US Pat. No. 9,068,114

METAL FLUORIDE EUTECTIC, NEUTRON SCINTILLATOR AND NEUTRON IMAGING DEVICE

TOKUYAMA CORPORATION, Sh...

1. A metal fluoride eutectic comprising a lithium fluoride crystal phase and a Ca1-xSrxF2 (where x denotes a number greater than 0, but not larger than 1) crystal phase.
US Pat. No. 9,056,774

ALUMINUM NITRIDE POWDER AND METHOD OF PRODUCING THE SAME

TOKUYAMA CORPORATION, Sh...

1. A method of producing an aluminum nitride powder including following steps of:
preparing a powder of alumina or hydrated alumina having a primary grain size of 0.001 to 6 ?m as an Al source, a powder of
a rare earth metal compound having an average grain size (D50) in a range of 2 to 80 ?m, the average grain size (D50) thereof being not less than 6 times as great as the primary grain size of said Al source, and a carbon powder,

mixing the powder of said Al source, the powder of the rare earth metal compound and the carbon powder together, and
reducing and nitriding said Al source by holding the mixed powder in a nitrogen-containing atmosphere at a temperature of
1620 to 1900° C. for not less than 2 hours,

wherein the aluminum nitride powder that is produced comprises aluminum nitride particles having a sphericalness expressed
by the ratio (DS/DL) of the short diameter (DS) thereof and the long diameter (DL) thereof of not less than 0.75.

US Pat. No. 9,316,765

PHOTOCHROMIC COMPOSITION

Tokuyama Corporation, Ya...

1. A photochromic composition comprising:
(A) a polyurethane-urea resin having a urea bond in a molecular chain, in which a tetrahydrofuran insoluble content is 20.0
to 90.0% by mass; and

(B) a photochromic compound.

US Pat. No. 9,374,893

PRODUCTION METHOD OF METALLIZED SUBSTRATE

TOKUYAMA CORPORATION, Sh...

1. A production method of a metallized substrate comprising a wiring pattern, the metallized substrate comprising: a sintered
nitride ceramic substrate; a titanium nitride layer formed on the sintered substrate; and a metal layer being the wiring pattern
and containing copper, silver and titanium formed on the titanium nitride layer, the method comprising:
a step of layering a first paste layer by means of a first paste composition containing copper powder and titanium hydride
powder and having a thixotropic index of 0.2 to 1.0 on a part of the sintered nitride ceramic substrate, to produce a first
layered body, wherein the part of the sintered nitride ceramic substrate is a part where the wiring pattern is to be formed,
and wherein the copper powder is a mixed powder of copper powder A having an average particle size of 0.1 ?m or more and less
than 1.0 ?m and copper powder B having an average particle size of 1.0 to 5.0 ?m;

a step of layering a second paste layer by means of a second paste composition containing silver-copper alloy powder and not
containing a titanium component on the first paste layer of the first layered body, to produce a second layered body, wherein
the silver-copper alloy powder has a melting point of 630 to 850° C. and an average particle size of 0.1 to 20 ?m; and

a step of firing the second layered body, at a temperature such that the second paste composition melts wherein the temperature
is not greater than melting point of copper and wherein the firing is carried out under a condition such that a shape of the
first paste layer is maintained, to thereby form the titanium nitride layer and the metal layer on the sintered nitride ceramic
substrate.

US Pat. No. 9,343,525

ALUMINUM NITRIDE SUBSTRATE AND GROUP-III NITRIDE LAMINATE

Tokuyama Corporation, Ya...

3. A group III nitride layered product, comprising:
an aluminum nitride substrate comprising at least on a surface thereof an aluminum nitride single crystal layer having a principal
plane inclined to “m” axis direction within a range of 0.05° or more and 0.40° or less and inclined to “a” axis direction
within a range of 0.00° or more and 0.24° or less from (0001) plane of the wurzite structure, and

an AlGaInBN layer which satisfies a composition shown by Al1?(x+y+z)GaxInyBzN, wherein x, y, and z are independently a rational number of 0 or more and less than 0.5 respectively, and a sum of x, y,
and z is less than 0.5, on the principal plane of the aluminum nitride single crystal layer of the aluminum nitride substrate.

US Pat. No. 9,303,841

ULTRAVIOLET LIGHT-EMITTING MODULE AND ULTRAVIOLET IRRADIATION DEVICE

TOKUYAMA CORPORATION, Ya...

1. An ultraviolet light-emitting module characterized by comprising:
a base where a plurality of ultraviolet light-emitting devices are disposed on a side surface of a cylindrical or polygonal
columnar base such that a light axis of each ultraviolet light-emitting device passes through a center axis of the cylindrical
or polygonal columnar base to emit ultraviolet rays radially to the center axis;

a cover formed by an ultraviolet transmitting material,
the cover covering the base where the ultraviolet light-emitting devices are disposed and being air-tightly mounted to the
base where the ultraviolet light-emitting devices are disposed such that inside thereof is filled with an inert gas or dried
air; and

a flow path for a cooling medium formed inside of the cylindrical or polygonal columnar base to flow a cooling medium through
the flow path for a cooling medium.

US Pat. No. 9,307,637

METALLIZED VIA-HOLED CERAMIC SUBSTRATE, AND METHOD FOR MANUFACTURE THEREOF

TOKUYAMA CORPORATION, Sh...

1. A metallized via-holed ceramic substrate comprising: a sintered ceramic substrate; an electroconductive via formed in the
sintered ceramic substrate, said electroconductive via having an electroconductive metal closely filled in a through-hole
of the sintered ceramic substrate, said electroconductive metal containing a metal (A) having a melting point of 600° C. to
1100° C., a metal (B) having a melting point higher than the melting point of the metal (A), and an active metal; a wiring
pattern on at least one face of the sintered ceramic substrate, said wiring pattern having an electroconductive surface layer
and a plating layer on a surface of the electroconductive surface layer, said electroconductive surface layer consisting of
an electroconductive metal containing the metal (A), the metal (B), and the active metal; an active layer formed in an interface
between the electroconductive via and the sintered ceramic substrate; and an active layer formed in an interface between the
electroconductive surface layer and the sintered ceramic substrate, wherein said metal (A) having a melting point of 600°
C. to 1100° C. is one or more selected from a group consisting of gold solder, silver solder, and copper; and said metal (B)
having a melting point higher than the melting point of the metal (A) is one or more selected from a group consisting of silver,
copper, and gold.

US Pat. No. 9,388,337

METAL FLUORIDE CRYSTAL, LIGHT EMITTING ELEMENT, SCINTILLATOR, METHOD OF DETECTING NEUTRON, AND METHOD OF PRODUCING METAL FLUORIDE CRYSTAL

TOKUYAMA CORPORATION, Ya...

1. A neutron scintillator, comprising a metal fluoride crystal including a crystal represented by a chemical formula LiM1M2F6 wherein Li includes 6Li, M1 represents at least one alkaline earth metal element selected from the group consisting of Mg, Ca, Sr, and Ba, and M2 represents at least one metal element selected from the group consisting of Al, Ga, and Sc, the crystal containing not less
than 0.02 mol % of Eu, and the crystal having a concentration of Eu2+ of less than 0.01 mol %.

US Pat. No. 9,228,035

PHOTO-CURABLE NANOIMPRINT COMPOSITION, METHOD FOR FORMATTING PATTERN USING THE COMPOSITION, AND NANOIMPRINT REPLICA MOLD COMPRISING CURED PRODUCT OF THE COMPOSITION

TOKUYAMA CORPORATION, Ya...

1. A photo-curable nanoimprint composition, said composition comprising:
(A) partial hydrolysate,
(B) polymerizable monomer having (meth)acrylic group; and
(C) photoinitiator,wherein said partial hydrolysate (A) is selected from a group consisting of
(A-1) mixture of partial hydrolysate of organic silicon compound having a general formula (1):
(wherein, each of (R1)s is, same or different, C1-4 alkyl group; n is an integer of 1-10; and partial hydrolysate of (meth)acrylic group-containing silicon compound having a
general formula (2):
wherein R2 is hydrogen atom or methyl group; R3 is C1-10 alkylene group, C3-10 cycloalkylene group, or C3-10 polymethylene group; R4 is C1-4 alkyl group, C3-4 cycloalkyl group, or C6-12 aryl group; R5 is C1-4 alkyl group or C3-4 cycloalkyl group; l is an integer of 1-3, m is an integer of 0-2, and k is an integer of 1-3, but (l+m+k) is 4; in case that
each of R2, R3, R4 and R5 is present in plural, each of (R2)s, (R3)s, (R4)s and (R5)s may be same or different;
(A-2) mixture of partial hydrolysate of fluorinated organic silane compound having a general formula (3):
wherein each of R6 and R8 is C1-10 alkyl group or C3-10 cycloalkyl group; R7 is C1-100 fluorine-containing alkyl group, fluorine-containing cycloalkyl group, or fluorine-containing alkoxy ether group; a is an
integer of 1-3and b is an integer of 0-2, but (a+b) is 1-3; in case that each of R6, R7 and R8 is present in plural, each of (R6) s, (R7)s and (R8)s may be same or different and said partial hydrolysate of (meth)acrylic group-containing silicon compound having the general
formula (2); and
(A-3) mixture of said partial hydrolysate of organic silicon compound having the general formula (1), said partial hydrolysate
of (meth)acrylic group-containing silicon compound having the general formula (2), and said partial hydrolysate of fluorinated
organic silane compound having the general formula (3), and

wherein said partial hydrolysate (A) comprises further partial hydrolysate of metal alkoxide having a general formula (5)

wherein, M is zirconium or titanium and each of (R9)s is, same or different, C1-10 alkyl group).

US Pat. No. 9,216,909

AEROGEL AND METHOD FOR MANUFACTURE THEREOF

TOKUYAMA CORPORATION, Sh...

1. A method for manufacturing an aerogel comprising the successive steps of:
(i) preparing an aqueous silica sol;
(ii) dispersing the aqueous silica sol into a hydrophobic solvent, thereby forming a W/O emulsion;
(iii) causing gelation of the silica sol, thereby converting the W/O emulsion into a dispersion of a gel;
(iv) replacing water in the gel with a solvent which has a surface tension at 20° C. of no more than 30 mN/m;
(v) treating the gel with a hydrophobing agent; and
(vi) removing the solvent used in the replacing step (iv),
wherein the hydrophobing agent is capable of reacting with a silanol group represented by the following formula (1) existing
on the silica surface:

?Si—OH  (1)[In the formula (1), the symbol “?” represents remaining three valences of the Si atom;] thereby converting the silanol group
into a group represented by the following formula (2):
(?Si—O—)(4-n)SiRn  (2)[In the formula (2), n is an integer of 1 to 3; each R is independently a hydrocarbyl group; and two or more R may be the
same or different with each other where n is 2 or more.]

US Pat. No. 9,500,754

NEUTRON SCINTILLATOR AND NEUTRON DETECTOR

Tokuyama Corporation, Ya...

1. A neutron scintillator comprising:
a resin composition having a resin, and
inorganic phosphor particles having at least one neutron-capturing-isotope selected from the group consisting of lithium 6
and boron 10,

wherein a content of lithium 6 and boron 10 are 0.2 to 30×1018 atom/mm3 and 0.05 to 8×1018 atom/mm3 respectively; and

the resin composition has a shape so that an average diameter of inscribed spheres is 5 mm or less.

US Pat. No. 9,177,819

METHOD FOR MANUFACTURING SILICON SUBSTRATE HAVING TEXTURED STRUCTURE

Tokuyama Corporation, Ya...

1. A method for manufacturing a silicon substrate having texture structure, said method comprising steps of:
(A) forming a pattern with a resin-comprising composition on the silicon substrate,
(B) irradiating an etching gas to the silicon substrate surface other than the pattern portion, and
(C) processing the silicon substrate irradiated with the etching gas with an alkaline etching liquid to form concave structure
under the pattern portion,

wherein said resin-comprising composition comprises:
(a) polymerizable monomer having (meth)acrylic group,
(b) photoinitiator, and
(c) hydrolysate of akloxysilane,
wherein said hydrolysate of alkoxysilane is at least one selected from a group consisting of:
hydrolysate of a mixture of general alkoxysilane having a general formula (2):

(wherein (R5)s are, same or different, C1-4 alkyl group; n is an integer of 1-10) and (meth)acrylic group-containing alkoxysilane having a general formula (3):


(wherein R6 is hydrogen atom or methyl; R7 is C1-10 alkylene, C3-10 cycloalkylene or C3-10 polymethylene; R8 is C1-4 alkyl, C3-4 cycloalkyl or C6-12 aryl; R9 is C1-4 alkyl or C3-4 cycloalkyl; l is an integer of 1-3, m is an integer of 0-2, k is an integer of 1-3 and (l+m+k) is 4; in case that respective
R6, R7, R8 or R9 is present in plural, each of R6(s), R7(s), R8(s) or R9(s) may be same to or different from each other);

hydrolysate of the (meth)acrylic group-containing alkoxysilane of the general formula (3); and
hydrolysate of a mixture of the general alcoxysilane of the general formula (2), the (meth)acrylic group-containing alkoxysilane
of the general formula (3) and metal alkoxide having a general formula (6):

M-(OR13)4  (6)

(wherein M is zirconium or titanium; and (R13)s are, same or different, C1-10 alkyl group).

US Pat. No. 9,090,469

METHOD OF PRODUCING A SPHERICAL ALUMINUM NITRIDE POWDER

TOKUYAMA CORPORATION, Sh...

1. A method of producing a spherical aluminum nitride powder, comprising:
(A) mixing 100 parts by mass of an alumina or an alumina hydrate having an average particle diameter of not more than 2 ?m,
2 to 10 parts by mass of a compound containing a rare earth metal per 100 parts by mass of said alumina or said alumina hydrate,
and 38 to 46 parts by mass of a carbon powder per 100 parts by mass of said alumina or said alumina hydrate to obtain a mixture
thereof; and

(B) reductively nitriding the alumina or the alumina hydrate in a state where said alumina or said alumina hydrate is dissolved
in a liquid phase by holding said mixture in a nitrogen-containing atmosphere at a temperature of 1680 to 1750° C. for 8 to
17 hours.

US Pat. No. 9,593,272

SILICA FOR CMP, AQUEOUS DISPERSION, AND PROCESS FOR PRODUCING SILICA FOR CMP

TOKUYAMA CORPORATION, Ya...

1. A silica for CMP, which satisfies the following (A) to (C):
(A) a BET specific surface area of 40 m2/g or more and 180 m2/g or less;

(B) a particle density measured by a He-gas pycnometer method of 2.24 g/cm3 or more; and

(C) a coefficient of variation in primary particle diameter calculated by TEM/image analysis of 0.40 or less.

US Pat. No. 9,308,764

SHEET FOR INK-JET PRINTING

TOKUYAMA CORPORATION, Sh...

1. A sheet for ink jet printing including a base sheet and a printing layer formed on a surface of said base sheet and containing
a plaster (shikkui) and an organic binder,
wherein said printing layer, further, contains at least one kind of additive selected from the group consisting of glycerin,
water-soluble polymer and non-ionic surfactant, and

wherein said printing layer has a thickness of 0.1 mm to 0.5 mm.

US Pat. No. 9,199,853

METAL OXIDE POWDER AND METHOD FOR MANUFACTURE THEREOF

TOKUYAMA CORPORATION, Sh...

1. A metal oxide powder comprising globular independent particles as main component,
said metal oxide powder having:
BET specific surface area of 400 to 1000 m2/g;

BJH pore volume of 2 to 8 mL/g; and
oil absorption measured by refined linseed oil method specified in JIS K5101-13-1 of no less than 250 mL/100 g,
wherein each said independent particle includes therein one or more hollow space having a size of 0.5 to 15 ?m; and
wherein the metal oxide powder has been hydrophobized by one or more silylating agent represented by the following general
formulae (6) to (8)

RnSiX(4-n)  (6)

wherein in the general formula (6), n represents an integer of 1 to 3; R represents methyl group; and X represents a leaving
group which can leave the molecule by cleavage of bond thereof with the Si atom in a reaction with a compound having a hydroxyl
group,


wherein in the general formula (7), R1 represents an alkylene group; R2 and R3 each represent methyl group; and R4 and R5 independently represent a hydrogen atom or a hydrocarbyl group,


wherein in the general formula (8), R6 and R7 each represent methyl group; and m represents an integer of 3 to 6.

US Pat. No. 9,073,755

SPHERICAL ALUMINUM NITRIDE POWDER

TOKUYAMA CORPORATION, Sh...

1. A spherical aluminum nitride powder having an average particle diameter of 3 to 30 ?m, a sphericalness of not less than
0.75, and an oxygen concentration which is suppressed to be not more than 1% by weight wherein, when said average particle
diameter is d (?m), the specific surface area S (m2/g) satisfies the following formula (1),
(1.84/d)?S?(1.84/d+0.5)  (1)

wherein, “d” is said average particle diameter; and
wherein a lattice constant of C-axis of aluminum nitride crystal particles in the aluminum nitride powder is not smaller than
4.9800.

US Pat. No. 9,462,698

METALLIZED SUBSTRATE, METAL PASTE COMPOSITION, AND METHOD FOR MANUFACTURING METALLIZED SUBSTRATE

TOKUYAMA CORPORATION, Sh...

2. A method for manufacturing a metallized substrate comprising the steps of:
(i) applying a metal paste composition on a whole surface of a side of a nitride ceramic sinter where a metallized pattern
is to be formed, wherein the metal paste composition comprises: a metal component containing a copper powder and a titanium
hydride powder, and not containing a silver powder; and a high-viscosity solvent having a viscosity at 25° C. of no less than
100 Pa-s, and wherein the metal paste composition contains 5 to 50 mass parts of said titanium hydride powder and 10 to 50
mass parts of said high-viscosity solvent per 100 mass parts of said copper powder,

(ii) firing a substrate obtained through the step (i), thereby forming a titanium nitride layer and an adhesion layer in the
order mentioned on or above the nitride ceramic sinter;

(iii) forming a resist pattern on a part of the adhesion layer where a wiring pattern is not to be formed, by a photolithographic
method;

(iv) forming a copper plating layer on a part of the adhesion layer where the resist pattern is not formed;
(v) removing the resist pattern;
(vi) etching an exposed part of the adhesion layer; and
(vii) etching an exposed part of the titanium nitride layer.
US Pat. No. 9,321,653

PROCESS FOR PRODUCING TRICHLOROSILANE

TOKUYAMA CORPORATION, Sh...

1. A process for producing trichlorosilane, including, independently from each other, a first production process for forming
said trichlorosilane by reacting metallic silicon with hydrogen chloride and a second production process for forming said
trichlorosilane by reacting metallic silicon with tetrachlorosilane and hydrogen; wherein
said trichlorosilane and other chlorosilane compounds are separated by condensation from trichlorosilane-containing gases
formed by reaction in said first production process, and waste gases from which said trichlorosilane and other chlorosilane
compounds have been separated by condensation are continuously fed without being refined as a hydrogen source to the second
production process,

wherein the metallic silicon is used in the first production process in an amount not less than twice as much as the amount
of the metallic silicon used in the second production process.

US Pat. No. 9,297,093

LAYERED BODY HAVING A SINGLE CRYSTAL LAYER

Tokuyama Corporation, Ya...

1. A layered body having a single crystal layer comprising a group III nitride satisfying a composition shown by AlXGaYInZN (wherein, X, Y and Z are rational numbers respectively satisfying 0.9?X?1.0, 0.0?Y?0.1, 0.0?Z?0.1, and X+Y+Z=1.0) on a sapphire
substrate, and said layered body has an initial single crystal layer comprising the group III nitride satisfying said composition
and containing oxygen in a concentration of 1×1020 cm?3 or more and 5×1021 cm?3 or less in a thickness of 15 nm or more and 40 nm or less on said sapphire substrate, and a second group III nitride single
crystal layer comprising the group III nitride satisfying said composition having reduced oxygen concentration than the initial
single crystal layer.
US Pat. No. 9,234,984

PHOTOCHROMIC COMPOSITION

Tokuyama Corporation, Ya...

1. A photochromic composition, comprising:
(A) a polyurethane-urea resin having an urea bond in a molecular chain; and
(B) a photochromic compound,
wherein (A) the polyurethane-urea resin has a piperidine structure, a hindered phenol structure, a triazine structure, or
a benzotriazol structure at a terminal end.

US Pat. No. 9,215,801

VIA-HOLED CERAMIC SUBSTRATE, METALLIZED VIA-HOLED CERAMIC SUBSTRATE, AND METHOD FOR MANUFACTURING THE SAME

TOKUYAMA CORPORATION, Sh...

1. A via-holed ceramic substrate comprising:
a sintered ceramic substrate;
an electroconductive via formed in the sintered ceramic substrate, said electroconductive via having an electroconductive
metal closely filled in a through-hole, said electroconductive metal containing a metal (A) having a melting point of 600°
C. to 1100° C., a metal (B) having a melting point higher than the melting point of the metal (A), and an active metal; and

an active layer formed in the interface between the electroconductive via and the sintered ceramic substrate,
wherein the sintered ceramic substrate is a sintered aluminum nitride substrate;
the metal (A) having the melting point of 600° C. to 1100° C. is one or more selected from a group consisting of gold solder,
silver solder, and copper; and

the metal (B) having the melting point higher than the melting point of the metal (A) is one or more selected from a group
consisting of silver, copper, and gold.

US Pat. No. 9,145,301

METHOD FOR PRODUCING ALUMINUM NITRIDE POWDER

Tokuyama Corporation, Ya...

1. A method for producing an aluminum nitride powder, comprising reductively nitriding an alumina powder, wherein:
the alumina powder having an average particle diameter of not more than 5 ?m, an eutectic melting agent, and a carbon powder
are mixed to obtain a mixture thereof, and

the mixture is reductively nitrided by firing at a higher temperature than a melting point of the eutectic melting agent,
while maintaining a nitrogen percentage within a range of 60 to 85 vol % in an atmosphere of mixed gases of nitrogen and carbon
monoxide until an aluminum nitride conversion percentage of the alumina powder reaches at least 50%.

US Pat. No. 9,132,365

REMOVAL METHOD AND REMOVAL APPARATUS FOR ENTRAINED AIR COATING FLUID

TOKUYAMA CORPORATION, Sh...

1. A method for removing air from a photochromic coating fluid containing entrained air comprising the steps of:
(A) preparing a coating unit comprising a cylindrical vessel storing the photochromic coating fluid, a check valve connecting
with the vessel and an outlet of the photochromic coating fluid existing downstream of the check valve, wherein the check
valve prevents back flow of the photochromic coating fluid from the outlet toward the vessel by urging a valve hail against
a valve seat by a spring,

(B) plugging the outlet; and
(C) after step (B), rotating the coating unit on an axis of the vessel and orbiting the coating unit on a revolution axis
simultaneously whereby the photochromic coating fluid within the vessel presses the valve ball in opposition to the pressing
force of the spring and the photochromic coating fluid enters the check valve, while air within the check valve flows into
the vessel, and further removing air incorporated in the photochromic coating fluid from the photochromic coating fluid.

US Pat. No. 9,079,777

METHOD FOR PRODUCING INORGANIC OXIDE PARTICLES

TOKUYAMA CORPORATION, Sh...

1. A method for producing inorganic oxide particles, comprising at least the following steps of:
coagulating a dispersion obtained by carrying out the hydrolysis reaction and the polycondensation reaction of a metal alkoxide
in the presence of a basic catalyst by using of a mixture of water and an alcohol as a solvent;

filtering the dispersion to obtain particles; and
drying the particles, wherein
the step of coagulating the dispersion is carried out by adding a coagulant comprising at least one compound selected from
the group consisting of carbon dioxide, ammonium carbonate, ammonium hydrogen carbonate and ammonium carbamate to the dispersion.

US Pat. No. 9,447,224

URETHANE (METH) ACRYLATE MONOMER AND PRODUCTION PROCESS THEREOF

TOKUYAMA CORPORATION, Sh...

1. A urethane (meth)acrylate monomer, which comprises
a urethane (meth)acrylate monomer represented by the following formula (I):

wherein, each a is independently an integer of 1 to 3, b, c and d are each independently an integer of 0 to 100, R1 is a hydrogen atom or methyl group, R2 is a divalent to tetravalent, aliphatic hydrocarbon group which may have a substituent, R3 is a divalent organic residue selected from a divalent group having an aromatic ring, a divalent group having an aliphatic
ring and an alkylene group, R4 is a divalent organic residue selected from a divalent group having a polyether structure, a divalent group having a polycarbonate
structure and a divalent group having a polyester structure, and R5 is a divalent group having a urea bond or a divalent group having a urethane bond;

water; and
an acid,
wherein the content of water is greater than zero and not more than 700 ppm (mass) and the content of the acid is such that
the acid value of the urethane (meth)acrylate monomer is not more than 0.2 mgKOH/g.

US Pat. No. 9,301,390

PROCESS FOR PRODUCING METALLIZED SUBSTRATE, AND METALLIZED SUBSTRATE

TOKUYAMA CORPORATION, Sh...

1. A process for producing a metallized substrate in which a sintered nitride ceramic substrate and a metal layer having a
predetermined shape that covers a partial area of a surface of the substrate are bonded to each other through a titanium nitride
layer having a thickness of 0.2 ?m or more and 0.7 ?m or less, comprising:
a step of preparing a metal paste composition comprising 100 parts by mass of a copper powder, 20 parts by mass or more and
60 parts by mass or less of a silver powder, and 2.0 parts by mass or more and 7.5 parts by mass or less of a titanium hydride
powder, the copper powder being a mixed powder of a copper powder having an average particle size of 1.0 ?m or more and 5.0
?m or less, and a copper powder having an average particle size of 0.2 ?m or more and 0.6 ?m or less, the silver powder having
an average particle size of 0.1 ?m or more and 1.0 ?m or less, and the titanium hydride powder having an average particle
size of 1.0 ?m or more and 7.0 ?m or less,

a first-precursor-substrate-forming step of applying the metal paste composition to the sintered nitride ceramic substrate,
thereby forming a first precursor substrate having the sintered nitride ceramic substrate, and a metal paste layer comprising
the metal paste composition, which is formed over the substrate, and which has a shape turning into the above-mentioned predetermined
shape after the precursor substrate is fired, and

a firing step of holding the first precursor substrate in a heat-resistant container arranged in a firing furnace, and firing
the substrate at a temperature of 800° C. or more and 950° C. or less and under a pressure of 1.33×10?5 Pa or more and 1.33×10?2 Pa or less, such that a titanium nitride layer is formed on the sintered nitride ceramic substrate and a metal layer is formed
on the titanium nitride layer,

wherein in the firing step, the titanium component contained in the metal paste layer is caused to react preferentially with
a nitride ceramic that constitutes the sintered nitride ceramic substrate, thereby forming the titanium nitride layer; and
further the content of titanium in the metal layer obtained after the firing is set to 2.0% by mass or less, and further is
set to ½ or less of the amount of titanium contained in the metal paste layer.

US Pat. No. 9,153,830

SEPARATION MEMBRANE FOR SOLID POLYMER FUEL CELL AND SEPARATION MEMBRANE-CATALYST ELECTRODE ASSEMBLY

Tokuyama Corporation, Ya...

1. A membrane for polymer electrolyte fuel cell used for preparing a membrane-electrode assembly, which comprises:
a hydrocarbon anion-exchange resin membrane wherein an anion-exchange group is covalently bonded to a hydrocarbon resin, and
an adhesive layer used for bonding a catalyst electrode layer formed on at least one side of the hydrocarbon anion-exchange
resin membrane,

wherein the adhesive layer consist essentially of a hydrocarbon anion-exchange resin, which hydrocarbon anion-exchange resin
is made of a styrene-based anion-exchange resin in which a quaternary ammonium salt group is covalently bonded to a non-crosslinked
styrene-based elastomer, and has a Young's modulus of 1 to 1,000 MPa, and

wherein the adhesive layer has a solubility of less than 1% by mass in water of 20° C. and has a thickness of 1 to 10 ?m.

US Pat. No. 9,145,621

PRODUCTION METHOD OF AN ALUMINUM BASED GROUP III NITRIDE SINGLE CRYSTAL

Tokuyama Corporation, Ya...

1. A production method of aluminum based group III nitride single crystal, comprising:
a reaction step, wherein a halogenated gas and an aluminum are made contact at a temperature of 300° C. or more to 700° C.
or less, and a mixed gas including an aluminum trihalide gas and an aluminum monohalide gas is produced,

a converting step, wherein the aluminum monohalide gas in the mixed gas is converted to a solid substance by setting a temperature
of the mixed gas equal to or higher than a temperature to which a solid aluminum trihalide deposit, and lower by 50° C. or
more than a temperature to which the halogenated gas and the aluminum contact in the reaction step,

a separation step, wherein the aluminum trihalide gas is taken out by separating the solid substance and the gas, and
a crystal growth step, wherein the aluminum trihalide gas is used for a raw material of aluminum based group III nitride single
crystal without lowering its temperature and keeping the temperature equal to or higher than a temperature of the converting
step.

US Pat. No. 9,457,120

AIR PURIFIER

TOKUYAMA CORPORATION, Sh...

1. An air purifier comprising:
an air sterilizing unit;
an air blowing unit arranged such that air flows in the air sterilizing unit;
the air sterilizing unit comprising:
a housing comprising a box body;
a substrate removably fixed in the housing; and
a plurality of ultraviolet light emitting diode arranged on the substrate and emitting deep ultraviolet ray having wavelength
of 200 to 350 nm;

the housing comprising a sterilizing room;
the sterilizing room being an inner space of the housing and facing a face of the substrate on which light emitting devices
are arranged, and comprising an air intake opening and an air outlet opening; and

the ultraviolet light emitting diode being arranged in a package having a structure such that light is emitted with strengthened
directivity, and being arranged in the housing such that the deep ultraviolet ray is emitted toward inside of the sterilizing
room,

wherein (A) at least a part of an inner wall surface of the sterilizing room comprises an ultraviolet reflective material
which may be covered with an ultraviolet ray transmitting material, and/or (B) one or more reflector plate which is a plate
body is arranged and fixed in the sterilizing room wherein at least a part of the surface of the reflector plate comprises
the ultraviolet reflective material; and

the deep ultraviolet ray emitted from the ultraviolet light emitting diode passes through air in the sterilizing room and
thereafter further passes through the air in the sterilizing room once or more, by being reflected on the inner wall surface
which comprises the ultraviolet reflective material or on the surface of the reflector plate which comprises the ultraviolet
reflective material.

US Pat. No. 9,199,848

PROCESS FOR PRODUCING SPHERICAL ALUMINUM NITRIDE POWDER AND SPHERICAL ALUMINUM NITRIDE POWDER PRODUCED BY THE SAME PROCESS

TOKUYAMA CORPORATION, Sh...

1. A process for producing a spherical aluminum nitride powder by using a spherical granulated product of an alumina powder
or an alumina hydrate powder as a starting material, and feeding said spherical granulated product to the step of reductive
nitrogenation so as to be reductively nitrogenated;
wherein said spherical granulated product of said alumina powder or said alumina hydrate powder has a BET specific surface
area of 30 to 500 m2/g;

further including the step of heat treatment for once heat-treating said spherical granulated product to lower the BET specific
surface area of said spherical granulated product prior to conducting said step of reductive nitrogenation;

wherein said heat treatment is conducted to such a degree that the BET specific surface area is lowered but is maintained
to be at least not less than 2 m2/g.

US Pat. No. 9,377,664

PHOTOCROMIC COMPOSITION

Tokuyama Corporation, Ya...

1. An optical article having a multilayer structure wherein two optical sheets or optical films facing each other are bound
via an adhesive layer comprising a photochromic composition comprising a polyurethane resin (A) having an isocyanurate structure
and a photochromic compound (B), wherein said polyurethane resin (A) having the isocyanurate structure is the polyurethane
resin obtained by reacting,
a polyol compound (A1) having two or more hydroxyl groups in the molecule, and having a number-average molecular weight of
400 to 3,000,

an isocyanurate compound (A2a) having an isocyanurate structure and three isocyanate groups in the molecule,
a diisocyanate compound (A2b) having two isocyanate groups in the molecule, and
a chain extender (A3) having two or more groups capable of reacting with the isocyanate groups in the molecule, and having
a molecular weight of 50 to 300.

US Pat. No. 9,403,680

METHOD FOR PRODUCING SINTERED ALUMINUM NITRIDE GRANULES

Tokuyama Corporation, Ta...

1. A method for producing sintered aluminum nitride granules comprising the steps of:
reductively nitrogenating porous alumina granules having an average particle size of 10 to 200 ?m and a BET specific surface
area of 2 to 250 m2/g at a temperature of 1400° C. or more and 1700° C. or less so as to obtain porous aluminum nitride granules; and

sintering the porous aluminum nitride granules obtained in the step of reduction-nitridation at a temperature of 1580° C.
or more and 1900° C. or less so as to obtain sintered aluminum nitride granules having an average particle size of 10 to 200
?m and a BET specific surface area of 0.05 to 0.5 m2/g.

US Pat. No. 9,399,577

METHOD FOR PRODUCING WATER-RESISTANT ALUMINUM NITRIDE POWDER

TOKUYAMA CORPORATION, Sh...

1. A method for producing a water-resistant aluminum nitride powder by surface treatment of aluminum nitride powder particles
having yttria on a surface thereof as a result of a production process thereof, the method comprising the successive steps
of:
(i) making an aluminum nitride powder contact with an acid solution which can dissolve yttria, wherein yttria exists at least
on a particle surface of the aluminum nitride powder;

(ii) removing the acid from the aluminum nitride powder; and
(iii) making the aluminum nitride powder contact with a phosphorus acid compound,
wherein an amount of yttria which remains on the surface of the aluminum nitride powder after the step (i) is determined by
carrying out the following successive steps of (a) to (e) on the aluminum nitride powder filtered, washed with water, and
dried after the step (i) and is no more than 1000 mg per 100 g of the aluminum nitride powder filtered, washed with water,
and dried:

(a) adding 10 g of the aluminum nitride powder filtered, washed with water, and dried to 25 mL of 1 mol/L hydrochloric acid
in a 50 mL vial bottle at 25° C.;

(b) holding the vial bottle in a ultrasonic bath and sonicating the vial bottle at 43 kHz for 30 minutes at 25° C.;
(c) filtering the content of the vial bottle and thereby obtaining a filtrate;
(d) measuring yttrium content in the filtrate by means of inductively coupled plasma atomic emission spectrometry; and
(e) converting the yttrium content in the filtrate into the content in terms of yttria.
US Pat. No. 9,513,407

PHOTOCHROMIC COMPOSITION AND OPTICAL ARTICLE USING PHOTOCHROMIC COMPOSITION

Tokuyama Corporation, Ya...

1. A photochromic composition, comprising:
an urethane polymer (A) having a polymerizable group within a molecule,
a photochromic compound (B),
an isocyanate compound (C) having at least one isocyanate group within a molecule, and
an optional monomer having the polymerizable group,
wherein said urethane polymer (A) is a prepolymer obtained by reacting:
a polyol compound (A1) of a number average molecular weight of 400 to 3000 having two or more of hydroxyl groups within a
molecule,

a polyisocyanate compound (A2) having two or more isocyanate groups within a molecule,
a chain extender (A3) of a molecular weight of 50 to 300 having two or more groups capable of reacting with isocyanate group
in a molecule, and

a compound (A4) being a polymerizable group imparting compound which can introduce the polymerizable group at the end terminal
of said urethane polymer (A),

wherein said polymerizable group is any one selected from the group consisting of silanol group or a group capable of forming
a silanol group by hydrolysis, (meth)acrylate group, epoxy group, and vinyl group,

wherein an amount ratio of (A1) component, (A2) component, (A3) component, and (A4) component used for obtaining said urethane
polymer (A) is n1:n2:n3:n4=0.33 to 0.85:1:0.1 to 0.65:0.01 to 0.3; and n1+n3+n4=1, wherein:

a total mol number of the hydroxyl group included in said (A1) component is n1,
a total mol number of isocyanate group included in said (A2) component is n2,
a total mol number of a group capable of reacting with isocyanate group included in said (A3) component is n3, and
a total mol number of a group capable of reacting with isocyanate group included in said (A4) component is n4, and
wherein a mol number of the polymerizable group per 100 gram of a total of said urethane polymer (A) and said optional monomer
is

(1) 10 mmol or more and 250 mmol or less, in case the polymerizable group is a silanol group or a group forming the silanol
group by hydrolysis;

(2) 10 mmol or more and 200 mmol or less, in case the polymerizable group is (meth)acrylate group, epoxy group, or vinyl group.

US Pat. No. 9,487,693

CHROMENE COMPOUND

TOKUYAMA CORPORATION, Sh...

1. A chromene compound represented by the following formula (5):
wherein R1 is a hydroxyl group, alkyl group, haloalkyl group, cycloalkyl group, alkoxy group, amino group, heterocyclic group having
a ring member nitrogen atom and bonded to a benzene ring to which the heterocyclic group is bonded via the nitrogen atom,
cyano group, nitro group, formyl group, hydroxycarbonyl group, alkylcarbonyl group, alkoxycarbonyl group, halogen atom, aralkyl
group, aralkoxy group, aryloxy group, aryl group, heteroaryl group, alkylthio group, cycloalkylthio group, arylthio group,
heteroarylthio group or group having a siloxane bond, “a” is an integer of 0 to 4, provided that when “a” is 2 to 4, a plurality
of R1's can be the same or different, or two R1's are bonded together to form a ring, R2 and R3 are each an alkyl group, aryl group, heteroaryl group, group represented by the following formula (2), or group represented
by the following formula (3):
wherein R4 is an aryl group or heteroaryl group, R5 is a hydrogen atom, alkyl group or halogen atom, and “m” is an integer of 1 to 3,
wherein R6 is an aryl group or heteroaryl group, and “n” is an integer of 1 to 3, or R2 and R3 form an aliphatic ring together with carbon atoms to which R2 and R3 are bonded, C* is a Spiro carbon atom, a spiro ring A represented by the following formula is a saturated hydrocarbon ring
or unsaturated hydrocarbon ring having 4 to 12 carbon atoms constituting the ring, and at least one ring member carbon atom
constituting the Spiro ring A is a group represented by the following formula (4):

wherein R7 and R8 are each an alkyl group having 3 or more carbon atoms, aralkyl group, cycloalkyl group, aryl group or heteroaryl group, and
R9 is a hydroxyl group, alkyl group, haloalkyl group, cycloalkyl group, alkoxy group, amino group, heterocyclic group having
a ring member nitrogen atom and bonded to a benzene ring to which the heterocyclic group is bonded via the nitrogen atom,
cyano group, nitro group, formyl group, hydroxycarbonyl group, alkylcarbonyl group, alkoxycarbonyl group, halogen atom, aralkyl
group, aralkoxy group, aryloxy group, aryl group, heteroaryl group, alkylthio group, cycloalkylthio group, arylthio group,
heteroarylthio group or group having a siloxane bond, “b” is an integer of 0 to 4, provided that when “b” is 2 to 4, a plurality
of R9's can be the same or different, or two R9's are bonded together to form a ring.

US Pat. No. 9,567,517

NEUTRON SCINTILLATOR, NEUTRON DETECTION METHOD AND NEUTRON DETECTOR

TOKUYAMA CORPORATION, Ya...

1. A neutron scintillator composed of a resin composition comprising (A) an inorganic phosphor containing at least one neutron
capture isotope selected from lithium 6 and boron 10 and (B) a resin, wherein
the inorganic phosphor is a particle having a specific surface area of 50 to 3,000 cm2/cm3, and the internal transmittance based on 1 cm of optical path length of the resin composition is 30%/cm or more at the emission
wavelength of the inorganic phosphor.

US Pat. No. 9,784,858

NEUTRON SCINTILLATOR, NEUTRON DETECTOR AND METHOD FOR MANUFACTURING NEUTRON SCINTILLATOR

Tokuyama Corporation, Ya...

1. A neutron scintillator comprising:
a resin based complex comprising:
a phosphor part (A) comprising a resin composition including a resin, and inorganic phosphor particles comprising at least
one neutron-capturing isotope comprising lithium 6 or boron 10; and

at least one wavelength converting part (B) comprising a wavelength converting fiber or a wavelength converting sheet.
US Pat. No. 9,691,942

SINGLE-CYSTALLINE ALUMINUM NITRIDE SUBSTRATE AND A MANUFACTURING METHOD THEREOF

National University Corpo...

1. A single-crystalline aluminum nitride, comprising:
a single-crystalline aluminum nitride having a predetermined amount of carbon and chlorine impurities, wherein:
a carbon concentration is 1×1014 atoms/cm3 or more and less than 3×1017 atoms/cm3,

a chlorine concentration is 1×1014 to 1×1017 atoms/cm3, and

an absorption coefficient at 265 nm wavelength is 40 cm?1 or less.

US Pat. No. 9,748,410

N-TYPE ALUMINUM NITRIDE SINGLE-CRYSTAL SUBSTRATE AND VERTICAL NITRIDE SEMICONDUCTOR DEVICE

Tokuyama Corporation, Ya...

1. A laminated body stacked with a layer represented by AIxGa1-xN, wherein X is a rational number satisfying 0.3?X?0.8 and having a Si content of 1×1018 to 5×1019 cm?3, on at least one principal plane of an n-type aluminum nitride single crystal substrate, wherein said n-type aluminum nitride
single crystal substrate has an Si content of 3×1017 to 1×1020 cm?3, a dislocation density of 106 cm?2 or less, and a thickness of 50 to 500 ?m.

US Pat. No. 9,806,205

N-TYPE ALUMINUM NITRIDE MONOCRYSTALLINE SUBSTRATE

Tokuyama Corporation, Ya...

1. A n-type aluminum nitride single crystal substrate doped with silicon, comprising:
an impurity concentration other than silicon which functions as a donor impurity and is equal or less than a silicon concentration,
wherein:
a ratio (I1/I2) between a luminescence spectrum intensity (I1) of a peak at 370 to 390 nm and a luminescence peak intensity (I2) of a band edge of aluminum nitride is 0.5 or less by a photoluminescence measurement at 23° C.,

a thickness is 25 to 500 ?m, and
a ratio between an electron concentration and a silicon concentration at 23° C. is 0.0005 to 0.001.

US Pat. No. 9,643,905

PHENYLNAPHTHOL DERIVATIVES

TOKUYAMA CORPORATION, Sh...

1. Phenylnaphthol derivatives represented by the following general formula (1):

wherein,
R1, R2 and R3 are hydrogen atoms, alkyl groups or aryl groups, and R2 and R3 may be bonded together to form an aliphatic hydrocarbon ring or a heterocyclic ring,

a is an integer of 0 to 4,
b is an integer of 0 to 4,
R4 and R5 are hydroxyl groups, alkyl groups, haloalkyl groups, cycloalkyl groups, alkoxy groups, amino groups, heterocyclic groups having
a nitrogen atom as a hetero atom and are bonded together via the nitrogen atom, cyano groups, nitro groups, formyl groups,
hydroxycarbonyl groups, alkylcarbonyl groups, alkoxycarbonyl groups, halogen atoms, aralkyl groups, aralkoxy groups, aryloxy
groups, aryl groups, heteroaryl groups bonded together via a carbon atom in the ring, alkylthio groups, cycloalkylthio groups,
arylthio groups or heteroarylthio groups, and

if R4 or R5 are present in a plural number, the plurality of R4 or the plurality of R5 may be the same or different, or 2 R4s or 2 R5s may be bonded together to form an alicyclic hydrocarbon ring or a heterocyclic ring.

US Pat. No. 9,840,421

CHLOROSILANE PRODUCTION METHOD

TOKUYAMA CORPORATION, Sh...

1. A method of producing a trichloromonosilane, which comprises
flowing a starting material chlorosilane liquid comprising dichloromonosilane and silicon tetrachloride through a catalyst-packed
layer which is packed with a weakly basic anion exchange resin as a reaction catalyst to react dichloromonosilane and silicon
tetrachloride to form trichloromonosilane,

wherein a step of bringing the reaction catalyst contained in the catalyst-packed layer into contact with a processing gas
obtained by diluting a silicon tetrachloride with an inert gas until a temperature rise in the catalyst-packed layer comes
to an end and a step of cleaning the reaction catalyst that has been brought into contact with the processing gas by flowing
a silicon tetrachloride liquid through the catalyst-packed layer to remove solid matter are carried out before flowing the
starting material chlorosilane liquid through the catalyst-packed layer.

US Pat. No. 9,753,161

NEUTRON SCINTILLATOR AND NEUTRON DETECTOR

TOKUYAMA CORPORATION, Ya...

1. A neutron scintillator comprising a resin composition containing a resin and eutectic particles, wherein
the resin has an internal transmittance of 10%/cm or more at an emission wavelength of the eutectic particles,
the eutectic particles are composed of lithium fluoride (LiF) and an inorganic fluorescent material, and
an equal specific surface area sphere equivalent diameter of the eutectic particles is in a range of 50 to 1000 ?m.

US Pat. No. 9,588,257

PHOTOCHROMIC CURABLE COMPOSITION

Tokuyama Corporation, Ya...

1. A photochromic coating agent comprising a photochromic curable composition which includes:
as radically polymerizable component (A), a silsesquioxane component (A1) having a radically polymerizable group and a bifunctional
radically polymerizable monomer (A2), and a photochromic compound (B);

said silsesquioxane component (A1) being contained in an amount of 1 to 150 parts by mass per 100 parts by mass of the bifunctional
radically polymerizable monomer (A2);

said silsesquioxane component (A1) having a weight average molecular weight of 2,000 to 10,000 and containing said radically
polymerizable groups in a number at a ratio of 70 to 100% per the total number of substituents bonded to the silicon atoms;
and

said bifunctional radically polymerizable monomer (A2) being represented by the following general formula (1);

wherein,
“a” is a number of 0 to 30, and “b” is a number of 0 to 30 on condition that an average value of “a+b” is 2 to 30,
R1, R2, R3 and R4 are each a hydrogen atom or a methyl group, and

“A” is a divalent organic group, on condition that the number of carbon atoms is 1 to 20, which is selected from the group
consisting of:

alkylene group;
unsubstituted phenylene group;
phenylene group having, as a substituent, a halogen atom or an alkyl group having 1 to 4 carbon atoms; and
a divalent group represented by the following formula (1a), (1b) or (1c);

wherein in the formula (1 c),
R5 and R6 are alkyl groups having 1 to 4 carbon atoms or halogen atoms,

c and d are integers of 0 to 4,
6-membered ring B is a benzene ring or a cyclohexane ring, and when the 6-membered ring B is the benzene ring, X is a divalent
group represented by —O—, —S—, —S(O)2—, —C(O)—, —CH2—, —CH?CH—, —C(CH3)2—, —C(CH3)(C6H5)— or by the following formula (1c-1),


and when the 6-membered ring B is the cyclohexane ring, X is a divalent group represented by —O—, —S—, —CH2— or —C(CH3)2—, and

said silsesquioxane component (A1) being an organopolysiloxane comprising a basic constituent unit represented by the following
composition formula (3),

(R—SiO3/2)g
wherein R represents substituents bonded to silicon atoms, at least one of which being a radically polymerizable group, and
g is a number in a range of 4 to 100.

US Pat. No. 9,840,790

HIGHLY TRANSPARENT ALUMINUM NITRIDE SINGLE CRYSTALLINE LAYERS AND DEVICES MADE THEREFROM

Hexatech, Inc., Morrisvi...

1. A highly transparent single crystalline AlN layer having a refractive index in the a-axis direction in the range of 2.250
to 2.400 and an absorption coefficient less than or equal to 15 cm?1 at a wavelength of 265 nm.

US Pat. No. 9,708,733

METHOD FOR MANUFACTURING ALUMINUM-BASED GROUP III NITRIDE SINGLE CRYSTAL BY HYDRIDE VAPOR PHASE EPITAXY

TOKUYAMA CORPORATION, Sh...

1. A method for manufacturing an aluminum-based group III nitride single crystal comprising the step of:
supplying at least one aluminum halide gas and a nitrogen source gas onto a base substrate, such that a reaction of the at
least one aluminum halide gas and the nitrogen source gas is conducted on the base substrate,

wherein the reaction of the at least one aluminum halide gas and the nitrogen source gas is conducted under coexistence of
a halogen-based gas other than any aluminum halide gas such that a halogen-based gas ratio (H) represented by the following
formula (1) is no less than 0.1 and less than 1.0:

H=VH/(VH+VAl)  (1)
wherein in the formula (1), VH represents a supply of the halogen-based gas other than any aluminum halide gas; VAl represents a total supply of the at least one aluminum halide gas; and VH and VAl are simultaneous supplies per unit time in terms of volumes in a standard state; and
a growth rate of the aluminum-based group Ill nitride single crystal is no less than 10 ?m/h.
US Pat. No. 9,809,682

HYDROPHOBIZED SPHERICAL POLYALKYLSILSESQUIOXANE FINE PARTICLE, EXTERNAL ADDITIVE FOR TONER, DRY TONER FOR ELECTROPHOTOGRAPHY, AND METHOD OF MANUFACTURING HYDROPHOBIZED SPHERICAL POLYALKYLSILSESQUIOXANE FINE PARTICLE

TOKUYAMA CORPORATION, Ya...

1. A hydrophobized spherical polyalkylsilsesquioxane fine particle, which has a mass-based median diameter in a centrifugal
sedimentation method within a range of from 0.05 ?m to 0.3 ?m,
wherein the hydrophobized spherical polyalkylsilsesquioxane fine particle has a disintegration strength in a crushing strength
measurement method of 0.20 N or less.

US Pat. No. 9,944,565

METAL/CERAMIC BONDING SUBSTRATE AND METHOD FOR PRODUCING SAME

DOWA METALTECH CO., LTD.,...

1. A metal/ceramic bonding substrate comprising:a ceramic substrate of aluminum nitride; anda metal plate bonded to the ceramic substrate, wherein the ceramic substrate has a residual stress of not higher than ?50 MPa and wherein a bonded surface of the ceramic substrate to the metal plate has an arithmetic average roughness Ra of 0.15 to 0.30 ?m, andwherein said ceramic substrate has a flexural strength of 250-450 MPa.

US Pat. No. 9,828,250

METHOD OF PREVENTING POLYSILICON FROM BEING CONTAMINATED WITH METALS

TOKUYAMA CORPORATION, Sh...

1. A member to be contacted with polysilicon arranged at a position where the polysilicon comes into contact therewith, wherein:
said member to be contacted with the polysilicon is a chute, a hopper, or a crusher bed arranged in a course of up to introducing
the polysilicon right after it is produced into a step of producing single crystals of silicon,

wherein said member to be contacted with the polysilicon comprises a metal substrate and a resin cover provided on said metal
substrate,

said resin cover comprises two kinds of resin sheets in a state of being overlapped one upon the other on said metal substrate,
a surface of a resin sheet positioned on an upper surface comes into contact with the polysilicon,
the two kinds of resin sheets are detachably attached to the metal substrate by resin bolts;
the two kinds of resin sheets have flexibilities different from each other, wherein a resin sheet having a higher flexibility
is arranged on a lower side, and a sheet having a lower flexibility is arranged on an upper side where the polysilicon comes
into contact therewith,

the two kinds of resin sheets have color tones different from each other; and the resin sheet having the higher flexibility,
and which is arranged on the lower side, is closely attached to an entire surface of the metal substrate.

US Pat. No. 9,890,324

PHOTOCHROMIC CURABLE COMPOSITION, CURED PRODUCT THEREOF AND LAMINATE INCLUDING THE CURED PRODUCT

TOKUYAMA CORPORATION, Sh...

1. A photochromic curable composition comprising (A) as a polymerizable (meth)acrylate component:
[A1] a polymerizable carbonate monomer represented by the following formula (1):

wherein A and A? are each a linear or branched alkylene group having 2 to 15 carbon atoms, “a” is an average value of 1 to
20, when there are a plurality of A's, A's may be the same or different, R1 is a hydrogen atom or methyl group, and R2 is a (meth)acryloyloxy group or hydroxyl group;

[A2] a polyfunctional polymerizable monomer represented by the following formula (2):

wherein R3 is a hydrogen atom or methyl group, R4 is a hydrogen atom or alkyl group having 1 to 2 carbon atoms, R5 is a trivalent to hexavalent organic group having 1 to 10 carbon atoms, “b” is an average value of 0 to 3, “c” is an integer
of 3 to 6; and

[A3] another polymerizable (meth)acrylate monomer different from the above components [A1] and [A2], and
(B) a photochromic compound (B),
wherein the polymerizable (meth)acrylate component (A) contains 5 to 50 mass % of the component [A1], more than 30 mass %
to 70 mass % or less of the component [A2] and 1 mass % or more to less than 65 mass % of the component [A3] (the total content
of the components [A1], [A2] and [A3] is 100 mass %), and the photochromic compound (B) is contained in an amount of 0.0001
to 10 parts by mass based on 100 parts by mass of the polymerizable (meth)acrylate component (A).

US Pat. No. 10,125,309

PHOTOCHROMIC COMPOSITION

TOKUYAMA CORPORATION, Sh...

1. A photochromic composition comprising:(A) a polyrotaxane having a composite molecular structure comprising an axial molecule and a plurality of cyclic molecules clathrating the axial molecule; and
(B) a photochromic compound, which is at least one compound selected from the group consisting of a fulgide compound, a spirooxazine compound, and a chromene compound.

US Pat. No. 9,977,161

CURABLE COMPOSITION, CURED ARTICLE OBTAINED THEREFROM, AND PHOTOCHROMIC OPTICAL MATERIAL AND PROCESS FOR PRODUCING THE SAME

TOKUYAMA CORPORATION, Sh...

1. A curable composition comprising:(1) 100 parts by weight of radically polymerizable monomers;
(2) 1 to 10 parts by weight of an amine compound represented by the following formula (17)

wherein R06 is methyl, R07 is a hydroxyl group, R08 is a hydrogen atom or a hydroxyl group, A? is an alkylene group having 2 to 6 carbon atoms, and A? is a methylene group when R08 is a hydrogen atom, or A? is an alkylene group having 2 to 6 carbon atoms when R08 is a hydroxyl group; and
(3) 0.01 to 20 parts by weight of a photochromic compound, said radically polymerizable monomers comprising (a) a radically polymerizable monomer having a group which forms a silanol group by hydrolysis, represented by the following formula:

wherein R5 is a hydrogen atom or methyl group, R6 is an alkylene group having 1 to 3 carbon atoms, R7 is an alkoxyl group having 1 to 2 carbon atoms and a is an integer of 3, (b) a radically polymerizable monomer which is selected from the group consisting of glycidyl acrylate and glycidyl methacrylate, (c) a monomer having a homopolymer L-scale Rockwell hardness of 40 or less and represented by the following formula (13):

where R26 is a hydrogen atom or methyl group, R27 and R28 are each independently a hydrogen atom or methyl group, I is a divalent organic residual group represented by the following formula:

i? and j? are each an integer that ensures that the average value of i?+j? is 9 to 30, and (d) a monomer having a homopolymer L-scale Rockwell hardness of 60 or more and represented by the following formula (7):

wherein R13 is a hydrogen atom or methyl group, R14 is a hydrogen atom, R15 is a tervalent to hexavalent organic residual group having 1 to 16 carbon atoms, f is an integer of 0 to 3, f is an integer of 0 to 1, and g is an integer of 3 to 6,
said radically polymerizable monomer (a) being in an amount of 1 to 10 wt % based on the total amount of all the radically polymerizable monomers, said radically polymerizable monomer (b) being in an amount of 0.1 to 20 wt % based on the total of all the radically polymerizable monomers excluding the radically polymerizable monomer (a), said monomer (c) being in an amount of 5 to 70 wt % based on all the radically polymerizable monomers excluding the radically polymerizable monomer (a), and said radically polymerizable monomer (d) being in an amount of 10 to 94.9 wt % based on all the radically polymerizable monomers excluding the radically polymerizable monomer (a), wherein
the curable composition has a viscosity at 25° C. of 20 to 500 cp.

US Pat. No. 9,920,243

SCINTILLATOR, RADIATION DETECTOR, AND METHOD FOR DETECTING RADIATION

TOKUYAMA CORPORATION, Sh...

1. A method for detecting radiation by scintillation, comprising:
entering radiation, at a high temperature of not lower than 100° C., into a scintillator, the scintillator comprising a colquiriite-type
crystal represented by the following chemical formula:

LiM1M2X6
wherein M1 represents at least one alkaline earth metal element selected from the group consisting of magnesium (Mg), calcium (Ca), strontium
(St) and barium (Ba), M2 represents at least one metal element selected from the group consisting of aluminum (Al), gallium (Ga) and scandium (Sc),
and X represents at least one halogen element selected from the group consisting of fluorine (F), chlorine (Cl), bromine (Br)
and iodine (I),
to emit fluorescence; and
detecting the fluorescence by a photodetector.

US Pat. No. 9,873,819

CURABLE COMPOSITION AND PHOTOCHROMIC COMPOSITION

Tokuyama Corporation, Sh...

1. A curable composition comprising (A) a silsesquioxane monomer having a radically polymerizable group in the molecule, a
weight average molecular weight measured by gel permeation chromatography (GPC) of 2,000 to 4,700 and a content of a component
having a weight average molecular weight of not less than 10,000 of less than 9 mass % and (B) a bifunctional polymerizable
monomer represented by the following formula (1),
wherein B and B? are each a linear or branched alkylene group having 2 to 15 carbon atoms, “c” is an average number of 1 to
20, when a plurality of B's are existent, B's may be the same or different, and R5 and R6 are each a hydrogen atom or methyl group.
US Pat. No. 10,095,145

SILICONE OIL-TREATED SILICA PARTICLES AND TONER FOR ELECTROPHOTOGRAPHY

TOKUYAMA CORPORATION, Sh...

1. A silicone oil-treated silica particle comprising a silica particle body and silicone oil, wherein:the silica particle body has a BET specific surface area of 70 m2/g to 120 m2/g,
the silica particle body has been surface-treated with the silicone oil,
the silica particle body is fumed silica,
the silica particle body has a particle density of 2.23 g/cm3 or more as measured by a helium (He) gas pycnometer, with an apparent density of 20 g/l to 35 g/l,
the amount of free silicone oil liberated from the surface of the silica particle body in the silicone oil accounts for 2.0 mass % to 5.0 mass % with respect to the silica particle body,
a surface-treated styrene acrylic resin particle, in which 2 parts by mass of the silicone oil-treated silica particle has been added to 100 parts by mass of a styrene acrylic resin particle having a particle size median of 5 um to 8 um, has a degree of agglomeration of 18% or less, and
wherein respective fractal shape parameter a values of the silica particle body in measurement ranges of 20-30 nms, 30-40 nm, and 50-70 nm have a maximum value ?max of 2.9 or more.
US Pat. No. 10,128,010

RADIATION SHIELDING MATERIAL AND PRODUCTION METHOD THEREFOR

Tokuyama Corporation, Sh...

1. A radiation shielding material, comprising:a resin composition containing a proportion of 20 to 80 vol % of fluoride powder containing barium as a constituent element, wherein
a difference between a refractive index of resin constituting the resin composition and a refractive index of the fluoride powder is within ±0.05.

US Pat. No. 10,307,763

POLYCRYSTALLINE SILICON FRAGMENT, METHOD FOR MANUFACTURING POLYCRYSTALLINE SILICON FRAGMENT, AND POLYCRYSTALLINE SILICON BLOCK FRACTURE DEVICE

Tokuyama Corporation, Ya...

1. A polycrystalline silicon fragment obtained by fracturing a polycrystalline silicon block which is not carried out with a wet chemical cleaning using acid, comprising:i) 90 wt % or more of said polycrystalline silicon fragment has the particle size of 4 to 60 mm;
ii) a content ratio of polycrystalline silicon powder having the particle size of 500 to 1000 ?m is 1 to 30 ppmw;
iii) a content ratio of the silicon dust having the particle size of less than 500 ?m is 10 to 60 ppmw, and
iv) a metal of a surface contamination including at least one metal selected from the group consisting of Na, Cr, Fe, Ni, Cu, Zn, Co, and W is 3 to 15 ppbw.
US Pat. No. 10,301,485

COATING COMPOSITION AND OPTICAL ARTICLE HAVING A COAT LAYER MADE OF THE COATING COMPOSITION

TOKUYAMA CORPORATION, Sh...

1. A coating composition comprising (A) inorganic oxide fine particles containing at least one element selected from the group consisting of Ti, Zr, Sn and Sb, (B) a hydrolysable group-containing organic silicon compound, and (C1) a surfactant having an HLB value of 8 or less and (C2) a surfactant having an HLB value of more than 8 as (C) surfactants, wherein the mass ratio (C1/C2) of the surfactant having an HLB value of 8 or less (C1) and the surfactant having an HLB value of more than 8 (C2) is 0.3 to 1.0.

US Pat. No. 10,287,704

PROCESS FOR PRODUCING SILICON SINGLE CRYSTAL

Tokuyama Corporation, Sh...

1. A process for producing a silicon single crystal by heating a silicon raw material held in a crucible to provide a silicon melt and allowing a silicon single crystal to grow during the pulling-up of a silicon single crystal ingot from the silicon melt, the process comprising using, as at least part of the silicon raw material, crushed materials of a polycrystalline silicon rod produced by Siemens process, the crushed materials obtained by crushing an end of the rod in the vicinity contacting a carbon core wire holding member,wherein a carbon concentration of the crushed materials is from 0.04 to 2.8 ppma,
wherein the crushed materials are obtained by removing a core including both the carbon core wire holding member embedded into the rod end and a polycrystalline silicon surrounding the carbon core wire holding member and covering a distance of 3 mm or more from an interface of the polycrystalline silicon with the carbon core wire holding member from the rod end cut off from the polycrystalline silicon rod to give a rod end hollow body, and thereafter crushing the rod end hollow body,
wherein the polycrystalline silicon is in direct contact with a surface of the carbon core wire holding member, and
wherein carbon from the carbon core wire holding member is incorporated into the polycrystalline silicon while silicon is being deposited.

US Pat. No. 10,494,488

POLYROTAXANE, PRODUCTION METHOD THEREFOR, AND OPTICAL COMPOSITION CONTAINING SAID POLYROTAXANE

Tokuyama Corporation, Sh...

1. A polyrotaxane, comprising a composite molecular structure formed of an axle molecule and a plurality of cyclic molecules clathrating the axle molecule, wherein the polyrotaxane satisfies at least one of requirements (X) and (Y):requirement (X): a side chain having a tertiary hydroxyl group is introduced into at least part of the cyclic molecule of the polyrotaxane; and
requirement (Y): a side chain having a group represented by the following formula (1):
-A  (1)
wherein, A is an organic group having 1 to 10 carbon atoms and contains at least one hydroxyl group is introduced into at least part of the cyclic molecule of the polyrotaxane; and a pKa of a hydroxyl group of a compound represented by the following formula (2):
H-A  (2)
is 6 or more and less than 14,
wherein the side chain having the tertiary hydroxyl group comprises a structure represented by the following formula (1?):

wherein, Q is formed of at least one kind selected from structures represented by the following formulas (Q-1), (Q-2) and (Q-3):

wherein, G is a straight-chain alkylene group or alkenylene group having 1 to 8 carbon atoms; a branched-chain alkylene group or alkenylene group having 3 to 20 carbon atoms; an alkylene group or alkenylene group formed by replacement a part of the alkylene group or alkenylene group by a —O— bond, a —NH— bond, a —SO— bond or a —SiO— bond; or an alkylene group formed by replacement of a part of hydrogen of the alkylene group by at least one kind selected from the group consisting of a hydroxyl group, a carboxyl group, an acyl group, a phenyl group, a halogen atom and an olefin group, and when a plurality of G exist, each G may be a same group or a different group, and n1, n2, n3 are each independently an integer from 1 to 200, and
when Q is formed of two or more kinds selected from the formulas (Q-1), (Q-2) and (Q-3), G constituting (Q-1) to (Q-3) may be a same group or a different group, a total of n1, n2 and n3 is an integer from 1 to 200, Xis an alkylene group or alkenylene group having 2 to 20 carbons, or an alkylene group or alkenylene group formed by replacement of a part of the alkylene group or alkenylene group by a —O— bond or a —NH— bond; R3 and R4 are each independently selected from a straight-chain alkyl group having 1 to 6 carbon atoms or a branched-chain alkyl group having 1 to 6 carbon atoms; and R5 is carbon or sulfur, and
wherein a side chain represented by the following formula (3?) is introduced into at least part of the cyclic molecule:

wherein, Q is formed of at least one kind selected from structures represented by the following formulas (Q-1), (Q-2) and (Q-3):

wherein, G is a straight-chain alkylene group or alkenylene group having 1 to 8 carbon atoms; a branched-chain alkylene group or alkenylene group having 3 to 20 carbon atoms; an alkylene group or alkenylene group formed by replacement of a part of the alkylene group or alkenylene group by a —O— bond, a —NH— bond, a —SO— bond or a —SiO— bond; or an alkylene group formed by replacement of a part of hydrogen of the alkylene group by at least one kind selected from the group consisting of a carboxyl group, an acyl group, a phenyl group, a halogen atom and an olefin group, and when a plurality of G exist, each G may be a same group or a different group, and n1, n2 and n3 are each independently an integer from 1 to 200, and
when Q is formed of two or more kinds selected from the formulas (Q-1), (Q-2) and (Q-3), G constituting (Q-1) to (Q-3) may be a same group or a different group, a total of n1, n2 and n3 is an integer from 1 to 200, and R6 is carbon or sulfur, X is an alkylene group or alkenylene group having 2 to 20 carbons; or an alkylene group or alkenylene group formed by replacement of a part of the alkylene group or alkenylene group by a —O— bond or a —NH— bond, and A is an organic group having 1 to 10 carbon atoms and contains at least one hydroxyl group.

US Pat. No. 10,526,533

PROCESS FOR PRODUCING A PHOTOCHROMIC CURED BODY

TOKUYAMA CORPORATION, Ya...

1. A process for producing a photochromic cured body by curing a photochromic composition comprising (A) a polyiso(thio)cyanate compound having at least two isocyanate groups and/or isothiocyanate groups in one molecule, (B) a poly(thi)ol compound having at least two hydroxyl groups and/or thiol groups in one molecule, (C) a mono(thi)ol compound having one hydroxy group or thiol group in one molecule, (D) a photochromic compound, and (E) a polyrotaxane having a composite molecular structure composed of an axial molecule and a plurality of cyclic molecules clathrating the axial molecule.

US Pat. No. 10,518,964

POLYSILICON PACKAGE

TOKUYAMA CORPORATION, Sh...

1. A polysilicon package in which a bag formed from a linear low-density polyethylene (LLDPE)-based resin film having an average thickness of 300 ?m or less is filled with crushed polysilicon that is obtained by mechanically crushing a polysilicon rod, wherein:the bag has a heat-sealed bonded part at a bottom and filled with crushed polysilicon to ensure that a maximum expansion of the bag is not less than 0% but is 5% or less while the bag is held in an upright state with the bottom as a ground contact surface, and
the linear low-density polyethylene-based resin film forming the bag is metallocene-catalyzed linear low-density polyethylene.

US Pat. No. 10,354,862

APPARATUS FOR MANUFACTURING GROUP III NITRIDE SINGLE CRYSTAL, METHOD FOR MANUFACTURING GROUP III NITRIDE SINGLE CRYSTAL USING THE APPARATUS, AND ALUMINUM NITRIDE SINGLE CRYSTAL

TOKUYAMA CORPORATION, Sh...

1. A method of manufacturing a group III nitride single crystal comprising the step of:(a) supplying a group III source gas and a nitrogen source gas to the reaction area of an apparatus for manufacturing the group III nitride single crystal comprising:
a reaction vessel comprising a reaction area, wherein in the reaction area, a group III source gas and a nitrogen source gas are reacted such that a group III nitride crystal is grown on a substrate;
a susceptor arranged in the reaction area and supporting the substrate;
a group III source gas supply nozzle supplying the group III source gas to the reaction area; and
a nitrogen source gas supply nozzle supplying the nitrogen source gas to the reaction area,
wherein the nitrogen source gas supply nozzle is configured to supply the nitrogen source gas and at least one halogen-based gas selected from the group consisting of a hydrogen halide gas and a halogen gas to the reaction area;
wherein the nitrogen source gas supply nozzle comprises:
a nitrogen source gas inlet from which the nitrogen source gas is introduced to the reaction vessel;
a nitrogen source gas outlet from which the nitrogen source gas flows out to the reaction area; and
a junction arranged between the nitrogen source gas inlet and the nitrogen source gas outlet, wherein a halogen-based gas inlet nozzle is joined to the nitrogen source gas supply nozzle at the junction, and wherein the halogen-based gas inlet nozzle supplies at least one halogen-based gas selected from a group consisting of a hydrogen halide gas and a halogen gas, such that the group III source gas and the nitrogen source gas react,
wherein in the step (a), the nitrogen source gas and at least one halogen-based gas selected from a hydrogen halide gas and a halogen gas are supplied to the reaction area from the nitrogen source gas supply nozzle; and
wherein in the step (a), the nitrogen source gas joins with the halogen-based gas at the junction, and thereafter is supplied from the nitrogen source gas outlet to the reaction area.

US Pat. No. 10,428,813

STATE MONITORING SYSTEM OF MOVING APPARATUS

Tokuyama Corporation, Ya...

1. A state monitoring system of a reciprocating-type compressor comprising:a personal computer including a processor and a memory, and
a vibration sensor configured to measure the vibrations of the reciprocating-type compressor during operation of said reciprocating-type compressor and to output a waveform of measured vibration data, wherein:
the reciprocating-type compressor comprises one or more constituent members that are to be monitored and that are to be located inside a casing of said reciprocating type compressor;
the vibration sensor is located at one or plural sites of the reciprocating-type compressor including at least one of a lower part of the crank case, a casing of the distance piece or cylinder, or the constituent member;
the processor functions as a simulator comprising a model of said reciprocating-type compressor;
the simulator replaces vibrations caused by characteristics of said constituent members and/or a connecting part between constituent members and/or a sliding part with vibrations caused by said characteristics of a viscoelastic member; and
the processor is configured to output virtual vibration data having vibrations equivalent to synthesized vibrations of the viscoelastic member;
the memory functions as a parameter memory unit for storing the parameter of a spring constant or the spring constant and a viscous damping coefficient of said viscoelastic member;
the stored parameter is obtained by operating said simulator so that the waveform of said virtual vibration data output from said model of said simulator is made substantially to match the measured waveform output by the vibration sensor during normal operation of the reciprocating-type compressor;
the processor functions as a parameter identifying part in which by changing the parameters of said viscoelastic member, the waveforms of the virtual vibration data output from the model are made substantially to match the vibration waveforms obtained at the arbitrary one or plural sites during actual operation of the reciprocating-type compressor;
the processor functions as a parameter-change verifying part which verifies how said parameters change during actual operation identified by said parameter-identifying part in comparison with parameters of said reciprocating-type compressor during normal operation stored in said parameter-memory unit; and
the processor outputs a warning when the change in said parameters indicates that a breakdown is estimated.

US Pat. No. 10,531,640

TEAT OPENING PROTECTION PATCH FOR LIVESTOCK

TOKUYAMA CORPORATION, Ya...

1. A teat opening protection patch to be stuck to portions inclusive of a teat opening of livestock, including a laminate of an elastic sheet and an adhesive layer laminated on one surface of the elastic sheet, said laminate having a double-stretched tensile stress in range of 0.1 to 5 N, wherein,(a) the laminate has a circular planar shape or elliptic planar shape, and
(b) the planar shape is imparted to a part to be adhered to the teat opening,and wherein a removable protection film is laminated on the surface of said laminate on the side opposite to the adhesive layer, and a parting sheet is stuck to the surface of said adhesive layer.

US Pat. No. 10,508,035

ALUMINUM NITRIDE POWDERS

TOKUYAMA CORPORATION, Sh...

1. Aluminum nitride single crystal particles, each having a flat octahedral shape in a direction where hexagonal faces are opposed to each other, which is composed of two opposed hexagonal faces and six rectangular faces, whereinan average distance “D” between two opposed corners within each of the hexagonal faces is 19.1 to 110 ?m, a length “L” of the short side of each of the rectangular faces is 2 to 45 ?m, and L/D is 0.05 to 0.33; each of the hexagonal faces and each of the rectangular faces cross each other to form a curve without forming a single ridge; and the true density is 3.20 to 3.26 g/cm3.

US Pat. No. 10,640,385

CORE WIRE HOLDER AND METHOD FOR PRODUCING SILICON

TOKUYAMA CORPORATION, Ya...

1. A core wire holder attached on a metal electrode placed on a bottom panel of a device for producing silicon by Siemens process, the core wire holder comprising:a silicon core wire holding portion being generally circular truncated cone-shaped, and configured to hold and energize a silicon core wire, wherein:
the silicon core wire holding portion is inscribed and includes a generally circular truncated cone having an upper surface formed with a silicon core wire insertion hole for holding the silicon core wire,
the circular truncated cone includes an upper surface in a shape of a first circle with a diameter “a”,
the circular truncated cone includes a bottom surface in a shape of a second circle with a diameter “b”,
the circular truncated cone has a height “h”,
the silicon core wire holding portion includes a chamfered portion having a curved surface formed on a ridge formed by the upper surface and a side surface of the silicon core wire holding portion,
the curved surface has a radius “R” of curvature, and
“a”, “b”, “h”, and “R” satisfy the following conditions: a

US Pat. No. 10,689,349

METHOD FOR PRODUCING INTERMEDIATE OF BIOTIN AND METHOD FOR PRODUCING BIOTIN

Tokuyama Corporation, Ya...

1. A method for producing a lactone compound in which an ureido compound represented by the following formula (11)
wherein, R1 and R2 may be the same or different and represent a hydrogen atom or a protecting group of an ureylene group, is dehydrated by refluxing in a reaction solvent comprising mesitylene, thereby producing an anhydride compound represented by the following formula (7)

the anhydride compound and an optically active amine compound represented by the following formula (8)

wherein, R4 represents an alkyl group, an aralkyl group, or an aryl group, and each of R5, R6, and R7 represents a hydrogen atom, an alkyl group, an alkoxy group, or a halogen atom, are reacted in a reaction solvent comprising mesitylene, thereby producing a mixture which comprises an amide compound I represented by the following formula (9)

and an amide compound II represented by the following formula (10)

a first reaction solution comprising the obtained mixture and mesitylene is refluxed to dehydrate the mixture, thereby producing a trione compound represented by the following formula (1)

the trione compound is (ii) reduced by calcium borohydride in ethanol, thereby producing an amide alcohol compound represented by the following formula (3)

and the amide alcohol compound is cyclized in the presence of hydrogen chloride in a solvent comprising an alkylene glycol monoalkyl ether in which the total number of carbon atoms in a molecule is 2 to 12, thereby producing a lactone compound represented by the following formula (4)

US Pat. No. 10,690,943

LAMINATE AND OPTICAL ARTICLE COMPRISING THE SAME

TOKUYAMA CORPORATION, Sh...

1. A laminate comprising a pair of polycarbonate optical sheets or films which are laminated together through a polarizing film layer and an adhesive layer of a photochromic composition comprising (I) a polyurethane urea resin and (II) a photochromic compound,wherein the photochromic composition further comprises (III) a polyisocyanate compound having at least two isocyanate groups in the molecule, and the polyisocyanate compound having at least two isocyanate groups in the molecule (III) comprises (IIIA) a compound having an isocyanate group bonded to a secondary carbon and (IIIB) at least one compound selected from the group consisting of hexamethylene diisocyanate, burette compound of hexamethylene diisocyanate, isocyanurate compound of hexamethylene diisocyanate and adduct compound of hexamethylene diisocyanate.

US Pat. No. 10,884,334

PHOTOCURABLE RESIN COMPOSITION

TOKUYAMA CORPORATION, Sh...

1. A photocurable resin composition comprising:(A) an N-vinyl amide compound represented by the following formula (1):

wherein R1 and R2 are each independently a hydrogen atom or hydrocarbon group having 1 to 5 carbon atoms, or R1 and R2 may be bonded together to form a hydrocarbon group having 2 to 6 carbon atoms;
(B) a polyfunctional (meth)acrylate monomer represented by the following formula (2):

wherein R4 and R5 are each independently a hydrogen atom or methyl group, R3 is a trivalent to hexavalent organic residue, “a” is an integer of 0 to 3, and “b” is an integer of 3 to 6;
(C) a photopolymerization initiator; and
(D) a compound having a 2,2,6,6-tetramethyl-4-piperidyl skeleton and represented by the following formula (4) as a radical scavenger;

wherein R9 and R10 are each independently a hydrogen atom or methyl group, and “e” is an integer of 5 to 12.

US Pat. No. 10,953,469

METHOD OF PRODUCING METAL POWDER

TOKUYAMA CORPORATION, Sh...

1. A method of producing a metal powder including:a preparatory step of providing a metal chloride gas and a reducing gas;
a gas phase reduction step in which said metal chloride gas and said reducing gas are contacted and mixed together so as to undergo a gas phase reduction reaction to form metal particles in a mixed gas stream formed by said metal gas and said reducing gas; and
a collection step of obtaining a metal powder by collecting the metal particles from the gas stream after said gas phase reduction reaction; wherein,
in said preparatory step, said metal chloride gas and said reducing gas are heated separately from each other, said metal chloride gas being maintained at a temperature lower than a thermal decomposition temperature of said metal chloride;
in said preparatory step, a multiple tube is used, the metal chloride gas is fed into at least one tube of said multiple tube, and the reducing gas is fed into at least the other tube of said multiple tube such that said metal chloride gas and said reducing gas are separately heated in said multiple tube;
in said gas phase reduction step, said metal chloride gas and said reducing gas are contacted together so that the temperature of the mixed gas of said metal chloride gas and said reducing gas becomes higher than a temperature at which said gas phase reduction reaction takes place;
the metal powder obtained through said collection step has a BET specific surface area of 5 to 250 m2/g, and
wherein said reducing gas is a hydrogen gas.
US Pat. No. 10,947,155

RECYCLING METHOD OF DIHYDRATE GYPSUM FROM WASTE GYPSUM BOARDS

TOKUYAMA CORPORATION, Ya...

1. A method of recycling dihydrate gypsum from waste gypsum boards, the method comprising:calcining gypsum derived from waste gypsum boards to convert the gypsum into hemihydrate and/or anhydrous type III gypsum granules;
dropping the gypsum granules after calcination into water to mix the gypsum granules with water to prepare a gypsum slurry; and
crystalizing dihydrate gypsum particles in the gypsum slurry; wherein
a temperature of the gypsum granules just before being dropped into the water is 90° C. or higher.
US Pat. No. 10,920,007

URETHANE RESIN COMPRISING A POLYROTAXANE AND POLISHING PAD

TOKUYAMA CORPORATION, Ya...

1. A urethane resin obtained by polymerizing a polymerizable composition, which comprises (A) a polyrotaxane having a composite molecular structure comprising an axial molecule and a plurality of cyclic molecules clathrating the axial molecule, wherein side chains having a group with active hydrogen which are introduced into at least some of the cyclic molecules, and (B) a polyiso(thio)cyanate compound,wherein the polyiso(thio)cyanate compound (B) contains (B2) a urethane prepolymer having an iso(thio)cyanate group at the end of the molecule which is obtained by reacting (C1) a bifunctional active hydrogen-containing compound having two groups with active hydrogen in the molecule with (B1) a bifunctional iso(thio)cyanate group-containing compound having two iso(thio)cyanate groups in the molecule.

US Pat. No. 10,906,021

STAINLESS STEEL MEMBER AND PRODUCTION METHOD THEREOF

TOKUYAMA CORPORATION, Ya...

1. An austenite stainless steel member comprising:a base material made of austenite stainless steel; and
a passivation layer formed on a surface of the base material made of austenite stainless steel, wherein the passivation layer has a thickness of 2 nm to 20 nm, a concentration of chromium atoms in an outermost surface of the passivation layer is 0.1 atomic % to 1.0 atomic %, and a concentration of silicon atoms in the outermost surface of the passivation layer is 2 atomic % to 10 atomic %.

US Pat. No. 10,822,718

METHOD FOR PRODUCING ALUMINUM NITRIDE SINGLE CRYSTAL SUBSTRATE

TOKUYAMA CORPORATION, Sh...

1. A method for producing an aluminum nitride single crystal substrate, the method comprising:i) preparing a first base substrate consisting of a first aluminum nitride single crystal, the first base substrate having a main face;
ii) growing a first aluminum nitride single crystal layer having a thickness of no less than 500 ?m over the main face of the first base substrate, to obtain a layered body comprising the first base substrate and the first aluminum nitride single crystal layer grown over the main face of the first base substrate, wherein the ii) comprises supplying an aluminum source and a nitrogen source onto the main face of the first base substrate;
iii) cutting the first aluminum nitride single crystal layer of the layered body, to separate the layered body into a second base substrate and a first part of the first aluminum nitride single crystal layer, the second base substrate comprising the first base substrate and a thin film layered thereon, the thin film being a second part of the first aluminum nitride single crystal layer;
iv) polishing a surface of the thin film in the second base substrate, to obtain a third base substrate consisting of a second aluminum nitride single crystal; and
v) growing a second aluminum nitride single crystal layer over the polished surface of the third base substrate;
wherein an X-ray omega rocking curve of an inclined crystal face of the first base substrate has a half width of no more than 100 arcsec, wherein the X-ray omega rocking curve of the inclined crystal face is measured under a condition that an incident angle between an incident X-ray and the main face of the first base substrate is no less than 10°.
US Pat. No. 10,753,011

CLEANING METHOD AND LAMINATE OF ALUMINUM NITRIDE SINGLE-CRYSTAL SUBSTRATE

Tokuyama Corporation, Ya...

1. A cleaning method of an aluminum nitride single crystal substrate, comprising:a scrub cleaning step wherein a surface of the aluminum nitride single crystal substrate is scrubbed by moving a polymer compound material in a parallel direction of the surface of said substrate while said polymer compound material contacts the surface of said substrate, and
wherein said polymer compound material has a lower hardness than the aluminum nitride single crystal and absorbed with an alkaline aqueous solution having concentration of 0.01 to 1 wt % of an alkaline which is selected from the group consisting of potassium hydroxide and sodium hydroxide.

US Pat. No. 10,945,412

METHOD OF PROTECTING TEAT OPENING

TOKUYAMA CORPORATION, Sh...

1. A method of protecting a teat opening of livestock, which comprises sticking a surface of a teat opening protection patch including a laminate of an elastic sheet and an adhesive layer laminated on one surface of the elastic sheet, on a side of the adhesive layer to a teat so as to cover the teat opening of the livestock, said laminate having a double-stretched tensile stress in a range of 0.1 to 5 N,wherein,
(a) the laminate has a circular or elliptic planar shape, and
(b) the planar shape is imparted to a part to be adhered to the teat opening.

US Pat. No. 10,919,767

HEXAGONAL BORON NITRIDE POWDER AND PRODUCTION PROCESS THEREFOR

TOKUYAMA CORPORATION, Sh...

1. A hexagonal boron nitride powder whose maximum absorption peak within the range of 3,100 to 3,800 cm?1 is existent at 3,530 to 3,590 cm?1 in the diffuse reflectance fourier transform infrared spectrum.

US Pat. No. 10,900,143

POLYCRYSTALLINE SILICON ROD

Tokuyama Corporation, Ya...

1. A polycrystalline silicon rod, comprising:a silicon core wire; and
radially-deposited polycrystalline silicon including needle shape crystals around the silicon core wire,
wherein the polycrystalline rod has a column shape, and
wherein, at a cross section face of the polycrystalline silicon rod perpendicular to an axial direction, an area ratio of needle shape crystals having a long diameter of 50 ?m or more is 35% or more among crystals observed at the cross section face excluding the silicon core wire.

US Pat. No. 10,899,663

PROCESS FOR PRODUCING MODIFIED FLY ASH

TOKUYAMA CORPORATION, Sh...