JP2005289797A5 - Method for producing nitride crystal - Google Patents

Method for producing nitride crystal Download PDF

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JP2005289797A5
JP2005289797A5 JP2005066543A JP2005066543A JP2005289797A5 JP 2005289797 A5 JP2005289797 A5 JP 2005289797A5 JP 2005066543 A JP2005066543 A JP 2005066543A JP 2005066543 A JP2005066543 A JP 2005066543A JP 2005289797 A5 JP2005289797 A5 JP 2005289797A5
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すなわち、本発明の課題は、以下の窒化物結晶の製造方法により達成される。
(1)反応容器に原料とアンモニア溶媒を充填して前記反応容器を密閉した後、さらに前記反応容器を耐圧性容器内に挿入し、前記反応容器と前記耐圧性容器との間の空隙に第二溶媒を充填して前記耐圧性容器を密閉した後、昇温することにより窒化物結晶を得ることを特徴とする窒化物結晶の製造方法。
(2)少なくとも内側の表面が耐食性の反応容器に原料とアンモニア溶媒を充填して前記反応容器を密閉した後、さらに前記反応容器を耐圧性容器内に挿入し、前記反応容器と前記耐圧性容器との間の空隙に第二溶媒を充填して前記耐圧性容器を密閉した後、昇温することにより窒化物結晶を得ることを特徴とする窒化物結晶の製造方法。
(3)少なくとも内側の表面が貴金属製の反応容器に原料とアンモニア溶媒を充填して前記反応容器を密閉した後、さらに前記反応容器を耐圧性容器内に挿入し、前記反応容器と前記耐圧性容器との間の空隙に第二溶媒を充填して前記耐圧性容器を密閉した後、昇温することにより窒化物結晶を得ることを特徴とする窒化物結晶の製造方法。
(4)前記貴金属がRh、Pd、Ag、Ir、PtおよびAuからなる群から選ばれる少なくとも1種類の貴金属を主成分とすることを特徴とする(3)に記載の製造方法。
(5)前記反応容器がPtまたはPtを含む合金を主成分とする容器であることを特徴とする(4)に記載の製造方法。
(6)前記反応容器が少なくともひとつのバルブを付属していることを特徴とする(1)〜(5)のいずれか一項に記載の製造方法。
(7)前記第二溶媒がアンモニア溶媒であることを特徴とする(1)〜(6)のいずれか一項に記載の製造方法。
(8)前記反応容器内のアンモニア溶媒を亜臨界状態または超臨界状態で保持することを特徴とする(1)〜(7)のいずれか一項に記載の製造方法。
(9)少なくとも前記耐圧性容器内を20〜500MPaに保持することを特徴とする(1)〜(8)のいずれかの窒化物結晶の製造方法。
(10)少なくとも前記耐圧性容器内を200〜700℃に昇温することを特徴とする(1)〜(9)のいずれか一項に記載の製造方法。
(11)前記反応容器内に少なくとも1種類の添加物を添加することを特徴とする(1)〜(10)のいずれか一項に記載の製造方法。
(12)前記添加物が少なくとも1種類のハロゲン原子を含むことを特徴とする(11)に記載の製造方法。
(13)前記原料中の酸素含有量が5質量%以下であることを特徴とする(1)〜(12)のいずれか一項に記載の製造方法。
(14)前記原料中に窒化ガリウムを含有することを特徴とする(1)〜(13)のいずれか一項に記載の製造方法。
(15)前記反応容器内に少なくとも1種類の種結晶を設置し、アンモニア溶媒に溶解した原料が前記種結晶上に析出することを特徴とする(1)〜(14)のいずれか一項に記載の窒化物結晶の製造方法
That is, the object of the present invention is achieved by the following method for producing a nitride crystal.
(1) After filling the reaction vessel with a raw material and an ammonia solvent and sealing the reaction vessel, the reaction vessel is further inserted into the pressure-resistant vessel, and is inserted into the gap between the reaction vessel and the pressure-resistant vessel. A method for producing a nitride crystal, comprising filling a two-solvent and sealing the pressure-resistant container and then raising the temperature to obtain the nitride crystal.
(2) At least the inner surface is filled with a raw material and an ammonia solvent in a corrosion-resistant reaction vessel and the reaction vessel is sealed, and then the reaction vessel is inserted into the pressure-resistant vessel, and the reaction vessel and the pressure-resistant vessel A nitride crystal is obtained by filling a space between the second solvent and sealing the pressure-resistant container and then raising the temperature.
(3) At least the inner surface is filled with a raw material and an ammonia solvent in a reaction vessel made of a noble metal, and the reaction vessel is sealed. Then, the reaction vessel is further inserted into a pressure resistant vessel, and the reaction vessel and the pressure resistant property are sealed. A method for producing a nitride crystal, comprising filling a space between the container and a second solvent, sealing the pressure-resistant container, and then obtaining a nitride crystal by raising the temperature.
(4) The production method according to (3) , wherein the noble metal contains at least one kind of noble metal selected from the group consisting of Rh, Pd, Ag, Ir, Pt and Au as a main component.
(5) The manufacturing method according to (4) , wherein the reaction vessel is a vessel mainly composed of Pt or an alloy containing Pt.
(6) The production method according to any one of (1) to (5) , wherein the reaction vessel is provided with at least one valve.
(7) Said 2nd solvent is an ammonia solvent, The manufacturing method as described in any one of (1)- (6) characterized by the above-mentioned.
(8) The production method according to any one of (1) to (7) , wherein the ammonia solvent in the reaction vessel is maintained in a subcritical state or a supercritical state.
(9) The method for producing a nitride crystal according to any one of (1) to (8) , wherein at least the pressure-resistant container is maintained at 20 to 500 MPa.
(10) The method according to any one of (1) to (9) , wherein at least the inside of the pressure-resistant container is heated to 200 to 700 ° C.
(11) The production method according to any one of (1) to (10) , wherein at least one kind of additive is added to the reaction vessel.
(12) The production method according to (11) , wherein the additive contains at least one kind of halogen atom.
(13) The production method according to any one of (1) to (12) , wherein an oxygen content in the raw material is 5% by mass or less.
(14) The manufacturing method according to any one of (1) to (13) , wherein the raw material contains gallium nitride.
(15) At least one type of seed crystal is placed in the reaction vessel, and a raw material dissolved in an ammonia solvent is deposited on the seed crystal. (1) to (14) The manufacturing method of the nitride crystal of description .

Claims (15)

反応容器に原料とアンモニア溶媒を充填して前記反応容器を密閉した後、さらに前記反応容器を耐圧性容器内に挿入し、前記反応容器と前記耐圧性容器との間の空隙に第二溶媒を充填して前記耐圧性容器を密閉した後、昇温することにより窒化物結晶を得ることを特徴とする窒化物結晶の製造方法。After filling the reaction vessel with raw materials and an ammonia solvent and sealing the reaction vessel, the reaction vessel is further inserted into the pressure-resistant vessel, and a second solvent is placed in the gap between the reaction vessel and the pressure-resistant vessel. A method for producing a nitride crystal, comprising filling and sealing the pressure-resistant container and then obtaining a nitride crystal by heating. 少なくとも内側の表面が耐食性の反応容器に原料とアンモニア溶媒を充填して前記反応容器を密閉した後、さらに前記反応容器を耐圧性容器内に挿入し、前記反応容器と前記耐圧性容器との間の空隙に第二溶媒を充填して前記耐圧性容器を密閉した後、昇温することにより窒化物結晶を得ることを特徴とする窒化物結晶の製造方法。At least the inner surface is filled with a raw material and an ammonia solvent in a corrosion-resistant reaction vessel and the reaction vessel is sealed, and then the reaction vessel is inserted into the pressure-resistant vessel, and between the reaction vessel and the pressure-resistant vessel. A nitride crystal is obtained by filling a void in the second solvent and sealing the pressure-resistant container, followed by heating to obtain a nitride crystal. 少なくとも内側の表面が貴金属製の反応容器に原料とアンモニア溶媒を充填して前記反応容器を密閉した後、さらに前記反応容器を耐圧性容器内に挿入し、前記反応容器と前記耐圧性容器との間の空隙に第二溶媒を充填して前記耐圧性容器を密閉した後、昇温することにより窒化物結晶を得ることを特徴とする窒化物結晶の製造方法。 At least the inner surface is filled with a raw material and an ammonia solvent in a noble metal reaction vessel and the reaction vessel is sealed, and then the reaction vessel is inserted into the pressure vessel, and the reaction vessel and the pressure vessel A method for producing a nitride crystal, comprising filling a space between the second solvent and sealing the pressure-resistant container, followed by heating to obtain a nitride crystal. 前記貴金属がRh、Pd、Ag、Ir、PtおよびAuからなる群から選ばれる少なくとも1種類の貴金属を主成分とすることを特徴とする請求項に記載の製造方法。 The manufacturing method according to claim 3 , wherein the noble metal contains at least one kind of noble metal selected from the group consisting of Rh, Pd, Ag, Ir, Pt and Au as a main component. 前記反応容器がPtまたはPtを含む合金を主成分とする容器であることを特徴とする請求項に記載の製造方法。 The manufacturing method according to claim 4 , wherein the reaction vessel is a vessel mainly composed of Pt or an alloy containing Pt. 前記反応容器が少なくともひとつのバルブを付属していることを特徴とする請求項1〜のいずれか一項に記載の製造方法。 The process according to any one of claims 1 to 5, characterized in that said reaction vessel is supplied with at least one valve. 前記第二溶媒がアンモニア溶媒であることを特徴とする請求項1〜のいずれか一項に記載の製造方法。 The method according to any one of claims 1 to 6 , wherein the second solvent is an ammonia solvent. 前記反応容器内のアンモニア溶媒を亜臨界状態または超臨界状態で保持することを特徴とする請求項1〜のいずれか一項に記載の製造方法。 The production method according to any one of claims 1 to 7 , wherein the ammonia solvent in the reaction vessel is maintained in a subcritical state or a supercritical state. 少なくとも前記耐圧性容器内を20〜500MPaに保持することを特徴とする請求項1〜のいずれかの窒化物結晶の製造方法。 The method for producing a nitride crystal according to any one of claims 1 to 8 , wherein at least the pressure-resistant container is maintained at 20 to 500 MPa. 少なくとも前記耐圧性容器内を200〜700℃に昇温することを特徴とする請求項1〜のいずれか一項に記載の製造方法。 The manufacturing method according to any one of claims 1 to 9 , wherein at least the inside of the pressure-resistant container is heated to 200 to 700 ° C. 前記反応容器内に少なくとも1種類の添加物を添加することを特徴とする請求項1〜10のいずれか一項に記載の製造方法。 The manufacturing method according to any one of claims 1 to 10 , wherein at least one kind of additive is added to the reaction vessel. 前記添加物が少なくとも1種類のハロゲン原子を含むことを特徴とする請求項11に記載の製造方法。 The manufacturing method according to claim 11 , wherein the additive contains at least one kind of halogen atom. 前記原料中の酸素含有量が5質量%以下であることを特徴とする請求項1〜12のいずれか一項に記載の製造方法。 The process according to any one of claims 1 to 12, characterized in that the oxygen content in said raw material is not more than 5 wt%. 前記原料中に窒化ガリウムを含有することを特徴とする請求項1〜13のいずれか一項に記載の製造方法。 The manufacturing method according to any one of claims 1 to 13 , wherein the raw material contains gallium nitride. 前記反応容器内に少なくとも1種類の種結晶を設置し、アンモニア溶媒に溶解した原料が前記種結晶上に析出することを特徴とする請求項1〜14のいずれか一項に記載の窒化物結晶の製造方法。 The nitride crystal according to any one of claims 1 to 14 , wherein at least one kind of seed crystal is placed in the reaction vessel, and a raw material dissolved in an ammonia solvent is deposited on the seed crystal. Manufacturing method.
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