PROCESS FOR SYNTHESIZING INDIUM PHOSPHIDE BY LIQUID PHOSPHORUS INJECTION METHOD | Matter42 Literature
Patent
Atlas literature
Patent
US 12,116,690 B2
PROCESS FOR SYNTHESIZING INDIUM PHOSPHIDE BY LIQUID PHOSPHORUS INJECTION METHOD
Lijie Fu, Niefeng Sun, Shujie Wang, Xiaolan Li et al.
THE 13TH RESEARCH INSTITUTE OF CHINA ELECTRONICS TECHNOLOGY GROUP CORPORATION, Hebei (CN)·Oct. 15, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
process chamber schematic
FIG. 1 is a schematic view showing a structure of a system for synthesizing indium phosphide by liquid phosphorus injection method in an example. In the …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 8 dependent
1
IndependentInPP₄InPB₂O₃Ga-In
A process for synthesizing indium phosphide by liquid phosphorus injection method based on a synthesis system comprising a quartz phosphorus bubble, a condenser, a phosphorus source furnace, a lifting crucible, a low tem-perature inert gas random delivery system and a monocrystal furnace, characterized in that the method comprises the following steps: 1) Indium cleaning: performing a surface cleaning treat-ment on indium, and drying the cleaned indium for later use; 2) Phosphorus charging: charging red phosphorus into the quartz phosphorus bubble under the protection of a nitrogen atmosphere; 3) Furnace loading: placing the quartz phosphorus bubble into the phosphorus source furnace for heating; then loading the phosphorus source furnace equipped with the quartz phosphorus bubble, the condenser, a seed crystal, the crucible filled with indium and a mated graphite support, an insulation jacket and a heater into a hearth of the monocrystal furnace, and placing a boron oxide protective agent; 4) Communication of condenser: communicating an inlet of the condenser with the low temperature inert gas random delivery system and a mouth of the quartz phosphorus bubble, and checking whether there is air leakage; 5) Synthesis: A, closing a furnace door, vacuuming the furnace, ran-domly delivering a low temperature inert gas by the low temperature inert gas random delivery system into the furnace through the condenser, and maintaining the pressure in the furnace greater than the dissociation pressure of indium phosphide; B, heating the indium in the crucible until the indium melts, C, lifting the crucible to allow an outlet end of the condenser to inserted into the indium melt, and intro-ducing a circulating cooling liquid into the condenser; and D, vaporizing the phosphorus in the quartz phosphorus bubble by heating the phosphorus source furnace, con-densing the vaporized phosphorus vapor into liquid white phosphorus through the condenser, and flowing the liquid white phosphorus into the indium melt to react and synthesize a proportioned indium phosphide; and 6) Preparation of crystals: after the phosphorus in the quartz phosphorus bubble is completely vaporized and injected into the indium melt, lowering the crucible away from the outlet of the condenser, and then low-ering the seed crystal to perform a high-pressure liquid encapsulation Czochralski (HP-LEC) crystal growth; wherein a condensing medium in the condenser is a gallium indium alloy.
2
Dependent← claim 1In
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that: the indium cleaning in step 1) com-prises removing oxides and residual impurities on the indium surface, wherein after cleaning, the indium reaches a purity of 6N, and has no dust impurities on the surface.
3
Dependent← claim 1P
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the purity of phosphorus in step 2) is 6N.
4
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the degree of vacuum in the phospho-rus source furnace in step 5) is 30-100 Pa.
7
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the heating power of the phosphorus source furnace in step 5) is increased from 0 W to 3000 W within 2 hours, and phosphorus is gradually vaporized by 770 K.
8
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the temperature in the crucible in step 5) is 1300-1400 K.
9
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the low temperature inert gas random delivery system includes a differential pressure controller that controls the pressure. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
indium
In
Precursor Metal
red phosphorus
P
Precursor Nonmetal
Process steps
Additional fabrication and treatment steps described in the patent.
1
InP Synthesis Liquid Phosphorus Injection
Step 1
Ambient
inert gas (nitrogen or argon) at >dissociation pressure of InP
Process details
encapsulant:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
—
0–3000 W
—
Temperature
Cited prior art
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 1
US 3,899,572 A3,899,572 A * 8/1975 Watanabe............... C01B 25/06examiner
Cited non-patent literature · 1
New Direct Synthesis Technique for Indium Phosphide Using Liquid Phosphorus T. Inada et al Journal of Crystal Growth 82 1987 pp. 561-565.
Patent
Atlas literature
Patent
US 12,116,690 B2
PROCESS FOR SYNTHESIZING INDIUM PHOSPHIDE BY LIQUID PHOSPHORUS INJECTION METHOD
Lijie Fu, Niefeng Sun, Shujie Wang, Xiaolan Li et al.
THE 13TH RESEARCH INSTITUTE OF CHINA ELECTRONICS TECHNOLOGY GROUP CORPORATION, Hebei (CN)·Oct. 15, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
process chamber schematic
FIG. 1 is a schematic view showing a structure of a system for synthesizing indium phosphide by liquid phosphorus injection method in an example. In the …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 8 dependent
1
IndependentInPP₄InPB₂O₃Ga-In
A process for synthesizing indium phosphide by liquid phosphorus injection method based on a synthesis system comprising a quartz phosphorus bubble, a condenser, a phosphorus source furnace, a lifting crucible, a low tem-perature inert gas random delivery system and a monocrystal furnace, characterized in that the method comprises the following steps: 1) Indium cleaning: performing a surface cleaning treat-ment on indium, and drying the cleaned indium for later use; 2) Phosphorus charging: charging red phosphorus into the quartz phosphorus bubble under the protection of a nitrogen atmosphere; 3) Furnace loading: placing the quartz phosphorus bubble into the phosphorus source furnace for heating; then loading the phosphorus source furnace equipped with the quartz phosphorus bubble, the condenser, a seed crystal, the crucible filled with indium and a mated graphite support, an insulation jacket and a heater into a hearth of the monocrystal furnace, and placing a boron oxide protective agent; 4) Communication of condenser: communicating an inlet of the condenser with the low temperature inert gas random delivery system and a mouth of the quartz phosphorus bubble, and checking whether there is air leakage; 5) Synthesis: A, closing a furnace door, vacuuming the furnace, ran-domly delivering a low temperature inert gas by the low temperature inert gas random delivery system into the furnace through the condenser, and maintaining the pressure in the furnace greater than the dissociation pressure of indium phosphide; B, heating the indium in the crucible until the indium melts, C, lifting the crucible to allow an outlet end of the condenser to inserted into the indium melt, and intro-ducing a circulating cooling liquid into the condenser; and D, vaporizing the phosphorus in the quartz phosphorus bubble by heating the phosphorus source furnace, con-densing the vaporized phosphorus vapor into liquid white phosphorus through the condenser, and flowing the liquid white phosphorus into the indium melt to react and synthesize a proportioned indium phosphide; and 6) Preparation of crystals: after the phosphorus in the quartz phosphorus bubble is completely vaporized and injected into the indium melt, lowering the crucible away from the outlet of the condenser, and then low-ering the seed crystal to perform a high-pressure liquid encapsulation Czochralski (HP-LEC) crystal growth; wherein a condensing medium in the condenser is a gallium indium alloy.
2
Dependent← claim 1In
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that: the indium cleaning in step 1) com-prises removing oxides and residual impurities on the indium surface, wherein after cleaning, the indium reaches a purity of 6N, and has no dust impurities on the surface.
3
Dependent← claim 1P
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the purity of phosphorus in step 2) is 6N.
4
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the degree of vacuum in the phospho-rus source furnace in step 5) is 30-100 Pa.
7
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the heating power of the phosphorus source furnace in step 5) is increased from 0 W to 3000 W within 2 hours, and phosphorus is gradually vaporized by 770 K.
8
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the temperature in the crucible in step 5) is 1300-1400 K.
9
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the low temperature inert gas random delivery system includes a differential pressure controller that controls the pressure. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
indium
In
Precursor Metal
red phosphorus
P
Precursor Nonmetal
Process steps
Additional fabrication and treatment steps described in the patent.
1
InP Synthesis Liquid Phosphorus Injection
Step 1
Ambient
inert gas (nitrogen or argon) at >dissociation pressure of InP
Process details
encapsulant:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
—
0–3000 W
—
Temperature
Cited prior art
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 1
US 3,899,572 A3,899,572 A * 8/1975 Watanabe............... C01B 25/06examiner
Cited non-patent literature · 1
New Direct Synthesis Technique for Indium Phosphide Using Liquid Phosphorus T. Inada et al Journal of Crystal Growth 82 1987 pp. 561-565.
Patent
Atlas literature
Patent
US 12,116,690 B2
PROCESS FOR SYNTHESIZING INDIUM PHOSPHIDE BY LIQUID PHOSPHORUS INJECTION METHOD
Lijie Fu, Niefeng Sun, Shujie Wang, Xiaolan Li et al.
THE 13TH RESEARCH INSTITUTE OF CHINA ELECTRONICS TECHNOLOGY GROUP CORPORATION, Hebei (CN)·Oct. 15, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
process chamber schematic
FIG. 1 is a schematic view showing a structure of a system for synthesizing indium phosphide by liquid phosphorus injection method in an example. In the …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 8 dependent
1
IndependentInPP₄InPB₂O₃Ga-In
A process for synthesizing indium phosphide by liquid phosphorus injection method based on a synthesis system comprising a quartz phosphorus bubble, a condenser, a phosphorus source furnace, a lifting crucible, a low tem-perature inert gas random delivery system and a monocrystal furnace, characterized in that the method comprises the following steps: 1) Indium cleaning: performing a surface cleaning treat-ment on indium, and drying the cleaned indium for later use; 2) Phosphorus charging: charging red phosphorus into the quartz phosphorus bubble under the protection of a nitrogen atmosphere; 3) Furnace loading: placing the quartz phosphorus bubble into the phosphorus source furnace for heating; then loading the phosphorus source furnace equipped with the quartz phosphorus bubble, the condenser, a seed crystal, the crucible filled with indium and a mated graphite support, an insulation jacket and a heater into a hearth of the monocrystal furnace, and placing a boron oxide protective agent; 4) Communication of condenser: communicating an inlet of the condenser with the low temperature inert gas random delivery system and a mouth of the quartz phosphorus bubble, and checking whether there is air leakage; 5) Synthesis: A, closing a furnace door, vacuuming the furnace, ran-domly delivering a low temperature inert gas by the low temperature inert gas random delivery system into the furnace through the condenser, and maintaining the pressure in the furnace greater than the dissociation pressure of indium phosphide; B, heating the indium in the crucible until the indium melts, C, lifting the crucible to allow an outlet end of the condenser to inserted into the indium melt, and intro-ducing a circulating cooling liquid into the condenser; and D, vaporizing the phosphorus in the quartz phosphorus bubble by heating the phosphorus source furnace, con-densing the vaporized phosphorus vapor into liquid white phosphorus through the condenser, and flowing the liquid white phosphorus into the indium melt to react and synthesize a proportioned indium phosphide; and 6) Preparation of crystals: after the phosphorus in the quartz phosphorus bubble is completely vaporized and injected into the indium melt, lowering the crucible away from the outlet of the condenser, and then low-ering the seed crystal to perform a high-pressure liquid encapsulation Czochralski (HP-LEC) crystal growth; wherein a condensing medium in the condenser is a gallium indium alloy.
2
Dependent← claim 1In
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that: the indium cleaning in step 1) com-prises removing oxides and residual impurities on the indium surface, wherein after cleaning, the indium reaches a purity of 6N, and has no dust impurities on the surface.
3
Dependent← claim 1P
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the purity of phosphorus in step 2) is 6N.
4
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the degree of vacuum in the phospho-rus source furnace in step 5) is 30-100 Pa.
7
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the heating power of the phosphorus source furnace in step 5) is increased from 0 W to 3000 W within 2 hours, and phosphorus is gradually vaporized by 770 K.
8
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the temperature in the crucible in step 5) is 1300-1400 K.
9
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the low temperature inert gas random delivery system includes a differential pressure controller that controls the pressure. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
indium
In
Precursor Metal
red phosphorus
P
Precursor Nonmetal
Process steps
Additional fabrication and treatment steps described in the patent.
1
InP Synthesis Liquid Phosphorus Injection
Step 1
Ambient
inert gas (nitrogen or argon) at >dissociation pressure of InP
Process details
encapsulant:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
—
0–3000 W
—
Temperature
Cited prior art
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 1
US 3,899,572 A3,899,572 A * 8/1975 Watanabe............... C01B 25/06examiner
Cited non-patent literature · 1
New Direct Synthesis Technique for Indium Phosphide Using Liquid Phosphorus T. Inada et al Journal of Crystal Growth 82 1987 pp. 561-565.
Patent
Atlas literature
Patent
US 12,116,690 B2
PROCESS FOR SYNTHESIZING INDIUM PHOSPHIDE BY LIQUID PHOSPHORUS INJECTION METHOD
Lijie Fu, Niefeng Sun, Shujie Wang, Xiaolan Li et al.
THE 13TH RESEARCH INSTITUTE OF CHINA ELECTRONICS TECHNOLOGY GROUP CORPORATION, Hebei (CN)·Oct. 15, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
process chamber schematic
FIG. 1 is a schematic view showing a structure of a system for synthesizing indium phosphide by liquid phosphorus injection method in an example. In the …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 8 dependent
1
IndependentInPP₄InPB₂O₃Ga-In
A process for synthesizing indium phosphide by liquid phosphorus injection method based on a synthesis system comprising a quartz phosphorus bubble, a condenser, a phosphorus source furnace, a lifting crucible, a low tem-perature inert gas random delivery system and a monocrystal furnace, characterized in that the method comprises the following steps: 1) Indium cleaning: performing a surface cleaning treat-ment on indium, and drying the cleaned indium for later use; 2) Phosphorus charging: charging red phosphorus into the quartz phosphorus bubble under the protection of a nitrogen atmosphere; 3) Furnace loading: placing the quartz phosphorus bubble into the phosphorus source furnace for heating; then loading the phosphorus source furnace equipped with the quartz phosphorus bubble, the condenser, a seed crystal, the crucible filled with indium and a mated graphite support, an insulation jacket and a heater into a hearth of the monocrystal furnace, and placing a boron oxide protective agent; 4) Communication of condenser: communicating an inlet of the condenser with the low temperature inert gas random delivery system and a mouth of the quartz phosphorus bubble, and checking whether there is air leakage; 5) Synthesis: A, closing a furnace door, vacuuming the furnace, ran-domly delivering a low temperature inert gas by the low temperature inert gas random delivery system into the furnace through the condenser, and maintaining the pressure in the furnace greater than the dissociation pressure of indium phosphide; B, heating the indium in the crucible until the indium melts, C, lifting the crucible to allow an outlet end of the condenser to inserted into the indium melt, and intro-ducing a circulating cooling liquid into the condenser; and D, vaporizing the phosphorus in the quartz phosphorus bubble by heating the phosphorus source furnace, con-densing the vaporized phosphorus vapor into liquid white phosphorus through the condenser, and flowing the liquid white phosphorus into the indium melt to react and synthesize a proportioned indium phosphide; and 6) Preparation of crystals: after the phosphorus in the quartz phosphorus bubble is completely vaporized and injected into the indium melt, lowering the crucible away from the outlet of the condenser, and then low-ering the seed crystal to perform a high-pressure liquid encapsulation Czochralski (HP-LEC) crystal growth; wherein a condensing medium in the condenser is a gallium indium alloy.
2
Dependent← claim 1In
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that: the indium cleaning in step 1) com-prises removing oxides and residual impurities on the indium surface, wherein after cleaning, the indium reaches a purity of 6N, and has no dust impurities on the surface.
3
Dependent← claim 1P
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the purity of phosphorus in step 2) is 6N.
4
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the degree of vacuum in the phospho-rus source furnace in step 5) is 30-100 Pa.
7
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the heating power of the phosphorus source furnace in step 5) is increased from 0 W to 3000 W within 2 hours, and phosphorus is gradually vaporized by 770 K.
8
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the temperature in the crucible in step 5) is 1300-1400 K.
9
Dependent← claim 1
The process for synthesizing indium phosphide by liquid phosphorus injection method according to claim 1, characterized in that, the low temperature inert gas random delivery system includes a differential pressure controller that controls the pressure. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
indium
In
Precursor Metal
red phosphorus
P
Precursor Nonmetal
Process steps
Additional fabrication and treatment steps described in the patent.
1
InP Synthesis Liquid Phosphorus Injection
Step 1
Ambient
inert gas (nitrogen or argon) at >dissociation pressure of InP
Process details
encapsulant:
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
—
0–3000 W
—
Temperature
Cited prior art
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 1
US 3,899,572 A3,899,572 A * 8/1975 Watanabe............... C01B 25/06examiner
Cited non-patent literature · 1
New Direct Synthesis Technique for Indium Phosphide Using Liquid Phosphorus T. Inada et al Journal of Crystal Growth 82 1987 pp. 561-565.