Method for growing gallium phosphide single crystals

Abstract

The invention relates to a method for growing gallium phosphide single crystals. The method comprises the following steps of: preparing materials, charging, vacuumizing, filling gas, heating for dissolving, welding seed crystals, seeding, shouldering, removing a floating needle for the first time, removing the floating needle for the second time, performing equal-diameter control, and ending, wherein gallium phosphide polycrystals, a floating boat, a doping agent and boron oxide are put into a crucible in the material preparation process, the floating boat is made of silicon nitride and has the internal diameter of phi20 to 80mm, and pressure is controlled to be 1.0 to 5.0MPa (absolute pressure) after a hearth is filled with nitrogen. The method has the advantages that: the diameter of the crystals is controlled by the floating boat, the density of the floating boat is between the density of the boron oxide and the density of gallium phosphide, the floating boat can float on a melting surface of the gallium phosphide, and the diameter is slightly influenced by the ascending or descending of a solid liquid interface in the floating boat due to temperature change, so the diameter of the crystals can be well controlled by controlling the rotating speed of the floating boat, the gallium phosphide single crystals with the size of 1 to 3 inches are grown, the yield of the single crystals is improved, the crystallization quality of the single crystals is high, and a mobility index in electrical parameters can stably reach 130-140cm<2> / v.s.

Description

technical field

[0001] The invention relates to a compound semiconductor single crystal growth process, in particular to a gallium phosphide single crystal growth method. Background technique

[0002] Gallium phosphide single crystal material can be used to manufacture general red, yellow, and green light-emitting diodes. It has low-current, high-efficiency light-emitting characteristics and is one of the main materials for visible light LEDs. At the same time, gallium phosphide single crystal materials can also be used as bonding materials for high-brightness light-emitting diodes, making the quaternary LED grains change from the original single-side light to six-side light, and its luminous brightness is increased by more than 60%, and the original The GaAs substrate absorbs energy, increasing the lifetime of the LED.

[0003] At present, the growth methods of gallium phosphide single crystal include high-pressure single crystal furnace liquid-sealed Czochralski method, v...

Examples

Embodiment 1

[0023] 1. Preparation: Carry out vacuum dehydration on boron oxide, corrode gallium phosphide polycrystal with aqua regia and wash it with deionized water, treat the quartz vessel with aqua regia and wash it with deionized water.

[0024] 2. Material preparation: Put 1.0 kg of gallium phosphide polycrystalline that has been etched and cleaned into a quartz crucible, put a float boat with an inner diameter of φ30 mm in the center of the crucible, add 40 mg of dopant sulfur, and then put 200 g of smashed boron oxide into the crucible crucible.

[0025] 3. Furnace installation: Install the seed crystal, cross, floating needle and lens, adjust the verticality of the crucible rod with a dial indicator, configure the graphite heater and heat preservation parts, and place the quartz crucible with polycrystalline material in the graphite crucible In the wall, the furnace body is sealed.

[0026] 4. Use a vacuum pump to pump out the air in the furnace, and the final air pressure is le...

Embodiment 2

[0037] 1. Preparation: Carry out vacuum dehydration on boron oxide, corrode gallium phosphide polycrystal with aqua regia and wash it with deionized water, treat the quartz vessel with aqua regia and wash it with deionized water.

[0038] 2. Material preparation: Put 1.5 kg of gallium phosphide polycrystalline that has been etched and cleaned into a quartz crucible, put a float boat with an inner diameter of φ45 mm in the center of the crucible, add 80 mg of dopant sulfur, and then put 400 g of smashed boron oxide into the crucible crucible.

[0039] 3. Furnace installation: Install the seed crystal, cross, floating needle and lens, adjust the verticality of the crucible rod with a dial indicator, configure the graphite heater and heat preservation parts, and place the quartz crucible with polycrystalline material in the graphite crucible In the wall, the furnace body is sealed.

[0040] 4. Use a vacuum pump to pump out the air in the furnace, and the final air pressure is le...

Embodiment 3

[0051] 1. Preparation: Carry out vacuum dehydration on boron oxide, corrode gallium phosphide polycrystal with aqua regia and wash it with deionized water, treat the quartz vessel with aqua regia and wash it with deionized water.

[0052] 2. Material preparation: Put 2.0 kg of gallium phosphide polycrystalline that has been etched and cleaned into a quartz crucible, put a float boat with an inner diameter of φ55 mm in the center of the crucible, put 900 mg of dopant tellurium, and then put 500 g of smashed boron oxide into the crucible crucible.

[0053] 3. Furnace installation: Install the seed crystal, cross, floating needle and lens, adjust the verticality of the crucible rod with a dial indicator, configure the graphite heater and heat preservation parts, and place the quartz crucible with polycrystalline material in the graphite crucible In the wall, the furnace body is sealed.

[0054] 4. Use a vacuum pump to pump out the air in the furnace, and the final air pressure i...

technical field

[0001] The invention relates to a compound semiconductor single crystal growth process, in particular to a gallium phosphide single crystal growth method. Background technique

[0002] Gallium phosphide single crystal material can be used to manufacture general red, yellow, and green light-emitting diodes. It has low-current, high-efficiency light-emitting characteristics and is one of the main materials for visible light LEDs. At the same time, gallium phosphide single crystal materials can also be used as bonding materials for high-brightness light-emitting diodes, making the quaternary LED grains change from the original single-side light to six-side light, and its luminous brightness is increased by more than 60%, and the original The GaAs substrate absorbs energy, increasing the lifetime of the LED.

[0003] At present, the growth methods of gallium phosphide single crystal include high-pressure single crystal furnace liquid-sealed Czochralski method, v...

Examples

Embodiment 1

[0023] 1. Preparation: Carry out vacuum dehydration on boron oxide, corrode gallium phosphide polycrystal with aqua regia and wash it with deionized water, treat the quartz vessel with aqua regia and wash it with deionized water.

[0024] 2. Material preparation: Put 1.0 kg of gallium phosphide polycrystalline that has been etched and cleaned into a quartz crucible, put a float boat with an inner diameter of φ30 mm in the center of the crucible, add 40 mg of dopant sulfur, and then put 200 g of smashed boron oxide into the crucible crucible.

[0025] 3. Furnace installation: Install the seed crystal, cross, floating needle and lens, adjust the verticality of the crucible rod with a dial indicator, configure the graphite heater and heat preservation parts, and place the quartz crucible with polycrystalline material in the graphite crucible In the wall, the furnace body is sealed.

[0026] 4. Use a vacuum pump to pump out the air in the furnace, and the final air pressure is le...

Embodiment 2

[0037] 1. Preparation: Carry out vacuum dehydration on boron oxide, corrode gallium phosphide polycrystal with aqua regia and wash it with deionized water, treat the quartz vessel with aqua regia and wash it with deionized water.

[0038] 2. Material preparation: Put 1.5 kg of gallium phosphide polycrystalline that has been etched and cleaned into a quartz crucible, put a float boat with an inner diameter of φ45 mm in the center of the crucible, add 80 mg of dopant sulfur, and then put 400 g of smashed boron oxide into the crucible crucible.

[0039] 3. Furnace installation: Install the seed crystal, cross, floating needle and lens, adjust the verticality of the crucible rod with a dial indicator, configure the graphite heater and heat preservation parts, and place the quartz crucible with polycrystalline material in the graphite crucible In the wall, the furnace body is sealed.

[0040] 4. Use a vacuum pump to pump out the air in the furnace, and the final air pressure is le...

Embodiment 3

[0051] 1. Preparation: Carry out vacuum dehydration on boron oxide, corrode gallium phosphide polycrystal with aqua regia and wash it with deionized water, treat the quartz vessel with aqua regia and wash it with deionized water.

[0052] 2. Material preparation: Put 2.0 kg of gallium phosphide polycrystalline that has been etched and cleaned into a quartz crucible, put a float boat with an inner diameter of φ55 mm in the center of the crucible, put 900 mg of dopant tellurium, and then put 500 g of smashed boron oxide into the crucible crucible.

[0053] 3. Furnace installation: Install the seed crystal, cross, floating needle and lens, adjust the verticality of the crucible rod with a dial indicator, configure the graphite heater and heat preservation parts, and place the quartz crucible with polycrystalline material in the graphite crucible In the wall, the furnace body is sealed.

[0054] 4. Use a vacuum pump to pump out the air in the furnace, and the final air pressure i...

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