CN113235166B - Preparation method of large-size antimony selenide single crystal material - Google Patents
Preparation method of large-size antimony selenide single crystal material Download PDFInfo
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- CN113235166B CN113235166B CN202110520744.6A CN202110520744A CN113235166B CN 113235166 B CN113235166 B CN 113235166B CN 202110520744 A CN202110520744 A CN 202110520744A CN 113235166 B CN113235166 B CN 113235166B
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
Abstract
The preparation method of the large-size antimony selenide single crystal material comprises the steps of synthesizing an antimony selenide polycrystalline raw material and growing an antimony selenide single crystal in sequence, wherein the antimony selenide polycrystalline raw material is sealed in a quartz ampoule and placed in a crystal growing furnace, the temperature of a high-temperature region is controlled to be 710-750 ℃, the temperature of a low-temperature region is controlled to be 400-420 ℃, the length of a gradient region is about 15cm, the temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient near a crystallization interface is 8-15 ℃/cm. The large-size antimony selenide single crystal prepared by the invention is a single crystal formed by 1 single grain, the grain size reaches more than 5.3cm, when the large-size antimony selenide single crystal is used for preparing a solar cell, the prepared antimony selenide can still obtain a smooth surface through cutting, polishing and other treatments, short circuit is not easy to occur, the carrier mobility is high, and due to the large size of the antimony selenide single crystal, the antimony selenide single crystal can be directly applied to the field of photoelectric detection in a single crystal structure, so that the performance of a detector is improved.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a preparation method of a large-size antimony selenide single crystal material.
Background
Antimony selenide (Sb)2Se3) The material has a direct forbidden band width of 1.15 eV and a large extinction coefficient, is a light absorption layer material with excellent performance, and has wide application prospects in the fields of solar cells, photocatalytic hydrolysis hydrogen production and photoelectric detectors. For example, the document Nature Communications 2018, 9:2179 reports that antimony selenide thin film materials are used for manufacturing thin film solar cells, and the photoelectric conversion efficiency reaches 7.6%. Antimony selenide materials are generally commonly polycrystalline, but the polycrystalline structure can degrade the optical and electrical properties of the material. The preparation of single crystal materials in the prior art is extremely small and the size is extremely small, which limits the single crystal Sb2Se3The large-size single crystal has not been reported yet in the fields of detection, battery plates and the like. CN105603532A preparation of Sb by solid phase sintering2Se3The size of the micron single crystal particles is 50-60 mu m, and if the micron single crystal particles are used for a solar cell, countless single crystal particles are needed, crystal boundaries exist among crystal grains, large pores exist, a smooth P-N junction interface cannot be formed, carriers can be scattered, the carrier mobility is reduced, and the photovoltaic performance or the light mobility is causedThe reduction of the electric detection sensitivity limits the application of antimony selenide in the occasions of photoelectric detection and the like. Therefore, it is desired to directly prepare a centimeter-level single crystal with 1 crystal grain to form 1 crystal, however, due to the technical reasons that antimony selenide is easy to decompose at high temperature and volatilize components, the growth of the antimony selenide single crystal is difficult, the uniformity of the crystal is poor, the defects are many, and no large-size antimony selenide single crystal and related products exist in the market.
Disclosure of Invention
The invention aims to provide a preparation method of a large-size antimony selenide single crystal material. The prepared antimony selenide is single crystal formed by single crystal particles of one centimeter grade, has good component uniformity and few defects, and is suitable for the fields of solar cells and photoelectric detection.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a large-size antimony selenide single crystal material is characterized by comprising the following steps: the synthesis of the antimony selenide polycrystalline raw material and the growth of the antimony selenide single crystal are sequentially carried out, wherein the growth of the antimony selenide single crystal is that the antimony selenide polycrystalline raw material is sealed in a quartz ampoule and is placed in a crystal growth furnace, the crystal growth furnace comprises a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area in the growth furnace is controlled to be 710-750 ℃, the temperature of the low-temperature area in the growth furnace is controlled to be 400-420 ℃, the length of the gradient area is about 15cm, the maximum temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient near a crystallization interface is 8-15 ℃/cm.
According to the invention, the temperature gradient is adjusted by controlling the temperature difference between the high-temperature area and the low-temperature area, and the temperature gradient of the crystallization interface is controlled at 8-15 ℃/cm. When the sealed quartz ampoule descends from the high-temperature area to the low-temperature area, the high temperature in the high-temperature area enables the upper selenium-rich molten polycrystalline raw material in the quartz ampoule to generate saturated vapor pressure to be increased, the large temperature difference generated by the high-temperature area and the low-temperature area and the regulation and control of the temperature gradient enable a large pressure difference to exist between the space at the upper end of the melt of the quartz ampoule and the melt, the components decomposed and volatilized by the quartz ampoule in the descending process are pressed into the melt with small pressure again by the high vapor pressure generated by the upper end, a single crystal is formed in the process of moving the quartz ampoule downwards, the distribution stability of each component in the crystal is guaranteed, the component uniformity is improved, the defects in the gradually formed single crystal are reduced, and therefore a large-size single crystal structure can be formed better.
Further, the synthesis of the antimony selenide polycrystalline raw material comprises the steps of mixing antimony particles and selenium powder, then placing the mixture in a quartz tube for baking, then heating to 550-800 ℃, preserving heat for 6-12 hours, and cooling to room temperature to obtain the antimony selenide polycrystalline ingot.
Further, the roasting in the synthesis process of the antimony selenide polycrystalline raw material is to heat the antimony selenide polycrystalline raw material at 40-80 ℃ for more than 30min while vacuumizing, and when the air pressure is lower than 10 DEG C-3And Pa, sealing the quartz tube.
Further, the mass ratio of the antimony particles to the selenium powder is 1: 1.02-1.05.
Further, the polycrystalline ingot is ground and then placed in a quartz ampoule to be baked, then the quartz ampoule is placed in a crystal growth furnace, before the quartz ampoule descends, the tip temperature is 650-660 ℃, the top temperature is 710-720 ℃, after heat preservation is carried out for 12 hours, the quartz ampoule descends at a speed of 1.5-5 mm/day until the whole quartz ampoule passes through a crystallization interface (solid-liquid interface), and then descending is stopped, so that single crystal growth is completed.
Further, after the quartz ampoule stops descending, the temperature of the high-temperature area is adjusted to 420-425 ℃ at the rate of 1-3 ℃/min, then the equipment is closed, and the crystal is taken out after cooling.
Most particularly, the preparation method of the large-size antimony selenide single crystal material is characterized by comprising the following steps:
the method comprises the following steps: synthesis of antimony selenide polycrystal raw material
Mixing antimony particles (with purity of 99.999%) and selenium powder (with purity of 99.999%) according to a ratio of 1: 1.02-1: 1.05, pouring into a quartz tube, baking at 40-80 ℃ for more than 30min while vacuumizing, and when the air pressure is lower than 10%-3Sealing is performed when Pa is less than Pa. Then placing the sealed quartz tube into a tube furnace, heating to 550-800 ℃, preserving heat for 6-12 hours, cooling to room temperature, and taking out the synthesized polycrystalline ingot from the quartz tube;
step two: growth of antimony selenide single crystals
Grinding the polycrystalline ingot into 200-400 mesh, pouring into a quartz ampoule with a tip, baking at 40-80 deg.C for more than 30min while vacuumizing, and when the air pressure is lower than 3 × 10-3Sealing when the temperature is below Pa, and suspending the quartz ampoule in a vertical Bridgman crystal growth furnace, wherein the growth furnace comprises a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area is controlled to be 710-750 ℃, the temperature of the low-temperature area is controlled to be 400-420 ℃, the length of the gradient area is about 15cm, the maximum temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient near a crystallization interface is 8-15 ℃/cm; before the quartz ampoule descends, the temperature of the tip is 650-660 ℃, the temperature of the top is 710-720 ℃, after heat preservation is carried out for 12h, the quartz ampoule descends at the speed of 1.5-5 mm/day until the whole quartz ampoule passes through a crystallization interface, then the descent is stopped, the growth of single crystal is completed, then the temperature of a high-temperature area is controlled, the temperature is reduced to 420-425 ℃ at the speed of 1-3 ℃/min, then the equipment is closed, and the crystal is taken out after cooling.
The invention has the following technical effects:
the large-size antimony selenide monocrystal prepared by the invention is a monocrystal formed by 1 single grain, the grain size reaches more than 5.3cm, the grain component uniformity is good, the defects are few, the antimony selenide prepared by the invention can still obtain a smooth surface through cutting, polishing and other treatments, short circuit is not easy to occur, the carrier mobility is high, and due to the large size of the antimony selenide, the antimony selenide can be directly applied to the field of photoelectric detection in a monocrystal structure, so that the performance of a detector is improved.
Drawings
FIG. 1: the structure of the crystal growing furnace adopted by the invention is schematically shown.
FIG. 2: the X-ray diffraction spectrum of the antimony selenide polycrystalline raw material synthesized by the invention.
FIG. 3: the X-ray diffraction spectrum of the antimony selenide single crystal material synthesized by the invention
FIG. 4: the centimeter-sized antimony selenide monocrystal substance prepared by the method is provided.
Detailed Description
The present invention will be further illustrated with reference to the following examples for better understanding, but the present invention is not limited to the following examples and should not be construed as being limited to the scope of the present invention, and those skilled in the art can make various insubstantial modifications and adaptations of the present invention based on the above-described present invention.
Example 1
A preparation method of a large-size antimony selenide single crystal material comprises the following steps:
the method comprises the following steps: synthesis of antimony selenide polycrystal raw material
Mixing 99.999% antimony particles and 99.999% selenium powder at a ratio of 1:1.05, pouring into a quartz tube, baking at 80 deg.C for more than 40min while vacuumizing, and when the air pressure is lower than 10%-3Sealing when the pressure is lower than Pa, then putting the sealed quartz tube into a tube furnace, heating to 800 ℃, preserving heat for 6 hours, cooling to room temperature, and taking out the synthesized polycrystalline ingot from the quartz tube;
step two: growth of antimony selenide single crystals
Grinding polycrystalline ingot into 400 mesh, pouring into quartz ampoule with tip, baking at 40 deg.C for 50min while vacuumizing, and when the air pressure is lower than 3 × 10-3Sealing when the temperature is below Pa, and suspending the quartz ampoule in a vertical Bridgman crystal growth furnace, wherein the growth furnace comprises a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area is controlled to be 750 ℃, the temperature of the low-temperature area is controlled to be 420 ℃, the length of the gradient area is about 15cm, the temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient near a crystallization interface is 8-15 ℃/cm; before the quartz ampoule descends, the temperature of the tip is 660 ℃, the temperature of the top is 720 ℃, after heat preservation is carried out for 12 hours, the quartz ampoule descends at the speed of 1.5mm/day until the whole quartz ampoule passes through a crystallization interface, then descending is stopped, single crystal growth is completed, then the temperature of a high-temperature area is controlled, the temperature is reduced to 420 ℃ at the speed of 3 ℃/min, then equipment is closed, and crystals are taken out after cooling.
The large-size antimony selenide single crystal material prepared by the embodiment has the size diameter of 21mm, the height of 53.4mm, good uniformity of crystal grain components and few defects, and the antimony selenide prepared by the invention can still obtain a smooth surface through cutting, polishing and other treatments, so that short circuit is not easy to occur, and the carrier mobility is high.
FIG. 2 is an X-ray diffraction pattern of the synthetic antimony selenide polycrystalline powder prepared in step one, which is known by comparison with card JCPDS 15-0861; FIG. 3 is an X-ray diffraction pattern of the antimony selenide single crystal material prepared by the invention, wherein only the diffraction peak of antimony selenide [061] appears, which shows that the whole crystal is uniformly oriented and is a complete single crystal grown along the [061] direction.
Example 2
A preparation method of a large-size antimony selenide single crystal material comprises the following steps:
the method comprises the following steps: synthesis of antimony selenide polycrystal raw material
Mixing antimony particles with purity of 99.999% and selenium powder with purity of 99.999% at a ratio of 1:1.02, pouring into a quartz tube, baking at 40 deg.C for 60min while vacuumizing, and when the air pressure is less than 10%-3Sealing is performed when Pa is less than Pa. Then placing the sealed quartz tube into a tube furnace, heating to 550 ℃, preserving heat for 12 hours, cooling to room temperature, and taking out the synthesized polycrystalline ingot from the quartz tube;
step two: growth of antimony selenide single crystals
Grinding into 200 mesh, pouring into quartz ampoule with tip, baking at 40 deg.C for 30min while vacuumizing, and controlling air pressure below 3 × 10-3Sealing is performed when Pa is less than Pa. The method comprises the following steps of suspending a quartz ampoule in a vertical Bridgman crystal growth furnace, wherein the growth furnace comprises a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area is controlled to be 710 ℃, the temperature of the low-temperature area is controlled to be 400 ℃, the length of the gradient area is about 15cm, the temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient near a crystallization interface is 8-15 ℃/cm; before the quartz ampoule descends, the temperature of the tip is 650 ℃, the temperature of the top is 710 ℃, after heat preservation is carried out for 12h, the quartz ampoule descends at the speed of 5mm/day until the whole quartz ampoule passes through a crystallization interface, then the descent is stopped, the growth of a single crystal is completed, then the temperature of a high-temperature area is controlled, the temperature is reduced to 425 ℃ at the speed of 1 ℃/min, then equipment is closed, and the crystal is taken out after cooling.
The large-size antimony selenide single crystal material prepared by the embodiment has the size diameter of 24mm, the height of 62.7mm, good uniformity of crystal grain components and few defects, and the antimony selenide prepared by the invention can still obtain a smooth surface through cutting, polishing and other treatments, so that short circuit is not easy to occur, and the carrier mobility is high.
Example 3
A preparation method of a large-size antimony selenide single crystal material comprises the following steps:
the method comprises the following steps: synthesis of antimony selenide polycrystal raw material
Mixing 99.999% antimony particles and 99.999% selenium powder at a ratio of 1:1.03, pouring into a quartz tube, baking at 50 deg.C for 50min while vacuumizing, and allowing the pressure to be lower than 10%-3Sealing is performed when Pa is less than Pa. Then putting the sealed quartz tube into a tube furnace, heating to 700 ℃, preserving heat for 8 hours, cooling to room temperature, and taking out the synthesized polycrystalline ingot from the quartz tube;
step two: growth of antimony selenide single crystals
Grinding polycrystalline ingot into 300 mesh, pouring into quartz ampoule with tip, baking at 60 deg.C for 40min while vacuumizing, and when the air pressure is lower than 3 × 10-3Sealing is performed when Pa is less than Pa. The method comprises the following steps of suspending a quartz ampoule in a vertical Bridgman crystal growth furnace, wherein the growth furnace comprises a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area is controlled to be 720 ℃, the temperature of the low-temperature area is controlled to be 410 ℃, the length of the gradient area is about 15cm, the temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient near a crystallization interface is 8-15 ℃/cm; before the quartz ampoule descends, the temperature of the tip is 655 ℃, the temperature of the top is 715 ℃, after heat preservation is carried out for 12 hours, the quartz ampoule descends at the speed of 3mm/day until the whole quartz ampoule passes through a crystallization interface, then the descent is stopped, the growth of a single crystal is completed, then the temperature of a high-temperature area is controlled to be reduced to 420 ℃ at the speed of 2 ℃/min, then equipment is closed, and the crystal is taken out after cooling.
The large-size antimony selenide single crystal material prepared by the embodiment has the size diameter of 26mm, the height of 66.9mm, good uniformity of crystal grain components and few defects, and the antimony selenide prepared by the invention can still obtain a smooth surface through cutting, polishing and other treatments, so that short circuit is not easy to occur, and the carrier mobility is high.
Claims (5)
1. A preparation method of a large-size antimony selenide single crystal material is characterized by comprising the following steps: the method comprises the steps of synthesizing an antimony selenide polycrystalline raw material and growing an antimony selenide single crystal in sequence, wherein the antimony selenide polycrystalline raw material is sealed in a quartz ampoule and placed in a crystal growing furnace, the temperature of the tip of the quartz ampoule is 650-660 ℃, the temperature of the top of the quartz ampoule is 710-720 ℃, the quartz ampoule is lowered at the speed of 1.5-5 mm/day after heat preservation is carried out for 12 hours until the whole quartz ampoule passes through a crystallization interface, then lowering is stopped, and single crystal growth is completed, the crystal growing furnace comprises three intervals of a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area in the growing furnace is controlled to be 710-750 ℃, the temperature of the low-temperature area is controlled to be 400-420 ℃, the length of the gradient area is 15cm, the maximum temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient of the crystallization interface is 8-15 ℃/cm.
2. The method for preparing a large-size antimony selenide single crystal material according to claim 1, wherein: the synthesis of the antimony selenide polycrystalline raw material comprises the steps of mixing antimony particles and selenium powder, then placing the mixture in a quartz tube for baking, then heating to 550-800 ℃, preserving heat for 6-12 hours, and cooling to room temperature to obtain antimony selenide polycrystalline ingots.
3. The method for preparing a large-size antimony selenide single crystal material according to claim 2, wherein: the mass ratio of the antimony particles to the selenium powder is 1: 1.02-1.05.
4. The method for preparing a large-size antimony selenide single crystal material according to claim 3, wherein: and after the quartz ampoule stops descending, adjusting the temperature of the high-temperature area to be reduced to 420-425 ℃ at the speed of 1-3 ℃/min, then closing the equipment, and taking out the crystal after cooling.
5. A preparation method of a large-size antimony selenide single crystal material is characterized by comprising the following steps:
the method comprises the following steps: synthesis of antimony selenide polycrystal raw material
Mixing antimony particles and selenium powder according to the mass ratio of 1: 1.02-1: 1.05, pouring the mixture into a quartz tube, baking while vacuumizing, and when the air pressure is lower than 10-3Sealing when the pressure is lower than Pa, then placing the sealed quartz tube into a tube furnace, heating to 550-800 ℃, preserving the heat for 6-12 hours, cooling to room temperature, and obtaining a crystal ingot;
step two: growth of antimony selenide single crystals
Grinding the polycrystalline ingot into 200-400 mesh, pouring into a quartz ampoule with a tip, baking at 40-80 deg.C for more than 30min while vacuumizing, and when the air pressure is lower than 3 × 10-3Sealing when the temperature is below Pa, and suspending the quartz ampoule in a vertical Bridgman crystal growth furnace, wherein the growth furnace comprises a high-temperature area, a gradient area and a low-temperature area, the temperature of the high-temperature area is controlled to be 710-750 ℃, the temperature of the low-temperature area is controlled to be 400-420 ℃, the length of the gradient area is 15cm, the maximum temperature gradient is controlled to be 20-24 ℃/cm, and the temperature gradient of a crystallization interface is 8-15 ℃/cm; before descending the quartz ampoule, the temperature of the tip is 650-660 ℃, the temperature of the top is 710-720 ℃, after heat preservation is carried out for 12 hours, the quartz ampoule descends at the speed of 1.5-5 mm/day until the whole quartz ampoule passes through a crystallization interface, then descending is stopped, single crystal growth is completed, then the temperature of a high-temperature area is controlled, the temperature is reduced to 420-425 ℃ at the speed of 1-3 ℃/min, then equipment is closed, and crystals are taken out after cooling.
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