CN113293429B - Preparation method of monoclinic phase Ga2S3 single crystal - Google Patents
Preparation method of monoclinic phase Ga2S3 single crystal Download PDFInfo
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- CN113293429B CN113293429B CN202110603475.XA CN202110603475A CN113293429B CN 113293429 B CN113293429 B CN 113293429B CN 202110603475 A CN202110603475 A CN 202110603475A CN 113293429 B CN113293429 B CN 113293429B
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- 239000013078 crystal Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 229910005228 Ga2S3 Inorganic materials 0.000 title description 2
- 238000002425 crystallisation Methods 0.000 claims abstract description 23
- 230000008025 crystallization Effects 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims description 17
- 238000007789 sealing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000002834 transmittance Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 description 20
- 239000010453 quartz Substances 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 239000000203 mixture Substances 0.000 description 12
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 150000004770 chalcogenides Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002109 crystal growth method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
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- 238000005457 optimization Methods 0.000 description 1
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- 230000008569 process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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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
-
- 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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a monoclinic phase Ga 2 S 3 The preparation method of the single crystal adopts a vacuum closed fluxing agent Bridgman-Stockbarge method. Introduction ofFluxing agent Sb 2 S 3 To reduce monoclinic phase Ga 2 S 3 The crystallization temperature of the single crystal is controlled by the crystal growth parameters (temperature gradient, descending speed and the like) to prepare centimeter-level high-quality large-size monoclinic-phase Ga which can meet the practical requirement 2 S 3 The size of the single crystal can reach phi 10 multiplied by 20mm, and the transmittance in the ultraviolet visible light region can reach more than 90%.
Description
Technical Field
The invention belongs to the technical field of single crystal growth, and particularly relates to monoclinic phase Ga 2 S 3 Flux crucible descent method for single crystal.
Background
Monoclinic phase Ga 2 S 3 The crystal is a mid-far infrared band nonlinear optical crystal with excellent physicochemical performance, has frequency doubling response under the excitation of 2 mu m laser, presents phase matching characteristic, has no absorption at 2 mu m, and has a laser damage threshold of commercial AgGaS 2 30 times of the total birefringence, and AgGaS 2 And (4) the equivalent. Thus monoclinic phase Ga 2 S 3 The crystal is a potential high-power middle and far infrared nonlinear laser material.
It is well known that chalcogenide crystals cannot be synthesized and grown in open space due to their strong volatility and susceptibility to oxidation, but rather need to be performed in a closed anhydrous oxygen-free environment.
It is reported that Ga 2 S 3 There are 3 phases (low temperature cubic phase, medium temperature monoclinic phase, high temperature hexagonal phase), and overcoming the phase transition between the phases is to grow high quality monoclinic phase Ga 2 S 3 The first problem faced by crystals. However, the current single crystal growth technology is still in the laboratory research stage and cannot meet the requirement of high technology development due to the inexperience of the single crystal growth beam of the chalcogenide with inconsistent melting (or phase change), so that the industrialization technical level of the laboratory achievement for converting into productivity still falls behind. Therefore, it is of great interest to explore a method suitable for the crystal growth of such compounds.
Disclosure of Invention
The invention aims to provide a monoclinic phase Ga 2 S 3 Method for preparing monocrystals to obtain centimeter-sized large-size monoclinic-phase Ga meeting practical requirements 2 S 3 The single crystal has good quality and high transmittance, and the method is simple to operate, efficient, economical and practical.
In order to achieve the purpose, the invention adopts the following technical scheme:
monoclinic phase Ga 2 S 3 The preparation method of the single crystal comprises the following steps: the vacuum sealing fluxing agent falling crucible method is adopted. The method comprises the following steps:
1) ga is prepared from 2 S 3 Polycrystalline feedstock and Sb 2 S 3 Mixing and grinding uniformly, and then sealing in vacuum;
2) heating and melting the vacuum-sealed material at high temperature, and then cooling to obtain the monoclinic phase Ga 2 S 3 And (3) single crystal.
Ga in step 1) 2 S 3 Polycrystalline feedstock and Sb 2 S 3 In a molar ratio of 1: 0.8 to 1.2, vacuum degree of 10 -4 Pa。
The specific steps of the step 2) are as follows: placing the vacuum-sealed material in a high-temperature area in a growth device with a high-temperature area and a low-temperature area, heating to make the high-temperature area and the low-temperature area in the growth device reach preset temperatures, and carrying out heat preservation and melting to obtain a molten liquid; searching the position of a crystallization point in a growing device, and enabling the molten liquid to uniformly pass through the position of the crystallization point in a descending mode; cooling the high-temperature area and the low-temperature area to obtain the monoclinic-phase Ga 2 S 3 And (3) single crystal.
The preset temperature of the high-temperature area is 800-1000 ℃, the preset temperature of the low-temperature area is 450-650 ℃, and the temperature gradient in the growth device is 20-30 ℃/cm.
The melt is first lowered to a position 1-3 cm above the crystallization point, then uniformly passes through the crystallization point at a lowering speed of 0.1-0.2 mm/h, and then is kept stand.
And cooling the high-temperature area and the low-temperature area to room temperature at the speed of 15-25 ℃/h.
Preferably, Ga in step 1) 2 S 3 Polycrystalline feedstock and Sb 2 S 3 In a molar ratio of 1: 1; the preset temperature of the high-temperature area is 900 ℃, the preset temperature of the low-temperature area is 600 ℃, and the temperature gradient in the growth device is 25 ℃/cm; both the high temperature zone and the low temperature zone were cooled down to room temperature at a rate of 20 ℃/h.
The invention has the beneficial effects that: the invention adopts a vacuum closed fluxing agent Bridgman method to prepare monoclinic phase Ga 2 S 3 Single crystals based on synthesis and crystal growth of such compounds at a previous stageExploration, mixing a certain proportion of Sb with synthesized polycrystalline raw materials 2 S 3 The single-inclined-phase Ga is sealed in a closed quartz tube by melting, grows by adopting a Bridgman-Stockbarge method, and obtains centimeter-grade high-quality large-size monoclinic-phase Ga which can meet practical requirements by adjusting parameters such as temperature, descending speed and the like in the growth process 2 S 3 The size of the single crystal can reach phi 10 multiplied by 20mm, and the transmittance in the ultraviolet visible light region can reach more than 90%. The single crystal growth method is practical, simple to operate, economical, efficient, low in cost and environment-friendly.
Drawings
FIG. 1 is a diagram of monoclinic phase Ga obtained in example 1 2 S 3 A photograph of a single crystal.
FIG. 2 is a monoclinic phase Ga of example 1 2 S 3 Transmittance curve of single crystal.
FIG. 3 is a monoclinic phase Ga obtained in example 2 2 S 3 Photo of single crystal.
FIG. 4 shows monoclinic phase Ga obtained in example 3 2 S 3 A photograph of a single crystal.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
The invention provides a monoclinic phase Ga 2 S 3 The single crystal growth method adopts a closed fluxing agent Bridgman-Stockbarge method to grow high-quality large-size monoclinic-phase Ga of centimeter level 2 S 3 And (3) single crystal. The growth method comprises the steps of polycrystalline material mixing, vacuum sealing and melt sealing, descending growth and the like, and preferably comprises the following steps:
1) using polycrystalline raw material Ga 2 S 3 And Sb 2 S 3 According to a molar ratio of 1: (0.8-1.2) mixing and grinding to obtain a uniform raw material mixture, and carrying out vacuum sealing on the raw material mixture. The invention is preferably weighed in a glove box filled with argon. Using Sb 2 S 3 The crystallization temperature is reduced, and the crystal growth temperature is in a monoclinic phase interval.
Preferably, the step of vacuum sealing the raw material mixture may be performed by charging the ground raw material mixture into a specially manufactured quartz crucible, and then removing the glove box, and charging the quartz crucible into a vacuum line at a gas pressure of 10 -4 Sealing by fusing when in Pao.
2) Heating and melting the raw material mixture subjected to vacuum sealing at high temperature, and then cooling to obtain the monoclinic phase Ga 2 S 3 And (3) single crystal.
The high-temperature heating and melting step of the step 2) further comprises the following steps:
21) and placing the raw material mixture after vacuum sealing in a high-temperature area in a growth device with a high-temperature area and a low-temperature area, heating to ensure that the high-temperature area and the low-temperature area in the growth device reach preset temperatures, and carrying out heat preservation and melting to obtain a molten liquid.
Preferably, the preset temperature of the high-temperature zone is 800-1000 ℃, and further preferably 900 ℃. The preset temperature of the low-temperature area is 450-650 ℃, and the further optimization is 600 ℃. The temperature gradient is (20-30) DEG C/cm; preferably 25 deg.c/cm. The invention controls the temperature of the high-temperature area within the range, mainly considering the optimal temperature gradient of crystal growth, the service life and the safety of the electric furnace wire, and being more economic and safe within the range.
In order to grow the crystal at a proper speed and prevent the crystal from growing too fast to become polycrystalline, the temperature of the melt in step 3) needs to be reduced. Preferably, the cooling step in step 3) includes:
22) searching a position, called a crystallization point position, in the growing device, wherein the position is the same as the crystallization temperature of the melt, and enabling the melt to uniformly pass through the crystallization point position in a descending mode;
23) cooling the high-temperature area and the low-temperature area, preferably cooling the high-temperature area and the low-temperature area at the speed of 15-25 ℃/h, more preferably cooling the high-temperature area and the low-temperature area to room temperature at the speed of 20 ℃/h, and obtaining the centimeter-grade high-quality large-size monoclinic-phase Ga 2 S 3 And (3) single crystal.
In the step 22), the melt passes through the crystallization point at a constant speed of 0.1-0.2 mm/hThen standing, completely crystallizing the melt, and finishing the growth, and finally obtaining the centimeter-grade high-quality large-size monoclinic-phase Ga by adopting the method 2 S 3 And (3) single crystal.
Example 1
1) Ga having a purity of 99.99% is commercially available 2 S 3 As the raw material, a polycrystalline raw material and Sb 2 S 3 Uniformly mixing according to the stoichiometric ratio of 1: 1, and grinding to obtain a uniform raw material mixture.
3) The homogeneous raw material mixture was charged into a quartz crucible. Then the vacuum degree reaches 10 -4 Sealing by the handkerchief. And fixing the sealed quartz tube in a descending furnace to enable the quartz tube to reach a high-temperature region of a growth device.
And heating the hearth to raise the temperature, so that the high temperature region reaches 900 ℃ of the preset temperature, the low temperature region reaches 600 ℃ of the preset temperature, and the temperature gradient is 25 ℃/cm. Then standing and preserving the heat for 48 hours to ensure that the material to be heated forms uniform molten liquid. The temperature thermocouple arranged in the crucible supporting rod is adopted to measure the position of a crystallization point in the hearth, the descending motor is started, so that the quartz crucible slowly descends at a constant speed at the speed of 0.2mm/h and uniformly passes through the position of the crystallization point to be cooled, and the quartz tube stops descending after passing through the position of the crystallization point. Then cooling the high-temperature area and the low-temperature area to room temperature at a cooling rate of 20 ℃/h, and finally taking out crystals to obtain centimeter-sized large-sized monoclinic-phase Ga with the size of phi 10 multiplied by 20mm 2 S 3 A single crystal having good quality and high transmittance.
Determination of the monoclinic Ga in the order of centimeters obtained in example 1 2 S 3 Transmittance of single crystal:
1) monoclinic phase Ga 2 S 3 Cutting and polishing a single crystal: subjecting the obtained monoclinic phase Ga 2 S 3 The single crystal is cut to a size of about 5X 2mm 3 And each side is polished.
2) A circular hole with a diameter of about 2mm is punched in a black sheet, and then polished monoclinic phase Ga is put in 2 S 3 Sticking the single crystal on the hole to block the hole, measuring the transmittance with the black sheet with single crystal, and allowing laser to pass through the hole. The monoclinic phase Ga in example 1 was determined by this method 2 S 3 The ultraviolet and visible light transmittance of the single crystal is as high as more than 90%.
Example 2
1) Ga having a purity of 99.99% is used as it is on the market 2 S 3 As the raw material, a polycrystalline raw material and Sb 2 S 3 According to a stoichiometric ratio of 1: 1.2 mixing evenly and grinding to obtain a uniform raw material mixture.
3) The homogeneous raw material mixture was charged into a quartz crucible. Then the vacuum degree reaches 10 -4 And sealing. And fixing the sealed quartz tube in a descending furnace to enable the quartz tube to reach a high-temperature region of a growth device.
And heating the hearth to raise the temperature, so that the high temperature region reaches the preset temperature of 800 ℃, the low temperature region reaches the preset temperature of 450 ℃, and the temperature gradient is 20 ℃/cm. Then standing and preserving the heat for 48 hours to ensure that the material to be heated forms uniform molten liquid. The temperature thermocouple arranged in the crucible supporting rod is adopted to measure the position of a crystallization point in the hearth, the descending motor is started, so that the quartz crucible slowly descends at a constant speed at the speed of 0.2mm/h and uniformly passes through the position of the crystallization point to be cooled, and the quartz tube stops descending after passing through the position of the crystallization point. Then cooling the high-temperature area and the low-temperature area to room temperature at a cooling rate of 25 ℃/h, and finally taking out crystals to obtain centimeter-sized large-sized monoclinic-phase Ga with the size of phi 10 multiplied by 12mm 2 S 3 And (3) single crystal.
Example 3
1) Ga having a purity of 99.99% is commercially available 2 S 3 As the raw material, a polycrystalline raw material and Sb 2 S 3 According to the stoichiometric ratio of 1: 0.8, and grinding to obtain a uniform raw material mixture.
3) The homogeneous raw material mixture was charged into a quartz crucible. Then the vacuum degree reaches 10 -4 And sealing. And fixing the sealed quartz tube in a descending furnace to enable the quartz tube to reach a high-temperature region of a growth device.
And heating the hearth to raise the temperature, so that the high temperature region reaches the preset temperature of 1000 ℃, the low temperature region reaches the preset temperature of 650 ℃, and the temperature gradient is 30 ℃/cm. Then standing and preserving heat 4For 8 hours, the material to be heated is formed into a homogeneous melt. The position of a crystallization point in a hearth is measured by adopting a temperature thermocouple arranged in a crucible supporting rod, a descending motor is started, so that the quartz crucible slowly descends at a constant speed at a speed of 0.1mm/h and uniformly passes through the position of the crystallization point to be cooled, and the quartz tube stops descending after passing through the position of the crystallization point. Then cooling the high-temperature area and the low-temperature area to room temperature at a cooling rate of 15 ℃/h, and finally taking out crystals to obtain centimeter-sized large-sized monoclinic-phase Ga with the size of phi 10 multiplied by 10mm 2 S 3 And (3) single crystal.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. Monoclinic phase Ga 2 S 3 A method for producing a single crystal, characterized in that: a vacuum closed fluxing agent crucible descending method is adopted;
the method comprises the following steps:
1) ga is prepared from 2 S 3 Polycrystalline feedstock and Sb 2 S 3 Mixing and grinding uniformly, and then sealing in vacuum;
2) heating and melting the vacuum-sealed material at high temperature, and then cooling to obtain the monoclinic phase Ga 2 S 3 Single crystal;
ga in step 1) 2 S 3 Polycrystalline feedstock and Sb 2 S 3 In a molar ratio of 1: 0.8-1.2, vacuum degree of 10 -4 Pa。
2. The production method according to claim 1, characterized in that: ga in step 1) 2 S 3 Polycrystalline feedstock and Sb 2 S 3 In a molar ratio of 1: 1.
3. the method of claim 1, wherein: the specific steps of the step 2) are as follows: placing the vacuum sealed material in a high temperature region of a growth device having a high temperature region and a low temperature region, and heating to make the high temperature region and the low temperature region in the growth deviceAll the zones reach the preset temperature, and melting is carried out in a heat preservation manner to obtain a molten liquid; searching the position of a crystallization point in a growing device, and enabling the molten liquid to uniformly pass through the position of the crystallization point in a descending mode; cooling the high-temperature area and the low-temperature area to obtain the monoclinic-phase Ga 2 S 3 And (3) single crystal.
4. The production method according to claim 3, characterized in that: the preset temperature of the high-temperature area is 800-1000 ℃, the preset temperature of the low-temperature area is 450-650 ℃, and the temperature gradient in the growth device is 20-30 ℃/cm.
5. The method of claim 4, wherein: the preset temperature of the high temperature zone is 900 ℃, the preset temperature of the low temperature zone is 600 ℃, and the temperature gradient in the growth device is 25 ℃/cm.
6. The production method according to claim 3, characterized in that: the melt is first lowered to a position 1-3 cm above the crystallization point, then uniformly passes through the crystallization point at a lowering speed of 0.1-0.2 mm/h, and then is kept stand.
7. The production method according to claim 3, characterized in that: and cooling the high-temperature area and the low-temperature area to room temperature at a speed of 15-25 ℃/h.
8. The method of claim 7, wherein: both the high temperature zone and the low temperature zone were cooled down to room temperature at a rate of 20 ℃/h.
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