CN113930844A - Method for seed crystal induction and self-fluxing agent growth of CdTe crystal - Google Patents
Method for seed crystal induction and self-fluxing agent growth of CdTe crystal Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 135
- 229910004613 CdTe Inorganic materials 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 44
- 230000006698 induction Effects 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000010453 quartz Substances 0.000 claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000007789 sealing Methods 0.000 claims abstract description 16
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 11
- 238000001816 cooling Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000005086 pumping Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000010587 phase diagram Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000012808 vapor phase Substances 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
- 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
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/06—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using as solvent a component of the crystal composition
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Abstract
The invention discloses a method for seed crystal induction and self fluxing agent growth of CdTe crystal. The method of the invention comprises the following steps: weighing raw materials according to a stoichiometric ratio, putting the raw materials into a quartz crucible, vacuumizing, sealing, and putting the quartz crucible into a swinging furnace to synthesize a polycrystalline material; the CdTe single crystal with required orientation is loaded into PBN as seed crystal, and then self fluxing agent Te and synthesized CdTe polycrystal material are mixed homogeneously in certain proportion, and the mixture is loaded into PBN crucible and set inside quartz tube, and through vacuum pumping and sealing, CdTe crystal grows at high temperature. The invention adopts CdTe single crystal as seed crystal and Te as self-fluxing agent, controls the temperature field, the cooling rate and the growth rate of the crystal furnace, reduces the growth temperature, can prepare CdTe single crystal with required orientation, large size and high quality, and can also be used for growing CdTe-doped single crystal, thereby solving the growth problem of CdTe crystal.
Description
Technical Field
The invention relates to a method for seed crystal induction and self-fluxing agent growth of CdTe crystal, belonging to the technical field of crystal semiconductors.
Background
CdTe crystals are one of the most important II-VI compound semiconductors and are widely used in X-ray detection and infrared detection materials. The forbidden band width at room temperature is 1.5eV, and the direct transition type energy band is providedStructure with lattice constant of 0.6481nm and room temperature electron mobility of 1050cm2/(Vs), room temperature hole mobility 80cm2/(Vs). The detector prepared by utilizing CdTe crystal has better energy resolution and sensitivity compared with the traditional semiconductor Si, Ge and scintillation crystal NaI detectors, and is the most ideal semiconductor material for manufacturing room-temperature X-ray and gamma-ray detectors found so far. Electrons in the wide-bandgap semiconductor material are not easy to ionize, so that the wide-bandgap semiconductor material can bear very high voltage and temperature, has higher breakdown electric field, high thermal conductivity, high electronic saturation rate and higher radiation resistance, is more suitable for manufacturing high-temperature, high-frequency and high-power devices, and has great application prospects in the aspects of laser photoelectric modulation, high-efficiency solar medical molding, industrial and environmental monitoring, nuclear detection, celestial body physics and the like.
The melting point of CdTe crystal is 1098 ℃, the growth temperature is usually higher than the temperature by more than 50 ℃, the quartz crucible starts to soften at the temperature, and the larger high-temperature steam easily causes the potential safety hazard of crystal growth. In addition, the CdTe crystal also has a weak Cd-Te bond, and is easy to decompose and break; the critical shear stress is small, and dislocation is easy to generate; stacking defect energy is very low, and twin crystals are easily caused; and the problems of low thermal conductivity, easy component segregation and the like are caused, and the growth of large-size and high-quality CdTe crystals is extremely difficult.
At present, mainly high-pressure Bridgman method, vertical gradient condensation method (VGF), physical vapor transport method (PVT), mobile heating method (THM) and other techniques are used for CdTe crystal growth. The diameter of the single crystal grown by the vertical gradient condensation method is large, but the temperature gradient is difficult to control, so that the growth speed of the crystal cannot be controlled, and the crystallization quality is influenced; the physical vapor transport method is a process for growing crystals by a vapor phase method, the EPD of the crystals grown by the method is low, but large-size single crystals are difficult to grow; at present, the related reports of growing CdTe crystals by adopting a mobile heating method are less, and the method is a growing method using Te as a fluxing agent. According to the phase diagram, the combination of seed crystal induction and self-fluxing agent is adopted to grow CdTe crystals from high-temperature solution, so that the method is a feasible preparation method. By accurately controlling the temperature field, the cooling rate and the descending rate of the growth furnace, large-size and high-quality crystals can be grown, and a plurality of CdTe crystals with different specifications and different dopes can be further grown in one furnace.
Disclosure of Invention
The technical problem solved by the invention is as follows: the existing methods for growing CdTe crystals reported in the prior art have the problems of difficult growth, non-uniformity of crystal components, poor crystal quality, uncontrollable size and the like.
In order to solve the technical problem, the invention discloses a method for growing CdTe crystals by seed crystal induction and self fluxing agent, which comprises the following steps:
step 1: weighing the elemental Cd powder and the elemental Te powder according to a stoichiometric ratio, mixing, grinding, putting into a quartz crucible, vacuum sealing, and synthesizing the CdTe polycrystalline material in a swinging furnace;
step 2: placing prepared CdTe seed crystals at the bottom of the PBN crucible, then filling a self-fluxing agent Te and the CdTe polycrystalline material synthesized in the step (1) according to a certain molar ratio, placing the CdTe seed crystals in a quartz container and sealing in vacuum; and (3) moving the quartz container to a crystal furnace, adjusting the height of the quartz container to a proper height, heating the quartz container to a temperature higher than the melting temperature, keeping the temperature for a period of time, adjusting the height to enable the position of a solid-liquid interface to reach an oversaturated temperature, starting a descending device to start crystal growth, and after the growth is finished, reducing the temperature to room temperature, and taking out the crystal.
Preferably, the purity of the elemental Cd powder and the purity of the elemental Te powder in the step 1 are both 99.999%.
Preferably, the molar ratio of the self-fluxing agent Te to the CdTe polycrystal material in the step 2 is 0.5-8: 1, the temperature for crystal growth needs to be 30-60 ℃ higher than the melting point temperature of CdTe crystal.
Preferably, the grinding in step 1 needs to be carried out in an agate mortar for grinding and mixing.
Preferably, the temperature of the rocking furnace in step 1 is set to 1100 ℃ or higher, and a stepwise temperature increase is used.
Preferably, the CdTe seed crystal in the step 2 is a CdTe seed crystal formed by precisely orienting CdTe crystals by an X-ray orientation instrument, and then cutting and grinding the CdTe seed crystal.
Preferably, the diameter of the CdTe seed crystal is 10-30 mm.
Preferably, the orientation of the CdTe seed crystal is (100) or (111).
Preferably, the vacuum sealing in step 2 is: vacuumizing to 10 ℃ below zero by using a tube sealing machine-4Pa and then the quartz tube was sealed with a quartz plug by means of an oxyhydrogen flame.
Preferably, the temperature of the crystal furnace in the step 2 is controlled to be 700-1050 ℃, the temperature is kept after the temperature reaches the set temperature, then the position of the quartz container is adjusted to enable a solid-liquid interface to be positioned at the top of the seed crystal, the solid-liquid interface starts to descend after being stabilized, and the descending rate is 0.4-1 mm/h.
Compared with the prior art, the invention has the following beneficial effects:
1. the CdTe crystal is grown by the fluxing agent method, the CdTe single crystal with a specific orientation is used as the seed crystal, and the Te-rich component is used as the self fluxing agent, so that the growth temperature is effectively reduced, and the damage to a quartz crucible and the influence on the purity of the crystal caused by overhigh growth temperature are overcome; on the other hand, the existence of the seed crystal can effectively improve the quality and the size of the single crystal, and a plurality of equivalent stations in the growth furnace can simultaneously grow a plurality of crystals, thereby reducing the growth cost and effectively realizing industrialization;
2. the Te-rich component serving as the self-fluxing agent can reduce the growth temperature, overcome the growth difficulty caused by overhigh melting point and overlarge vapor pressure of CdTe crystals, soften a quartz crucible to bring potential safety hazards due to the fact that the melting point of the CdTe crystals is 1098 ℃, and the high growth temperature, and then, the difference between the melting points of Cd and Te is large, the partial pressure of Cd is 1-2 orders of magnitude higher than the partial pressure of Te, so that deviation of the stoichiometric ratio is easily generated, and a large amount of Cd vacancies and Te inversion defects are generated in the crystals; the method of the invention overcomes the problems of non-uniformity of components and the like existing in the past solidification growth, and large-size and high-quality CdTe single crystal can be grown by adopting the seed crystal induction and self-fluxing agent method of the invention; the growth process of the invention can also realize the growth of a plurality of CdTe crystals with different specifications and different dopings in one furnace.
Drawings
FIG. 1 is the phase diagram of CdTe.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
Example 1
A method for seed crystal induction and self fluxing agent growth of CdTe crystals comprises the following steps:
the method comprises the following steps: a fluxing agent method is utilized to grow CdTe crystal, raw materials are Cd powder and Te powder with the purity of 99.999 percent, the materials are accurately weighed according to the stoichiometric ratio, the materials are put into an agate mortar for grinding and mixing, the mixture is put into a quartz crucible, and a tube sealing machine is used for vacuumizing to 10 percent-4Pa and then sealed with a quartz plug by means of an oxyhydrogen flame. Cleaning the outer wall of the quartz crucible with ethanol, then loading the quartz crucible into a swinging furnace, setting the temperature rise to 1120 ℃ in 3 stages, preserving the heat for 1 hour, starting the swinging device to enable the raw materials to fully react in the crucible, stopping swinging after 3 hours, cooling to 300 ℃ at the speed of 50 ℃/h, turning off a power supply, and then cooling along with the furnace.
Step two: the prepared CdTe single crystal is oriented and cut by an X-ray orientation device, the seed crystal is oriented to (100), and the CdTe single crystal is processed into a cylinder with the diameter of 15mm and the length of 50 mm. Placing the processed seed crystal at the bottom of the PBN crucible, and mixing self-fluxing agent Te and the synthesized CdTe polycrystal material according to a molar ratio of 4: 3, uniformly mixing, placing into a PBN crucible with the diameter of 2 inches, placing into a quartz crucible, and then sealing in vacuum.
Step three: moving a quartz crucible into a growth furnace, wherein the growth temperature is 40-50 ℃ higher than the corresponding melting point in a phase diagram of figure 1 (namely 940-950 ℃), raising the temperature to 950 ℃ after 20 hours, shaking the furnace to a high temperature region, keeping the temperature for 4 hours after the seed crystal position temperature reaches 950 ℃, melting the raw materials and the top of the seed crystal, starting a descending device to descend the crucible at the rate of 0.5mm/h, starting crystal growth, gradually reducing the temperature at the rate of 50 ℃/h after the growth is finished, turning off a power supply after the temperature is reduced to 300 ℃, cooling the crystal along with the furnace, and finally taking out the crystal.
Example 2
A method for seed crystal induction and self fluxing agent growth of CdTe crystals comprises the following steps:
the method comprises the following steps: a fluxing agent method is utilized to grow CdTe crystal, raw materials are Cd powder and Te powder with the purity of 99.999 percent, the materials are accurately weighed according to the stoichiometric ratio, the materials are put into an agate mortar for grinding and mixing, the mixture is put into a quartz crucible, and a tube sealing machine is used for vacuumizing to 10 percent-4Pa and then sealed with a quartz plug by means of an oxyhydrogen flame. Cleaning the outer wall of the quartz crucible with ethanol, then loading the quartz crucible into a swinging furnace, setting the temperature rise to 1120 ℃ in 3 stages, preserving the heat for 1 hour, starting the swinging device to enable the raw materials to fully react in the crucible, stopping swinging after 3 hours, cooling to 300 ℃ at the speed of 50 ℃/h, turning off a power supply, and then cooling along with the furnace.
Step two: the prepared CdTe single crystal is oriented and cut by an X-ray orientation device, the seed crystal is oriented to (100), and the CdTe single crystal is processed into a cylinder with the diameter of 10mm and the length of 50 mm. Placing the processed seed crystal at the bottom of the PBN crucible, and mixing self-fluxing agent Te and the synthesized CdTe polycrystal material according to a molar ratio of 3: 1, charging into a PBN crucible with a diameter of 1 inch, placing in a quartz crucible, and then vacuum sealing.
Step three: moving a quartz crucible into a growth furnace, wherein the growth temperature is 40-50 ℃ higher than the corresponding melting point in a phase diagram of figure 1 (namely 830-840 ℃), setting the program to heat to 840 ℃ after 16 hours, shaking the furnace to a high temperature region, keeping the temperature for 4 hours after the seed crystal position temperature reaches 840 ℃, melting the raw material and the top of the seed crystal, starting a descending device to descend the crucible at a speed of 0.7mm/h, starting crystal growth, gradually reducing the temperature at a speed of-50 ℃/h after the growth is finished, turning off a power supply after the temperature is reduced to 300 ℃, cooling the crystal along with the furnace, and finally taking out the crystal.
Example 3
A method for seed crystal induction and self fluxing agent growth of CdTe crystals comprises the following steps:
the method comprises the following steps: a fluxing agent method is utilized to grow CdTe crystal, raw materials are Cd powder and Te powder with the purity of 99.999 percent, the materials are accurately weighed according to the stoichiometric ratio, the materials are put into an agate mortar for grinding and mixing, the mixture is put into a quartz crucible, and a tube sealing machine is used for vacuumizing to 10 percent-4Pa and then sealed with a quartz plug by means of an oxyhydrogen flame. Cleaning the outer wall of the quartz crucible with ethanol, loading the quartz crucible into a swinging furnace, setting the temperature rise to 1120 ℃ in 3 stages,after the temperature is kept for 1 hour, the swinging device is started to ensure that the raw materials fully react in the crucible, the swinging is stopped after 3 hours, the temperature is reduced to 300 ℃ at the speed of 50 ℃/h, the power supply is turned off, and then the furnace is cooled.
Step two: the prepared CdTe single crystal is oriented and cut by an X-ray orientation device, the seed crystal is oriented to (111), and the CdTe single crystal is processed into a cylinder with the diameter of 15mm and the length of 50 mm. Placing the processed seed crystal at the bottom of the PBN crucible, and mixing self-fluxing agent Te and the synthesized CdTe polycrystal material according to a molar ratio of 3: 1, after being uniformly mixed, the mixture was put into a PBN crucible having a diameter of 2 inches, and placed in a quartz crucible, followed by vacuum sealing.
Step three: moving a quartz crucible into a growth furnace, wherein the growth temperature needs to be 40-50 ℃ higher than the corresponding melting point (namely 830-840 ℃) in a phase diagram of figure 1, the temperature is increased to 840 ℃ after 16 hours, then the furnace is shaken to a high temperature region, the temperature of the seed crystal reaches 840 ℃ and then is kept for 4 hours, so that the raw materials and the top of the seed crystal are melted, then a descending device is started to descend the crucible at the speed of 0.5mm/h, crystal growth is started, the temperature is gradually reduced at the speed of-50 ℃/h after the growth is finished, a power supply is turned off after the temperature is reduced to 300 ℃, the crystal is cooled along with the furnace, and finally the crystal is taken out.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for seed crystal induction and self fluxing agent growth of CdTe crystal is characterized by comprising the following steps:
step 1: weighing the elemental Cd powder and the elemental Te powder according to a stoichiometric ratio, mixing, grinding, putting into a quartz crucible, vacuum sealing, and synthesizing the CdTe polycrystalline material in a swinging furnace;
step 2: placing prepared CdTe seed crystals at the bottom of the PBN crucible, then filling a self-fluxing agent Te and the CdTe polycrystalline material synthesized in the step (1) according to a certain molar ratio, placing the CdTe seed crystals in a quartz container and sealing in vacuum; and (3) moving the quartz container to a crystal furnace, adjusting the height of the quartz container to a proper height, heating the quartz container to a temperature higher than the melting temperature, keeping the temperature for a period of time, adjusting the height to enable the position of a solid-liquid interface to reach an oversaturated temperature, starting a descending device to start crystal growth, and after the growth is finished, reducing the temperature to room temperature, and taking out the crystal.
2. The seed crystal induction and self-fluxing agent CdTe crystal growing method of claim 1, wherein the purity of the elemental Cd powder and the purity of the elemental Te powder in the step 1 are both 99.999%.
3. The seed crystal induction and self-fluxing agent CdTe crystal growing method in the claim 1, wherein the mole ratio of the self-fluxing agent Te to the CdTe polycrystal material in the step 2 is 0.5-8: 1, the temperature for crystal growth needs to be 30-60 ℃ higher than the melting point temperature of CdTe crystal.
4. The seed crystal induction, self-fluxing agent CdTe crystal growing method according to claim 1, wherein the grinding in the step 1 is carried out in an agate mortar for grinding and mixing.
5. The seed-induced, self-fluxing agent method for growing CdTe crystals as claimed in claim 1, wherein the rocking furnace temperature in step 1 is set above 1100 ℃ and staged temperature elevation is used.
6. The seed crystal induction, self-fluxing agent CdTe crystal growing method of claim 1, wherein the seed crystal in the step 2 is a CdTe seed crystal formed by precisely orienting CdTe crystal through an X-ray orientation instrument, and then cutting and grinding.
7. The seed-induced, self-fluxing agent growth method of CdTe crystals as claimed in claim 6, wherein the diameter of the CdTe seed crystals is 10-30 mm.
8. The seed induced, self fluxing agent growth method of CdTe crystals according to claim 1, wherein the orientation of the CdTe seeds is (100) or (111).
9. The seed-induced, self-fluxing agent method for growing CdTe crystals as claimed in claim 1, wherein the vacuum sealing in step 2 is: vacuumizing to 10 ℃ below zero by using a tube sealing machine-4Pa and then the quartz tube was sealed with a quartz plug by means of an oxyhydrogen flame.
10. The seed crystal induction and self-fluxing agent CdTe crystal growing method in the step 2, which is characterized in that the temperature of the crystal furnace in the step 2 is controlled to be 700-1050 ℃, the temperature is kept after the temperature reaches the set temperature, then the position of the quartz container is adjusted, a solid-liquid interface is positioned at the top of the seed crystal, the solid-liquid interface starts to descend after being stabilized, and the descending rate is 0.4-1 mm/h.
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| CN105063741A (en) * | 2015-08-04 | 2015-11-18 | 西北工业大学 | Preparation method of ZnTe monocrystals |
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2021
- 2021-10-14 CN CN202111196947.0A patent/CN113930844A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409800A (en) * | 2013-07-17 | 2013-11-27 | 武汉高芯科技有限公司 | Large-diameter CdTe or CdZnTe polycrystalline rod synthesis apparatus and preparation method thereof |
| CN105063741A (en) * | 2015-08-04 | 2015-11-18 | 西北工业大学 | Preparation method of ZnTe monocrystals |
| CN106480495A (en) * | 2016-10-26 | 2017-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | The method that a kind of travelling heating method of similar Bridgman thermal field grows tellurium manganese cadmium crystal |
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Application publication date: 20220114 |