CN117702274B - Growth process of indium phosphide crystal - Google Patents
Growth process of indium phosphide crystal Download PDFInfo
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- CN117702274B CN117702274B CN202410161454.0A CN202410161454A CN117702274B CN 117702274 B CN117702274 B CN 117702274B CN 202410161454 A CN202410161454 A CN 202410161454A CN 117702274 B CN117702274 B CN 117702274B
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- 239000013078 crystal Substances 0.000 title claims abstract description 235
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 57
- 239000010453 quartz Substances 0.000 claims abstract description 271
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 271
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 239000000523 sample Substances 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 26
- 238000009413 insulation Methods 0.000 claims description 20
- 229910052738 indium Inorganic materials 0.000 claims description 13
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 11
- 230000002194 synthesizing effect Effects 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 229910052810 boron oxide Inorganic materials 0.000 claims description 8
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 238000000859 sublimation Methods 0.000 claims description 8
- 230000008022 sublimation Effects 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000002019 doping agent Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 230000002159 abnormal effect Effects 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
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- 238000006243 chemical reaction Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
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- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
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- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 230000005856 abnormality Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
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- 238000002309 gasification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention provides a growth process of an indium phosphide crystal, which comprises the following steps: the method comprises the steps of utilizing a special-shaped quartz tube to synthesize an indium phosphide crystal, pre-installing a growth raw material in a single crystal furnace, carrying out exhaust treatment on the single crystal furnace, sublimating red phosphorus, melting the indium phosphide crystal, carrying out crystal growth and cooling the crystal, completing the synthesis of indium phosphide polycrystal through the special-shaped quartz tube, and then realizing the growth of the indium phosphide crystal by matching with the control of temperature and pressure so as to ensure the smooth progress of a processing technology in the whole growth process of the indium phosphide crystal and improve the stability of the growth process of the indium phosphide single crystal.
Description
Technical Field
The application relates to the field of indium phosphide crystals, in particular to a growth process of an indium phosphide crystal.
Background
With the progress of the age and the innovation of the technology, the second generation compound semiconductor material represented by indium phosphide is vigorously developed, and the InP crystal has the advantages of high saturated electron drift speed, strong radiation resistance, good heat conductivity, high photoelectric conversion efficiency and the like, and is widely applied to the fields of optical communication, high-frequency millimeter wave devices, photoelectric integrated circuits, solar cells for outer space and the like. Indium has a melting point of 1070 ℃, at this temperature, an indium phosphide material has a very high dissociation pressure, the dissociation pressure at the melting point is 2.75MPa, the calculation is performed according to the formula lgp=a-B/(t+c) of the functional relation between the Antoine saturation vapor pressure and the temperature, and under this condition, the phosphorus vapor pressure has exceeded 10MPa and is far greater than the dissociation pressure of indium phosphide, so that it is very difficult to directly synthesize indium phosphide single crystals from phosphorus and indium in a single crystal furnace, so that in general, high-purity indium and high-purity phosphorus are synthesized through polycrystal, indium phosphide single crystals are grown by using indium phosphide crystals after synthesizing indium phosphide crystals, and the preparation of indium phosphide single crystals by using a high-pressure single crystal furnace is the most dominant method, and the dislocation density of the crystals is reduced by using a method of doping an isoelectric impurity.
In the current indium phosphide crystal synthesis process, mainly a quartz tube is adopted to load raw materials red phosphorus and indium into the quartz tube, then the quartz tube is vacuum sealed and loaded into a single crystal furnace for high-temperature synthesis, the method has extremely high requirement on air pressure control in the synthesis process, the tube cracking rate is extremely high, the red phosphorus is burnt in the furnace after tube cracking, irreparable damage is caused to equipment, and the air pressure control is extremely difficult, so that the synthesized yield is extremely unstable.
In the process of growing the indium phosphide single crystal by the indium phosphide crystal, mainly, an indium phosphide raw material is placed in a quartz tube of a high-pressure single crystal furnace, a high-temperature and high-pressure environment suitable for the growth of the indium phosphide single crystal is established by heating and applying pressure, the indium phosphide single crystal is gradually grown on the surface of a seed crystal by controlling parameters such as temperature, pressure, raw material supply rate and the like, the temperature and the pressure are gradually reduced after the growth of the single crystal is completed, the indium phosphide single crystal in a reaction container is cooled and solidified, and the container is opened to take out the indium phosphide single crystal after the reaction container is cooled to a safe temperature. The internal temperature of the quartz tube can not be directly measured in the single crystal growth process, the internal temperature can only be estimated by indirectly measuring the temperature of the tube wall of the quartz tube, and the axial temperature gradient in the quartz tube needs to be controlled in the process of heating, so that the pressure is very difficult to control in the indium phosphide single crystal growth process, and the quartz tube is extremely easy to crack in the growth process.
In the single crystal growth process, the air pressure in the furnace body is kept balanced with the air pressure in the quartz tube, if the pressure difference is too large, the pressure difference can damage the quartz tube to cause tube cracking, red phosphorus can corrode a heater and platinum rhodium wires for temperature measurement after coming out, and the tube cracking at the high temperature stage can cause crystal decomposition to cause loss of raw materials; in addition, the instability of the air pressure can cause fluctuation of a temperature field, thereby affecting the growing indium phosphide monocrystal, generating twin crystals or polycrystal and affecting the crystal yield. It is necessary to exercise strict control over the gas pressure during the production of the indium phosphide single crystal.
In other words, the problems of difficult control of air pressure and high cracking rate of quartz tube in the synthesis and growth processes of indium phosphide crystal at present, which result in low quality of the final single crystal or low synthesis rate.
Disclosure of Invention
The invention aims to provide a growth process of an indium phosphide crystal, which is characterized in that synthesis of indium phosphide polycrystal is completed through a special-shaped quartz tube, and then growth of the indium phosphide crystal is realized by controlling temperature and pressure in combination, so that smooth progress of a processing process is ensured in the whole growth process of the indium phosphide crystal, and stability of the growth process of the indium phosphide monocrystal is improved.
In order to achieve the above object, the present solution provides a growth process of an indium phosphide crystal, comprising the steps of:
1) Synthesizing indium phosphide crystals: placing red phosphorus in a red phosphorus part of a special-shaped quartz tube, placing an indium strip in a crystal part of the special-shaped quartz tube, sealing a first quartz tube of the special-shaped quartz tube, placing the sealed special-shaped quartz tube into a polycrystalline furnace, connecting a quartz probe of the special-shaped quartz tube with a displacement sensor of the polycrystalline furnace, closing the polycrystalline furnace, adjusting the pressure of the polycrystalline furnace according to the quartz probe, and then completing crystal synthesis to obtain an indium phosphide crystal;
2) Preassembling growth raw materials in a single crystal furnace: after indium phosphide crystal, red phosphorus, doping agent and liquid sealing agent are filled into a boron oxide crucible, the boron oxide crucible is filled into a quartz tube and then sealed, the sealed quartz tube is filled into a single crystal furnace and then the single crystal furnace is sealed, wherein a heating element, a temperature measuring element and an air valve are arranged on the single crystal furnace;
3) Single crystal furnace exhaust treatment: heating the interior of the single crystal furnace and vacuumizing the interior of the single crystal furnace in the heating process, wherein the heating condition is that the temperature is raised from 25 ℃ to 380 ℃, the vacuumizing time is controlled to be 50-70 minutes, and the pressure requirement of the interior of the single crystal furnace is lower than-10 psi;
4) Sublimating red phosphorus: stopping vacuumizing treatment and inflating the single crystal furnace when the temperature in the single crystal furnace reaches 380 ℃, wherein the inflating condition is that inert gas is uniformly inflated until the pressure reaches 300psi;
5) Melting indium phosphide crystal: setting a temperature rise curve according to process parameters, wherein the temperature rise curve is formed by raising the temperature from 380 ℃ to 1065-1085 ℃ in a plurality of stages, and controlling the pressure in the single crystal furnace to 405-420 psi by supplementing or discharging air to the single crystal furnace;
6) Crystal growth: reducing the air pressure of the single crystal furnace according to the pressure of the special-shaped quartz tube until the air pressure of the single crystal furnace is maintained to be 395-405 psi;
7) And (3) cooling the crystal: the single crystal furnace is controlled to be cooled slowly according to a set cooling program in the first stage until the temperature in the single crystal furnace is 300 ℃, and an air valve of the single crystal furnace is closed in the first stage; and in the second stage, an air valve of the single crystal furnace is opened, and heating is closed for cooling.
In a second aspect, the present invention provides an indium phosphide crystal as described above, prepared according to the growth process of an indium phosphide crystal as described above.
Compared with the prior art, the scheme has the following characteristics and beneficial effects:
The special-shaped quartz tube consisting of the first quartz tube and the second quartz tube which are connected in a sealing way is designed, raw materials are placed into the first quartz tube and the second quartz tube, and pressure detection is carried out by utilizing quartz probes in the special-shaped quartz tube, so that operators can conveniently adjust the pressure in the polycrystalline furnace according to the detected pressure value, the quartz tube is prevented from being broken, and the crystallization yield is improved; meanwhile, due to the design of the special-shaped quartz tube, the influence on the feedback of pressure change in the high-temperature baking process can be avoided, the quartz diaphragm and the quartz probe can be reused, and the synthesis cost is reduced. By controlling the temperature and the pressure in the synthesis process of the indium phosphide crystal, the pipe cracking accident of the indium phosphide single crystal in the production process is greatly reduced, the loss of materials and equipment is reduced, the stability of the growth process of the indium phosphide single crystal can be improved, and the smooth production is ensured. The details of one or more embodiments of the application are set forth in the accompanying drawings and the description below to provide a more thorough understanding of the other features, objects, and advantages of the application.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 is a schematic view of the overall structure of a profiled quartz tube according to an embodiment of the present disclosure;
FIG. 2 is a schematic view of a partial structure of a profiled quartz tube according to an embodiment of the present disclosure;
FIG. 3 is a graph of temperature pressure versus time;
fig. 4 is a temperature pressure graph of indium phosphide growth.
In the figure: 11-first quartz tube, 111-crystal part, 112-first heat insulation part, 113-red phosphor part, 12-second quartz tube, 121-connection part, 122-second heat insulation part, 123-diaphragm detection part, 1231-diaphragm part, 1232-probe part, 20-quartz boat, 30-quartz cap, 41-quartz diaphragm, 42-quartz ring, 43-quartz probe, 51-first heat preservation layer, 52-second heat preservation layer.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary embodiments do not represent all implementations consistent with one or more embodiments of the present specification. Rather, they are merely examples of apparatus and methods consistent with aspects of one or more embodiments of the present description as detailed in the accompanying claims.
It should be noted that: in other embodiments, the steps of the corresponding method are not necessarily performed in the order shown and described in this specification. In some other embodiments, the method may include more or fewer steps than described in this specification. Furthermore, individual steps described in this specification, in other embodiments, may be described as being split into multiple steps; while various steps described in this specification may be combined into a single step in other embodiments.
Example 1
The technical scheme provides a growth process of indium phosphide crystals, firstly, a special-shaped quartz tube which is favorable for synthesizing the indium phosphide crystals is designed, so that the scheme can timely adjust the pressure of a polycrystalline furnace based on quartz diaphragms and probes in the special-shaped quartz tube after detecting the pressure, and further, the effects of accurately controlling the pressure and avoiding tube cracking are achieved; and secondly, a set of method for effectively maintaining the stability of the indium phosphide crystal in the growth process is designed in a matched manner so as to improve the quality of the finally grown indium phosphide.
The following describes the special-shaped quartz tube designed by the scheme, and fig. 1 is a schematic structural diagram of the special-shaped quartz tube provided by the scheme. As shown in fig. 1, the special-shaped quartz tube designed according to this scheme includes: a first quartz tube 11 and a second quartz tube 12 which are hermetically connected, wherein the first quartz tube 11 includes a crystal portion 111 and a red phosphorus portion 113 which are separated by a first heat insulating portion 112, the quartz boat 20 is disposed in the crystal portion 111 and the quartz cap 30 seals an opening position of the crystal portion 111 away from the first heat insulating portion 112; the second quartz tube 12 includes a connection portion 121 and a diaphragm probe portion 123 separated by a second heat insulating portion 122, the diaphragm probe portion 123 includes a diaphragm portion 1231 contacting the second heat insulating portion 122 and a probe portion 1232 contacting the diaphragm portion 1231, the quartz diaphragm 41 is disposed at the diaphragm portion 1231, at least two quartz rings 42 are disposed at intervals on the probe portion 1232, the quartz probe 43 passes through the quartz rings 42 to contact the quartz diaphragm 41, and the quartz probe 43 is used to detect the pressure of the quartz tube by sensing the deformation of the quartz rings 42.
In some embodiments, the diameter of the first heat insulation part 112 in the first quartz tube 11 is smaller than the diameters of the crystal part 111 and the red phosphorus part 113, and the diameter of the position of the crystal part 111 close to the second heat insulation part 112 gradually becomes smaller toward the position of the first heat insulation part 112, and the diameter of the position of the red phosphorus part 113 close to the second heat insulation part 112 gradually becomes larger away from the position of the first heat insulation part 112, and the first quartz tube 11 of the special-shaped quartz tube of the present embodiment takes a dumbbell shape. The crystal portion 111, the first heat insulating portion 112, and the red phosphorus portion 113 are provided in order.
In some embodiments, the diameters of the main portions of the crystal portions 111 and 113 of the first quartz tube 11 are the same, and the quartz boat 20 is placed in the crystal portion 111 for placing indium strips and the red phosphorus portion 113 is for placing red phosphorus.
Specifically, the quartz boat 20 is composed of a bottom and walls disposed on both sides of the bottom, and the bottom and walls form a chamber for accommodating indium strips. In some embodiments, the boat walls on both sides of the boat bottom are designed to be arc-shaped to wrap around to form the boat cavity, and the boat wall on one side is provided with a guide strip protruding outwards.
In order to achieve sealing of the first quartz tube 11, the quartz cap 30 is provided at an opening position of the crystal portion 111 away from the first heat insulating portion 112 to seal the first quartz tube 11. After indium and red phosphorus were added to the corresponding positions, the quartz cap 30 was placed in the position of the crystal portion 111 away from the opening of the first heat insulating portion 112 and welded.
In some embodiments, the second Dan Yingbu is sealingly connected to the first quartz portion 11, and the connecting portion 121 of the second quartz portion 12 has a diameter smaller than the diameter of the red phosphor portion 113. Specifically, the diameter of the red phosphorus portion 113 at a position close to the connection portion 121 gradually decreases toward a position where the connection portion 121 is located, and the diameter of the main body position of the connection portion 121 is uniform.
Likewise, the diameter of the second heat insulating portion 122 is smaller than the diameters of the connection portion 121 and the diaphragm detecting portion 123. Specifically, the diameter of the connection portion 121 at a position close to the second heat insulating portion 122 gradually becomes smaller toward the second heat insulating portion 122, and the diameter of the second heat insulating portion 122 at a position close to the diaphragm detecting portion 123 gradually becomes smaller toward the diaphragm detecting portion 123. In other words, the diameter of the connection portion 121 is smaller than the diameter of the red phosphorus portion 113 and larger than the diameter of the second heat insulation portion 122, and the diameter of the diaphragm portion of the diaphragm detecting portion 123 is larger than the diameter of the second heat insulation portion 122.
In addition, the diaphragm detecting portion 123 of this embodiment includes a diaphragm portion 1231 and a probe portion 1232 that are sequentially connected, wherein the diameter of the position of the diaphragm portion 1231 near the probe portion 1232 is gradually reduced, and the probe portion 1232 is designed to be in a straight cylindrical shape in contact with the diaphragm portion 1231.
As shown in fig. 2, the quartz diaphragm 41 is horizontally laid in the diaphragm part 1231, the quartz probe 43 is placed in the probe part 1232 and one end of the quartz probe 43 contacts the quartz diaphragm 41, so that the design has the advantages that: after the reaction of the crystal, the pressure in the quartz tube is transmitted to the sensor for detection through the quartz diaphragm 41 and the quartz probe 43, so that an operator can conveniently adjust the pressure in the polycrystalline furnace according to the detection value, the quartz tube is prevented from being broken, and the yield of the crystal is improved.
In some embodiments, the quartz diaphragm 41 is designed to be a flat plate with uniform thickness, so that the deformation amount of the quartz diaphragm 41 caused by pressure change is larger than that of a round shape or an oval shape, and by enlarging the diameter of the deformation part, the quartz diaphragm 41 can accurately feed back the pressure change in the crystal synthesis process, so that the breakage of the quartz tube caused by the fact that the pressure change does not adjust the air pressure in time is avoided.
In addition, in order to enable the quartz probe 43 to always contact the quartz diaphragm 41 to detect pressure, at least two quartz rings 42 are provided at intervals inside the probe portion 1232, and the quartz probe 43 is fixed against the quartz diaphragm 41 through the quartz rings 42.
In some embodiments, the first heat insulation layer 51 is sleeved outside the first heat insulation portion 112, and the second heat insulation layer 52 is sleeved outside the second heat insulation portion 122, which has the following design advantages: the first heat insulation part 112 and the first heat preservation layer 51 are matched to conduct heat insulation, so that heat of the crystal part 111 is less transferred to the red phosphorus part 113, the second heat insulation part 122 and the second heat preservation layer 52 are matched to conduct heat insulation, the heat of the red phosphorus part 113 is less transferred to the second quartz tube 12, the quartz membrane 41 in the second quartz tube 12 is always in a low-temperature state, feedback to pressure change due to high-temperature baking is avoided, meanwhile, the quartz membrane 41 can be reused, the service life is prolonged, and the whole second quartz tube 12 can be reused after being cut off after one use.
After introducing the structure of the special-shaped quartz tube, the scheme provides a growth process of indium phosphide crystal based on the special-shaped quartz tube, which comprises the following steps:
1) Synthesizing indium phosphide crystals: placing red phosphorus in a red phosphorus part 113 of a special-shaped quartz tube, placing an indium strip in a crystal part 111 of the special-shaped quartz tube, sealing a first quartz tube 11 of the special-shaped quartz tube, placing the sealed special-shaped quartz tube into a polycrystalline furnace, connecting a quartz probe 43 of the special-shaped quartz tube with a displacement sensor of the polycrystalline furnace, closing the polycrystalline furnace, adjusting the pressure of the polycrystalline furnace according to the quartz probe 43, and completing crystal synthesis to obtain indium phosphide crystals;
2) Preassembling growth raw materials in a single crystal furnace: after indium phosphide crystal, red phosphorus, doping agent and liquid sealing agent are filled into a boron oxide crucible, the boron oxide crucible is filled into a quartz tube and then sealed, the sealed quartz tube is filled into a single crystal furnace and then the single crystal furnace is sealed, wherein a heating element, a temperature measuring element and an air valve are arranged on the single crystal furnace;
3) Single crystal furnace exhaust treatment: heating the interior of the single crystal furnace, vacuumizing the interior of the single crystal furnace in the heating process, heating to 380 ℃ from room temperature in the vacuumizing process, controlling the time to be 50-70 minutes, and controlling the pressure requirement of the interior of the single crystal furnace to be lower than-10 psi;
4) Sublimating red phosphorus: stopping vacuumizing treatment and inflating the single crystal furnace when the temperature in the single crystal furnace reaches 380 ℃, wherein the inflating condition is that inert gas is uniformly inflated until the pressure reaches 300psi;
5) Melting indium phosphide crystal: setting a temperature rise curve according to process parameters, wherein the temperature rise curve is formed by raising the temperature from 380 ℃ to 1065-1085 ℃ in a plurality of stages, and controlling the pressure in the single crystal furnace to 405-420 psi by supplementing or discharging air to the single crystal furnace;
6) Crystal growth: reducing the air pressure of the single crystal furnace according to the pressure of the special-shaped quartz tube until the air pressure of the single crystal furnace is maintained to be 395-420 psi;
7) And (3) cooling the crystal: the single crystal furnace is controlled to be cooled slowly according to a set cooling program in the first stage until the temperature in the single crystal furnace is 300 ℃, and an air valve of the single crystal furnace is closed in the first stage; and in the second stage, an air valve of the single crystal furnace is opened, and heating is closed for cooling.
Regarding the step of synthesizing the indium phosphide crystal, the mode of synthesizing the indium phosphide crystal by adopting the special-shaped quartz tube in the scheme can sense the pressure in the special-shaped quartz tube at any time through the quartz probe, so that an operator can conveniently adjust the pressure in the polycrystalline furnace at any time, the special-shaped quartz tube is prevented from being broken, and the crystallization yield is improved. Simultaneously, carry out the heat separation through the cooperation of first thermal-insulated portion and first heat preservation for the heat of crystal portion is less to be transmitted to red phosphorus portion, and rethread second thermal-insulated portion carries out the heat separation with the cooperation of second heat preservation, makes the heat of red phosphorus portion less to be transmitted to the second quartz capsule, makes the quartz diaphragm in the second quartz capsule be in low temperature state all the time, makes it avoid influencing the feedback to pressure variation because of high temperature toasting, can also make quartz diaphragm used repeatedly simultaneously, increase of service life, after accomplishing once using, cuts off whole second quartz capsule and can used repeatedly.
Specifically, in the step of "synthesizing indium phosphide crystal", a special-shaped quartz tube is vertically placed so that the first quartz tube 11 is positioned above the second quartz tube 12, a set amount of red phosphorus is introduced from the upper end opening of the first quartz tube 11 and placed in the red phosphorus portion 113, then the upper end opening of the first quartz tube 11 is sealed with dust-free cloth, then the special-shaped quartz tube is horizontally placed and then the dust-free cloth is removed, a set amount of indium strips are placed in the quartz boat 20 and pushed into the crystal portion 111 and then the upper end opening of the first quartz tube 11 is sealed with dust-free cloth, then the special-shaped quartz tube is transferred into an oven and then the dust-free cloth is removed and then is put into the quartz cap 30, and after the special-shaped quartz tube is vacuumized, the temperature is raised and baked and the quartz cap 30 and the first quartz tube 11 are welded.
In some embodiments, the profiled quartz tube is first welded prior to loading the red phosphorus and indium strips into the profiled quartz tube. Specifically, the lower end of the first quartz tube 11 and the upper end of the second quartz tube 12 are welded together by oxyhydrogen flame to form an integral special-shaped quartz tube, the welding positions of the first quartz tube 11 and the second quartz tube 12 are required to be subjected to leak detection treatment, if no abnormality exists in leak detection, the special-shaped quartz tube is cleaned and baked, after evaporation of the moisture, the opening end of the special-shaped quartz tube is plugged by dust-free cloth, then the special-shaped quartz tube is vertically placed on a specific tube rack to enable the first quartz tube 11 to be located above the second quartz tube 12, and high-purity argon is blown into the special-shaped quartz tube by using a hose to replace air in the special-shaped quartz tube.
It should be noted that, in this embodiment, firstly, when the special-shaped quartz tube is in a vertical state, red phosphorus is poured into the quartz tube from the upper end opening of the first quartz tube 11 so that the red phosphorus is placed in the red phosphorus portion 113, then, when the special-shaped quartz tube is in a flat state, an indium strip is placed on the quartz boat 20, and the small mouth of the quartz boat 20 is pushed forward slowly into the crystal portion 111.
In the stage of welding the quartz cap 30, the quartz cap 30 is placed in the upper end of the opening of the first quartz tube 11, the special-shaped quartz tube is vacuumized after the chuck of the vacuum unit is connected, and after heating and baking are carried out for a period of time, the upper end of the special-shaped quartz tube is welded by oxyhydrogen flame, so that the quartz cap 30 and the first quartz tube 11 are welded into a whole.
In addition, in the step of 'synthesizing indium phosphide crystal', after the quartz cap 30 is welded, the special-shaped quartz tube cap is cooled to room temperature and then is put into a polycrystalline furnace, after the polycrystalline furnace is put into the polycrystalline furnace, a probe part 1232 of the second quartz tube 12 is put into a quartz ring 42, the upper end of a quartz probe 43 penetrates through the quartz ring 42 and contacts with a quartz diaphragm 41, the lower end of the quartz probe 43 is connected with a displacement sensor, the polycrystalline furnace is closed, and the temperature of the polycrystalline furnace is calibrated and raised, wherein the pressure in the furnace body of the polycrystalline furnace is continuously adjusted according to the deformation amount of the quartz diaphragm 41 in the heating process, so that the internal and external pressure difference is always kept basically balanced.
In some embodiments, two quartz rings 42 are provided, with two quartz rings 42 being provided in tandem. And the quartz ring 42 is provided so that the quartz probe 43 can be easily slid horizontally without being hindered substantially.
After the synthesis of the indium phosphide crystal is completed in the special-shaped quartz tube in the present embodiment, the quartz cap 30 is cut off, the synthesized indium phosphide crystal is taken out from the first quartz tube 11, and the first quartz tube 11 and the second quartz tube 12 are cut after the special-shaped quartz tube is cleaned. Since the first quartz tube 11 is subjected to a high temperature treatment, the risk of reuse is large and the price is relatively inexpensive and can be no longer used; since the second quartz tube 12 is located at the edge of the low temperature zone, the bearing temperature is low and can be reused for many times until damage occurs.
In the step of preassembling growth raw materials in the single crystal furnace, when the boron oxide crucible is placed in the quartz tube, vacuumizing treatment is carried out on the boron oxide crucible, then the quartz tube is sealed by using oxyhydrogen flame high-temperature sintering, and the sealed quartz tube is placed in the single crystal furnace and then the single crystal furnace is sealed.
It should be noted that, the quartz tube is different from the special-shaped quartz tube in the stage of synthesizing indium phosphide crystal, the quartz tube preloaded with growth raw material in the single crystal furnace is cylindrical, and the sealing cap is outward hemispherical. Because the quartz tube can bear a part of pressure, according to the design of the shape and the stress characteristics of the quartz tube, when the quartz tube is subjected to uniform and outward force in the tube wall, the quartz tube can be destroyed even if the acting force is very small, when the uniform force is applied inwards from the outer wall, the quartz tube can be destroyed by the larger pressure, so in the growth process of the indium phosphide, when the in-tube pressure of the quartz tube is smaller than the out-tube pressure, the quartz tube can be broken by the larger pressure difference, and when the in-tube pressure of the quartz tube is larger than the out-tube pressure, the quartz tube can be broken by the smaller pressure difference. Therefore, in the actual production process, the pressure outside the quartz tube is required to be controlled to be always 5-15psi higher than the pressure inside the tube, so that a larger safe space for tube cracking can be provided when the internal pressure and the external pressure fluctuate.
Regarding the step of exhaust treatment of the single crystal furnace, the main purpose of the step is to replace gas in the single crystal furnace, and as the water in the furnace body of the single crystal furnace gradually gasifies into water vapor after the temperature in the single crystal furnace is higher than 100 ℃, the water vapor has adverse effects on equipment and a temperature field in the growth process of indium phosphide, so the vaporized water vapor needs to be pumped away. Specifically, the heating element in the single crystal furnace is utilized to heat the single crystal furnace so that the temperature of the single crystal furnace is raised to 380 ℃ from 25 ℃, a vacuum pump is started to vacuumize the single crystal furnace in the heating process, specifically, the single crystal furnace is vacuumized through a vacuum pump connecting pipeline, a needle valve is arranged on the vacuum pipeline, the vacuumizing time is controlled to be 50-70 minutes, preferably 60 minutes, and the pressure requirement in the furnace body of the single crystal furnace is always kept to be lower than-10 psi.
And (3) regarding the step of sublimating red phosphorus, stopping vacuumizing treatment and inflating the single crystal furnace when the temperature inside the single crystal furnace reaches 380 ℃, wherein the inflating condition is that the inflating speed is 8 psi/min, the pressure in the single crystal furnace reaches 300psi at a constant speed according to the inflating speed, the required inflating time is about 40+/-1 min, and after the inflating is finished, closing an air valve, and the temperature in the single crystal furnace is about 550 ℃.
In this stage of sublimating red phosphorus, the outside temperature of the quartz tube immediately after the start of the inert gas filling is 380 ℃, and the inside temperature of the quartz tube is less than 380 ℃, in some embodiments, about 350 ℃, although specific inside temperatures are associated with different insulating materials and different quartz product sizes. The temperature of the quartz tube in the heating stage rises faster, the internal pressure of the Shi Danying tube rises faster when the temperature of the red phosphorus reaches the sublimation temperature of about 420 ℃, so that the temperature in the tube of the quartz tube is not yet increased to the sublimation temperature, namely, the quartz tube is inflated to a single crystal furnace outside the quartz tube, so that the internal red phosphorus ensures a certain pressure outside when the sublimation begins, the air pressure in the tube of the quartz tube is suddenly increased to cope with the rapid sublimation of the red phosphorus caused by the rapid sublimation of the red phosphorus when the temperature reaches the sublimation temperature, the internal pressure and the external pressure of the quartz tube are synchronously increased in the sublimation process of the red phosphorus, and after the sublimation of the red phosphorus is finished, 5psi high-purity nitrogen is continuously inflated to the single crystal furnace, so that the external air pressure of the quartz tube is always higher than the air pressure in the quartz tube, and the air valve is closed when the air pressure in the single crystal furnace is about 300 psi.
In other words, the scheme fills inert gas before the temperature in the quartz tube is lower than the temperature of the red phosphorus until the red phosphorus sublimates, and continuously fills high-purity nitrogen into the single crystal furnace until the air pressure in the single crystal furnace is about 300psi.
Regarding the melting step of indium phosphide polycrystal material, after the single crystal furnace is inflated to 300psi in the previous step, the temperature of the single crystal furnace is raised, the pressure in the single crystal furnace and the pressure in the quartz tube are both raised continuously along with the temperature rise, when the temperature in the quartz tube reaches 1065-1085 ℃, the temperature of the polycrystal material in the quartz tube is slightly higher than the melting point, the polycrystal material starts to melt gradually, the pressure in the quartz tube is about 400psi (the pressure is the vapor pressure of indium phosphide near the melting point 1062 ℃), in order to prevent the material in the tube from leaking and cracking, the pressure in the furnace is always higher than the vapor pressure of indium phosphide by 5-20psi, so that the pressure in the single crystal furnace needs to be kept at 405-420psi all the time, the maintaining pressure is mainly regulated by a pressure reducing valve or controlled by an electromagnetic valve, the redundant pressure is removed by removing the pressure higher than 420psi, the single crystal furnace is slowly inflated to the single crystal furnace after the waiting for the pressure stabilization, the temperature is regulated, and the upper part of the crystal is melted is made to enter the growth stage. In other words, as the temperature increases to the melting temperature (1065 ℃ -1085 ℃), the pressure in the single crystal furnace does not reach 405psi, the single crystal furnace is replenished with air, and if the pressure is higher than 420psi, the pressure is required to be relieved, so that the pressure in the single crystal furnace is maintained between 405psi and 420 psi.
And in the step of crystal growth, the air pressure of the single crystal furnace is reduced according to the pressure of the special-shaped quartz tube until the air pressure of the single crystal furnace is maintained to be 395-405 psi, and the air inlet rate and the air inlet amount are controlled in the adjusting process so as to avoid the change of the furnace pressure and the temperature fluctuation of the single crystal furnace caused by the large air inlet amount and the high air inlet rate. In the stage of the crystal growth, the crystal growth is a process of slowly reducing the temperature, the temperature is reduced to be lower than 0.5 ℃ in about one hour, and the pressure in the quartz tube is reduced along with the slow reduction of the temperature, so that the air pressure in the external single crystal furnace is required to be correspondingly reduced, and the scheme is used for continuously adjusting the air pressure in the single crystal furnace in the crystal growth process.
And in the cooling step, when the crystal is grown, the crystal enters the cooling step, and in the first cooling stage, the single crystal furnace is in a high-temperature environment, the temperature is about 1040 ℃, and the single crystal furnace is controlled to slowly cool down according to a set cooling program until the temperature in the single crystal furnace is 300 ℃ under the condition that the power supply and the air valve of the single crystal furnace are not closed. In the first stage of cooling, as the temperature is reduced, the pressure of the single crystal furnace and the pressure in the quartz tube are reduced, and the temperature in the quartz tube is higher than the temperature outside the tube in the stage, so that the pressure outside the tube is slightly reduced more than the pressure inside the tube.
And in the second stage of cooling, opening a gas valve of the single crystal furnace, closing heating to deflate, controlling the deflating speed to be slow and then fast, keeping the average speed to be 2.5psi/min until the pressure of the single crystal furnace is 0psi, and then opening the single crystal furnace and taking out the grown single crystal. It should be noted that the second stage of cooling is slower in temperature reduction, at this time, the temperature outside the quartz tube is 300 ℃, and the temperature inside the tube is close to 420 ℃ of the condensation temperature of red phosphorus.
In order to facilitate understanding of the growth of the indium phosphide single crystal in the scheme, the temperature and pressure change chart of the single crystal furnace along with the processing process is shown in fig. 3, the growth temperature and pressure chart of the indium phosphide single crystal is shown in fig. 4, and the method adopted in the scheme can reduce pipe cracking accidents of the indium phosphide single crystal in the production process, reduce loss of materials and equipment, improve the stability of the growth process of the indium phosphide single crystal, and ensure smooth production.
FIG. 3 is a graph of pressure, temperature and time during the growth of an indium phosphide single crystal; the whole growth process of the indium phosphide monocrystal mainly comprises the steps of heating (heating is divided into vacuumizing, air inlet and pressure rising stages), melting, growing, cooling and pressure relief; FIG. 4 shows the pressure required in the single crystal furnace at different temperatures in the indium phosphide growing process, the pressure in the quartz tube of indium phosphide and the bearing pressure of the quartz tube are required to be ensured to be approximately equal to the pressure in the single crystal furnace in the whole production process, the pressure in the quartz tube is mainly generated by red phosphorus gasification, so that the pressure in each stage is related to the gasification, condensation and temperature of red phosphorus, the pressure in each temperature has a reference effect on the process change and the pressure control when abnormality occurs in the production process, and the following table shows the relation between the specific pressure temperature and time in each stage:
table one pressure temperature time relationship of each stage
。
The present application is not limited to the above-mentioned preferred embodiments, and any person who can obtain other various products under the teaching of the present application can make any changes in shape or structure, and all the technical solutions that are the same or similar to the present application fall within the scope of the present application.
Claims (6)
1. A process for growing an indium phosphide crystal, comprising the steps of:
1) Synthesizing indium phosphide crystals: placing red phosphorus in a red phosphorus part of a special-shaped quartz tube, placing an indium strip in a crystal part of the special-shaped quartz tube, sealing a first quartz tube of the special-shaped quartz tube, placing the sealed special-shaped quartz tube into a polycrystalline furnace, connecting a quartz probe of the special-shaped quartz tube with a displacement sensor of the polycrystalline furnace, closing the polycrystalline furnace, adjusting the pressure of the polycrystalline furnace according to the quartz probe, completing crystal synthesis to obtain an indium phosphide crystal, wherein the special-shaped quartz tube comprises the first quartz tube and a second quartz tube which are in sealed connection, the first quartz tube comprises a crystal part and a red phosphorus part which are distinguished by a first heat insulation part, the second quartz tube comprises a connecting part and a diaphragm probe part which are distinguished by a second heat insulation part, the diaphragm probe part comprises a diaphragm part which is connected with the second heat insulation part and a probe part which is connected with a diaphragm, the quartz diaphragm is arranged in the diaphragm part, and at least two quartz rings are arranged at intervals on the probe part, the quartz probe passes through the quartz ring to be in contact with the quartz membrane, the special-shaped quartz tube is vertically placed so that the first quartz tube is positioned above the second quartz tube, a set amount of red phosphorus is led in from the upper end opening of the first quartz tube and then is placed in the red phosphorus part, the upper end opening of the first quartz tube is sealed by dust-free cloth, then the special-shaped quartz tube is horizontally placed and then is taken down, the dust-free cloth is used for sealing the upper end opening of the first quartz tube, then the special-shaped quartz tube is transported into the oven, the dust-free cloth is taken down and then is placed in the oven, the special-shaped quartz tube is vacuumized and then is heated, the quartz cap and the first quartz tube are welded, the membrane detection part comprises a membrane part and a probe part which are sequentially conducted, the quartz membrane is horizontally placed in the membrane part, the quartz probe is placed in the probe part, one end of the quartz probe is in contact with the quartz membrane, the quartz diaphragm is designed into a flat plate shape with uniform thickness;
2) Preassembling growth raw materials in a single crystal furnace: after indium phosphide crystal, red phosphorus, doping agent and liquid sealing agent are filled into a boron oxide crucible, the boron oxide crucible is filled into a quartz tube and then sealed, the sealed quartz tube is filled into a single crystal furnace and then the single crystal furnace is sealed, wherein a heating element, a temperature measuring element and an air valve are arranged on the single crystal furnace;
3) Single crystal furnace exhaust treatment: heating the interior of the single crystal furnace and vacuumizing the interior of the single crystal furnace in the heating process, wherein the heating condition is that the temperature is raised from 25 ℃ to 380 ℃, the vacuumizing time is controlled to be 50-70 minutes, and the pressure requirement of the interior of the single crystal furnace is lower than-10 psi;
4) Sublimating red phosphorus: stopping vacuumizing treatment and inflating the single crystal furnace when the temperature in the single crystal furnace reaches 380 ℃, wherein the inflating condition is that inert gas is uniformly inflated until the pressure reaches 300psi;
5) Melting indium phosphide crystal: setting a temperature rise curve according to process parameters, wherein the temperature rise curve is formed by raising the temperature from 380 ℃ to 1065-1085 ℃ in a plurality of stages, and controlling the pressure in the single crystal furnace to 405-420 psi by supplementing or discharging air to the single crystal furnace;
6) Crystal growth: reducing the air pressure of the single crystal furnace according to the pressure of the special-shaped quartz tube until the air pressure of the single crystal furnace is maintained to be 395-405 psi;
7) And (3) cooling the crystal: the single crystal furnace is controlled to be cooled slowly according to a set cooling program in the first stage until the temperature in the single crystal furnace is 300 ℃, and an air valve of the single crystal furnace is closed in the first stage; and in the second stage, an air valve of the single crystal furnace is opened, and heating is closed for cooling.
2. The process for growing indium phosphide crystals as set forth in claim 1, wherein the quartz tube preloaded with the raw material for growth in the single-crystal furnace is cylindrical, the sealing cap is outwardly hemispherical, and the pressure outside the quartz tube is required to be controlled to be always 5-15psi higher than the pressure inside the tube during actual production.
3. The process for growing indium phosphide crystal according to claim 1, wherein inert gas is introduced before the temperature in the tube of the quartz tube is lower than the temperature of the red phosphorus until the sublimation of the red phosphorus is completed, and high-purity nitrogen gas of 5psi is continuously introduced into the single crystal furnace until the gas pressure in the single crystal furnace is 300psi.
4. The process for growing indium phosphide crystals according to claim 1, wherein in the first stage of cooling, the single crystal furnace is controlled to slowly cool down according to a set cooling program until the temperature in the single crystal furnace is 300 ℃ under the condition that the power supply and the air valve of the single crystal furnace are not closed; in the second stage of cooling, the air valve of the single crystal furnace is opened and the heating is closed for deflation, the deflation speed is controlled to be slow and then fast, and the average speed is kept at 2.5psi/min until the pressure of the single crystal furnace is 0psi.
5. The process for growing an indium phosphide crystal according to claim 1, wherein the lower end of the first quartz tube and the upper end of the second quartz tube are welded by oxyhydrogen flame, the welded position of the first quartz tube and the second quartz tube is subjected to leak detection treatment, if the leak detection is not abnormal, the special-shaped quartz tube is cleaned and baked with all moisture, the open end of the special-shaped quartz tube is plugged with dust-free cloth after the moisture is evaporated, and high-purity argon is blown into the special-shaped quartz tube by using a hose to replace air in the special-shaped quartz tube.
6. The process for growing an indium phosphide crystal according to claim 1, wherein a first heat-insulating layer is provided on the outer side of the first heat-insulating portion and a second heat-insulating layer is provided on the outer side of the second heat-insulating portion.
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