CN115537921A - Synthesis method of indium phosphide - Google Patents
Synthesis method of indium phosphide Download PDFInfo
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- CN115537921A CN115537921A CN202211301629.0A CN202211301629A CN115537921A CN 115537921 A CN115537921 A CN 115537921A CN 202211301629 A CN202211301629 A CN 202211301629A CN 115537921 A CN115537921 A CN 115537921A
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- indium
- quartz boat
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- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000001308 synthesis method Methods 0.000 title claims description 11
- 239000010453 quartz Substances 0.000 claims abstract description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052738 indium Inorganic materials 0.000 claims abstract description 26
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 24
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 13
- 239000011574 phosphorus Substances 0.000 claims abstract description 13
- 238000004857 zone melting Methods 0.000 claims abstract description 11
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000002904 solvent Substances 0.000 claims description 22
- -1 alkyl indium salt Chemical class 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 7
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 3
- RTXSBTHBRXWZBH-UHFFFAOYSA-K indium(3+) propanoate Chemical compound [In+3].CCC([O-])=O.CCC([O-])=O.CCC([O-])=O RTXSBTHBRXWZBH-UHFFFAOYSA-K 0.000 claims description 2
- LKEDUJPRSZGTHZ-UHFFFAOYSA-H indium(3+);oxalate Chemical compound [In+3].[In+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O LKEDUJPRSZGTHZ-UHFFFAOYSA-H 0.000 claims description 2
- SBFKENUEAOCRNR-UHFFFAOYSA-K indium(3+);triformate Chemical compound [In+3].[O-]C=O.[O-]C=O.[O-]C=O SBFKENUEAOCRNR-UHFFFAOYSA-K 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 27
- 230000000052 comparative effect Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 16
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 6
- 239000003708 ampul Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000006837 decompression Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000011043 treated quartz Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
-
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
Abstract
The invention relates to the field of compound semiconductor materials, in particular to a method for synthesizing indium phosphide. The invention provides a method for synthesizing indium phosphide, which comprises the following steps: in is formed on the inner surface of the quartz boat 2 O 3 And coating, namely adding phosphorus and indium into the quartz boat, and carrying out zone melting to obtain indium phosphide. The method provided by the invention can be used for obtaining the indium phosphide with low silicon impurity content, and the method is low in production cost. Experiments show that the indium phosphide polycrystal with the impurity Si content of 6.5ppb is obtained by the method of the invention, the impurity Si content is far lower than that of the indium phosphide polycrystal of other comparative examples, and the contents of the impurity O and the impurity C are not obviously increased.
Description
Technical Field
The invention relates to the field of compound semiconductor materials, in particular to a method for synthesizing indium phosphide.
Background
Indium phosphide (InP) is a group III-V compound semiconductor material with a sphalerite structure and excellent performance, has the advantages of high saturated electron drift velocity, strong radiation resistance, good thermal conductivity, high photoelectric conversion efficiency, high forbidden bandwidth 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.
The melting point of indium is 1070 ℃, the indium phosphide material has high decompression pressure at the melting point, the decompression pressure at the melting point is 2.75MPa, and the phosphorus vapor pressure is over 10MPa and far greater than the decompression pressure of indium phosphide under the condition calculated according to the formula of the functional relation between the Antoine saturated vapor pressure and the temperature, i.e., lgP = A-B/(T + C), so that the synthesis of indium phosphide single crystal by directly synthesizing high-purity indium and high-purity phosphorus in a single crystal furnace is very difficult, and the synthesis of indium phosphide polycrystal by polycrystalline synthesis of high-purity indium and high-purity phosphorus is generally carried out, and then the indium phosphide single crystal is grown by using the indium phosphide polycrystal.
At present, the horizontal Bridgman method is mainly used for producing the indium phosphide polycrystal, the method is used for synthesizing the indium phosphide polycrystal by phosphorus steam and indium melt, and because the indium phosphide polycrystal contacts a quartz ampoule bottle and a quartz boat at high temperature for a long time, the content of Si in the indium phosphide polycrystal is very high, and the performance of a product is seriously influenced. The impurity content of Si can be reduced by adopting the PBN (pyrolytic boron nitride) boat, but the production cost is greatly increased, and the method is not suitable for long-term development of enterprises.
In the production process of indium phosphide polycrystal, a quartz boat is generally used to replace a PBN (pyrolytic boron nitride) boat because the price of the quartz boat with the same size is only 1/10 of that of the PBN boat, but in the production process, under the environment of high temperature and high pressure for a long time, siO in the indium and quartz boats 2 Reaction is carried out:
the content of Si impurity element in the indium phosphide polycrystal material is increased, the performance of the product is seriously influenced, and the quality of the product of the subsequent single crystal growth is influenced.
Therefore, a new method is needed to reduce the impurity content of Si without increasing the production cost.
Disclosure of Invention
In view of the above, the present invention provides a method for synthesizing indium phosphide, which can obtain indium phosphide with low silicon impurity content and has low production cost.
The invention provides a method for synthesizing indium phosphide, which comprises the following steps: in is formed on the inner surface of the quartz boat 2 O 3 A coating layer ofAnd adding phosphorus and indium into the quartz boat, and carrying out zone melting to obtain indium phosphide.
In is first formed on the inner surface of the quartz boat 2 O 3 Coating, in which the concentration of the product is increased In a reversible reaction under otherwise unchanged conditions according to the principle of chemical equilibrium shift, and the reaction is carried out In the reverse direction, using In 2 O 3 The coated quartz boat can reversibly react In 2 O 3 The concentration value of (2) is increased, and the positive reaction is inhibited, so that the generation of Si is reduced, and the aim of reducing the content of Si impurities is fulfilled.
Specifically, in is formed on the inner surface of the quartz boat 2 O 3 The coating specifically comprises: the inner surface of the quartz boat is soaked in a mixed solution of alkyl indium salt and alcohol solvent and then calcined. In some embodiments of the present invention, the mixed solution of the alkyl indium salt and the alcohol solvent is obtained by stirring and mixing the alkyl indium salt and the alcohol solvent, and the inner surface of the quartz boat is soaked in the mixed solution of the alkyl indium salt and the alcohol solvent, and then dried and calcined. In one embodiment, the method comprises the steps of putting alkyl indium salt into a clean quartz boat, adding an alcohol solvent, stirring and mixing to obtain a mixed solution of the alkyl indium salt and the alcohol solvent, infiltrating the inner surface of the quartz boat into the mixed solution of the alkyl indium salt and the alcohol solvent, volatilizing the alcohol solvent, drying, and calcining. In one embodiment, the In 2 O 3 The thickness of the coating is 0.5 mm-1 mm.
In can not be directly added into the alcohol solvent 2 O 3 Or In (OH) 3 Due to In 2 O 3 Or In (OH) 3 The quartz boat is not dissolved in water or alcohol solvents, clear and transparent solution cannot be obtained, and the inner surface of the whole quartz boat cannot be uniformly soaked. In one embodiment, the purity of the alkyl indium salt is 6N or more, and the alcoholic solvent is an UP grade alcoholic solvent. In one embodiment, the hydrocarbyl indium salt is selected from at least one of indium acetate, indium formate, indium propionate, indium oxalate; the alcohol solvent is at least one selected from ethanol, glycol and glycerol. In one embodiment, the hydrocarbyl indium saltAnd the dosage proportion of the alcohol solvent is 5 g-10 g:30 mL-50 mL.
The invention mixes alkyl indium salt and alcohol solvent, which can generate the following reaction equation: in 3+ +6AC - →In(AC) 6 3- Complexing to obtain a clear and transparent solution, and fully soaking the clear and transparent solution into a quartz boat; in (AC) 6 In pure Water phase 3- Exists only in weakly hydrated ionic forms, according to the reaction equation: in (AC) 6 3- +H 2 O→In(OH) 3 In (AC) In pure Water phase 6 3- Easily hydrolyzed to obtain In (OH) 3 ，In(OH) 3 Is insoluble in water, and a clear and transparent solution cannot be obtained; in the alcohol solvent, the number of hydroxyl groups is increased, and the number of bonding of trivalent indium ions and the hydroxyl groups is also increased, so that the reaction equation is as follows: in (AC) 6 3- +CH 3 CH 2 OH→In[CH 3 CH 2 O] 2+ +H + +6AC - Shown, hydrolysis was inhibited, in (OH) was reduced 3 And (4) generating. In one embodiment, the time of mixing is 10min or more.
The invention mixes the solution of alkyl indium salt and alcohol solvent to fully soak the quartz boat, volatilizes the alcohol solvent and dries, in [ CH ] 3 CH 2 O] + Uniformly attached to the inner surface of the quartz boat. In one embodiment, the soaking time is 3min to 5min. In one embodiment, the temperature of the drying is 40 to 80 ℃, preferably 60 ℃.
The invention calcines the quartz boat which is fully soaked by the mixed solution of the alkyl indium salt and the alcohol solvent, and the quartz boat is prepared by the following steps: in [ CH ] 3 CH 2 O] 2+ →In 2 O 3 A uniform In layer is formed on the inner surface 2 O 3 The film and the water and the carbon-oxygen compound generated simultaneously are changed into gaseous state along with the temperature rise and are continuously discharged, so that the product is prevented from being polluted by excessive C element and O element. In one embodiment, the temperature of the calcination is from 450 ℃ to 500 ℃, preferably 500 ℃; the calcining time is 4-6 h, preferably 5h; the temperature rise rate of the calcination is 80-100 ℃/h.
In some embodiments of the invention, indium acetate is used as alkyl indium salt to form In on the inner surface of the quartz boat 2 O 3 Coating, in is formed on the inner surface of the quartz boat by using indium acetate as alkyl indium salt 2 O 3 A typical process flow for coating is as follows: adding 5-10 g of indium acetate and 30-50 mL of UP-grade alcohol solution into a quartz boat, and stirring for more than 10min to obtain clear transparent solution; shaking the solution to wet the inner surface of the whole quartz boat; putting the quartz boat into a constant-temperature oven at 60 ℃ for drying; putting the quartz boat into a heater to be heated to 450-500 ℃, and preserving heat for 4-6 h to form In on the inner surface of the quartz boat 2 O 3 And (4) coating.
In is formed on the inner surface of the quartz boat 2 O 3 And after coating, adding phosphorus and indium into the quartz boat, and carrying out zone melting to obtain indium phosphide. In certain embodiments of the present invention, the phosphorus is red phosphorus and the indium is elemental indium. In certain embodiments of the invention, the zone melting process is a bridgman growth process; the Bridgman method is essentially a zone melting technique, and impurities can be removed from the product by adjusting the temperature of a heating zone, so that the purpose of purification is achieved. In some embodiments of the invention, in is formed on the inner surface of the quartz boat 2 O 3 And after coating, adding phosphorus and indium into the quartz boat, and performing zone melting on the quartz boat added with the phosphorus and the indium at 1200-1500 ℃ for more than 10h to obtain the indium phosphide.
In 2 O 3 Has a melting point of 2000 deg.C, a melting point of 1070 deg.C, and a large difference between the melting points of In and InP to ensure that In is In 2 O 3 Easier to remove from the InP product. Even if a small amount of In remains 2 O 3 In, which cannot be removed completely 2 O 3 In and O elements In the InP have little influence on InP products, in is a main element and cannot influence the product quality, and the O elements can be removed In the subsequent annealing process. In some embodiments of the invention, the quartz boat added with phosphorus and indium is placed on a heater provided with more than 3 temperature zones for zone melting, the temperature of each temperature zone is ensured to be 1200-1500 ℃ in the synthesis stage, andpreserving the heat for more than 10 hours; when the temperature is reduced, firstly, the temperature of the temperature zone at one end of the head of the crystal bar is set to be 1100-1200 ℃, and the temperature of other temperature zones is kept unchanged at 1200-1500 ℃ so that In is enabled 2 O 3 Si and other impurities with high melting points are gradually condensed in the head area of the crystal bar, and then the indium phosphide is kept in a molten state, and then the temperature of the temperature zone of the heater is adjusted to gradually cool from the temperature zone at one end of the head of the crystal bar to the temperature zone at one end of the tail of the crystal bar, so that the indium phosphide product is condensed in the middle of the crystal bar, and finally the impurities with low melting points are all condensed at the tail of the crystal bar; and cutting off the head and the tail of the crystal bar to obtain the indium phosphide with low impurity content.
The invention provides a method for synthesizing indium phosphide, which comprises the following steps: in is formed on the inner surface of the quartz boat 2 O 3 And coating, namely adding phosphorus and indium into the quartz boat, and carrying out zone melting to obtain indium phosphide. The process provided by the invention utilizes a hydrocarbyl indium salt and an alcoholic solvent to convert In 2 O 3 The coating reduces the generation of Si impurity elements, does not introduce other impurity elements, improves the performance of products, and provides high-quality raw materials for the subsequent single crystal process. The alkyl indium salt and the alcohol solution in the invention have wide sources, are simple and easy to obtain, are nontoxic and harmless, have low price, have lower production cost of indium phosphide polycrystal materials compared with the PBN boat with high price in the traditional method, improve the market competitiveness of enterprises, and meet the long-term development requirements of the enterprises. The invention has simple and convenient manufacturing process, safety and reliability, does not generate waste slag, waste water and waste gas, does not influence the environment, and is safe and environment-friendly. Experiments show that the indium phosphide polycrystal with the impurity Si content of 6.5ppb is obtained by the method of the invention, the impurity Si content is far lower than that of the indium phosphide polycrystal of other comparative examples, and the contents of the impurity O and the impurity C are not obviously increased.
Detailed Description
The invention discloses a method for synthesizing indium phosphide. Those skilled in the art can modify the process parameters appropriately to achieve the desired results with reference to the disclosure herein. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention is further illustrated by the following examples:
example 1
1, 10g of 6N indium acetate is put into a clean quartz boat, 50mL of UP-grade ethanol solution is measured, and is stirred for 10min with force, and clear and transparent solution is obtained by complexation. Slowly shaking the quartz boat to enable the solution to completely soak the inner surface of the whole quartz boat for 5min; after the ethanol solution is volatilized, putting the quartz boat into a drying oven with the constant temperature of 60 ℃ for drying; placing the dried quartz boat In a heater, heating to 500 deg.C, and maintaining for 5 hr to form a layer of uniform In on the inner surface of the quartz boat 2 O 3 And (3) a membrane.
Slowly putting the indium strips into the quartz boat by using the treated quartz boat, calculating the weight of the required red phosphorus according to the loading amount of the indium strips, filling the red phosphorus into an ampoule bottle, sealing the tube for later use, then carrying out a synthesis process by using a horizontal Bridgman method, and carrying out InP and In synthesis according to InP and In 2 O 3 The heater is arranged in 3 sections of temperature areas, the temperature of the 3 sections of temperature areas is ensured to be about 1400 ℃ in the synthesis stage, and the temperature is kept for 12 hours; when the temperature is reduced, firstly, the temperature zone at one end of the head of the crystal bar is set to be 1200 ℃, and the temperature of other temperature zones is kept to be 1400 ℃ to ensure that In is kept unchanged 2 O 3 Si and other impurities with high melting points are gradually condensed in the head area of the crystal bar, and then the indium phosphide is kept in a molten state, and then the temperature of a temperature zone of the heater is adjusted to gradually cool from the head of the crystal bar to the tail of the crystal bar, so that an indium phosphide product is condensed in the middle of the crystal bar, and finally, the impurities with low melting points are all condensed at the tail of the crystal bar; and cutting off the head and the tail of the crystal bar to obtain an indium phosphide product with low impurity content.
Comparative example 1
1, putting 10g of 6N indium acetate into a clean quartz boat, measuring 50mL of ultrapure water, and stirring for 10min with force; slowly shaking the quartz boat to make the solution infiltrate the whole stoneThe inner surface of the quartz boat; putting the quartz boat into a constant-temperature oven at 60 ℃ for drying; placing the dried quartz boat In a heater, heating to 500 deg.C, and maintaining for 5 hr to generate In on the inner surface of the quartz boat 2 O 3 And (3) a film.
Using the treated quartz boat, the indium strips were slowly placed in the quartz boat, and the required weight of red phosphorus was calculated from the amount of indium strips charged, and red phosphorus was put into an ampoule and sealed for further use, and then indium phosphide product was obtained according to the synthesis method of example 1.
Comparative example 2
10g 6N of In (OH) 3 Putting the quartz boat into a clean quartz boat, measuring 50mL of UP-grade ethanol solution, and stirring for 10min with force; slowly shaking the quartz boat to enable the liquid to infiltrate the inner surface of the whole quartz boat; putting the quartz boat into a constant-temperature oven at 60 ℃ for drying; placing the dried quartz boat In a heater, heating to 500 deg.C, and maintaining for 5 hr to generate In on the inner surface of the quartz boat 2 O 3 And (3) a membrane.
Using the treated quartz boat, the indium strips were slowly placed in the quartz boat, and the required weight of red phosphorus was calculated from the amount of indium strips charged, and red phosphorus was put into an ampoule and sealed for further use, and then indium phosphide product was obtained according to the synthesis method of example 1.
Comparative example 3
Taking a quartz boat which is not treated by the method of the invention, slowly putting indium strips into the quartz boat, calculating the weight of red phosphorus according to the loading amount of the indium strips, filling the red phosphorus into an ampoule bottle, sealing the tube for standby, and then obtaining an indium phosphide product according to the synthesis method of the embodiment 1.
The products obtained in example 1 and comparative examples 1 to 3 were sampled for electrical property and GDMS detection, and the detection results are shown in table 1:
TABLE 1
From Table 1, it can be seen from the results of the tests of example 1 that example 1 has stone treated by the method of the present inventionThe inner surface of the quartz boat forms a layer of uniform In 2 O 3 The film effectively inhibits the reaction of indium and the quartz boat, reduces the generation of Si impurity elements, and achieves the purpose of reducing the content of silicon impurities in the indium phosphide polycrystal material. Meanwhile, it can be seen from the results of the tests of comparative examples 1 to 3 that the Si impurity elements in the product are far more than those in the examples without the quartz boat processed by the method of the present invention or without some steps of processing. In addition, from the test results of the examples and the comparative examples, the impurity contents of the O element and the C element in the invention are not obviously improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A method for synthesizing indium phosphide is characterized by comprising the following steps:
in is formed on the inner surface of the quartz boat 2 O 3 And coating, namely adding phosphorus and indium into the quartz boat, and carrying out zone melting to obtain indium phosphide.
2. The synthesis method according to claim 1, wherein In is formed on the inner surface of the quartz boat 2 O 3 The coating specifically comprises:
the inner surface of the quartz boat is soaked in the mixed solution of alkyl indium salt and alcohol solvent and then calcined.
3. The method of claim 2, wherein said alkyl indium salt is selected from at least one of indium acetate, indium formate, indium propionate, and indium oxalate.
4. The synthesis method according to claim 2, wherein the alcoholic solvent is at least one selected from ethanol, ethylene glycol and glycerol.
5. The synthesis method as claimed in claim 2, wherein the ratio of the amount of said alkyl indium salt to said alcohol solvent is 5-10 g:30 mL-50 mL.
6. The method of claim 2, wherein the soaking time is 3min to 5min.
7. The synthesis method according to claim 2, characterized in that the calcination temperature is 450-500 ℃ and the calcination time is 4-6 h.
8. The synthesis method according to claim 7, characterized in that the heating rate of the calcination is 80-100 ℃/h.
9. The synthesis method according to claim 1 or 2, characterized in that the temperature of the zone melting is 1200 ℃ to 1500 ℃;
the zone melting time is more than 10 h.
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