CN112725901A - Method for eliminating CVD-ZnSe defect - Google Patents
Method for eliminating CVD-ZnSe defect Download PDFInfo
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- CN112725901A CN112725901A CN202011582585.4A CN202011582585A CN112725901A CN 112725901 A CN112725901 A CN 112725901A CN 202011582585 A CN202011582585 A CN 202011582585A CN 112725901 A CN112725901 A CN 112725901A
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- znse
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- isostatic pressing
- hot isostatic
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000007547 defect Effects 0.000 title claims abstract description 25
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 38
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005498 polishing Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000011068 loading method Methods 0.000 claims abstract description 7
- 238000002955 isolation Methods 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000001179 sorption measurement Methods 0.000 claims description 9
- 125000006850 spacer group Chemical group 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000003110 molding sand Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 230000036760 body temperature Effects 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 8
- 230000003287 optical effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present disclosure provides a method of eliminating CVD-ZnSe defects, comprising the steps of: s1: grinding and polishing the CVD-ZnSe wafer to obtain a CVD-ZnSe polished wafer; s2: wiping the surface of the CVD-ZnSe polished wafer with alcohol, then placing the CVD-ZnSe polished wafer in a loading frame of a hot isostatic pressing furnace, respectively placing isolation gaskets on the upper surface and the lower surface of the CVD-ZnSe polished wafer, and then closing the furnace; s3: vacuumizing the hot isostatic pressing furnace, introducing argon, controlling the hot pressing pressure in the hot isostatic pressing furnace to be 100-800 MPa, raising the temperature of the furnace body until the hot pressing temperature reaches 500-800 ℃, and then carrying out hot isostatic pressing on the CVD-ZnSe polished wafer; s4: after the hot isostatic pressing is finished, cooling the hot isostatic pressing furnace to room temperature, and relieving pressure to recover the normal pressure; s5: the CVD-ZnSe polished wafer becomes a CVD-ZnSe wafer after hot isostatic pressing treatment, and the CVD-ZnSe wafer is taken out; s6: and grinding and polishing the CVD-ZnSe wafer to obtain the defect-free CVD-ZnSe wafer. The method for eliminating the CVD-ZnSe defect effectively eliminates the cloud defect and improves the optical light transmittance of the CVD-ZnSe polished wafer.
Description
Technical Field
The disclosure relates to the technical field of chemical industry, in particular to a method for eliminating CVD-ZnSe defects.
Background
Zinc selenide (ZnSe) belongs to II-VI semiconductor compounds, has broadband transmission characteristics, particularly has an extremely low absorption coefficient at 10.6 mu m, is an important infrared optical material, and at present, the main methods for preparing ZnSe comprise a hot pressing method, a Physical Vapor Deposition (PVD) method and a Chemical Vapor Deposition (CVD) method. Compared with a hot pressing method and a physical vapor deposition method, the chemical vapor deposition method has high purity and compact material, and can prepare large-size blocks with complex shapes, but the chemical vapor deposition process is a vapor phase reaction, the internal control is complex, the prepared material is easy to have defects such as microscopic fine particle inclusion, layering, microcrack, hole and the like, the inside of a crystal can be seen by naked eyes after the material is ground and polished to be in a cloud state, the internal uniformity of the material is seriously influenced, and further the transmittance of the material, especially the transmittance of a visible waveband, is influenced.
Disclosure of Invention
In view of the problems in the background art, the present disclosure is directed to a method for eliminating CVD-ZnSe defects, which can effectively eliminate cloud defects inside CVD-ZnSe and improve the optical transmittance of CVD-ZnSe.
In order to achieve the above object, the present disclosure provides a method of eliminating CVD-ZnSe defects, comprising the steps of: s1: grinding and polishing the CVD-ZnSe wafer to obtain a CVD-ZnSe polished wafer; s2: wiping the surface of the CVD-ZnSe polished wafer with alcohol, then placing the CVD-ZnSe polished wafer in a loading frame of a hot isostatic pressing furnace, respectively placing isolation gaskets on the upper surface and the lower surface of the CVD-ZnSe polished wafer, and then closing the furnace; s3: vacuumizing the hot isostatic pressing furnace, introducing argon, controlling the hot pressing pressure in the hot isostatic pressing furnace to be 100-800 MPa, raising the temperature of the furnace body until the hot pressing temperature reaches 500-800 ℃, and then carrying out hot isostatic pressing on the CVD-ZnSe polished wafer; s4: after the hot isostatic pressing is finished, cooling the hot isostatic pressing furnace to room temperature, and relieving pressure to recover the normal pressure; s5: the CVD-ZnSe polished wafer becomes a CVD-ZnSe wafer after hot isostatic pressing treatment, and the CVD-ZnSe wafer is taken out; s6: and grinding and polishing the CVD-ZnSe wafer to obtain the defect-free CVD-ZnSe wafer.
In one embodiment, in step S1, the CVD-ZnSe polished sheet has a surface roughness Ra <20 μm.
In one embodiment, in step S3, the furnace body temperature rise rate is 0.5 deg.C-5 deg.C/min.
In one embodiment, in step S4, the temperature reduction rate of the hot isostatic pressing furnace is 0.5 deg.C-5 deg.C/min.
In one embodiment, in step S2, the CVD-ZnSe polished sheets in the loading frame are provided in multiple layers, a spacer is interposed between two adjacent CVD-ZnSe polished sheets, and an adsorption film for adsorbing impurities on the surface of the CVD-ZnSe polished sheets is further interposed between each CVD-ZnSe polished sheet and the corresponding spacer.
In one embodiment, the spacer is graphite paper.
In one embodiment, the adsorption film is a silver film or a platinum film.
In one embodiment, in step S2, the charging frame of the hiping furnace is further filled with molding sand.
The beneficial effect of this disclosure: according to the method for eliminating the CVD-ZnSe defect, the CVD-ZnSe polished wafer can be uniformly pressed in all directions under the action of pressure transfer gas through the hot isostatic pressing technology, the cloud defect is effectively eliminated, and the optical light transmittance of the CVD-ZnSe polished wafer is improved.
Drawings
FIG. 1 is a schematic view of a CVD-ZnSe wafer placed in a hot isostatic pressing furnace.
Wherein the reference numerals are as follows:
1 charging frame 3 spacer
2CVD-ZnSe polished section 4 molding sand
Detailed Description
It should be noted that the CVD-ZnSe referred to in the present disclosure refers to a zinc selenide material prepared by a chemical vapor deposition method. The method for eliminating CVD-ZnSe defects according to the present disclosure comprises the steps of:
s1: and grinding and polishing the CVD-ZnSe wafer to obtain the CVD-ZnSe polished wafer 2. In one embodiment, the polished CVD-ZnSe polishing sheet 2 has a surface roughness Ra <20 μm.
S2: wiping the surface of the CVD-ZnSe polished wafer 2 with alcohol, placing the CVD-ZnSe polished wafer in a loading frame 1 of a hot isostatic pressing furnace, placing isolation gaskets 3 on the upper surface and the lower surface of the CVD-ZnSe polished wafer 2 respectively, and then closing the furnace. In one embodiment, the spacer is graphite paper. The graphite paper is flexible graphite paper, and can separate two adjacent CVD-ZnSe polished sheets 2 along the up-down direction, so that the risk of scratching caused by mutual contact of the surfaces of the adjacent CVD-ZnSe polished sheets 2 is avoided. The spacer is not limited to graphite paper, and may be made of other materials capable of preventing the surface of the CVD-ZnSe polished wafer 2 from being scratched. As shown in fig. 1, the CVD-ZnSe polished sheets 2 in the loading frame are arranged in a plurality of layers in the vertical direction, a spacer 3 is sandwiched between two adjacent CVD-ZnSe polished sheets 2, and preferably, an adsorption film (not shown) for adsorbing impurities on the surface of the CVD-ZnSe polished sheets 2 is further sandwiched between each CVD-ZnSe polished sheet 2 and the corresponding spacer 3. In one embodiment, the adsorption film is a silver film or a platinum film, and the adsorption film can effectively adsorb microscopic impurities such as hydrogen, zinc and the like on the surface of the CVD-ZnSe polished wafer 2. In one embodiment, the thickness of the graphite paper corresponds to the thickness of the CVD-ZnSe polished sheet 2, i.e., the thicker the CVD-ZnSe polished sheet 2, the thicker the graphite paper is required to effectively space the two adjacent CVD-ZnSe polished sheets 2 apart.
S3: vacuumizing the hot isostatic pressing furnace, introducing argon, controlling the hot pressing pressure in the hot isostatic pressing furnace to be 100-800 MPa, raising the temperature of the furnace body until the hot pressing temperature reaches 500-800 ℃, and then carrying out hot isostatic pressing on the CVD-ZnSe polished wafer 2. In one embodiment, the heating rate of the furnace body is 0.5-5 ℃/min. In a hot isostatic pressing furnace, argon is used as a pressure transmission medium, so that the CVD-ZnSe polished wafer 2 is pressed uniformly in all directions, and defects such as holes, inclusion, cloud mist and the like at a crystal boundary can be eliminated.
S4: after the hot isostatic pressing is completed, the hot isostatic pressing furnace is cooled to room temperature and depressurized to return to normal pressure. In one embodiment, the temperature reduction rate of the hot isostatic pressing furnace is 0.5-5 ℃/min.
S5: the CVD-ZnSe polished wafer 2 becomes a CVD-ZnSe wafer after hot isostatic pressing treatment, and the CVD-ZnSe wafer is taken out.
S6: and grinding and polishing the CVD-ZnSe wafer to obtain the defect-free CVD-ZnSe wafer.
The finally obtained defect-free CVD-ZnSe wafer is detected, the transmittance of the CVD-ZnSe wafer in an infrared band is obviously improved, and the transmittance at the position of 10.6 mu m is more than 70 percent, so that the CVD-ZnSe defect eliminating method disclosed by the invention can enable the CVD-ZnSe polished wafer 2 to be uniformly pressed in all directions under the action of pressure transfer gas through a hot isostatic pressing technology, effectively eliminates cloud and fog defects, and improves the optical transmittance of the CVD-ZnSe polished wafer 2.
In the method of eliminating CVD-ZnSe defects according to the present disclosure, as shown in fig. 1, the charging frame of the hot isostatic pressing furnace is also filled with molding sand 4. In the hot isostatic pressing furnace, the arrangement of the molding sand 4 can increase the all-directional extrusion of the CVD-ZnSe polished wafer 2, so that the adsorption film is tightly attached to the CVD-ZnSe wafer, the adsorption effect of the adsorption film is improved, and the hot pressing effect is increased.
Claims (8)
1. A method of eliminating CVD-ZnSe defects, comprising the steps of:
s1: grinding and polishing the CVD-ZnSe wafer to obtain a CVD-ZnSe polished wafer;
s2: wiping the surface of the CVD-ZnSe polished wafer with alcohol, then placing the CVD-ZnSe polished wafer in a loading frame of a hot isostatic pressing furnace, respectively placing isolation gaskets on the upper surface and the lower surface of the CVD-ZnSe polished wafer, and then closing the furnace;
s3: vacuumizing the hot isostatic pressing furnace, introducing argon, controlling the hot pressing pressure in the hot isostatic pressing furnace to be 100-800 MPa, raising the temperature of the furnace body until the hot pressing temperature reaches 500-800 ℃, and then carrying out hot isostatic pressing on the CVD-ZnSe polished wafer;
s4: after the hot isostatic pressing is finished, cooling the hot isostatic pressing furnace to room temperature, and relieving pressure to recover the normal pressure;
s5: the CVD-ZnSe polished wafer becomes a CVD-ZnSe wafer after hot isostatic pressing treatment, and the CVD-ZnSe wafer is taken out;
s6: and grinding and polishing the CVD-ZnSe wafer to obtain the defect-free CVD-ZnSe wafer.
2. The method of eliminating CVD-ZnSe defects according to claim 1, wherein in step S1, the surface roughness Ra of the CVD-ZnSe polished sheet is <20 μm.
3. The method of eliminating CVD-ZnSe defects according to claim 1, wherein in step S3, the furnace body temperature raising rate is in the range of 0.5 ℃ to 5 ℃/min.
4. The method of eliminating CVD-ZnSe defects according to claim 1, wherein in step S4, the temperature lowering rate of the hot isostatic pressing furnace is set to 0.5 ℃ to 5 ℃/min.
5. The method of eliminating CVD-ZnSe defects according to claim 1,
in step S2, the CVD-ZnSe polished sheets in the loading frame are provided in multiple layers, an isolation pad is sandwiched between two adjacent CVD-ZnSe polished sheets, and an adsorption film for adsorbing impurities on the surface of the CVD-ZnSe polished sheets is sandwiched between each CVD-ZnSe polished sheet and the corresponding isolation pad.
6. The method of eliminating CVD-ZnSe defects of claim 1, wherein the spacer is graphite paper.
7. The method of eliminating CVD-ZnSe defects according to claim 5, wherein the adsorbing film is a silver film or a platinum film.
8. The method of removing CVD-ZnSe defects according to claim 1, wherein in step S2, the charging frame of the hot isostatic pressing furnace is further filled with molding sand.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011582585.4A CN112725901A (en) | 2020-12-28 | 2020-12-28 | Method for eliminating CVD-ZnSe defect |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011582585.4A CN112725901A (en) | 2020-12-28 | 2020-12-28 | Method for eliminating CVD-ZnSe defect |
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| CN112725901A true CN112725901A (en) | 2021-04-30 |
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| CN202011582585.4A Pending CN112725901A (en) | 2020-12-28 | 2020-12-28 | Method for eliminating CVD-ZnSe defect |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320173A (en) * | 1998-09-30 | 2001-10-31 | 三菱硅材料株式会社 | Method for removing defects of single crystal material and single crystal material from which defects are removed by the method |
| CN104591736A (en) * | 2015-01-09 | 2015-05-06 | 中国科学院上海光学精密机械研究所 | Manufacturing method of infrared-transmitted ZnS cowling ceramic |
-
2020
- 2020-12-28 CN CN202011582585.4A patent/CN112725901A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320173A (en) * | 1998-09-30 | 2001-10-31 | 三菱硅材料株式会社 | Method for removing defects of single crystal material and single crystal material from which defects are removed by the method |
| CN104591736A (en) * | 2015-01-09 | 2015-05-06 | 中国科学院上海光学精密机械研究所 | Manufacturing method of infrared-transmitted ZnS cowling ceramic |
Non-Patent Citations (2)
| Title |
|---|
| NAIGUANG WEI: "a hot isostatic processing strategy for improving the optical transmission of poly crystalline CVD ZnSe", 《MATERIALS SCIENCE & PROCESSING》 * |
| 石红春: "热等静压（HIP）对CVDZnSe 透过率的影响", 《红外与激光工程》 * |
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Effective date of registration: 20210701 Address after: 239000 100 Nanjing Road, Langya Economic Development Zone, Chuzhou City, Anhui Province Applicant after: Anhui Zhongfei Technology Co.,Ltd. Address before: 511517 area B, no.27-9 Baijia Industrial Park, Qingyuan high tech Zone, Guangdong Province Applicant before: FIRST SEMICONDUCTOR MATERIALS Co.,Ltd. |
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Application publication date: 20210430 |