CN114250520A - Method for reducing diamond stress - Google Patents
Method for reducing diamond stress Download PDFInfo
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- CN114250520A CN114250520A CN202111614966.0A CN202111614966A CN114250520A CN 114250520 A CN114250520 A CN 114250520A CN 202111614966 A CN202111614966 A CN 202111614966A CN 114250520 A CN114250520 A CN 114250520A
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- diamond
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 78
- 239000010432 diamond Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000004140 cleaning Methods 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 18
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000011049 filling Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000945 filler Substances 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000758 substrate 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
- 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
- C30B29/02—Elements
- C30B29/04—Diamond
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Cleaning In General (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present disclosure provides a method of reducing diamond stress, comprising the steps of: step one, cleaning diamond: ultrasonically cleaning diamond with acetone, absolute ethyl alcohol and deionized water in sequence, drying and then preserving heat; step two, annealing diamond: putting the dried diamond into a tubular atmosphere furnace, sealing, opening a vacuum pump, annealing, and cooling to normal temperature after annealing is completed; step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling one of silicon carbide, silicon nitride and diamond micro powder into the beaker for ultrasonic treatment; step five, cleaning: ultrasonic cleaning with acetone, anhydrous alcohol, and deionized water for 5-30 min. The method utilizes heat energy and ultrasonic impact vibration to provide external power for dislocation motion and increment, can well remove the stress in the diamond, and reduces the breakage rate, and has simple process and low cost.
Description
Technical Field
The invention relates to the technical field of diamond preparation and processing treatment, in particular to a method for reducing diamond stress.
Background
Due to the limitation of equipment or process technology, the artificially synthesized single crystal or polycrystalline diamond has certain stress more or less, and the application of the diamond in various high and new technical fields such as precision machining, aerospace and the like can be limited by the overhigh stress.
In the field of diamond preparation and processing, common stress removal methods include heat treatment, cold treatment and hot pressing treatment, wherein the heat treatment and the hot pressing treatment cannot completely eliminate stress, and the cold treatment may cause cracking of the diamond.
Therefore, a new method is needed to remove diamond stress.
Disclosure of Invention
In view of the problems in the background art, it is an object of the present disclosure to provide a method of reducing diamond stress.
In order to achieve the above object, the present disclosure provides a method of reducing diamond stress, comprising the steps of: step one, cleaning diamond: ultrasonically cleaning diamond with acetone, absolute ethyl alcohol and deionized water in sequence, drying and then preserving heat; step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, carrying out annealing treatment, and cooling to normal temperature after annealing is finished; step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling one of silicon carbide, silicon nitride and diamond micro powder into the beaker for ultrasonic treatment; step five, cleaning: ultrasonic cleaning with acetone, anhydrous alcohol, and deionized water for 5-30 min.
In some embodiments, in step one, the time for the ultrasonic cleaning is 5-10 min.
In some embodiments, in step one, the drying temperature is 60-120 ℃.
In some embodiments, in step one, the incubation time is 10-30 min.
In some embodiments, in step two, the annealing process is performed by: and opening the MFC system, adjusting the argon flow to 200-600sccm, the pressure to 5-10kPa, the temperature to 400-800 ℃, the heating rate to 5-15 ℃/min and the heat preservation time to 10-30 h.
In some embodiments, in step three, the method of sonication is: and opening the ultrasonic cleaning instrument, wherein the power is 200-.
The beneficial effects of this disclosure are as follows:
the method combines heat treatment and ultrasonic treatment to treat the diamond, utilizes heat energy and ultrasonic impact vibration and irregular vibration of the filler to impact the diamond to provide external power for dislocation movement and increment, can better remove the internal stress of the diamond, reduces the breakage rate, provides a new mode for removing the internal stress of the diamond, and has simple process and low cost.
Detailed Description
The method of reducing diamond stress of the present disclosure is described in detail below, comprising the steps of: step one, cleaning diamond: ultrasonically cleaning diamond with acetone, absolute ethyl alcohol and deionized water in sequence, drying and then preserving heat; step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, carrying out annealing treatment, and cooling to normal temperature after annealing is finished; step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling one of silicon carbide, silicon nitride and diamond micro powder into the beaker for ultrasonic treatment; step five, cleaning: ultrasonic cleaning with acetone, anhydrous alcohol, and deionized water for 5-30 min.
According to the method, the diamond is treated by combining heat treatment and ultrasonic treatment, external power is provided for dislocation motion and increment by utilizing heat energy and ultrasonic impact vibration in the early stage, external power is provided for dislocation motion and increment by utilizing the ultrasonic impact vibration and irregular vibration of the filler to impact the diamond in the later stage, and internal stress of the diamond is removed.
In some embodiments, in step one, the time for the ultrasonic cleaning is 5-10 min. The surface of the diamond cannot be cleaned by the ultrasonic cleaning time which is too short.
In some embodiments, in step one, the drying temperature is 60-120 ℃. The drying temperature is too low, the drying time is too long, and the time cost is increased.
In some embodiments, in step one, the incubation time is 10-30 min.
In some embodiments, in step two, the annealing process is performed by: and opening the MFC system, adjusting the argon flow to 200-600sccm, the pressure to 5-10kPa, the temperature to 400-800 ℃, the heating rate to 5-15 ℃/min and the heat preservation time to 10-30 h.
In some embodiments, in step three, the method of sonication is: and opening the ultrasonic cleaning instrument, wherein the power is 200-. The ultrasonic power is too low, and the ultrasonic time is too short, so that the effect of removing stress cannot be achieved.
The disclosure is further illustrated with reference to the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure.
Example 1
Step one, cleaning diamond: ultrasonically cleaning diamond with acetone, anhydrous ethanol and deionized water for 5min, and maintaining at 60 deg.C for 30min in oven;
step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, opening an MFC system, adjusting the argon flow to 200sccm, the pressure to 5kPa, the temperature to 800 ℃, the heating rate to 15 ℃/min, preserving heat for 30 hours, carrying out annealing treatment, and cooling to normal temperature after the annealing is finished;
step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling diamond micro powder into the beaker for ultrasonic treatment;
step five, cleaning: and ultrasonically cleaning the glass substrate for 30min by using acetone, absolute ethyl alcohol and deionized water in sequence.
The raman shift results are shown in table 1.
Example 2
Step one, cleaning diamond: ultrasonically cleaning diamond with acetone, anhydrous ethanol and deionized water for 5min, and maintaining at 60 deg.C for 30min in oven;
step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, opening an MFC system, adjusting the argon flow to 200sccm, the pressure to 5kPa, the temperature to 400 ℃, the heating rate to 15 ℃/min, preserving heat for 30 hours, carrying out annealing treatment, and cooling to normal temperature after the annealing is finished;
step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling diamond micro powder into the beaker for ultrasonic treatment;
step four, cleaning: and ultrasonic cleaning with acetone, anhydrous ethanol and deionized water for 30 min.
The raman shift results are shown in table 1.
Comparative example 1
Step one, cleaning diamond: ultrasonically cleaning diamond with acetone, anhydrous ethanol and deionized water for 5min, and maintaining at 60 deg.C for 30min in oven;
step two, ultrasonic treatment: putting the diamond processed in the step one into an ultrasonic bracket, putting the ultrasonic bracket into a beaker, and filling diamond micro powder into the beaker for ultrasonic processing;
step three, cleaning: and ultrasonic cleaning with acetone, anhydrous ethanol and deionized water for 30 min.
The raman shift results are shown in table 1.
Comparative example 2
Step one, cleaning diamond: ultrasonically cleaning diamond with acetone, anhydrous ethanol and deionized water for 5min, and maintaining at 60 deg.C for 30min in oven;
step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, opening an MFC system, adjusting the argon flow to 200sccm, the pressure to 5kPa, the temperature to 800 ℃, the heating rate to 15 ℃/min, preserving heat for 30 hours, carrying out annealing treatment, and cooling to normal temperature after the annealing is finished;
step three, cleaning: the results of the Raman shift of the sample after ultrasonic cleaning with acetone, absolute ethyl alcohol and deionized water for 30min are shown in Table 1.
Comparative example 3
Step one, cleaning diamond: ultrasonically cleaning diamond with acetone, anhydrous ethanol and deionized water for 5min, and maintaining at 60 deg.C for 30min in oven;
step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, opening an MFC system, adjusting the argon flow to 200sccm, the pressure to 5kPa, the temperature to 800 ℃, the heating rate to 15 ℃/min, preserving heat for 30 hours, carrying out annealing treatment, and cooling to normal temperature after the annealing is finished;
step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling deionized water into the beaker for ultrasonic treatment;
step four, cleaning: and ultrasonic cleaning with acetone, anhydrous ethanol and deionized water for 30 min.
The raman shift results are shown in table 1.
TABLE 1 experimental results of Raman Shift testing of examples 1-2 and comparative examples 1-3
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| D peak change amount | 0.33cm-1 | 0.24cm-1 | 0.11cm-1 | 0.16cm-1 | 0.18cm-1 |
Note: untreated D Peak position 1333.16cm-1
The larger the variation of the raman shift is, the better the stress relief result is, and as shown in table 1, the raman test shifts of examples 1 and 2 are larger than those of comparative examples 1 to 3, which indicates that the effect of relieving the stress of the diamond by using the impact vibration of the thermal energy and the ultrasonic wave and the irregular vibration of the filler is good.
The above-disclosed features are not intended to limit the scope of practice of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (6)
1. A method of reducing diamond stress comprising the steps of:
step one, cleaning diamond: ultrasonically cleaning diamond with acetone, absolute ethyl alcohol and deionized water in sequence, drying and then preserving heat;
step two, annealing diamond: putting the diamond dried in the step one into a tubular atmosphere furnace, sealing the tubular atmosphere furnace, opening a vacuum pump, pumping out air of the tubular atmosphere furnace, carrying out annealing treatment, and cooling to normal temperature after annealing is finished;
step three, ultrasonic treatment: putting the diamond annealed in the step two into an ultrasonic support, putting the ultrasonic support into a beaker, and filling one of silicon carbide, silicon nitride and diamond micro powder in the beaker for ultrasonic treatment;
step five, cleaning: ultrasonic cleaning with acetone, anhydrous alcohol, and deionized water for 5-30 min.
2. A method of reducing diamond stress according to claim 1, wherein in step one, the time of the ultrasonic cleaning is 5-10 min.
3. A method of reducing diamond stress according to claim 1, wherein in step one, the baking temperature is 60-120 ℃.
4. A method of reducing diamond stress according to claim 1, wherein in step one, the holding time is 10-30 min.
5. A method of reducing diamond stress according to claim 1, wherein in step two, the annealing process is carried out by: and opening the MFC system, adjusting the argon flow to 200-600sccm, the pressure to 5-10kPa, the temperature to 400-800 ℃, the heating rate to 5-15 ℃/min and the heat preservation time to 10-30 h.
6. The method for reducing diamond stress according to claim 1, wherein in step three, the ultrasonic treatment method is: and opening the ultrasonic cleaning instrument, wherein the power is 200-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111614966.0A CN114250520A (en) | 2021-12-24 | 2021-12-24 | Method for reducing diamond stress |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111614966.0A CN114250520A (en) | 2021-12-24 | 2021-12-24 | Method for reducing diamond stress |
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| CN114250520A true CN114250520A (en) | 2022-03-29 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5451430A (en) * | 1994-05-05 | 1995-09-19 | General Electric Company | Method for enhancing the toughness of CVD diamond |
| CN103290482A (en) * | 2013-01-06 | 2013-09-11 | 河北同光晶体有限公司 | Method for removing stress of silicon carbide crystal with large diameter |
| CN104975343A (en) * | 2015-06-04 | 2015-10-14 | 哈尔滨工业大学 | Method for improving quality of diamond seed crystal with hydrogen plasma multiple etching/annealing cyclic process |
| CN113005517A (en) * | 2021-02-25 | 2021-06-22 | 廊坊西波尔钻石技术有限公司 | Treatment method for reducing internal stress of single crystal diamond |
| CN213835629U (en) * | 2020-09-01 | 2021-07-30 | 山东天岳先进科技股份有限公司 | Device for eliminating internal stress of crystal ingot |
-
2021
- 2021-12-24 CN CN202111614966.0A patent/CN114250520A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5451430A (en) * | 1994-05-05 | 1995-09-19 | General Electric Company | Method for enhancing the toughness of CVD diamond |
| CN103290482A (en) * | 2013-01-06 | 2013-09-11 | 河北同光晶体有限公司 | Method for removing stress of silicon carbide crystal with large diameter |
| CN104975343A (en) * | 2015-06-04 | 2015-10-14 | 哈尔滨工业大学 | Method for improving quality of diamond seed crystal with hydrogen plasma multiple etching/annealing cyclic process |
| CN213835629U (en) * | 2020-09-01 | 2021-07-30 | 山东天岳先进科技股份有限公司 | Device for eliminating internal stress of crystal ingot |
| CN113005517A (en) * | 2021-02-25 | 2021-06-22 | 廊坊西波尔钻石技术有限公司 | Treatment method for reducing internal stress of single crystal diamond |
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