CN113308745A - Preparation method of perforated diamond - Google Patents
Preparation method of perforated diamond Download PDFInfo
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- CN113308745A CN113308745A CN202110580903.1A CN202110580903A CN113308745A CN 113308745 A CN113308745 A CN 113308745A CN 202110580903 A CN202110580903 A CN 202110580903A CN 113308745 A CN113308745 A CN 113308745A
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- Prior art keywords
- diamond
- etching
- quartz boat
- perforated
- furnace
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 67
- 239000010432 diamond Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000001681 protective effect Effects 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000013532 laser treatment Methods 0.000 claims abstract description 4
- 238000011282 treatment Methods 0.000 claims abstract description 3
- 238000005530 etching Methods 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 17
- 239000010453 quartz Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 239000001307 helium Substances 0.000 claims 1
- 229910052734 helium Inorganic materials 0.000 claims 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims 1
- 229910052754 neon Inorganic materials 0.000 claims 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 12
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000009835 boiling Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000010355 oscillation Effects 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000001020 plasma etching Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron group metals Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012808 vapor phase 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
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
-
- 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
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a perforated diamond, and belongs to the field of diamond surface treatment. The main process is that diamond is pretreated, then laser treatment is carried out, the diamond and Ni powder which are subjected to laser treatment are heated and etched in a vacuum tube furnace under the protective atmosphere, and finally cleaning treatment is carried out, thus obtaining the perforated diamond. The method has the advantages of simple operation, cheap and easily obtained raw materials, simple equipment and suitability for batch production.
Description
Technical Field
The invention relates to the technical field of diamond surface treatment, in particular to a method for preparing a perforated diamond.
Background
The diamond has the advantages of high hardness, high strength, wear resistance, corrosion resistance, good insulativity, high heat transfer coefficient and the like, and is widely applied to various fields such as functional materials, grinding tools and the like. However, since the diamond itself has a smooth surface and a high surface energy, the application field of the diamond is limited, and therefore, etching of the diamond surface is one of important processing methods to process the diamond surface.
Currently, there are 4 main types of diamond etching methods: vapor phase etching, solid phase etching, gas solid phase etching, and plasma etching. The biggest defects of gas phase etching and plasma etching are high cost and complex etching equipment, and are not suitable for large-batch industrial production. Therefore, the solid phase etching and the gas-solid phase etching have advantages, and the gas-solid phase mixed etching and solid phase etching technology shows great cost and efficiency advantages, and is a trend of the surface treatment development of the diamond in the future.
At present, the diamond etchant is used as metal simple substances, metal oxides, metal salts and the like, wherein the metal simple substances comprise catalysts such as Fe, Co, Ni and the like, the metal oxides comprise oxides of catalytic metals, oxides of iron group metals and the like, and the metal salts comprise oxalates, sylvites and the like. However, after the diamond is etched, etching pits with different shapes and different depths are formed on the surface of the diamond. The {100} plane is an irregular quadrilateral or octagonal etch pit, and the {111} plane is an inverted pyramid etch pit. The etched diamond has certain improvement effect on the preparation of the diamond composite material, but the diamond in the prepared composite material is only simply coated and combined by other materials, and the most ideal combination mode is mutual occlusion type combination.
Disclosure of Invention
The purpose of the invention is: a method for preparing diamond having a perforated structure is provided.
To achieve the purpose of the invention, the following technical scheme is adopted to realize the purpose:
a. the surface pretreatment of the diamond comprises the following specific processes: 1 part of diamond is treated by acid, alkali and organic matter, and then is dried.
b. The laser treatment of diamond comprises the following specific processes: the treated diamond is irradiated with the laser for 5 to 10 seconds, most preferably 8 seconds.
c. The etching of the diamond comprises the following specific processes: uniformly mixing the treated diamond and the etching agent in a crucible, transferring the mixture into a quartz boat, slightly compacting, putting the quartz boat filled with the mixture into a vacuum tube furnace, carrying out gas replacement in the furnace to ensure that the quartz boat is filled with protective gas, then heating to 1000-1200 ℃ under the flowing protective gas atmosphere, keeping the temperature for 90-150 min, and then cooling to room temperature along with the furnace.
d. The specific process of etching the diamond comprises the following steps: and transferring the etched diamond into hydrochloric acid with the mass fraction of 10%, ultrasonically oscillating for 10min to 20min, filtering, washing with distilled water to be neutral, and drying to obtain the perforated diamond.
The acid treatment in the step a in the invention is preferably carried out by the following steps: putting the diamond into a dilute hydrochloric acid solution with the mass fraction of 10-30%, boiling for 10-50 minutes, and then cleaning.
The preferred alkali treatment process in step a of the invention is as follows: putting the diamond into NaOH solution with the mass fraction of 10-30%, boiling for 10-50 minutes and then cleaning.
The preferred process for removing organic matters in the step a in the invention is as follows: the diamond is put into an acetone solution and stirred for 10 to 50 minutes, and then washed, washed by absolute ethyl alcohol and washed by distilled water.
The diamond particle size range in the invention is 300-600 μm, and the optimal selection is 400 μm.
The etching agent in the invention is Ni powder.
The ratio of diamond to etchant in the invention is 1: 5-1: 10 is optimally selected to be 1: 5.
the diameter of the laser beam in the present invention is 2 to 8 μm, and preferably 5 μm.
The etching temperature is 1000-1200 ℃, and the heat preservation time is 90-150 min.
The protective gas in the invention is nitrogen, argon and the mixed gas thereof.
The invention has the beneficial effects that:
1. the holding force of the diamond and the bonding agent is greatly increased through the perforated structure, the cutting effect of the diamond grinding tool in the grinding process is increased, and the grinding quality is improved.
2. The etching conditions are simple, the etching agent is cheap, and the industrial production can be satisfied.
3. The diamond is etched into a perforated structure, and a foundation is provided for preparing high-performance diamond composite materials (diamond metal matrix, diamond resin matrix and diamond ceramic matrix).
Detailed Description
The invention is further described below with reference to specific examples:
example 1:
a. respectively putting 2g of 400-micron diamond into 50ml of 30-percent sodium hydroxide, boiling for 20 minutes, cleaning, adding into 50ml of 30-percent hydrochloric acid solution, boiling for 30 minutes, cleaning, stirring for 10 minutes in acetone solution, cleaning with absolute ethyl alcohol and distilled water, and drying for later use;
b. irradiating the diamond in the step a for 8s by using laser;
c. c, mixing the diamond obtained in the step b and Ni powder according to the proportion of 1: 5, uniformly mixing the mixture in the crucible, transferring the mixture into a quartz boat, slightly compacting, putting the quartz boat filled with the mixture into a vacuum tube furnace, carrying out gas replacement in the furnace to ensure that the quartz boat is filled with protective gas, heating to 1000 ℃ in a flowing protective gas atmosphere, keeping the temperature for 90min, and cooling to room temperature along with the furnace;
d. and c, placing the product obtained in the step c into hydrochloric acid with the mass fraction of 10% for ultrasonic oscillation for 20min, washing the product with distilled water to be neutral after oscillation, and drying the product to obtain the perforated diamond.
Example 2:
a. respectively putting 2g of 400-micron diamond into 50ml of 30-percent sodium hydroxide, boiling for 20 minutes, cleaning, adding into 50ml of 30-percent hydrochloric acid solution, boiling for 30 minutes, cleaning, stirring for 10 minutes in acetone solution, cleaning with absolute ethyl alcohol and distilled water, and drying for later use;
b. irradiating the diamond in the step a for 8s by using laser;
c. c, mixing the diamond obtained in the step b and Ni powder according to the proportion of 1: 5, uniformly mixing the mixture in the crucible, transferring the mixture into a quartz boat, slightly compacting, putting the quartz boat filled with the mixture into a vacuum tube furnace, carrying out gas replacement in the furnace to ensure that the quartz boat is filled with protective gas, heating to 1100 ℃ under the flowing protective gas atmosphere, keeping the temperature for 120min, and cooling to room temperature along with the furnace;
d. and c, placing the product obtained in the step c into hydrochloric acid with the mass fraction of 10% for ultrasonic oscillation for 20min, washing the product with distilled water to be neutral after oscillation, and drying the product to obtain the perforated diamond.
Example 3:
a. respectively putting 2g of 400-micron diamond into 50ml of 30-percent sodium hydroxide, boiling for 20 minutes, cleaning, adding into 50ml of 30-percent hydrochloric acid solution, boiling for 30 minutes, cleaning, stirring for 10 minutes in acetone solution, cleaning with absolute ethyl alcohol and distilled water, and drying for later use;
b. irradiating the diamond in the step a for 8s by using laser;
c. c, mixing the diamond obtained in the step b and Ni powder according to the proportion of 1: 5, uniformly mixing the mixture in the crucible, transferring the mixture into a quartz boat, slightly compacting, putting the quartz boat filled with the mixture into a vacuum tube furnace, carrying out gas replacement in the furnace to ensure that the quartz boat is filled with protective gas, heating to 1200 ℃ under the flowing protective gas atmosphere, keeping the temperature for 150min, and cooling to room temperature along with the furnace;
and placing the obtained product into hydrochloric acid with the mass fraction of 10% for ultrasonic oscillation for 20min, washing the product to be neutral by using distilled water after oscillation, and drying the product to obtain the perforated diamond.
Claims (5)
1. A method for etching a perforated diamond is characterized by comprising the following steps:
a. the surface pretreatment of the diamond comprises the following specific processes: treating 1 part of diamond with acid, alkali and organic matter, and drying;
b. the laser treatment of the diamond comprises the following specific processes: irradiating the processed diamond with laser for 5 to 10 seconds, optimally 8 seconds;
c. the etching treatment of the diamond comprises the following specific processes: uniformly mixing the treated diamond and an etching agent in a crucible, transferring the mixture into a quartz boat, slightly compacting, putting the quartz boat filled with the mixture into a vacuum tube furnace, carrying out gas replacement in the furnace to ensure that the quartz boat is filled with protective gas, heating to 1000-1200 ℃ under the flowing protective gas atmosphere, keeping the temperature for 90-150 min, and cooling to room temperature along with the furnace;
d. the specific process of etching the diamond comprises the following steps: and transferring the etched diamond into hydrochloric acid with the mass fraction of 10%, ultrasonically oscillating for 10min to 20min, filtering, washing with distilled water to be neutral, and drying to obtain the perforated diamond.
2. The etching method according to claim 1, characterized in that: the diamond particle size range is 300-600 μm, and the optimal selection is 400 μm.
3. The etching method according to claim 1, characterized in that: the main component of the etching agent is Ni powder.
4. Etching method according to claims 1 to 3, characterized in that: the protective gas is one or more of nitrogen, argon, helium and neon.
5. Etching method according to claims 1 to 4, characterized in that: during etching, the quartz boat is wrapped by graphite paper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110580903.1A CN113308745A (en) | 2021-05-26 | 2021-05-26 | Preparation method of perforated diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110580903.1A CN113308745A (en) | 2021-05-26 | 2021-05-26 | Preparation method of perforated diamond |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113308745A true CN113308745A (en) | 2021-08-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110580903.1A Pending CN113308745A (en) | 2021-05-26 | 2021-05-26 | Preparation method of perforated diamond |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113308745A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114572979A (en) * | 2022-03-12 | 2022-06-03 | 河南工业大学 | Diamond etching method for surface nano-pore channel |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101118378A (en) * | 2007-08-22 | 2008-02-06 | 武汉工程大学 | Preparation method of diamond surface graphics |
| CN104529527A (en) * | 2014-12-15 | 2015-04-22 | 湖南大学 | Method for increasing surface roughness of man-made diamond single crystal |
| CN107937783A (en) * | 2017-11-17 | 2018-04-20 | 湖南大学 | Increase the method for binding ability between diamond and metallic matrix |
| CN109502582A (en) * | 2018-12-22 | 2019-03-22 | 河南工业大学 | A kind of method of diamond perfectly roundization processing |
| CN110540200A (en) * | 2019-09-11 | 2019-12-06 | 河南工业大学 | method for etching diamond (100) surface in high orientation |
-
2021
- 2021-05-26 CN CN202110580903.1A patent/CN113308745A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101118378A (en) * | 2007-08-22 | 2008-02-06 | 武汉工程大学 | Preparation method of diamond surface graphics |
| CN104529527A (en) * | 2014-12-15 | 2015-04-22 | 湖南大学 | Method for increasing surface roughness of man-made diamond single crystal |
| CN107937783A (en) * | 2017-11-17 | 2018-04-20 | 湖南大学 | Increase the method for binding ability between diamond and metallic matrix |
| CN109502582A (en) * | 2018-12-22 | 2019-03-22 | 河南工业大学 | A kind of method of diamond perfectly roundization processing |
| CN110540200A (en) * | 2019-09-11 | 2019-12-06 | 河南工业大学 | method for etching diamond (100) surface in high orientation |
Non-Patent Citations (1)
| Title |
|---|
| 窦志强等: "金刚石表面刻蚀技术研究进展", 《表面技术》, vol. 47, pages 90 - 95 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114572979A (en) * | 2022-03-12 | 2022-06-03 | 河南工业大学 | Diamond etching method for surface nano-pore channel |
| CN114572979B (en) * | 2022-03-12 | 2024-01-26 | 河南工业大学 | Diamond etching method of surface nano pore canal |
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Application publication date: 20210827 |