CN114572979B - Diamond etching method of surface nano pore canal - Google Patents
Diamond etching method of surface nano pore canal Download PDFInfo
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- CN114572979B CN114572979B CN202210239887.4A CN202210239887A CN114572979B CN 114572979 B CN114572979 B CN 114572979B CN 202210239887 A CN202210239887 A CN 202210239887A CN 114572979 B CN114572979 B CN 114572979B
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- 239000010432 diamond Substances 0.000 title claims abstract description 82
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 82
- 238000005530 etching Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000011148 porous material Substances 0.000 title claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 238000010306 acid treatment Methods 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000001020 plasma etching Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical class [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical class [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical class [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004317 sodium nitrate Chemical class 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical class [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a diamond etching method for a surface nano pore canal, and belongs to the field of diamond surface treatment. The main process is that firstlyPretreating diamond, and hydrogen reducing ferric chloride (FeCl) on the surface of diamond 3 ·6H 2 O), obtaining diamond wrapped by nano iron powder, placing the diamond wrapped by nano iron powder into a tube furnace, heating and etching under the condition of continuously introducing hydrogen atmosphere, and finally cleaning to obtain the diamond with the nano pore canal on the surface. The invention has simple operation, cheap and easily obtained raw materials and simple equipment, and can meet the industrial production.
Description
Technical Field
The invention relates to the technical field of diamond surface treatment, in particular to a diamond etching method for a surface nano pore canal.
Background
Diamond has been widely used in precision manufacturing due to its special mechanical properties such as high hardness, high wear resistance and the ability to have extremely sharp cutting edges. In addition, the unique three-dimensional skeleton structure of diamond makes it show excellent properties in other fields such as heat, electricity and optics. However, since diamond surfaces are smooth and very inert, it is difficult to bond with other materials. In order to improve the functionality of diamond and increase its applicability in other related fields, extensive research is being conducted on the surface modification of diamond. The application of the diamond surface etching technology can increase the surface roughness of the diamond crystal and facilitate the combination of diamond and other materials.
3. The main methods of the current domestic diamond surface etching technology include plasma etching, molten salt etching, gas phase etching, solid phase etching, gas-solid phase mixed etching and the like. The plasma etching is mainly reactive ion etching, and the purpose of etching is achieved by utilizing high-energy active particle ion beams to bombard the atoms on the surface of the diamond and simultaneously reacting with the atoms on the surface layer of the diamond. The molten salt etching of diamond is realized by utilizing molten ionic compound to carry out oxidation-reduction reaction with carbon atoms on the surface of diamond. The gas phase etching is to chemically etch diamond by oxidation-reduction reaction of water vapor, hydrogen and oxygen gas at high temperature. The method has the advantages of low cost, simple process, no need of reprocessing the diamond after etching, high cleanliness of the obtained diamond surface and the like. The solid phase etching of diamond is the reverse process of the diamond synthesis process, and mainly uses the diamond in a thermodynamically unstable state under the conditions of high temperature and low pressure, and metals such as iron, cobalt, nickel and the like are not only catalysts for the mutual transformation of diamond and graphite, but also good solvents of carbon, and can dissolve graphite generated on the surface layer of the diamond, thereby causing the surface etching of the diamond. The gas-solid phase mixed etching is to utilize gas capable of reacting with carbon to etch the diamond surface under the catalysis of a metal catalyst.
Currently, the diamond etchant is used as a metal simple substance, a metal oxide, a metal salt and the like, wherein the metal simple substance comprises catalysts of iron, cobalt, nickel, cobalt, niobium, molybdenum, tungsten and the like, the metal oxide comprises transition metal oxide, main group metal oxide and the like, and the metal salt comprises strong oxidizing salts of potassium nitrate, sodium nitrate, potassium chlorate, sodium perchlorate and the like. The metal simple substance such as iron, cobalt, nickel and other catalysts are used as the traditional etchant, so that the research is more mature, and the etching effect is better. And under the reducing atmosphere of hydrogen and the like, the nano-scale metal particles etch the surface of the diamond, so that uniform nano holes can be obtained. The existence of the nano pore canal can greatly increase the specific surface area of diamond, and provides a foundation for preparing high-performance diamond composite materials (diamond metal base, diamond resin base and diamond ceramic base).
Disclosure of Invention
The purpose of the invention is that: a diamond etching method for surface nano-pore canal is provided.
The invention is realized by adopting the following technical scheme:
a. the diamond surface pretreatment comprises the following specific processes: 1 part of diamond is firstly subjected to acid treatment and alkali treatment to remove oil stains and other impurities on the surface, and finally is washed to be neutral by distilled water and dried for standby.
b. The preparation before diamond etching comprises the following specific processes: dilute ferric chloride (FeCl) 3 ·6H 2 O) solution was soaked on the diamond surface and then the sample was dried in a microwave oven.
c. The diamond etching process comprises the following specific steps: and (3) putting the prepared diamond sample into a tube furnace, introducing hydrogen before heating, exhausting air in the device by using the hydrogen, detecting the purity of the hydrogen in the tail gas, and heating to 700-1000 ℃ under flowing hydrogen atmosphere, wherein the heat preservation time is 50-150 min. After the reaction is completed, heating is stopped, and hydrogen is continuously introduced until the device is cooled to room temperature.
d. The diamond treatment after etching comprises the following specific processes: and (3) placing the etched diamond sample into hydrochloric acid with the mass fraction of 10% for cleaning, oscillating for 10-15 min by using ultrasonic waves, washing to be neutral by using distilled water after oscillating, and drying to obtain the diamond with the surface of the nano pore canal.
The acid treatment in step a of the invention preferably comprises the following steps: the diamond is put into a dilute hydrochloric acid solution with the mass fraction of 10% to 30% and is boiled for 10 minutes to 50 minutes and then washed.
In the invention, the alkali treatment in the step a preferably comprises the following steps: the diamond after the acid treatment is put into NaOH solution with the mass fraction of 10% to 30% and is boiled for 10 minutes to 50 minutes for cleaning.
The diamond particle size range described in the present invention is 300 μm to 600 μm, most preferably 400 μm.
The beneficial effects of the invention are as follows:
the method is low in cost, quick and effective, and can obtain the pyramid-shaped nano pore canal with the production size as low as 15nm without any electron beam lithography.
The highly porous nano pore canal greatly increases the specific surface area of diamond, can greatly strengthen the holding force of diamond and a bonding agent, and prolongs the service life of the diamond grinding tool.
The etching process is simple, the raw materials are rich and the cost is low, and the industrial production can be satisfied.
Detailed Description
The invention is further described below in connection with specific embodiments:
example 1:
a. 2g of 400 mu m diamond is respectively put into 50ml of 30% hydrochloric acid solution by mass fraction for 30 minutes and then washed, then added into 50ml of 30% sodium hydroxide solution by mass fraction for 20 minutes and then washed, and finally washed with absolute ethyl alcohol and distilled water and dried for standby.
b. Ferric chloride (FeCl) with concentration of 20% 3 ·6H 2 O) the solution wets the diamond surface obtained in step a, and then the sample is dried in a microwave oven for 2min.
c. And c, placing the diamond obtained in the step b in a tube furnace, introducing hydrogen before heating, exhausting air in the device by using the hydrogen, detecting the purity of the hydrogen in the tail gas, and heating to 700 ℃ at a speed of 5 ℃/min under the flowing hydrogen atmosphere, wherein the heat preservation time is 50min. After the reaction is completed, heating is stopped, and hydrogen is continuously introduced until the device is cooled to room temperature.
d. And c, cleaning the product obtained in the step c in hydrochloric acid with the mass fraction of 10%, oscillating for 15min by using ultrasonic waves, washing to be neutral by using distilled water after oscillating, and drying to obtain the diamond with the surface of the nano pore canal.
Example 2:
a. 2g of 400 mu m diamond is respectively put into 50ml of 30% hydrochloric acid solution by mass fraction for 30 minutes and then washed, then added into 50ml of 30% sodium hydroxide solution by mass fraction for 20 minutes and then washed, and finally washed with absolute ethyl alcohol and distilled water and dried for standby.
b. Ferric chloride (FeCl) with concentration of 20% 3 ·6H 2 O) the solution wets the diamond surface obtained in step a, and then the sample is dried in a microwave oven for 2min.
c. And c, placing the diamond obtained in the step b in a tube furnace, introducing hydrogen before heating, exhausting air in the device by using the hydrogen, detecting the purity of the hydrogen in the tail gas, and heating to 850 ℃ at a speed of 5 ℃/min under the flowing hydrogen atmosphere, wherein the heat preservation time is 100min. After the reaction is completed, heating is stopped, and hydrogen is continuously introduced until the device is cooled to room temperature.
d. And c, cleaning the product obtained in the step c in hydrochloric acid with the mass fraction of 10%, oscillating for 15min by using ultrasonic waves, washing to be neutral by using distilled water after oscillating, and drying to obtain the diamond with the surface of the nano pore canal.
Example 3:
a. 2g of 400 mu m diamond is respectively put into 50ml of 30% hydrochloric acid solution by mass fraction for 30 minutes and then washed, then added into 50ml of 30% sodium hydroxide solution by mass fraction for 20 minutes and then washed, and finally washed with absolute ethyl alcohol and distilled water and dried for standby.
b. Ferric chloride (FeCl) with concentration of 20% 3 ·6H 2 O) wetting the diamond surface obtained in step a with a solution,the sample was then dried in a microwave oven for 2min.
c. And c, placing the diamond obtained in the step b in a tube furnace, introducing hydrogen before heating, exhausting air in the device by using the hydrogen, detecting the purity of the hydrogen in the tail gas, and heating to 1000 ℃ at a speed of 5 ℃/min under the flowing hydrogen atmosphere, wherein the heat preservation time is 150min. After the reaction is completed, heating is stopped, and hydrogen is continuously introduced until the device is cooled to room temperature.
d. And c, cleaning the product obtained in the step c in hydrochloric acid with the mass fraction of 10%, oscillating for 15min by using ultrasonic waves, washing to be neutral by using distilled water after oscillating, and drying to obtain the diamond with the surface of the nano pore canal.
Claims (2)
1. The etching method of the perforated diamond is characterized by comprising the following steps:
a. the diamond surface pretreatment comprises the following specific processes: firstly, carrying out acid treatment and alkali treatment on diamond to remove oil stains and other impurities on the surface, and finally, washing the diamond to be neutral by distilled water and drying the diamond for later use;
b. the preparation before diamond etching comprises the following specific processes: soaking diluted ferric chloride solution on the surface of diamond, and then placing the sample into a microwave oven for drying;
c. the diamond etching process comprises the following specific steps: putting the prepared diamond sample into a tube furnace, introducing hydrogen before heating, exhausting air in the device by using the hydrogen, heating to 700-1000 ℃ under flowing hydrogen atmosphere after detecting the purity of the hydrogen in the tail gas, keeping the temperature for 50-150 min, stopping heating after the reaction is finished, and continuing introducing the hydrogen until the device is cooled to room temperature;
d. the diamond treatment after etching comprises the following specific processes: and (3) placing the etched diamond sample into hydrochloric acid with the mass fraction of 10% for cleaning, oscillating for 10-15 min by using ultrasonic waves, washing with distilled water to be neutral after oscillating, and drying to obtain the diamond with the surface of the nano pore canal.
2. The etching method according to claim 1, characterized in that: the diamond particle size range is 300-600 mu m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210239887.4A CN114572979B (en) | 2022-03-12 | 2022-03-12 | Diamond etching method of surface nano pore canal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210239887.4A CN114572979B (en) | 2022-03-12 | 2022-03-12 | Diamond etching method of surface nano pore canal |
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| Publication Number | Publication Date |
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| CN114572979A CN114572979A (en) | 2022-06-03 |
| CN114572979B true CN114572979B (en) | 2024-01-26 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106925775A (en) * | 2017-04-17 | 2017-07-07 | 河南工业大学 | A kind of method of diadust plated surface chromium carbide |
| CN107473768A (en) * | 2017-08-10 | 2017-12-15 | 中南钻石有限公司 | A kind of diamond surface is roughened processing method |
| CN110540200A (en) * | 2019-09-11 | 2019-12-06 | 河南工业大学 | method for etching diamond (100) surface in high orientation |
| CN113308745A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of perforated diamond |
-
2022
- 2022-03-12 CN CN202210239887.4A patent/CN114572979B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106925775A (en) * | 2017-04-17 | 2017-07-07 | 河南工业大学 | A kind of method of diadust plated surface chromium carbide |
| CN107473768A (en) * | 2017-08-10 | 2017-12-15 | 中南钻石有限公司 | A kind of diamond surface is roughened processing method |
| CN110540200A (en) * | 2019-09-11 | 2019-12-06 | 河南工业大学 | method for etching diamond (100) surface in high orientation |
| CN113308745A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of perforated diamond |
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| CN114572979A (en) | 2022-06-03 |
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