CN104073834A - Preparation method of nanometer diamond-like powder - Google Patents
Preparation method of nanometer diamond-like powder Download PDFInfo
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- CN104073834A CN104073834A CN201310097289.9A CN201310097289A CN104073834A CN 104073834 A CN104073834 A CN 104073834A CN 201310097289 A CN201310097289 A CN 201310097289A CN 104073834 A CN104073834 A CN 104073834A
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- diamond
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- electrolytic solution
- sodium
- nanometer diamond
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- 239000000843 powder Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 239000010959 steel Substances 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 235000013312 flour Nutrition 0.000 claims description 14
- 239000004575 stone Substances 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000703 high-speed centrifugation Methods 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005238 degreasing Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 229910003460 diamond Inorganic materials 0.000 abstract description 15
- 239000010432 diamond Substances 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 8
- 238000010891 electric arc Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000012254 powdered material Substances 0.000 description 6
- 244000137852 Petrea volubilis Species 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- 229910000975 Carbon steel Inorganic materials 0.000 description 3
- 239000010962 carbon steel Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- -1 opticglass Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention provides a method for preparing nanometer diamond-like powder by using cathodic micro-arc discharge phenomenon, and belongs to the technical field of preparation of nanometer materials. Steel serving as cathode and graphite serving as anode are dipped in a specific electrolyte solution; and the electrolyte comprises the following components in percentage by mass: 45-65% of glycerinum, 10-20% of methanol, 5-10% of sodium carbonate, 5-10% of sodium hydroxide, 3-5% of sodium chloride, and 10-20% of de-ionized water. 200-500 V of voltage is applied between the two electrodes at room temperature; the micro-arc discharge is generated on the surface of the cathode; the discharge processing time is 30 minutes; and then, turbid liquid containing diamond-like particles is obtained. The turbid liquid is separated by using a high-speed centrifuge; the alcohol cleaning and the drying are performed on separated powder repeatedly; and finally, the nanometer diamond-like powder is prepared. The nanometer diamond-like powder, prepared by the method, has the advantages of high purity, small particle size, good uniformity and low production cost, and can be applied to such products as abrasive paste, polishing agent and metallographic abrasive papers as a substitute for the diamond powder.
Description
Technical field
The invention belongs to technical field prepared by nano material, a kind of method of utilizing cathode micro arc electric discharge to prepare nanometer quasi-diamond powdered material in electrolytic solution is particularly provided.
Background technology
Quasi-diamond is the amorphous metastable state carbon material by decolorizing carbon and diamond phase composite, and it forms the novel material into people's primary study owing to having excellent machinery, electricity, acoustics, optics, calorifics, chemical property and good biocompatibility.Nanometer diamond-like stone flour has mechanics and the chemical property of similar diamond particles, can in multiple application, substitute diamond components, to reduce the production cost of diamond composition.It not only can prepare senior lapping paste and rumbling compound, and can also be used for retrofit quartz, opticglass, semi-conductor, metal and alloy surface, can effectively improve working accuracy.Because nano level diamond-like stone flour has very large specific surface area, contain kinds of surface functional group, available its preparation catalyzer, promotes reacting to each other of organic compound simultaneously.But the quasi-diamond powdered material ubiquity granularity problem such as film forming, preparation cost height of greatly, easily reuniting, has limited its development and application.There is bibliographical information, under strong magnetic field action, taking Nanoscale Iron as catalyzer, carbon black is carbon source, at normal pressure and 1100 DEG C, be incubated 100min and prepared nanometer diamond-like stone flour and the coated new diamond nano particle (Wen Bin of graphite, Li Tingju, Zhang Xingguo, Dong Chuan, Yao Shan, Cao Zhiqiang. high-intensity magnetic field catalysis method of carbon black is prepared the new bortz powder of nanometer. chemical journal, 2004,62 (23): 2361-2364), but the method needs high temperature and strong magnetic field circumstance, and length consuming time, preparation cost is high, is unfavorable for batch production.In recent years, the method of utilizing electric discharge phenomena in the aqueous solution to prepare nano-carbon material is subject to people's attention, patent 200610137895.9 discloses a kind of method of utilizing micro discharge of cathodic gaseous envelope to prepare carbon fullerene, carbon nanofiber and metallic surface diamond like carbon film, but the method for utilizing cathode micro arc discharge technology to prepare nanometer quasi-diamond powdered material there is not yet report.
The present invention adopts cathode micro arc discharge technology in specific electrolytic solution, to prepare nanometer diamond-like stone flour, and prepared powder has that purity is high, particle diameter is tiny and narrowly distributing, the feature of good uniformity.The method is using iron and steel as negative electrode, graphite is as anode, between two electrodes, apply certain voltage, heating effect of current gasifies rapidly near solution steel surface, forms the gas film of one deck encirclement negative electrode, and the further rising of voltage will make gas film puncture, near negative electrode, produce plasma sheath, and being attended by arc discharge, region of discharge produces local High Temperature High Pressure, has formed the synthetic environment of quasi-diamond.The organic components such as glycerine, methyl alcohol in electrolytic solution is decomposed in discharge process, produces carbon, hydrogen, oxygen isoreactivity particle.Under the katalysis of iron, between the active particle of High Temperature High Pressure region of discharge, form diamond-like carbon bunch by violent crash response, and be dispersed in solution, reacted solution can be obtained to the diamond-like stone flour that granularity is less than 100 nanometers after by high speed centrifugation separating treatment.
In electrolytic solution, micro-arc discharge technology, because operation is simple, cost is low, without vacuum or hot conditions, can effectively solve the bottleneck problem of restriction quasi-diamond powdered material development.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of quasi-diamond nano-powder material, is characterized in that, the preparation method of described nanometer quasi-diamond powdered material is the technology based on cathode micro arc discharge generation plasma body in specific electrolytic solution.Concrete technology flow process is as follows:
Step 1, the preparation cathode micro arc electrolytic solution used that discharges, each component is calculated by mass percentage: glycerine 45-65%, methyl alcohol 10-20%, sodium carbonate 5-10%, sodium hydroxide 5-10%, sodium-chlor 3-5%, deionized water 10-20%.
Step 2, ferrous materials is carried out to pre-treatment, with 360
#-1500
#sand paper is polished to steel surface, then cleans and remove surface and oil contaminant with alcohol, afterwards sample is dried.
Step 3, using pretreated ferrous materials as negative electrode, graphite is anode, is immersed in and fills in the electrolyzer of preparing electrolytic solution, applies 200V-500V voltage under room temperature condition between two electrodes, the treatment time is 30min;
Step 4, electric discharge finish rear electrolytic solution to be carried out to high speed centrifugation separation, and centrifuge speed is 12000r/min, finally isolated powder are carried out to alcohol cleans and drying and processing 3-5 time, prepare nanometer diamond-like stone flour, and its mean particle size is less than 100 nanometers.
Feature of the present invention is: (1) electrolytic solution solute used wide material sources, do not produce obnoxious flavour, cleanliness without any pollution in discharge process; (2) whole treating processes is carried out under normal temperature, atmospheric environment, and cost of equipment maintenance is low and operation simple, repeatability is strong, production efficiency is high; (3) prepared powdered material purity is high, particle diameter is tiny and narrowly distributing, good uniformity, can be used for preparing senior lapping paste, rumbling compound, catalyzer, for retrofit or add other materials to and form matrix material, to improve wear-resisting, the corrosion resisting property of material.
Brief description of the drawings
Figure of description 1 is the nanometer diamond-like stone flour stereoscan photograph of preparing with the present invention.
Embodiment
According to electrolyte system of the present invention and process flow, provide following examples:
Embodiment 1
Using T8 carbon steel as negative electrode, graphite is anode, first uses sand paper (360
#-1500
#) to the polish pre-treatment use alcohol degreasing of steel surface.Then prepare electrolytic solution: glycerine 720ml, methyl alcohol 510ml, sodium carbonate 100g, sodium hydroxide 100g, sodium-chlor 100g, deionized water 400ml, is immersed in two electrodes in the electrolyzer that fills above-mentioned electrolytic solution, and applies 360V voltage, and the treatment time is 30min.After processing finishes, solution is carried out to high speed centrifugation separation, centrifuge speed is 12000r/min, finally isolated powder is repeatedly cleaned and is dried 3 times with alcohol, can obtain nanometer diamond-like stone flour.
Embodiment 2
Using T8 carbon steel as negative electrode, graphite is anode, first uses sand paper (360
#-1500
#) to the polish pre-treatment use alcohol degreasing of steel surface.Then prepare electrolytic solution: glycerine 870ml, methyl alcohol 380ml, sodium carbonate 100g, sodium hydroxide 100g, sodium-chlor 100g, deionized water 300ml, is immersed in two electrodes in the electrolyzer that fills above-mentioned electrolytic solution, and applies 400V voltage, and the treatment time is 30min.After processing finishes, solution is carried out to high speed centrifugation separation, centrifuge speed is 12000r/min, finally isolated powder is repeatedly cleaned and is dried 3 times with alcohol, can obtain nanometer diamond-like stone flour.
Embodiment 3
Using T8 carbon steel as negative electrode, graphite is anode, first uses sand paper (360
#-1500
#) to the polish pre-treatment use alcohol degreasing of steel surface.Then prepare electrolytic solution: glycerine 1030ml, methyl alcohol 250ml, sodium carbonate 100g, sodium hydroxide 100g, sodium-chlor 100g, deionized water 200ml, is immersed in two electrodes in the electrolyzer that fills above-mentioned electrolytic solution, and applies 440V voltage, and the treatment time is 30min.After processing finishes, solution is carried out to high speed centrifugation separation, centrifuge speed is 12000r/min, finally isolated powder is repeatedly cleaned and is dried 3 times with alcohol, can obtain nanometer diamond-like stone flour.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (3)
1. for the preparation of an electrolytic solution for nanometer diamond-like stone flour, it is characterized in that, described electrolytic solution is the aqueous solution that contains glycerine, methyl alcohol, sodium carbonate, sodium hydroxide and sodium-chlor.
2. for electrolytic solution claimed in claim 1, it is characterized in that, each component is respectively by mass percentage: glycerine 45-65%, methyl alcohol 10-20%, sodium carbonate 5-10%, sodium hydroxide 5-10%, sodium-chlor 3-5%, deionized water 10-20%.
3.. a method of preparing nanometer diamond-like stone flour, is characterized in that, the method comprises the following steps:
Step 1, prepare electrolytic solution claimed in claim 2;
Step 2, iron and steel cathode material is carried out to surface preparation, comprise that sand papering and alcohol clean degreasing;
Step 3, using pretreated ferrous materials as negative electrode, graphite is anode, is immersed in the electrolyzer that fills electrolytic solution described in claim 2, applies 200V-500V voltage under room temperature condition between two electrodes, the treatment time is 30min;
Step 4, solution after processing is finished carry out high speed centrifugation separation, then isolated powder are carried out to alcohol cleans and drying and processing 3-5 time, prepare nanometer diamond-like stone flour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310097289.9A CN104073834B (en) | 2013-03-26 | 2013-03-26 | Preparation method of nanometer diamond-like powder |
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|---|---|---|---|
| CN201310097289.9A CN104073834B (en) | 2013-03-26 | 2013-03-26 | Preparation method of nanometer diamond-like powder |
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| Publication Number | Publication Date |
|---|---|
| CN104073834A true CN104073834A (en) | 2014-10-01 |
| CN104073834B CN104073834B (en) | 2017-01-18 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191902A (en) * | 2016-07-28 | 2016-12-07 | 北京科技大学 | A kind of method preparing hydrogen doping oxide ceramics micro Nano material |
| CN109504996A (en) * | 2017-09-14 | 2019-03-22 | 北京师范大学 | A kind of cathode micro arc oxidation solution and method for steel surface DLC combined oxidation film preparation |
| CN113004576A (en) * | 2021-02-20 | 2021-06-22 | 安徽瑞邦橡塑助剂集团有限公司 | Preparation method of supported nano zinc oxide |
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| CN1962431A (en) * | 2006-11-09 | 2007-05-16 | 北京科技大学 | Cathode gas film microarc discharging method for preparing carbon nanometer material in solution |
| CN102732851A (en) * | 2011-03-30 | 2012-10-17 | 陈伟 | Method for preparing diamond-like carbon film by pulsed discharge deposition |
-
2013
- 2013-03-26 CN CN201310097289.9A patent/CN104073834B/en not_active Expired - Fee Related
Patent Citations (2)
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| CN1962431A (en) * | 2006-11-09 | 2007-05-16 | 北京科技大学 | Cathode gas film microarc discharging method for preparing carbon nanometer material in solution |
| CN102732851A (en) * | 2011-03-30 | 2012-10-17 | 陈伟 | Method for preparing diamond-like carbon film by pulsed discharge deposition |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191902A (en) * | 2016-07-28 | 2016-12-07 | 北京科技大学 | A kind of method preparing hydrogen doping oxide ceramics micro Nano material |
| CN109504996A (en) * | 2017-09-14 | 2019-03-22 | 北京师范大学 | A kind of cathode micro arc oxidation solution and method for steel surface DLC combined oxidation film preparation |
| CN109504996B (en) * | 2017-09-14 | 2020-09-29 | 北京师范大学 | Cathode micro-arc oxidation solution and method for preparing DLC composite oxide film on steel surface |
| CN113004576A (en) * | 2021-02-20 | 2021-06-22 | 安徽瑞邦橡塑助剂集团有限公司 | Preparation method of supported nano zinc oxide |
| CN113004576B (en) * | 2021-02-20 | 2021-09-07 | 安徽瑞邦橡塑助剂集团有限公司 | Preparation method of supported nano zinc oxide |
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