CN104073834B - Preparation method of nanometer diamond-like powder - Google Patents
Preparation method of nanometer diamond-like powder Download PDFInfo
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- CN104073834B CN104073834B CN201310097289.9A CN201310097289A CN104073834B CN 104073834 B CN104073834 B CN 104073834B CN 201310097289 A CN201310097289 A CN 201310097289A CN 104073834 B CN104073834 B CN 104073834B
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- 239000000843 powder Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003792 electrolyte Substances 0.000 claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 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
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000004575 stone Substances 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005868 electrolysis reaction 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
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000010406 cathode material Substances 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910003460 diamond Inorganic materials 0.000 abstract description 14
- 239000010432 diamond Substances 0.000 abstract description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 8
- 238000010891 electric arc Methods 0.000 abstract description 6
- 238000005498 polishing Methods 0.000 abstract description 6
- 239000011780 sodium chloride Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 244000137852 Petrea volubilis Species 0.000 description 4
- 229910000975 Carbon steel Inorganic materials 0.000 description 3
- 239000010962 carbon steel Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000126 substance 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
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 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
- 150000001875 compounds Chemical class 0.000 description 1
- 235000009508 confectionery Nutrition 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
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 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
- 238000009413 insulation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 239000005304 optical glass Substances 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
- -1 quasiconductor Substances 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 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 the technical field of nano material preparation, in particular, provide one kind and discharged in electricity using cathode micro arc
The method preparing nanometer diamond like carbon dusty material in solution liquid.
Background technology
Diamond like carbon is that it is excellent due to having by the amorphous metastable state material with carbon element of amorphous carbon and diamond phase composition
Machinery, electricity, acoustics, optics, calorifics, chemical characteristic and good biocompatibility and become the green wood of people's primary study
Material.Nanometer diamond-like stone powder has mechanics and the chemical property of similar diamond particles, can substitute Buddha's warrior attendant in numerous applications
Stone composition, to reduce the production cost of diamond composition.It not only can prepare senior abrasive pastes and polishing agent, and can also use
In retrofit quartz, optical glass, quasiconductor, metal and alloy surface, machining accuracy can be effectively improved.Simultaneously because nanometer
The diamond-like stone powder of level has very big specific surface area, containing kinds of surface functional group, can use it to prepare catalyst, promotes organic
The reacting to each other of compound.But, diamond like carbon dusty material generally existing granularity is big, easily reunion film forming, preparation cost height etc.
Problem, limits its development and applies.There is document report, under strong magnetic field action, with Nanoscale Iron as catalyst, carbon black is carbon
Source, at normal pressure and 1100 DEG C, insulation 100min has prepared nanometer diamond-like stone powder and the new diamond nano-particles of graphite coat
(Wen Bin, Li Tingju, Zhang Xingguo, Dong Chuan, Yao Shan, Cao Zhiqiang. high-intensity magnetic field catalysis method of carbon black prepares the new bortz powder of nanometer. chemistry
Journal, 2004,62 (23): 2361-2364), but the method needs high temperature and strong magnetic field circumstance, and time-consuming, preparation cost is high,
It is unfavorable for producing in batches.In recent years, it is subject to the weight of people using the method that the electric discharge phenomena in aqueous solution prepare nano-carbon material
Depending on, patent 200610137895.9 disclose a kind of using micro discharge of cathodic gaseous envelope prepare carbon fullerene, carbon nano-fiber with
And the method for metal surface diamond like carbon film, but prepare nanometer diamond like carbon dusty material using cathode micro arc discharge technology
Method there is not been reported.
The present invention prepares a nanometer diamond-like stone powder, prepared powder using cathode micro arc discharge technology in specific electrolyte
End has that purity is high, particle diameter is tiny and narrowly distributing, the good feature of uniformity.The method is as negative electrode, graphite conduct using iron and steel
Anode, applies certain voltage between electrodes, and heating effect of current makes the solution near steel surface gasify rapidly, forms one
Layer surrounds the gas film of negative electrode, and voltage raises further will make gas film puncture, and produce plasma sheath near negative electrode, and
With arc discharge, region of discharge produces the High Temperature High Pressure of local, defines the synthetic environment of diamond like carbon.Sweet in electrolyte
The organic components such as oil, methanol are decomposed in discharge process, produce carbon, hydrogen, oxygen isoreactivity particle.Catalytic action in ferrum
Under, pass through violent crash response between the active particle of High Temperature High Pressure region of discharge and form diamond-like-carbon cluster, and be dispersed in molten
In liquid, can obtain, after reacted solution is processed by being centrifuged at a high speed, the diamond-like stone powder that granularity is less than 100 nanometers.
In electrolyte micro-arc discharge technology because operation is simple, low cost, without vacuum or hot conditionss, can effectively solving
The bottleneck problem of restriction diamond like carbon dusty material development.
Content of the invention
It is an object of the invention to provide a kind of preparation method of diamond like carbon nano-powder material is it is characterised in that described
The preparation method of nanometer diamond like carbon dusty material is the skill producing plasma based on cathode micro arc electric discharge in specific electrolyte
Art.Concrete technology flow process is as follows:
Step one, preparation cathode micro arc electric discharge electrolyte used, each component is calculated by mass percentage: glycerol 45-
65%, methanol 10-20%, sodium carbonate 5-10%, sodium hydroxide 5-10%, sodium chloride 3-5%, deionized water 10-20%.
Step 2, pretreatment is carried out to ferrous materials, use 360#-1500#Sand paper is polished to steel surface, then uses wine
Seminal plasma washes away except surface and oil contaminant, dries sample afterwards.
Step 3, using pretreated ferrous materials as negative electrode, graphite is anode, is immersed in fill and prepares electrolyte
Electrolysis bath in, under room temperature condition between two electrodes apply 200v-500v voltage, process time be 30min；
Step 4, electric discharge are centrifuged at a high speed to electrolyte after terminating, and centrifuge speed is 12000r/min, finally
The powder isolated is carried out with alcohol washes and drying and processing 3-5 time, prepares a nanometer diamond-like stone powder, its particle mean size is less than
100 nanometers.
Present invention is characterized in that electrolyte solute wide material sources used by (1), in discharge process, do not produce harmful gass,
Cleanliness without any pollution；(2) whole processing procedure is carried out under room temperature, atmospheric environment, and cost of equipment maintenance is low and operation is simple, can weigh
Renaturation is strong, production efficiency is high；(3) the dusty material purity prepared by is high, particle diameter is tiny and narrowly distributing, and uniformity is good, permissible
It is used for preparing senior abrasive pastes, polishing agent, catalyst, for retrofit or be added in other materials formation composite,
To improve wear-resisting, the corrosion resisting property of material.
Brief description
Figure of description 1 is the nanometer diamond-like stone powder stereoscan photograph prepared with the present invention.
Specific 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, uses sand paper (360 first#-1500#) pre- place of polishing is carried out to steel surface
Manage and use ethanol degreasing.Then prepare electrolyte: glycerol 720ml, methanol 510ml, sodium carbonate 100g, sodium hydroxide 100g,
Sodium chloride 100g, deionized water 400ml, two electrodes are immersed in the electrolysis bath filling above-mentioned electrolyte, and apply 360v voltage,
Process time is 30min.After process terminates, solution is centrifuged at a high speed, centrifuge speed is 12000r/min, finally
The powder ethanol isolated is cleaned repeatedly and dries 3 times, you can obtain a nanometer diamond-like stone powder.
Embodiment 2
Using t8 carbon steel as negative electrode, graphite is anode, uses sand paper (360 first#-1500#) pre- place of polishing is carried out to steel surface
Manage and use ethanol degreasing.Then prepare electrolyte: glycerol 870ml, methanol 380ml, sodium carbonate 100g, sodium hydroxide 100g,
Sodium chloride 100g, deionized water 300ml, two electrodes are immersed in the electrolysis bath filling above-mentioned electrolyte, and apply 400v voltage,
Process time is 30min.After process terminates, solution is centrifuged at a high speed, centrifuge speed is 12000r/min, finally
The powder ethanol isolated is cleaned repeatedly and dries 3 times, you can obtain a nanometer diamond-like stone powder.
Embodiment 3
Using t8 carbon steel as negative electrode, graphite is anode, uses sand paper (360 first#-1500#) pre- place of polishing is carried out to steel surface
Manage and use ethanol degreasing.Then prepare electrolyte: glycerol 1030ml, methanol 250ml, sodium carbonate 100g, sodium hydroxide 100g,
Sodium chloride 100g, deionized water 200ml, two electrodes are immersed in the electrolysis bath filling above-mentioned electrolyte, and apply 440v voltage,
Process time is 30min.After process terminates, solution is centrifuged at a high speed, centrifuge speed is 12000r/min, finally
The powder ethanol isolated is cleaned repeatedly and dries 3 times, you can obtain a nanometer diamond-like stone powder.
Above-described embodiment only technology design to illustrate the invention and feature, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implements according to this, can not be limited the scope of the invention with this.All according to the present invention
Equivalence changes or modification that spirit is made, all should be included within the scope of the present invention.
Claims (2)
1. a kind of electrolyte for preparing nanometer diamond-like stone powder is it is characterised in that the content of each component of described electrolyte is pressed
Percentage by weight calculates and is respectively as follows: glycerol 45-65%, methanol 10-20%, sodium carbonate 5-10%, sodium hydroxide 5-10%, chlorination
Sodium 3-5%, deionized water 10-20%.
2. a kind of nanometer method of diamond-like stone powder of preparing is it is characterised in that the method comprises the following steps:
Electrolyte described in step one, preparation claim 1；
Step 2, surface preparation is carried out to iron and steel cathode material, including sand papering and alcohol washes degreasing；
Step 3, using pretreated ferrous materials as negative electrode, graphite is anode, is immersed in and fills electricity described in claim 1
In the electrolysis bath of solution liquid, between two electrodes, under room temperature condition, apply 200-500v DC voltage, process time is 30min；
Step 4, process is terminated after solution be centrifuged at a high speed, then alcohol washes are carried out to the powder isolated
With drying and processing 3-5 time, prepare a nanometer diamond-like stone 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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| CN104073834A CN104073834A (en) | 2014-10-01 |
| CN104073834B true CN104073834B (en) | 2017-01-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106191902B (en) * | 2016-07-28 | 2018-11-27 | 北京科技大学 | A method of preparing hydrogen doping oxide ceramics micro Nano material |
| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| 强磁场碳黑催化法制备纳米新金刚石粉;温斌等;《化学学报》;20041231;第62卷(第23期);第2361-2364页 * |
| 液相电化学沉积类金刚石薄膜的研究进展;郭静等;《化学通报》;20071231(第7期);第521-526页 * |
| 阴极微弧电沉积表面处理钛的高温氧化行为;薛文斌等;《材料热处理学报》;20100930;第31卷(第9期);第124-127、132页 * |
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