CN102002264A - Preparation method of nano-diamond aqueous dispersion - Google Patents
Preparation method of nano-diamond aqueous dispersion Download PDFInfo
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- CN102002264A CN102002264A CN2010102898800A CN201010289880A CN102002264A CN 102002264 A CN102002264 A CN 102002264A CN 2010102898800 A CN2010102898800 A CN 2010102898800A CN 201010289880 A CN201010289880 A CN 201010289880A CN 102002264 A CN102002264 A CN 102002264A
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 56
- 239000006185 dispersion Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- -1 polypropylene Polymers 0.000 claims abstract description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 239000013543 active substance Substances 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 5
- PWJNDVAKQLOWRZ-UHFFFAOYSA-N 1-hydroxynaphthalene-2-sulfonic acid Chemical compound C1=CC=C2C(O)=C(S(O)(=O)=O)C=CC2=C1 PWJNDVAKQLOWRZ-UHFFFAOYSA-N 0.000 claims description 4
- 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 description 4
- 239000002253 acid Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000003945 anionic surfactant Substances 0.000 claims description 4
- 239000007859 condensation product Substances 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229960002050 hydrofluoric acid Drugs 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 13
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000002783 friction material Substances 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 2
- 239000004094 surface-active agent Substances 0.000 abstract 2
- 239000004743 Polypropylene Substances 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 229920001155 polypropylene Polymers 0.000 abstract 1
- 239000011257 shell material Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 20
- 239000002105 nanoparticle Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000004677 Nylon Substances 0.000 description 6
- 229920001778 nylon Polymers 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000005411 Van der Waals force Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 241000212978 Amorpha <angiosperm> Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a nano-diamond water dispersion, which comprises the steps of pretreating original nano-diamond, treating the surface of the nano-diamond and dispersing, purifying and acidifying the original nano-diamond, adding a dispersing agent and a surfactant during ball milling treatment to disperse the pretreated nano-diamond, and dispersing the modified nano-diamond in a water system by using the dispersing agent and the surfactant to obtain the nano-diamond water dispersion system which is uniform and stable, good in dispersity, stable for a long time, small in particle size and narrow in particle size distribution. The aqueous dispersion of nano-diamond prepared by the method can be used for blending with modified polypropylene polymer and applied to bearing friction materials or plastic shell materials.
Description
Technical field
The present invention relates to a kind of preparation method of Nano diamond water dispersion.
Background technology
Diamond is the new function material of the heat that integrates excellent, light, sound, electromagnetism, chemical property.It has the highest hardness, the fastest compressional wave velocity of sound, the wideest transparent scope, maximum Young's modulus, the highest thermal conductivity, best chemical stability and the consistency that coexists with other material.
Nano diamond is the newcomer of nano material circle, and it not only has the comprehensive excellent properties of diamond institute inherent, but also has the unusual characteristic of nano material.The applied research of Nano diamond still is in the starting stage, but experimental results show that Nano diamond has won initial success and formed certain industrial scale in the application of some traditional field.
The Nano diamond that uses the explosion method synthetic is as nano material, because its hardness height, granularity is little, specific surface area is big, can be filled in the macromolecular material, is used for improving its performance.And the functional group of the high activity of nano grain surface and absorption and chemical bond connection, make particle be not limited only to the rigid particles effect, also have the effect that forms chemical bond with matrix.But Nano diamond is of a size of 1-100nm, belong to the superfine powder particle, have great specific surface area and higher surface energy, surface lacks contiguous ligating atom, cause particle surface to have a large amount of unsaturated link(age)s, has very high surfactivity, be in thermodynamics utmost point unsteady state, very easily produce spontaneous agglomeration each other.Add the factors such as surface tension of solvent in intergranular Van der Waals force, electrostatic force and the suspension, make it in preparation and last handling process, interparticle reunion take place very easily, make particle diameter become big, form second particle, the final peculiar function that loses ultra-fine grain in use and possessed, thus giving full play to of superfine powder advantage hindered greatly.This is the problem of a general character existing in the application of Nano diamond and all nano materials.
In the material field, material evenly particularly important, certain element (material) degree of scatter in the material body has determined the performance and the quality of material.The homodisperse degree of the different substances of composition material is high more, and the performance of material is good more.In a word, in a lot of fields, disperse to have become and improve product (material) quality and performance, improve the indispensable and crucial technique means of process efficiency.Superfine powder is very easily reunited, and the very poor superfine powder of dispersing property is very difficult in actual use, has often lost many superiority of superfine powder, and its usefulness can not be given full play to.Can the many strangenesss of nano particle be given full play to, and depends on that to a great extent can nano particle disperse and keep the state of nanoparticle uniformly and stably in medium.In the application process of nano-powder, nano particle belongs to thermodynamic unstable system, because specific surface area is big, the surface atom number increases, Atomic coordinate deficiency, surface energy height, in different stepss such as powder preparing, drying and aftertreatments, easy formation has the size of some linkage interfaces than macro aggregate between particle.The existence of these coacervates makes that particle can not be with the nanometer grade evenly and stable dispersion, but is present in the system with the form of submicron even micron grade, and size-grade distribution is inhomogeneous, the sedimentation of poly-group takes place easily or is separated.Like this, synthetic nanometer grade powder can lose it when using should have physicals and function as nanoparticle, do not reach the purpose of the performance raising that makes material and system.
Nano diamond exists the problem of reunion equally as novel nano material, because it has high-ratio surface energy and strong surface effects, is in a kind of thermodynamic instability state, has formed firm coacervate in building-up process and subsequent treatment process.
Some conventional dispersing method, as grinding, ball milling, dispersed with stirring, ultra-sonic dispersion all is difficult to reach persistent dispersion effect to Nano diamond, can produce certain influence to subsequent applications.
All be to link to each other between the molecular chain of many macromolecular materials by Van der Waals force or hydrogen bond, reactive force is more weak each other, be easy to generate relative movement, usually have lower shearing modulus and shearing resistance as the pars amorpha between the crystalline region in the crystalline polymer material, be easy to take place deformation under external force, form smooth surface, therefore macromolecular material mostly has extremely low frictional coefficient, this is that the common metal material hardly matches, be widely used in preparing anti-friction wear-resistant spare, as sliding surface bearing, gear, machine tool guideway, slide block, piston ring etc.But surface energy and surface tension are low to be the shortcoming of macromolecular material, is difficult to produce surface adsorption with filler grain, wears no resistance, and wears away greatlyyer, and physical strength is lower, easy-cold flow, and poor thermal conductivity easily causes thermal expansion, thermal fatigue and thermal distortion.In order to overcome and to change these shortcomings, utilize weighting agents such as fiber, particle that macromolecule matrix is carried out modification, strengthen toughness reinforcing purpose to reach, effectively improve the performance of macromolecular material.But this type of method of modifying or be the mechanical property that cost improves material to sacrifice frictional behaviour, or be the frictional behaviour that cost improves material to sacrifice mechanical property, be difficult to take into account simultaneously the frictional behaviour and the mechanical property of material.Adopt nano-particles filled modification superpolymer in recent years, can utilize the toughness reinforcing characteristic of enhancing of nanoparticle on the one hand, can utilize the superhard material film of the small-size effect of nanoparticle on the other hand again, play the anti-friction wear-resistant effect at frictional interface formation nano-scale.
Summary of the invention
The purpose of this invention is to provide that a kind of to overcome in the prior art Nano diamond size-grade distribution inhomogeneous, the shortcoming that a poly-sedimentation takes place easily or be separated, have uniform and stable, the preparation method of the Nano diamond water dispersion of advantage such as good dispersity, long-term stability, particle diameter are little, narrow diameter distribution.
The object of the present invention is achieved like this:
The invention provides a kind of preparation method of Nano diamond water dispersion, original Nano diamond is purified, acidifying, adding dispersion agent and tensio-active agent when ball-milling processing will disperse through pre-treated Nano diamond, utilize dispersion agent and tensio-active agent that the Nano diamond of modification is scattered in the aqueous systems and obtain.
The preparation method of the water dispersion of above-mentioned Nano diamond comprises that wherein, original Nano diamond pre-treatment has following steps to original Nano diamond pre-treatment, Nano diamond surface treatment and dispersion treatment two big steps:
A. with original Nano diamond and strong oxidizing property acid-respons, this acid with strong oxidizing property is selected from dense H
2SO
4, dense HNO
3, KMnO
4, HClO
4One or more mixtures, wherein any acid with strong oxidizing property can account for the 25%-100% of total amount.Treatment temp is 200-300 ℃, and preferred process temperature is 240-280 ℃.Treatment step is for to be soaked in pending sample in the excessive acidic oxidation liquid, and heated and stirred, after solution becomes grey by black, solution is cooled to room temperature, and is extremely neutral with deionized water wash;
B. the product after handling through step a is handled at 50-80 ℃ with hydrofluoric acid, and the solution after handling is cooled to room temperature, and is extremely neutral with deionized water wash.
C. through 80-100 ℃ of vacuum-drying, obtain through pretreated Nano diamond.
Through pretreated Nano diamond surface treatment and dispersion treatment following steps are arranged:
D. in ball grinder, pack into the abrading-ball of 5-10 diameter 8-10mm, add aforementioned through pretreated Nano diamond 0.1-5g, add the 0.1-2g dispersion agent again in jar, drip appropriate amount of deionized water, add the 0.1-0.5g tensio-active agent again, the sealing ball grinder is put into ball mill with ball grinder, be ball milling 48 hours under the condition of 300-400rpm at rotating speed, obtain the water dispersion of Nano diamond.
Described dispersion agent is the mixture of sulfonaphthol and formaldehyde condensation products.
Described tensio-active agent is anion surfactant or nonionogenic tenside.Be advisable with anion surfactant, be selected from one or more mixture of alkyls sulfonate, alkylbenzene sulfonate or fatty acid methyl ester-α sodium sulfonate.
The invention has the beneficial effects as follows: the preparation method of a kind of Nano diamond water dispersion provided by the invention, can obtain uniform and stablely, good dispersity, particle diameter are little, the Nano diamond aqueous dispersion of narrow diameter distribution.The water dispersion of the Nano diamond of present method preparation can with the polyacrylic polymer blend of modification, in the bearing friction material or the application in the plastic housing material.
Embodiment
The water dispersion of a kind of Nano diamond of the present invention obtains by following examples:
Embodiment one
A. with original Nano diamond and dense H
2SO
4With dense HNO
3Two kinds mixing solutions (dense H
2SO
4With dense HNO
31: 1), treatment temp is 200 ℃, original Nano diamond is soaked in the excessive acidic oxidation liquid, and heated and stirred, after solution becomes grey by black, solution is cooled to room temperature, extremely neutral with deionized water wash;
B. the product after handling through step a is handled at 50 ℃ with the sufficient hydrogen fluoric acid, and the solution after handling is cooled to room temperature, and is extremely neutral with deionized water wash.
C. through 80 ℃ of vacuum-dryings, obtain through pretreated Nano diamond, its Particle Distribution is 2-20nm, mainly is distributed as 5-20nm.
D. in 100ml nylon jar, pack into the agate ball of 5 diameter 8mm, adding is through pretreated Nano diamond 0.1g, the mixture dispersion agent that adds 0.1g sulfonaphthol and formaldehyde condensation products (1: 1) again is in jar, drip appropriate amount of deionized water, add 0.1g fatty acid methyl ester-α sodium sulfonate again,, the nylon jar is put into ball mill with the sealing of nylon lid, be ball milling 48 hours under the condition of 300rpm at rotating speed, obtain the water dispersion of Nano diamond.
Embodiment two
A. the acid with strong oxidizing property among the embodiment one is dense H
2SO
4With dense HNO
3Two kinds mixing solutions (dense H
2SO
4With dense HNO
3Ratio be 2: 1); Treatment temp is 300 ℃, original Nano diamond is soaked in the excessive acidic oxidation liquid, and heated and stirred, after solution becomes grey by black, solution is cooled to room temperature, extremely neutral with deionized water wash;
B. the product after handling through step a is handled at 80 ℃ with hydrofluoric acid, and the solution after handling is cooled to room temperature, and is extremely neutral with deionized water wash;
C. through 100 ℃ of vacuum-dryings, obtain through pretreated Nano diamond, its Particle Distribution is 2-20nm, mainly is distributed as 5-20nm.
D. in 100ml nylon jar, pack into the zirconia ball of 10 diameter 10mm, add aforementioned through pretreated Nano diamond 5g, the dispersion agent of mixture that adds 2g sulfonaphthol and formaldehyde condensation products again is in jar, drip appropriate amount of deionized water, add 0.5g fatty acid methyl ester-α sodium sulfonate again, with the sealing of nylon lid, the nylon jar is put into ball mill, it at rotating speed ball milling 48 hours under the condition of 400rpm, obtain the water dispersion of Nano diamond, its Particle Distribution is 2-20nm, mainly is distributed as 5-20nm.
Embodiments of the present invention etc. can not limit protection scope of the present invention, so long as the variation of doing to be equal to according to claim protection domain of the present invention, still belong within the protection domain that the invention contains.
Claims (6)
1. the preparation method of a Nano diamond water dispersion is characterized in that: comprise that wherein original Nano diamond pre-treatment comprises following steps to original Nano diamond pre-treatment, Nano diamond surface treatment and dispersion treatment to having handled:
A. with original Nano diamond and strong oxidizing property acid-respons, treatment temp is 200-300 ℃, and treatment step is for to be soaked in pending sample in the excessive acidic oxidation liquid, and heated and stirred, after solution becomes grey by black, solution is cooled to room temperature, extremely neutral with deionized water wash;
B. the product after handling through step a is handled at 50-80 ℃ with the sufficient hydrogen fluoric acid, and the solution after handling is cooled to room temperature, and is extremely neutral with deionized water wash;
C. through 80-100 ℃ of vacuum-drying, obtain through pretreated Nano diamond;
Surface treatment and dispersion treatment through pretreated Nano diamond have following steps:
D. in ball grinder, pack into the abrading-ball of 5-10 diameter 8-10mm, add aforementioned through giving the Nano diamond 0.1-5g of processing, add the 0.1-2g dispersion agent again in jar, drip appropriate amount of deionized water, add the 0.1-0.5g tensio-active agent again, the sealing ball grinder is put into ball mill with ball grinder, be in water medium, to carry out ball milling 48 hours under the condition of 300-400rpm at rotating speed, obtain the water dispersion of Nano diamond.
2. preparation method according to claim 2 is characterized in that described acid with strong oxidizing property is selected from dense H
2SO
4, dense HNO
3, KMnO
4, HClO
4One or more mixtures.
3. preparation method according to claim 2 is characterized in that the treatment temp in the described a step is 240-280 ℃.
4. preparation method according to claim 2 is characterized in that described dispersion agent is the mixture of sulfonaphthol and formaldehyde condensation products.
5. preparation method according to claim 2 is characterized in that described tensio-active agent is anion surfactant or nonionogenic tenside.
6. preparation method according to claim 2 is characterized in that described tensio-active agent is an anion surfactant, is selected from one or more mixture of alkyls sulfonate, alkylbenzene sulfonate or fatty acid methyl ester-α sodium sulfonate.
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CN2010102898800A CN102002264A (en) | 2010-09-17 | 2010-09-17 | Preparation method of nano-diamond aqueous dispersion |
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Family
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105419089A (en) * | 2015-12-08 | 2016-03-23 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Melt grafting modified polypropylene and preparation method thereof and application |
CN106118596A (en) * | 2016-06-15 | 2016-11-16 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of novel nano carbon crystalline substance lapping liquid and preparation method thereof |
CN107304047A (en) * | 2016-04-21 | 2017-10-31 | 常州二维碳素科技股份有限公司 | A kind of process for dispersing of multi-layer graphene |
CN108970434A (en) * | 2018-08-17 | 2018-12-11 | 成都天成鑫钻纳米科技股份有限公司 | A kind of Nano diamond cluster crushes and dispersing method |
CN114717677A (en) * | 2022-03-31 | 2022-07-08 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano-gold non-woven fabric and preparation method and application thereof |
-
2010
- 2010-09-17 CN CN2010102898800A patent/CN102002264A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105419089A (en) * | 2015-12-08 | 2016-03-23 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Melt grafting modified polypropylene and preparation method thereof and application |
CN107304047A (en) * | 2016-04-21 | 2017-10-31 | 常州二维碳素科技股份有限公司 | A kind of process for dispersing of multi-layer graphene |
CN107304047B (en) * | 2016-04-21 | 2020-05-26 | 常州二维碳素科技股份有限公司 | Dispersing method of multilayer graphene |
CN106118596A (en) * | 2016-06-15 | 2016-11-16 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of novel nano carbon crystalline substance lapping liquid and preparation method thereof |
CN108970434A (en) * | 2018-08-17 | 2018-12-11 | 成都天成鑫钻纳米科技股份有限公司 | A kind of Nano diamond cluster crushes and dispersing method |
CN114717677A (en) * | 2022-03-31 | 2022-07-08 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano-gold non-woven fabric and preparation method and application thereof |
CN114717677B (en) * | 2022-03-31 | 2023-09-26 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano gold non-woven fabric and preparation method and application thereof |
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Application publication date: 20110406 |