CN101898761B - Method for dispersing detonation method nano-diamond in liquid phase - Google Patents
Method for dispersing detonation method nano-diamond in liquid phase Download PDFInfo
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- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The invention discloses a method for dispersing a detonation method nano-diamond in a liquid phase. The method comprises the following steps of: a, mixing commercial detonation method nano-diamond powder serving as a raw material into a liquid medium for the ultrasonic processing to form a suspension; b, bombarding the suspension by using a pulse laser with a laser power density of 106W/cm<2> in the action area for 1 to 3h to obtain stable suspension with no precipitate; and c, oxidizing the product which is subjected to the laser bombardment by using strong acid. The method has the advantages of overcoming the problem of easy product pollution in the conventional process for dispersing the detonation method nano-diamond, and aggregating the aggregated detonation method nano-diamond in multiple kinds of solution to obtain monodisperse nano-diamond particles, along with simple process and safe and controllable laser action process. The method can be widely used in the fields of paint, polymer composites, lubrication and the like.
Description
Technical field
The invention relates to the preparation method of Nano diamond, relate in particular in liquid phase dispersing detonation method nano-diamond, with the adamantine method of preparation pure nano.
Background technology
In meteorite, protoplanet nebula, interstellar dust or volcanical ash, exist natural diamond, some also can exist with the form of jewel level diamond, is the valuable ornaments that people like.In recent years along with the discovery and the application of development, especially carbon nanomaterial such as the carbon nanotube of nanometer material science, nano level diamond as the novel carbon nanomaterial of another kind gradually by people's understanding with use.Because Nano diamond has good biocompatibility, dimensional stability, electrical insulating property, high temperature high voltage resistant and chemicalstability; A lot of aspects have been applied at present, such as additive, pharmaceutical carrier and cell marking as lubricating oil or polymer composite.
So far; People have developed the multiple method for preparing Nano diamond, and wherein detonation method is to prepare the most frequently used in the diamond also to be the most successful a kind of method of industriallization, to be used for the production of extensive Nano diamond; Referring to Greiner NR; Phillips DS, Johnson JD, Volk F.Diamonds in detonation soot.Nature.1988; 333 (440): 440-2.In the detonation method, make parent material with the mixture of TNT and cyclotrimethylenetrinitramine usually, the former provides main source of carbon, and the latter provides main energy, and the HTHP that in encloses container, utilizes blast to produce will make carbonaceous change diamond into.The general original Nano diamond particle size less (about 5nm) that forms, surface coverage has graphite-structure or amorphous carbonaceous, and these non-diamond phase carbonaceous can be removed through the strong acid oxidation.Utilize the Nano diamond of this method preparation also to be known as detonation method nano-diamond.
Although in the sixties in 20th century; People just utilize the detonation method successfully to prepare Nano diamond; But subsequently 40 years; Because Nano diamond powder serious agglomeration makes that the microtexture of Nano diamond is not known always, Nano diamond also never obtains the researchist and extensively payes attention to and application.Up to 2003; People such as Japan scientist Osawa have recognized the true appearance of Nano diamond group clustering architecture through the experiment of ball milling Nano diamond; Just the level Four system---the first step is an original Nano diamond particle (4-5nm); The second stage is to be strapped in adhesion body (100-200nm) together by original Nano diamond particle through chemical bond; The third stage is the coacervate (2-3 μ m) that is flocked together and formed by the Van der Waals force between the second stage adhesion body, and the fourth stage is to pile up the block (30-50 μ m) that forms by third stage coacervate.And utilized the method for ball milling to prepare stable dispersion, non-setting Nano diamond colloidal sol in solution in 2005, utilize dynamic light scattering to record Nano diamond particle size distribution behind the ball milling about 5nm.Referring to Kruger A, Kataoka F, Ozawa M; Fujino T; Suzuki Y, Aleksenskii AE, et al.Unusually tight aggregation in detonation nanodiamond:Identification and disintegration.Carbon.2005 Jul; 43 (8): 1722-30.
But because the hardness of Nano diamond is very high, the method for mechanical ball milling unavoidably can be polluted the Nano diamond powder, influences its follow-up application; And up to the present, also really do not observe the existence of the real dispersion state of Nano diamond.Therefore, how in liquid phase dispersing detonation method nano-diamond still be a problem demanding prompt solution.
Summary of the invention
The objective of the invention is to solve that detonation method nano-diamond is seriously reunited, in the existing dispersing detonation method nano-diamond technology to the problems such as pollution of Nano diamond.Utilize laser technology to prepare the advantage of nano material, provide a kind of pollution-free, technology simple, product is purified after, can access the novel method of stable dispersion, non-setting Nano diamond suspension-s in liquid medium.
The present invention is achieved through following technical scheme:
The method of dispersing detonation method nano-diamond in liquid phase has following steps:
A, be raw material with commercial detonation method nano-diamond powder; Its particle diameter is 2-10nm, and it is mixed in the liquid medium, and said Nano diamond solution is 0.1-0.5mg/mL; Utilize UW to carry out supersound process then, to form the suspension-s of detonation method nano-diamond;
The detonation method nano-diamond suspension-s of b, use pulse laser implant steps a, laser beam converges at suspension surface, and the wavelength of pulse laser beam is 1.06 μ m, and PW is 1.0ms, and pulse-repetition is 10-30Hz, the laser power density of the zone of action is 10
6W/cm
2, the time of lasing is 1-3h; Detonation method nano-diamond effect suspension stabilization after the lasing, do not precipitate;
C, the product after the laser bombardment is carried out the strong acid oxide treatment, remove the carbonaceous of the non-diamond in the product, obtain purified detonation method nano-diamond.
The liquid medium of said step a is the mixed solution of deionized water or alcohol, ketone, ether and the arbitrary proportion that formed by arbitrary combination between them.
The Nd:YAG solid statelaser is adopted in the laser bombardment of said step b.
In the process of said step b, the reaction vessel that holds suspension-s is adopted the heat of outer loop water-bath type of cooling absorbing redundant, prevent the solution boiling, liquid medium is under the normal temperature.
The strong acid of said step c is perchloric acid.
The invention has the beneficial effects as follows that technology is simple, lasing process safety is controlled, has overcome the caused product pollution of method dispersing detonation method nano-diamond of utilizing ball milling, and in multiple solution, has realized the dispersion of detonation method nano-diamond.In addition, utilize in the laser bombardment liquid Nano diamond can directly make the Nano diamond particle surface produce organism and modify, help follow-up matrix material and biological aspect application, also make Nano diamond have more scientific research value.The dispersive detonation method nano-diamond can be used widely in coating, polymer composite, field such as lubricated.
Description of drawings
Fig. 1 is the laser liquid phase ablation device synoptic diagram of laser bombardment detonation method nano-diamond suspension-s;
Fig. 2 is the transmission electron microscope photo of detonation method nano-diamond raw material;
Fig. 3 is the Nano diamond particulate transmission electron microscope photo that obtains behind the Nano diamond suspension-s in the laser bombardment water among the embodiment 2;
Fig. 4 is the Nano diamond particulate transmission electron microscope photo that obtains behind the Nano diamond suspension-s in the laser bombardment vinylformic acid.
Reference numeral is among Fig. 1:
1---Nd:YAG solid statelaser 2---pulse laser beam 3---recirculated cooling water
4---ultrasonic generator 5---speculum 6---condensors
7---detonation method nano-diamond suspension-s
Embodiment
The device that the present invention adopts is as shown in Figure 1; Pulse laser beam 2 by 1 generation of Nd:YAG solid statelaser; Through converging through condensor 6 again after speculum 5 reflections; Pulse laser beam 2 is focused on the liquid level place of detonation method nano-diamond suspension-s 7, utilize 4 pairs of detonation method nano-diamond suspension-s of ultrasonic generator 7 to carry out supersound process, and outsidely cool off with 3 pairs of systems of recirculated cooling water at it.
With commercial detonation method nano-diamond powder is raw material, and its particle diameter is 2-10nm.
Specific embodiment is following:
Embodiment 1
A, 50mg detonation method nano-diamond powder is joined in the 100mL deionized water, the median size of Nano diamond powder is 5nm here, utilizes ultrasonic generator that it is carried out supersound process, to form detonation method nano-diamond suspension-s.
The detonation method nano-diamond suspension-s of b, use pulse laser implant steps a; Laser spot converges at the fluid surface place; In the liquid level microcell of laser beam effect, the amorphous carbonaceous in the Nano diamond coacervate can absorb laser and produce high temperature and decomposition, and the high temperature that amorphous carbon decomposes can make the covalent linkage between the Nano diamond particle break off; Thereby the detonation method nano-diamond of agglomerated is separated reunion, forms monodispersed diamond nano particle.The laser power density of the zone of action is 10
6W/cm
2, the time of lasing is 3h, and the wavelength of pulse laser beam is 1.06 μ m, and PW is 1.0ms, and pulse-repetition is 10Hz, adopts the Nd:YAG solid statelaser.
Utilize UW that Nano diamond powder suspension-s is disperseed; Can form uniform Nano diamond suspension-s; Thereby make laser act on different Nano diamond suspension-s microcells constantly, help improving the efficient of laser dispersing detonation method nano-diamond in difference.
The detonation method nano-diamond powder is the business level Nano diamond powder that utilizes the preparation of detonation method, and its particle diameter is 2-10nm.Referring to Fig. 2, be depicted as the transmission electron microscope photo of detonation method nano-diamond, can find out the Nano diamond particle agglomeration together, particle surface has the amorphous carbonaceous to exist.After the detonation method nano-diamond raw material is soluble in water, utilize ultrasonic echography after 30 minutes, leave standstill after tens minutes and promptly precipitate, show the detonation method nano-diamond serious agglomeration.
In the laser bombardment process, the reaction vessel that holds suspension-s is adopted the heat of outer loop water-bath type of cooling absorbing redundant, prevent the solution boiling, and liquid medium is under the normal temperature.
Nano diamond effect suspension stabilization after the lasing, do not precipitate.
C, the detonation method nano-diamond after the laser bombardment is carried out pickling, adopt perchloric acid, the carbonaceous of removing the non-diamond in the product obtains the pure nano diamond.
Embodiment 2
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.By Nd-YAG solid statelaser output wavelength is the pulse laser beam (PW 1.0ms, pulse-repetition is 20Hz) of 1.06 μ m, after converging through optical lens, focuses on the surface of detonation method nano-diamond suspension-s.Liquid medium is a deionized water, utilizes UW to disperse detonation method nano-diamond suspension-s, to form uniform detonation method nano-diamond suspension-s.The container that holds detonation method nano-diamond suspension-s is adopted outer loop water-bath cooling.Laser bombards 1h continuously, and reacted product is obtained gray diamond nano particle after pickling is purified, and median size is 4nm.Referring to Fig. 3, be depicted as the dispersive Nano diamond particulate transmission electron microscope photo that the detonation method nano-diamond suspension-s in the laser bombardment deionized water obtains, can find out that the Nano diamond particles dispersed that obtains exists, and does not reunite.
Embodiment 3
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.The pulse-repetition that changes pulse laser beam is 10Hz.Liquid medium is a deionized water, utilizes UW to disperse detonation method nano-diamond suspension-s, to form uniform detonation method nano-diamond suspension-s.The container that holds detonation method nano-diamond suspension-s is adopted outer loop water-bath cooling.Laser bombards 1h continuously, and reacted product is obtained gray diamond nano particle after pickling is purified, and median size is 4nm.
Embodiment 4
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.The pulse-repetition that changes pulse laser beam is 30Hz.Liquid medium is a deionized water, utilizes UW to disperse detonation method nano-diamond suspension-s, to form uniform detonation method nano-diamond suspension-s.The container that holds detonation method nano-diamond suspension-s is adopted outer loop water-bath cooling.Laser bombards 1h continuously, and reacted product is obtained gray diamond nano particle after pickling is purified, and median size is 4nm.
Embodiment 5
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.Only changing the continuous bombardment time of laser is 2h, and reacted product is obtained gray diamond nano particle after pickling is purified, and median size is 4nm.
Embodiment 6
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.Only changing the continuous bombardment time of laser is 3h, and reacted product is obtained gray diamond nano particle after pickling is purified, and median size is 4nm.
Embodiment 7
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.Detonation method nano-diamond suspension-s in the laser bombardment deionized water utilized perchloric acid to carry out oxide treatment after 2 hours.It still exists with the steady suspension form after 5 months with the detonation method nano-diamond suspension-s placement that obtains, and shows Nano diamond particle good dispersion in solution, and median size is 4nm.
Embodiment 8
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.The change liquid medium is an ethanol, and 10mg detonation method nano-diamond powder is mixed with 30mL vinylformic acid, and other condition is constant, and the product after the lasing is carried out obtaining gray diamond nano particle after pickling is purified, and median size is 5nm.Product after purifying is scattered in the ethanol still can forms the stabilized nano diamond suspension, show its good dispersibility.
Embodiment 9
In the same reaction unit, there are not the processing condition of explanation all identical with embodiment 1.The change liquid medium is a vinylformic acid, and other condition is constant, and the product after the lasing is carried out obtaining gray diamond nano particle after pickling is purified, and median size is 5nm.Referring to Fig. 4, be depicted as the dispersive Nano diamond particulate transmission electron microscope photo that laser bombardment goes the detonation method nano-diamond suspension-s in the vinylformic acid to obtain, can find out that the Nano diamond particles dispersed that obtains exists, and does not have agglomeration.
Claims (5)
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| GB2503643A (en) * | 2012-04-27 | 2014-01-08 | Univ Newcastle | Method for separation of diamond particle clusters |
| CN103657564B (en) * | 2013-10-12 | 2015-03-04 | 江苏大学 | Device and method for preparing nano diamonds by high-energy lamp pumping solid laser |
| CN103864070A (en) * | 2014-03-19 | 2014-06-18 | 中山大学 | Preparation method of superfine fluorescent nano diamond |
| CN104231712A (en) * | 2014-09-02 | 2014-12-24 | 河南工业职业技术学院 | Preparation method of automotive topcoat based on nano diamond packing with high wear resistance |
| KR102328995B1 (en) * | 2014-11-26 | 2021-11-23 | 나노리소스 주식회사 | Separation method of Detonation Nano Diamond |
| CN104479844A (en) * | 2014-12-18 | 2015-04-01 | 清华大学 | Water-based lubricating fluid with ultralow frictional coefficient and preparation method of water-based lubricating fluid |
| KR102610504B1 (en) * | 2017-04-05 | 2023-12-07 | 주식회사 다이셀 | Lubricant compositions and lubrication systems |
| CN109238974A (en) * | 2018-08-30 | 2019-01-18 | 南京理工大学 | A kind of preparation method of blind type deep ultraviolet plasma resonance nano particle |
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