CN1313366C - Method for synthesizing nano diamond by laser bombarding carbon powder - Google Patents
Method for synthesizing nano diamond by laser bombarding carbon powder Download PDFInfo
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- CN1313366C CN1313366C CNB2004100939730A CN200410093973A CN1313366C CN 1313366 C CN1313366 C CN 1313366C CN B2004100939730 A CNB2004100939730 A CN B2004100939730A CN 200410093973 A CN200410093973 A CN 200410093973A CN 1313366 C CN1313366 C CN 1313366C
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Abstract
The present invention relates to a method for synthesizing nanometer diamond by using lasers to bombard carbon powder, which solves the problem of special reaction condition or reaction yield in the existing preparation processes of the nanometer diamond. The method comprises: using the carbon powder as raw materials; suspending the carbon powder in a liquid medium and circulating the liquid medium; bombarding the carbon powder in the circulating liquid medium by pulses or continuous lasers; purifying products after the bombardment of the lasers to obtain nanometer diamond powder. The carbon powder can be various graphite particles and carbon black particles, and the particle size of the carbon powder can be less than or equal to 10 micrometers. The liquid medium can be any flowing liquid, such as water, alcohol, ketone and ether, or a solution formed from the liquid or a mixed solution in different proportions, wherein the mixed solution is formed from water, alcohol, ketone and ether. The method overcomes the disadvantages of special requirements for the reaction conditions or low reaction yield, etc. in the preparation processes of the nanometer diamond in the prior art, realizes the continuous synthesis of the nanometer diamond under the conditions of normal temperature and pressure, and obtains nanometer diamond powder materials with high purity.
Description
[technical field]: the present invention relates to a kind of method with the carbon dust synthesizing nano diamond.
[background technology]: diamond is widely used in many important science and technology and industrial circle owing to having unique physicochemical property.Nano diamond also has the characteristic of nano material except that having more adamantine essential propertys, application prospect is very wide.
Artificially synthesizing diamond mainly adopted the static high pressure method in the past, at first utilized graphite to be raw material as GE in 1954, used the static high pressure method to synthesize man-made diamond, referring to F.P.Bundy, H.T.Hall, H.M.Strong, et al., Nature, 1955,176:51～55.The diamond particles that this method is produced is all bigger, is not suitable for the preparation of nano material.
At present, the preparation method of synthetic Nano diamond powder mainly contains: it is that explosion method successfully makes diamond that 1, explosion method---DeCarli used the dynamic high-pressure method in 1961, referring to P.S.DeCarli, J.C.Jamieson, Science, 1961,133:1821～1822.Explosion method can manufacture the diamond powder of 4-8nm, but there is the deficiency of two aspects in it: one, extremely short owing to the blast process reaction times, and the reaction process complexity, reaction process is uncontrollable.Two, need utilize explosive and blast place, reaction conditions is restricted.2, Na-CCl
4Reduction method---Qian Yitai was in (about 700 degree) employing sodium Metal 99.5 reduction CCl under relatively low temperature in 1998
4Obtain Nano diamond, referring to Yadong Li, Yatai Qian etal, Science, 1998,281:246～247.Na-CCl
4Reduction method does not obtain practical application so far because productive rate is low excessively.3, pulse laser induced liquid liquid/solid interface reaction method---laser can make material heat, melt, vaporize or undergo phase transition in the extremely short time, thereby reaches the purpose of processing or modification.Laser has also obtained application aspect artificially synthesizing diamond, its dominant mechanism is that laser has high energy density, thereby can be with the transformation of substance activating recurring structure.Method with the reaction of pulse laser induced liquid liquid/solid interface, people such as Wang Jinbin 1998 are with the blocky graphite target of pulse laser corrode in the aqueous solution, it is nanocrystalline to have obtained six sides and cubic diamond, referring to Wang Jinbin, Liu Qiuxiang etc., the investigation of materials journal, 1998, the 12 volume third phase: 323～325.Induced liquid liquid/solid interface reaction method is because the lasing object is in static state (the blocky graphite target is fixed on the Glass Containers bottom), and the Nano diamond quantity that is obtained is few, and actual application value is little.
[summary of the invention]: the objective of the invention is to solve the problem that the requirement of Nano diamond preparation process reaction conditions is special or reaction yield is lower in the prior art, provide a kind of place and reaction conditions of not being subjected to limit, and the method for the synthesizing nano diamond by laser bombarding carbon powder that can manufacture.
The method of synthesizing nano diamond by laser bombarding carbon powder provided by the invention may further comprise the steps:
---a, be raw material with the carbon dust, its particle diameter should be smaller or equal to 10 microns;
---b, carbon dust is suspended in the liquid medium, and makes liquid medium keep circulation;
---the carbon dust in c, use pulse or the continuous laser bombardment circulating liquid medium, laser spot converges under the fluid surface; In order to prevent liquid splash, burning or blast, make the synthetic good reaction environment that is in simultaneously, feed shielding gas along laser incident coaxial direction; In order to make liquid medium be in the normal temperature state, in the laser bombardment process, to the unnecessary heat of container employing outer loop water-bath type of cooling absorption of contain fluid;
---d, to the product after the laser bombardment through purify obtaining the Nano diamond powder.
Carbon dust wherein can be graphite granule or carbon black granules.
The effect of liquid medium is that carbon dust is suspended in wherein, and can make the laser bombardment that can circulate, so liquid medium is can any liquid of mobile, can be mixture or the water and the alcoholic acid mixture of water or water and acetone.
In the lasing process, feed shielding gas along laser incident coaxial direction.This shielding gas can be argon gas or nitrogen or air.
The present invention has following advantage: the present invention has overcome in the above-mentioned prior art in the Nano diamond preparation process shortcomings such as the special or reaction yield of reaction conditions requirement is lower, realize Nano diamond continuous synthesizing at normal temperatures and pressures, obtained the higher Nano diamond powder material of purity.In addition, it is controlled that the method for synthesizing nano diamond of the present invention has reaction process safety, and reaction can be carried out continuously, the Nano diamond size distribution advantage of uniform that is obtained.
[embodiment]:
Embodiment 1
Micro fine carbon dust is suspended in the liquid medium, stirs with electromagnetic shock and make its homodisperse, and adopt electric pump to make liquid circulation, control suitable speed of circulation.Use the micro fine carbon dust in pulse or the continuous laser bombardment circulating liquid medium, laser spot converges at suitable distance under the fluid surface, has produced the microcell of a High Temperature High Pressure at the laser spot place, impels the micro fine carbon dust in the microcell to be transformed into the Nano diamond powder.
Wherein: the composition of liquid medium comprises water or alcohol, ketone, ether etc., and all can flowing fluid and the solution that formed by this liquid, or by the mixture of the different ratios that forms between them.Micro fine carbon dust should guarantee homodisperse in liquid medium.Because liquid medium carries the micro fine carbon dust particle and circulates, laser acts on different micro fine carbon dust particles constantly in difference, is of value to the productive rate that improves Nano diamond.
The composition of micro fine carbon dust raw material can be various types of graphite granules, carbon black granules or other carbonaceous particles, and its particle diameter should be smaller or equal to 10 microns.
Feed suitable shielding gas along laser incident coaxial direction, comprise argon gas, nitrogen or air etc.Shielding gas feeds reaction zone along the laser coaxial direction, and takes steam and issuable gaseous product that liquid phase in the building-up process produces out of reaction zone, recycles after treatment or emptying.Feed shielding gas and can prevent liquid splash, burning or blast, make the synthetic good reaction environment that is in simultaneously.
In the laser bombardment process, the unnecessary heat of container employing outer loop water-bath type of cooling absorption to contain fluid is under the normal temperature liquid medium.
Product after the laser bombardment is obtained the Nano diamond powder through the peroxidation purification.
Embodiment 2
By Nd-YAG solid statelaser output wavelength is the pulse laser beam (pulse width 1.2ms, pulse-repetition is 20Hz) of 1.06 μ m, after converging through optical lens, focuses on following 1mm place, circulating liquid medium surface.The round-robin liquid medium is a deionized water, and granularity is used being scattered in wherein that electromagnetic shock stirs less than the powdered graphite of 10 μ m.As shielding gas, and the container of contain fluid dielectric suspensions adopted outer loop water-bath cooling along laser incident coaxial direction bubbling air.Generated time is 5 hours continuously, and reacted product is obtained linen Nano diamond powder after oxidation is purified.
Embodiment 3
In the same reaction unit; changing the round-robin liquid medium is the miscellany (volume ratio is 3: 1) of acetone, water; micro fine carbon dust is a carbon black powders; feed argon gas as shielding gas along laser incident coaxial direction; other reaction conditionss are constant, and reacted product is obtained gray Nano diamond powder after oxidation is purified.
Embodiment 4
In the same reaction unit, use CO
2The gas laser output wavelength is the continuous laser beam of 10.6 μ m; changing the round-robin liquid medium is the miscellany (volume ratio is 2: 1) of ethanol, water; micro fine carbon dust is the Graphite Powder 99 of granularity less than 10 μ m; feed nitrogen as shielding gas along laser incident coaxial direction; other reaction conditionss are constant, and reacted product is obtained linen Nano diamond powder after oxidation is purified.
Claims (5)
1, a kind of method of synthesizing nano diamond by laser bombarding carbon powder is characterized in that this method may further comprise the steps:
---a, be raw material with the carbon dust, its particle diameter should be smaller or equal to 10 microns;
---b, carbon dust is suspended in the liquid medium, and makes liquid medium keep circulation;
---the carbon dust in c, use pulse or the continuous laser bombardment circulating liquid medium, laser spot converges under the fluid surface; In order to prevent liquid splash, burning or blast, make the synthetic good reaction environment that is in simultaneously, feed shielding gas along laser incident coaxial direction; In order to make liquid medium be in the normal temperature state, in the laser bombardment process, to the unnecessary heat of container employing outer loop water-bath type of cooling absorption of contain fluid;
---d, to the product after the laser bombardment through purify obtaining the Nano diamond powder.
2, the method for synthesizing nano diamond by laser bombarding carbon powder according to claim 1 is characterized in that described carbon dust is graphite granule or carbon black granules.
3, the method for synthesizing nano diamond according to claim 1 is characterized in that liquid medium is mixture or the water and the alcoholic acid mixture of water, water and acetone.
4, according to the method for claim 1 or 2 or 3 described synthesizing nano diamonds, its technical characterictic be lasing on liquid level, the focus of laser converges under the liquid level.
5,, it is characterized in that shielding gas is argon gas, nitrogen or air according to the method for claim 1 or 2 or 3 described synthesizing nano diamonds.
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| CNB2004100939730A CN1313366C (en) | 2004-12-20 | 2004-12-20 | Method for synthesizing nano diamond by laser bombarding carbon powder |
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| CNB2004100939730A CN1313366C (en) | 2004-12-20 | 2004-12-20 | Method for synthesizing nano diamond by laser bombarding carbon powder |
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| CN1313366C true CN1313366C (en) | 2007-05-02 |
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Families Citing this family (10)
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| CN101239391B (en) * | 2008-02-27 | 2010-06-02 | 天津大学 | Method for coating metal nano granule by laser synthesizing carbon |
| CN101898761B (en) * | 2010-07-13 | 2012-06-27 | 天津大学 | Method for dispersing detonation method nano-diamond in liquid phase |
| CN102210999B (en) * | 2011-06-10 | 2013-12-25 | 东北大学 | Method for synthesizing nano diamond by irradiating graphite suspension with high current pulsed electron beam |
| CN102409292A (en) * | 2011-11-18 | 2012-04-11 | 江苏大学 | Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser |
| CN103288074A (en) * | 2013-05-17 | 2013-09-11 | 燕山大学 | Preparation method of nano new diamond powder |
| CN103409729B (en) * | 2013-08-27 | 2015-11-18 | 江苏大学 | A kind of Irradiation of High prepares the method for diamond like carbon film |
| CN103508451A (en) * | 2013-10-09 | 2014-01-15 | 江苏大学 | Method and device for nanosecond pulse laser-assisted preparation of nano-diamond |
| 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 |
| CN112679995A (en) * | 2020-12-08 | 2021-04-20 | 安徽枡水新能源科技有限公司 | Method for improving electrochemical corrosion resistance of conductive carbon black |
| CN113088849B (en) * | 2021-03-09 | 2022-08-05 | 武汉大学 | Composite strengthening method for synthesizing nano diamond by laser induction |
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| JPH0640712A (en) * | 1992-07-22 | 1994-02-15 | Mitsubishi Materials Corp | Production of artificial diamond powder |
| US5690794A (en) * | 1995-06-07 | 1997-11-25 | Fizichesky Institut Imeni P.N./Lebedeva Rossiiskoi Akademii Nauk | Method of growing diamond from graphite |
| CN1347843A (en) * | 2001-10-16 | 2002-05-08 | 福建师范大学 | Laser impact process of synthesizing nanometer diamond bead (sol) continuously |
| CN1541937A (en) * | 2003-11-06 | 2004-11-03 | 东北大学 | Laser preparation and in-situ dispersion method for nanometer carbon granular material |
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2004
- 2004-12-20 CN CNB2004100939730A patent/CN1313366C/en not_active Expired - Fee Related
Patent Citations (4)
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|---|---|---|---|---|
| JPH0640712A (en) * | 1992-07-22 | 1994-02-15 | Mitsubishi Materials Corp | Production of artificial diamond powder |
| US5690794A (en) * | 1995-06-07 | 1997-11-25 | Fizichesky Institut Imeni P.N./Lebedeva Rossiiskoi Akademii Nauk | Method of growing diamond from graphite |
| CN1347843A (en) * | 2001-10-16 | 2002-05-08 | 福建师范大学 | Laser impact process of synthesizing nanometer diamond bead (sol) continuously |
| CN1541937A (en) * | 2003-11-06 | 2004-11-03 | 东北大学 | Laser preparation and in-situ dispersion method for nanometer carbon granular material |
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