CN1313366C - Method for synthesizing nano diamond by laser bombarding carbon powder - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
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Abstract
Description
【技术领域】：本发明涉及一种用碳粉合成纳米金刚石的方法。[technical field]: the present invention relates to a kind of method with carbon powder synthetic nano-diamond.
【背景技术】：金刚石由于具有独特的物理化学性质而被广泛地应用于许多重要的科学技术和工业领域。纳米金刚石除具有金刚石的一些基本性质外还具有纳米材料的特性，应用前景十分广阔。[Background Technology]: Diamond is widely used in many important fields of science, technology and industry due to its unique physical and chemical properties. In addition to some basic properties of diamond, nano-diamond also has the characteristics of nano-materials, and its application prospects are very broad.
以往人工合成金刚石主要采用静态高压法，如1954年美国通用电气公司首先利用石墨为原料，使用静态高压法合成了人造金刚石，参见F.P.Bundy，H.T.Hall，H.M.Strong，et al.，Nature，1955，176：51～55。这种方法生产的金刚石颗粒都比较大，不适合纳米材料的制备。In the past, artificially synthesized diamond mainly used the static high-pressure method. For example, in 1954, General Electric Company of the United States first used graphite as a raw material to synthesize artificial diamond using the static high-pressure method. See F.P.Bundy, H.T.Hall, H.M.Strong, et al., Nature, 1955, 176: 51-55. The diamond particles produced by this method are relatively large, which is not suitable for the preparation of nanomaterials.
目前，人工合成纳米金刚石粉体的制备方法主要有：1、爆炸法——DeCarli于1961年使用动态高压法即爆炸法成功制得金刚石，参见P.S.DeCarli，J.C.Jamieson，Science，1961，133：1821～1822。爆炸法已能批量生产4-8nm的金刚石粉体，但其存在两方面的不足：一、由于爆炸过程反应时间极短，反应过程复杂，反应过程不可控制。二、需要利用炸药和爆炸场地，反应条件受到限制。2、Na-CCl4还原法——钱逸泰于1998年在相对较低的温度下(约700度)采用金属钠还原CCl4得到纳米金刚石，参见Yadong Li，Yatai Qian etal，Science，1998，281：246～247。Na-CCl4还原法由于产率过低，迄今未获实际应用。3、脉冲激光诱导液固界面反应法——激光能在极短的时间内使材料加热、熔化、汽化或者发生相变，从而达到加工或改性的目的。激光在人工合成金刚石方面也已经得到了应用，其主要机理是激光具有极高的能量密度，能够将物质激活从而发生结构的转变。用脉冲激光诱导液固界面反应的方法，王金斌等人1998年用脉冲激光熔蚀在水溶液中的块状石墨靶，得到了六方和立方金刚石纳米晶，参见王金斌，刘秋香等，材料研究学报，1998年，第十二卷第三期：323～325。诱导液固界面反应法由于激光作用对象处于静态(块状石墨靶被固定在玻璃容器底部)，所获得的纳米金刚石数量极少，实际应用价值不大。At present, the preparation methods of artificially synthesized nano-diamond powder mainly include: 1. Explosion method——DeCarli used the dynamic high-pressure method, that is, the explosion method, to successfully prepare diamond in 1961. See PS DeCarli, JC Jamieson, Science, 1961, 133: 1821-1822 . The explosion method has been able to produce 4-8nm diamond powder in batches, but it has two shortcomings: 1. Due to the extremely short reaction time of the explosion process, the reaction process is complicated and uncontrollable. Two, it is necessary to utilize explosives and explosion sites, and the reaction conditions are limited. 2. Na-CCl 4 reduction method——Qian Yitai used metal sodium to reduce CCl 4 at a relatively low temperature (about 700 degrees) in 1998 to obtain nano-diamonds, see Yadong Li, Yatai Qian et al, Science, 1998, 281: 246-247. The Na-CCl 4 reduction method has not been practically applied so far due to the low yield. 3. Pulse laser-induced liquid-solid interface reaction method - laser can heat, melt, vaporize or undergo phase change in a very short period of time, so as to achieve the purpose of processing or modification. Lasers have also been applied in synthetic diamonds. The main mechanism is that lasers have extremely high energy density and can activate substances to undergo structural transformation. Using pulsed laser to induce liquid-solid interface reaction, Wang Jinbin and others used pulsed laser to ablate bulk graphite target in aqueous solution in 1998, and obtained hexagonal and cubic diamond nanocrystals, see Wang Jinbin, Liu Qiuxiang, etc., Materials Research Journal, 1998, Volume 12, Issue 3: 323-325. In the induced liquid-solid interface reaction method, since the target of the laser is static (the block graphite target is fixed at the bottom of the glass container), the number of nano-diamonds obtained is very small, and the practical application value is not great.
【发明内容】：本发明的目的是解决现有技术中纳米金刚石制备过程反应条件要求特殊或反应产率较低的问题，提供一种不受场地和反应条件限制，且能批量生产的激光轰击碳粉合成纳米金刚石的方法。[Content of the invention]: The purpose of the present invention is to solve the problem of special requirements for reaction conditions or low reaction yield in the preparation process of nano-diamonds in the prior art, and to provide a laser bombardment that is not limited by the site and reaction conditions and can be mass-produced. A method for synthesizing nano-diamonds from carbon powder.
本发明提供的激光轰击碳粉合成纳米金刚石的方法，包括以下步骤：The method for synthesizing nano-diamonds by laser bombarding carbon powder provided by the invention comprises the following steps:
——a、以碳粉为原料，其粒径应小于等于10微米；——a. Carbon powder is used as raw material, and its particle size should be less than or equal to 10 microns;
——b、将碳粉悬浮于液体介质中，并使液体介质保持循环；——b. Suspend the carbon powder in the liquid medium and keep the liquid medium in circulation;
——c、使用脉冲或连续激光轰击循环液体介质中的碳粉，激光焦点汇聚于液体表面下；为了防止液体飞溅、燃烧或爆炸，同时使合成处于良好的反应环境，沿着激光入射同轴方向通入保护气体；为了使液体介质处于常温状态，在激光轰击过程中，对盛放液体的容器采用外部循环水浴冷却方式吸收多余的热量；——c. Use pulsed or continuous laser to bombard the carbon powder in the circulating liquid medium, and the laser focus is concentrated under the surface of the liquid; in order to prevent the liquid from splashing, burning or exploding, and make the synthesis in a good reaction environment, along the laser incident coaxial In order to keep the liquid medium at normal temperature, during the laser bombardment process, the container containing the liquid is cooled by an external circulating water bath to absorb excess heat;
——d、对激光轰击后的产物经过提纯获得纳米金刚石粉末。——d. Purifying the product after laser bombardment to obtain nano-diamond powder.
其中的碳粉可以是石墨颗粒、或碳黑颗粒。The carbon powder can be graphite particles or carbon black particles.
液体介质的作用是使碳粉悬浮于其中，并可使激光能够循环轰击，因此液体介质为可以流动的任何液体，可以是水、或水与丙酮的混合物、或水与乙醇的混合物。The role of the liquid medium is to suspend the carbon powder in it and enable the laser to cyclically bombard it. Therefore, the liquid medium is any liquid that can flow, and it can be water, or a mixture of water and acetone, or a mixture of water and ethanol.
在激光作用过程中，沿着激光入射同轴方向通入保护气体。该保护气体可以是氩气、或氮气、或空气。During the laser action, the protective gas is introduced along the coaxial direction of the laser incident. The shielding gas can be argon, or nitrogen, or air.
本发明具有如下优点：本发明克服了上述现有技术中纳米金刚石制备过程中反应条件要求特殊或反应产率较低等缺点，实现了纳米金刚石在常温常压下的连续合成，获得了纯度较高的纳米金刚石粉体材料。此外，本发明所采用的合成纳米金刚石的方法具有反应过程安全可控，反应可连续进行，所获得的纳米金刚石粒径分布均匀的优点。The present invention has the following advantages: the present invention overcomes the shortcomings of special reaction conditions or low reaction yields in the preparation process of nano-diamonds in the above-mentioned prior art, realizes the continuous synthesis of nano-diamonds at normal temperature and pressure, and obtains high-purity nano-diamonds. High nano-diamond powder material. In addition, the method for synthesizing nano-diamonds adopted in the present invention has the advantages that the reaction process is safe and controllable, the reaction can be carried out continuously, and the particle size distribution of the obtained nano-diamonds is uniform.
【具体实施方式】：【Detailed ways】:
实施例1Example 1
将微细碳粉悬浮于液体介质中，用电磁震动搅拌使其均匀分散，并采用电泵使液体循环起来，控制适当的循环速度。使用脉冲或连续激光轰击循环液体介质中的微细碳粉，激光焦点汇聚于液体表面下适当距离，在激光焦点处产生了一个高温高压的微区，促使微区内的微细碳粉转变成纳米金刚石粉末。Suspend the fine carbon powder in the liquid medium, stir it with electromagnetic vibration to disperse it evenly, and use an electric pump to circulate the liquid to control the appropriate circulation speed. Use pulsed or continuous laser to bombard the fine carbon powder in the circulating liquid medium, the laser focus converges at an appropriate distance below the liquid surface, and a high-temperature and high-pressure micro-zone is generated at the laser focus, which promotes the micro-fine carbon powder in the micro-zone to transform into nano-diamond powder.
其中：液体介质的组成包括水或醇、酮、醚等一切可以流动的液体及由该液体形成的溶液，或由它们之间形成的不同比例的混合物。微细碳粉应保证在液体介质中均匀分散。由于液体介质载着微细碳粉粒子循环流动，激光在不同时刻作用于不同的微细碳粉粒子，有益于提高纳米金刚石的产率。Wherein: the composition of the liquid medium includes all flowable liquids such as water or alcohols, ketones, ethers, and solutions formed by the liquids, or mixtures of different proportions formed between them. Fine carbon powder should ensure uniform dispersion in the liquid medium. Because the liquid medium carries fine carbon powder particles and circulates, the laser acts on different fine carbon powder particles at different times, which is beneficial to improve the yield of nano-diamonds.
微细碳粉原料的组成可以是各种类型的石墨颗粒、碳黑颗粒或其它含碳颗粒，其粒径应小于等于10微米。The composition of the fine carbon powder raw material can be various types of graphite particles, carbon black particles or other carbon-containing particles, and its particle size should be less than or equal to 10 microns.
沿着激光入射同轴方向通入适当的保护气体，包括氩气、氮气或空气等。保护气体沿激光同轴方向通入反应区，并将合成过程中液相产生的蒸汽以及可能产生的气态产物带出反应区，经处理后循环使用或放空。通入保护气体可以防止液体飞溅、燃烧或爆炸，同时使合成处于良好的反应环境。Appropriate protective gas, including argon, nitrogen or air, is introduced along the laser incident coaxial direction. The protective gas is passed into the reaction area along the coaxial direction of the laser, and the steam generated in the liquid phase and the possible gaseous products during the synthesis process are taken out of the reaction area, and recycled or emptied after treatment. Introducing a protective gas can prevent the liquid from splashing, burning or exploding, and at the same time make the synthesis in a good reaction environment.
在激光轰击过程中，对盛放液体的容器采用外部循环水浴冷却方式吸收多余的热量，使液体介质处于常温之下。During the laser bombardment process, the container containing the liquid is cooled by an external circulating water bath to absorb excess heat, so that the liquid medium is at room temperature.
对激光轰击后的产物经过氧化提纯获得纳米金刚石粉末。The product after laser bombardment is oxidized and purified to obtain nano-diamond powder.
实施例2Example 2
由Nd-YAG固体激光器输出波长为1.06μm的脉冲激光束(脉冲宽度1.2ms，脉冲频率为20Hz)，经过光学透镜汇聚后，聚焦于循环液体介质表面以下1mm处。循环的液体介质为去离子水，将粒度小于10μm的石墨粉末使用电磁震动搅拌均匀的分散于其中。沿着激光入射同轴方向通入空气作为保护气体，并将盛放液体介质悬浮液的容器采用外部循环水浴冷却。连续合成时间5小时，将反应后的产物经氧化提纯后获得灰白色的纳米金刚石粉体。The Nd-YAG solid-state laser outputs a pulsed laser beam with a wavelength of 1.06 μm (pulse width 1.2 ms, pulse frequency 20 Hz), which is focused at 1 mm below the surface of the circulating liquid medium after being converged by an optical lens. The circulating liquid medium is deionized water, and the graphite powder with a particle size of less than 10 μm is evenly dispersed in it by electromagnetic vibration stirring. Air is introduced along the coaxial direction of the laser incident as a protective gas, and the container containing the liquid medium suspension is cooled by an external circulating water bath. The continuous synthesis time was 5 hours, and the off-white nano-diamond powder was obtained after the reaction product was oxidized and purified.
实施例3Example 3
在同上的反应装置中，改变循环的液体介质为丙酮、水的混和物(体积比为3∶1)，微细碳粉为碳黑粉末，沿激光入射同轴方向通入氩气作为保护气体，其他反应条件不变，将反应后的产物经氧化提纯后获得灰色的纳米金刚石粉体。In the above reaction device, the circulating liquid medium is changed to be a mixture of acetone and water (volume ratio is 3: 1), the fine carbon powder is carbon black powder, and argon gas is introduced along the laser incident coaxial direction as a protective gas. Other reaction conditions remain unchanged, and the reaction product is oxidized and purified to obtain gray nano-diamond powder.
实施例4Example 4
在同上的反应装置中，使用CO2气体激光器输出波长为10.6μm的连续激光束，改变循环的液体介质为乙醇、水的混和物(体积比为2∶1)，微细碳粉为粒度小于10μm的石墨粉，沿激光入射同轴方向通入氮气作为保护气体，其他反应条件不变，将反应后的产物经氧化提纯后获得灰白色的纳米金刚石粉体。In the above reaction device, use the CO2 gas laser to output a continuous laser beam with a wavelength of 10.6 μm, change the circulating liquid medium to be a mixture of ethanol and water (volume ratio is 2:1), and the fine carbon powder has a particle size of less than 10 μm Nitrogen gas was introduced along the coaxial direction of the laser incident as a protective gas, and the other reaction conditions remained unchanged. After the reaction product was oxidized and purified, off-white nano-diamond powder was obtained.
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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 of carbon nanoparticle materials |
-
2004
- 2004-12-20 CN CNB2004100939730A patent/CN1313366C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 of carbon nanoparticle materials |
Non-Patent Citations (3)
| Title |
|---|
| 一种新的金刚石合成方法——强激光冲击合成金刚石的初步研究 陈晓虎等，南京航空航天大学学报，第30卷第1期 1998 * |
| 脉冲激光诱导液-固界面反应制备金刚石纳米晶 王金斌等，材料研究学报，第12卷第3期 1998 * |
| 金刚石产品的脉冲激光制备与应用 任志昂等，湘潭矿业学院学报，第15卷第1期 2000 * |
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| CN1663909A (en) | 2005-09-07 |
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