CN101898761A - Method for Dispersing Detonation Nanodiamonds in Liquid Phase - Google Patents
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Abstract
本发明公开了一种在液相中分散爆轰法纳米金刚石的方法，步骤为：a、以商业爆轰法纳米金刚石粉末为原料，混合于液体介质中，利用超声波进行超声处理，形成悬浮液；b、使用脉冲激光轰击该悬浮液，作用区域的激光功率密度为106W/cm2，作用时间为1-3h，得到的悬浮液稳定、不沉淀；c、对激光轰击后的产物进行强酸氧化处理。本发明工艺简单，激光作用过程安全可控，克服了现有分散爆轰法纳米金刚石的工艺中容易引起的产物污染，并在各种溶液中使团聚的爆轰法纳米金刚石解团聚，得到单分散的金刚石纳米颗粒。本发明在涂料、高分子复合材料、润滑等领域可以得到广泛应用。
The invention discloses a method for dispersing detonation method nano-diamonds in a liquid phase. The steps are as follows: a. Commercial detonation method nano-diamond powders are used as raw materials, mixed in a liquid medium, and ultrasonically treated by ultrasonic waves to form a suspension ; b. Bombard the suspension with a pulsed laser, the laser power density in the action area is 10 6 W/cm 2 , and the action time is 1-3 hours. The obtained suspension is stable and does not precipitate; c. The product after laser bombardment is subjected to Strong acid oxidation treatment. The process of the invention is simple, the laser action process is safe and controllable, overcomes the product pollution that is easily caused in the existing process of dispersing detonation method nano-diamonds, and deagglomerates the agglomerated detonation method nano-diamonds in various solutions to obtain a single Dispersed diamond nanoparticles. The invention can be widely used in the fields of paint, polymer composite material, lubrication and the like.
Description
技术领域technical field
本发明是关于纳米金刚石的制备方法，尤其涉及在液相中分散爆轰法纳米金刚石、以制备纯净的纳米金刚石的方法。The invention relates to a preparation method of nano-diamonds, in particular to a method for dispersing detonation nano-diamonds in a liquid phase to prepare pure nano-diamonds.
背景技术Background technique
在陨星、原行星星云、星际尘埃或火山灰中，存在着天然的金刚石，有些还会以宝石级钻石的形式存在，是人们喜爱的贵重饰品。近年来随着纳米材料科学的发展，尤其是碳纳米材料如碳纳米管的发现与应用，纳米级的金刚石做为另一种新型的碳纳米材料逐渐被人们认识和应用。由于纳米金刚石具有优良的生物相容性、尺寸稳定性、电绝缘性、耐高温高压及化学稳定性，目前已经被应用于很多方面，比如用作润滑油或高分子复合材料的添加剂、药物载体及细胞标记。Diamonds exist naturally in meteorites, protoplanetary nebulae, interstellar dust or volcanic ash, and some exist in the form of gem-quality diamonds, which are precious jewelry that people love. In recent years, with the development of nanomaterials science, especially the discovery and application of carbon nanomaterials such as carbon nanotubes, nanoscale diamonds have gradually been recognized and applied as another new type of carbon nanomaterials. Due to its excellent biocompatibility, dimensional stability, electrical insulation, high temperature and high pressure resistance, and chemical stability, nanodiamonds have been used in many fields, such as additives for lubricating oil or polymer composites, and drug carriers. and cell markers.
目前为止，人们已经开发出多种制备纳米金刚石的方法，其中爆轰法是制备金刚石中最常用也是工业化最成功的一种方法，用于大规模纳米金刚石的生产，参见Greiner NR，Phillips DS，Johnson JD，Volk F.Diamonds in detonation soot.Nature.1988；333(440)：440-2。在爆轰法中，通常用TNT和环三次甲基三硝基胺的混合物作起始材料，前者提供主要的碳源，后者提供主要的能量，在密闭容器中利用爆炸产生的高温高压，就会使碳质转变为金刚石。一般形成的原始纳米金刚石颗粒尺寸较小(5nm左右)，表面覆盖有石墨结构或非晶碳质，这些非金刚石相碳质可以通过强酸氧化除去。利用这种方法制备的纳米金刚石也被称作爆轰法纳米金刚石。So far, people have developed a variety of methods for preparing nano-diamonds. Among them, the detonation method is the most commonly used and industrialized method for preparing diamonds. It is used for the production of large-scale nano-diamonds. See Greiner NR, Phillips DS, Johnson JD, Volk F. Diamonds in detonation soot. Nature. 1988; 333(440): 440-2. In the detonation method, a mixture of TNT and cyclotrimethyltrinitroamine is usually used as the starting material, the former provides the main carbon source, the latter provides the main energy, and the high temperature and pressure generated by the explosion is used in a closed container. It turns carbon into diamond. Generally, the original nano-diamond particles are small in size (about 5nm), and the surface is covered with graphite structure or amorphous carbon. These non-diamond phase carbon can be removed by strong acid oxidation. Nanodiamonds prepared by this method are also called detonation nanodiamonds.
尽管在20世纪60年代，人们就已经利用爆轰法成功制备了纳米金刚石，但随后的40年，由于纳米金刚石粉末团聚严重，使得纳米金刚石的微观结构一直不为人所知，纳米金刚石也一直没有得到研究人员广泛重视和应用。直到2003年，日本科学家Osawa等人通过球磨纳米金刚石的实验认识到了纳米金刚石团簇结构的真实面目，也就是四级体系——第一级为原始纳米金刚石颗粒(4-5nm)，第二级是由原始纳米金刚石颗粒通过化学键束缚在一起的粘着体(100-200nm)，第三级是由第二级粘着体之间的范德华力聚集在一起形成的团聚体(2-3μm)，第四级是由第三级团聚体堆积而成的块体(30-50μm)。并于2005年利用球磨的方法制备了在溶液中稳定分散、不沉淀的纳米金刚石溶胶，利用动态光散射测得球磨后的纳米金刚石颗粒尺寸分布在5nm左右。参见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.Although in the 1960s, people had successfully prepared nano-diamonds by the detonation method, but in the following 40 years, due to the serious agglomeration of nano-diamond powder, the microstructure of nano-diamonds has been unknown, and nano-diamonds have never been known. It has been widely valued and applied by researchers. Until 2003, Japanese scientists Osawa and others realized the true face of the nano-diamond cluster structure through the experiment of ball milling nano-diamonds, that is, the four-level system-the first level is the original nano-diamond particles (4-5nm), and the second level Adhesives (100-200nm) bound together by original nano-diamond particles through chemical bonds, the third level is agglomerates (2-3μm) formed by the van der Waals force between the second-level adherents, the fourth The first stage is a block (30-50 μm) formed by the accumulation of tertiary aggregates. In 2005, a nano-diamond sol that was stably dispersed in the solution without precipitation was prepared by ball milling. The size distribution of nano-diamond particles after ball milling was measured to be about 5nm by dynamic light scattering. See Kruger A, Kataoka F, Ozawa M, Fujino T, Suzuki Y, Aleksenskii AE, et al. Usually tight aggregation in detonation nanodiamond: Identification and disintegration. Carbon. 2005 Jul; 43(8): 1722-30.
但是，由于纳米金刚石的硬度很高，机械球磨的方法不可避免会污染纳米金刚石粉末，影响其后续的应用；并且到目前为止，还没有真正观察到纳米金刚石真实的分散状态的存在。因此，如何在液相中分散爆轰法纳米金刚石还是一个亟待解决的问题。However, due to the high hardness of nano-diamond, the method of mechanical ball milling will inevitably pollute the nano-diamond powder and affect its subsequent application; and so far, the existence of a true dispersed state of nano-diamond has not been observed. Therefore, how to disperse detonation nanodiamonds in the liquid phase is still an urgent problem to be solved.
发明内容Contents of the invention
本发明的目的是解决爆轰法纳米金刚石严重团聚、现有分散爆轰法纳米金刚石工艺中对纳米金刚石的污染等问题。利用激光技术制备纳米材料的优势，提供一种无污染、工艺简单的、对产物进行提纯后，能够得到在液体介质中稳定分散、不沉淀的纳米金刚石悬浮液的新方法。The purpose of the invention is to solve the problems of severe agglomeration of nano-diamonds in detonation method, pollution of nano-diamonds in the existing nano-diamond process of dispersed detonation method, and the like. Using the advantages of laser technology to prepare nano-materials, it provides a new method that is pollution-free, simple in process, and can obtain nano-diamond suspensions that are stably dispersed in liquid media without precipitation after purification of the products.
本发明通过以下技术方案予以实现：The present invention is achieved through the following technical solutions:
在液相中分散爆轰法纳米金刚石的方法，具有如下步骤：The method for dispersing detonation method nano-diamond in liquid phase has the following steps:
a、以商业爆轰法纳米金刚石粉末为原料，其粒径为2-10nm，将其混合于液体介质中，所述纳米金刚石溶液为0.1-0.5mg/mL，然后利用超声波进行超声处理，以形成爆轰法纳米金刚石的悬浮液；a. Using commercial detonation method nano-diamond powder as raw material, its particle size is 2-10nm, it is mixed in the liquid medium, the described nano-diamond solution is 0.1-0.5mg/mL, and then utilizes ultrasonic wave to carry out ultrasonic treatment, with Forming a suspension of detonation nanodiamonds;
b、使用脉冲激光轰击步骤a的爆轰法纳米金刚石悬浮液，激光束汇聚于悬浮液表面，脉冲激光束的波长为1.06μm，脉冲宽度为1.0ms，脉冲频率为10-30Hz，作用区域的激光功率密度为106W/cm2，激光作用的时间为1-3h；激光作用后的爆轰法纳米金刚石悬浮液稳定、不沉淀；b. Use the pulsed laser to bombard the detonation method nano-diamond suspension in step a, the laser beam converges on the surface of the suspension, the wavelength of the pulsed laser beam is 1.06 μm, the pulse width is 1.0 ms, and the pulse frequency is 10-30 Hz. The laser power density is 10 6 W/cm 2 , and the laser action time is 1-3h; the detonation nano-diamond suspension after laser action is stable and does not precipitate;
c、对激光轰击后的产物进行强酸氧化处理，除去产物中的非金刚石的碳质如非晶碳，得到纯净的爆轰法纳米金刚石。c. Perform strong acid oxidation treatment on the product after laser bombardment to remove non-diamond carbon such as amorphous carbon in the product to obtain pure detonation nano-diamond.
所述步骤a的液体介质为去离子水或醇、酮、醚等一切可以流动的液体以及由它们之间任意组合形成的任意比例的混合液。The liquid medium in the step a is deionized water or all flowable liquids such as alcohols, ketones, ethers, etc., and a mixed liquid in any proportion formed by any combination of them.
所述步骤b的激光轰击采用Nd:YAG固体激光器。The laser bombardment in step b uses a Nd:YAG solid-state laser.
所述步骤b的过程中，对盛放悬浮液的反应容器采用外部循环水浴冷却方式吸收多余的热量，防止溶液沸腾，使液体介质处于常温之下。In the process of step b, the reaction vessel containing the suspension is cooled by an external circulating water bath to absorb excess heat, prevent the solution from boiling, and keep the liquid medium at room temperature.
所述步骤c的强酸为高氯酸。The strong acid of the step c is perchloric acid.
本发明的有益效果是，工艺简单，激光作用过程安全可控，克服了利用球磨的方法分散爆轰法纳米金刚石所引起的产物污染，并在多种溶液中实现了爆轰法纳米金刚石的分散。此外，利用激光轰击液体中纳米金刚石可以直接使纳米金刚石颗粒表面产生有机物修饰，有利于后续在复合材料及生物方面的应用，也使纳米金刚石更具科学研究价值。分散的爆轰法纳米金刚石可以在涂料、高分子复合材料、润滑等领域得到广泛应用。The beneficial effect of the invention is that the process is simple, the laser action process is safe and controllable, the product pollution caused by the dispersion of detonation method nano-diamonds by the method of ball milling is overcome, and the dispersion of detonation method nano-diamonds is realized in various solutions . In addition, the use of laser bombardment of nano-diamond in liquid can directly modify the surface of nano-diamond particles with organic matter, which is beneficial to the subsequent application in composite materials and biology, and also makes nano-diamond more scientific research value. Dispersed detonation nano-diamonds can be widely used in coatings, polymer composites, lubrication and other fields.
附图说明Description of drawings
图1为激光轰击爆轰法纳米金刚石悬浮液的激光液相烧蚀装置示意图；Fig. 1 is the schematic diagram of the laser liquid phase ablation device of laser bombardment detonation method nano-diamond suspension;
图2为爆轰法纳米金刚石原料的透射电子显微镜照片；Fig. 2 is the transmission electron micrograph of detonation method nano-diamond raw material;
图3为实施例2中激光轰击水中的纳米金刚石悬浮液后得到的纳米金刚石颗粒的透射电子显微镜照片；Fig. 3 is the transmission electron micrograph of the nano-diamond particle that obtains after the nano-diamond suspension in the laser bombardment water in embodiment 2;
图4为激光轰击丙烯酸中的纳米金刚石悬浮液后得到的纳米金刚石颗粒的透射电子显微镜照片。Fig. 4 is a transmission electron micrograph of nano-diamond particles obtained after laser bombardment of nano-diamond suspension in acrylic acid.
图1中附图标记为：Reference numerals in Fig. 1 are:
1——Nd:YAG固体激光器 2——脉冲激光束 3——循环冷却水1——Nd:YAG solid-state laser 2——pulse laser beam 3——circulating cooling water
4——超声波发生器 5——反射镜 6——聚光镜4——ultrasonic generator 5——mirror 6——concentrating mirror
7——爆轰法纳米金刚石悬浮液7——Detonation method nano-diamond suspension
具体实施方式Detailed ways
本发明采用的装置如图1所示，由Nd:YAG固体激光器1产生的脉冲激光束2，经过反射镜5反射后再经聚光镜6汇聚，将脉冲激光束2聚焦于爆轰法纳米金刚石悬浮液7的液面处，利用超声波发生器4对爆轰法纳米金刚石悬浮液7进行超声处理，并在其外部用循环冷却水3对体系进行冷却。The device that the present invention adopts is as shown in Figure 1, and the pulsed laser beam 2 that is produced by Nd:YAG solid-state laser 1 is converged by condenser lens 6 again after reflecting mirror 5, and pulsed laser beam 2 is focused on detonation method nano-diamond suspension At the liquid level of the liquid 7, the detonation method nano-diamond suspension 7 is ultrasonically treated by an ultrasonic generator 4, and the system is cooled by circulating cooling water 3 outside it.
以商业爆轰法纳米金刚石粉末为原料，其粒径为2-10nm。The commercial detonation method nano-diamond powder is used as the raw material, and its particle size is 2-10nm.
具体实施例如下：Specific examples are as follows:
实施例1Example 1
a、将50mg爆轰法纳米金刚石粉末加入到100mL去离子水中，这里纳米金刚石粉末的平均粒径为5nm，利用超声波发生器对其进行超声处理，以形成爆轰法纳米金刚石悬浮液。a. Add 50 mg of detonation nano-diamond powder into 100 mL of deionized water, where the average particle size of the nano-diamond powder is 5 nm, and ultrasonically treat it with an ultrasonic generator to form a detonation nano-diamond suspension.
b、使用脉冲激光轰击步骤a的爆轰法纳米金刚石悬浮液，激光焦点汇聚于液体表面处，在激光束作用的液面微区内，纳米金刚石团聚体中的非晶碳质会吸收激光产生高温并分解，非晶碳分解的高温会使纳米金刚石颗粒之间的共价键断开，从而使团聚的爆轰法纳米金刚石解团聚，形成单分散的金刚石纳米颗粒。作用区域的激光功率密度在106W/cm2，激光作用的时间为3h，脉冲激光束的波长为1.06μm，脉冲宽度为1.0ms，脉冲频率为10Hz，采用Nd:YAG固体激光器。b. Use the pulsed laser to bombard the detonation method nano-diamond suspension in step a, the laser focus converges on the liquid surface, and in the micro-area of the liquid surface where the laser beam acts, the amorphous carbon in the nano-diamond aggregate will absorb the laser to generate High temperature and decomposition, the high temperature of amorphous carbon decomposition will break the covalent bonds between nano-diamond particles, so that the agglomerated detonation nano-diamonds will be deagglomerated to form monodisperse diamond nanoparticles. The laser power density in the action area is 10 6 W/cm 2 , the laser action time is 3h, the wavelength of the pulsed laser beam is 1.06μm, the pulse width is 1.0ms, and the pulse frequency is 10Hz. Nd:YAG solid-state laser is used.
利用超声波对纳米金刚石粉末悬浮液进行分散，可以形成均匀的纳米金刚石悬浮液，从而使得激光在不同时刻作用于不同的纳米金刚石悬浮液微区，有利于提高激光分散爆轰法纳米金刚石的效率。The use of ultrasound to disperse the nano-diamond powder suspension can form a uniform nano-diamond suspension, so that the laser can act on different micro-areas of the nano-diamond suspension at different times, which is conducive to improving the efficiency of the laser dispersion detonation method of nano-diamonds.
爆轰法纳米金刚石粉末为利用爆轰法制备的商业级纳米金刚石粉末，其粒径为2-10nm。参见图2，所示为爆轰法纳米金刚石的透射电子显微镜照片，可以看出纳米金刚石颗粒团聚在一起，颗粒表面有非晶碳质存在。爆轰法纳米金刚石原料溶于水中后，利用超声波超声30分钟后，静置十几分钟后即沉淀，表明爆轰法纳米金刚石团聚严重。The detonation method nano-diamond powder is a commercial-grade nano-diamond powder prepared by the detonation method, and its particle size is 2-10nm. Referring to FIG. 2 , it shows a transmission electron micrograph of nano-diamonds by detonation method. It can be seen that the nano-diamond particles are agglomerated together, and there is amorphous carbon on the surface of the particles. After the detonation method nano-diamond raw material is dissolved in water, after 30 minutes of supersonication, it will precipitate after standing for more than ten minutes, which shows that the detonation method nano-diamond agglomeration is serious.
在激光轰击过程中，对盛放悬浮液的反应容器采用外部循环水浴冷却方式吸收多余的热量，防止溶液沸腾，并使液体介质处于常温之下。During the laser bombardment process, the reaction vessel containing the suspension is cooled by an external circulating water bath to absorb excess heat, prevent the solution from boiling, and keep the liquid medium at room temperature.
激光作用后的纳米金刚石悬浮液稳定、不沉淀。The nano-diamond suspension after laser action is stable and does not precipitate.
c、对激光轰击后的爆轰法纳米金刚石进行酸洗，采用高氯酸，除去产物中的非金刚石的碳质，得到纯净的纳米金刚石。c. Pickling the detonation method nano-diamond after laser bombardment, using perchloric acid to remove non-diamond carbon in the product to obtain pure nano-diamond.
实施例2Example 2
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。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1.0ms，脉冲频率为20Hz)，经过光学透镜汇聚后，聚焦于爆轰法纳米金刚石悬浮液的表面处。液体介质为去离子水，将爆轰法纳米金刚石悬浮液利用超声波进行分散，以形成均匀的爆轰法纳米金刚石悬浮液。将盛放爆轰法纳米金刚石悬浮液的容器采用外部循环水浴冷却。激光连续轰击1h，将反应后的产物经酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为4nm。参见图3，所示为激光轰击去离子水中的爆轰法纳米金刚石悬浮液得到的分散的纳米金刚石颗粒的透射电镜照片，可以看出得到的纳米金刚石颗粒分散存在，不团聚。In the same reaction device, the processing conditions not described are all the same as in Example 1. The Nd-YAG solid-state laser outputs a pulsed laser beam with a wavelength of 1.06 μm (pulse width 1.0 ms, pulse frequency 20 Hz), which is focused on the surface of the detonation nano-diamond suspension after being converged by an optical lens. The liquid medium is deionized water, and the detonation method nano-diamond suspension is dispersed by ultrasonic waves to form a uniform detonation method nano-diamond suspension. The container containing the detonation nano-diamond suspension is cooled by an external circulating water bath. After continuous laser bombardment for 1 h, the reacted product was purified by acid washing to obtain gray diamond nanoparticles with an average particle size of 4 nm. Referring to FIG. 3 , it shows a transmission electron micrograph of dispersed nano-diamond particles obtained by laser bombarding deionized nano-diamond suspension in deionized water. It can be seen that the obtained nano-diamond particles are dispersed and not agglomerated.
实施例3Example 3
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。改变脉冲激光束的脉冲频率为10Hz。液体介质为去离子水，将爆轰法纳米金刚石悬浮液利用超声波进行分散，以形成均匀的爆轰法纳米金刚石悬浮液。将盛放爆轰法纳米金刚石悬浮液的容器采用外部循环水浴冷却。激光连续轰击1h，将反应后的产物经酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为4nm。In the same reaction device, the processing conditions not described are all the same as in Example 1. Change the pulse frequency of the pulsed laser beam to 10 Hz. The liquid medium is deionized water, and the detonation method nano-diamond suspension is dispersed by ultrasonic waves to form a uniform detonation method nano-diamond suspension. The container containing the detonation nano-diamond suspension is cooled by an external circulating water bath. After continuous laser bombardment for 1 h, the reacted product was purified by acid washing to obtain gray diamond nanoparticles with an average particle size of 4 nm.
实施例4Example 4
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。改变脉冲激光束的脉冲频率为30Hz。液体介质为去离子水，将爆轰法纳米金刚石悬浮液利用超声波进行分散，以形成均匀的爆轰法纳米金刚石悬浮液。将盛放爆轰法纳米金刚石悬浮液的容器采用外部循环水浴冷却。激光连续轰击1h，将反应后的产物经酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为4nm。In the same reaction device, the processing conditions not described are all the same as in Example 1. Change the pulse frequency of the pulsed laser beam to 30 Hz. The liquid medium is deionized water, and the detonation method nano-diamond suspension is dispersed by ultrasonic waves to form a uniform detonation method nano-diamond suspension. The container containing the detonation nano-diamond suspension is cooled by an external circulating water bath. After continuous laser bombardment for 1 h, the reacted product was purified by acid washing to obtain gray diamond nanoparticles with an average particle size of 4 nm.
实施例5Example 5
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。只改变激光连续轰击时间为2h，将反应后的产物经酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为4nm。In the same reaction device, the processing conditions not described are all the same as in Example 1. Only changing the continuous laser bombardment time to 2h, the reaction product was purified by pickling to obtain gray diamond nanoparticles with an average particle size of 4nm.
实施例6Example 6
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。只改变激光连续轰击时间为3h，将反应后的产物经酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为4nm。In the same reaction device, the processing conditions not described are all the same as in Example 1. Only changing the continuous laser bombardment time to 3h, the reaction product was purified by pickling to obtain gray diamond nanoparticles with an average particle size of 4nm.
实施例7Example 7
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。激光轰击去离子水中的爆轰法纳米金刚石悬浮液2小时后，利用高氯酸进行氧化处理。将得到的爆轰法纳米金刚石悬浮液放置5个月后其仍然以稳定的悬浮液形式存在，表明纳米金刚石颗粒在溶液中分散良好，平均粒径为4nm。In the same reaction device, the processing conditions not described are all the same as in Example 1. The detonation nanodiamond suspension in deionized water was laser bombarded for 2 hours and then oxidized with perchloric acid. The nano-diamond suspension obtained by the detonation method is still in the form of a stable suspension after being placed for 5 months, indicating that the nano-diamond particles are well dispersed in the solution, and the average particle size is 4nm.
实施例8Example 8
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。改变液体介质为乙醇，将10mg爆轰法纳米金刚石粉末与30mL丙烯酸混合，其它条件不变，将激光作用后的产物进行酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为5nm。将提纯后的产物分散于乙醇中仍可以形成稳定的纳米金刚石悬浮液，表明其分散性良好。In the same reaction device, the processing conditions not described are all the same as in Example 1. Change the liquid medium to ethanol, mix 10mg detonation nano-diamond powder with 30mL acrylic acid, and keep other conditions unchanged, pickle and purify the product after laser action to obtain gray diamond nanoparticles with an average particle size of 5nm. Dispersing the purified product in ethanol can still form a stable nano-diamond suspension, which shows that its dispersibility is good.
实施例9Example 9
在同上的反应装置中，没有说明的工艺条件均与实施例1相同。改变液体介质为丙烯酸，其它条件不变，将激光作用后的产物进行酸洗提纯后获得灰色的金刚石纳米颗粒，平均粒径为5nm。参见图4，所示为激光轰击去丙烯酸中的爆轰法纳米金刚石悬浮液得到的分散的纳米金刚石颗粒的透射电镜照片，可以看出得到的纳米金刚石颗粒分散存在，没有团聚现象。In the same reaction device, the processing conditions not described are all the same as in Example 1. The liquid medium is changed to acrylic acid, and other conditions remain unchanged, and the product after laser action is pickled and purified to obtain gray diamond nanoparticles with an average particle diameter of 5 nm. Referring to FIG. 4 , it shows a transmission electron micrograph of dispersed nano-diamond particles obtained by laser bombarding the detonation method nano-diamond suspension in acrylic acid. It can be seen that the obtained nano-diamond particles are dispersed and there is no agglomeration phenomenon.
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