CN1388182A - Composite particle of conductive polymer and nano crystalline oxide and its prepn - Google Patents
Composite particle of conductive polymer and nano crystalline oxide and its prepn Download PDFInfo
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- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 27
- 239000011246 composite particle Substances 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 239000002019 doping agent Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims abstract description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 6
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- QENGPZGAWFQWCZ-UHFFFAOYSA-N 3-Methylthiophene Chemical compound CC=1C=CSC=1 QENGPZGAWFQWCZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 3
- 229930192474 thiophene Natural products 0.000 claims description 3
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 5
- 239000002159 nanocrystal Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 8
- 239000002114 nanocomposite Substances 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 229920000767 polyaniline Polymers 0.000 description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000001706 oxygenating effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
导电聚合物/纳米晶氧化物复合粒子及其制备方法,其特征是将起始原料(按重量计)纳米晶氧化物粒子粒径为1～100nm0.5～20份,单体0.1～20份,氧化剂0.1～20份,掺杂剂0.1～20份,表面活性剂0.1～10份和溶剂40～200份加入超声辐照反应器中,插入超声波变幅杆,通入氮气,通循环水浴温度为－5－30℃，启动超声波仪,进行聚合反应,超声功率调节范围在50～1500w,频率为2×104～109Hz,反应时间10分钟～5小时,获得导电聚合物/纳米晶氧化物复合粒子。
The conductive polymer/nanocrystalline oxide composite particle and its preparation method are characterized in that the starting raw material (by weight) nanocrystalline oxide particle diameter is 1-100nm 0.5-20 parts, and the monomer is 0.1-20 parts , 0.1-20 parts of oxidant, 0.1-20 parts of dopant, 0.1-10 parts of surfactant and 40-200 parts of solvent are added to the ultrasonic irradiation reactor, an ultrasonic horn is inserted, nitrogen gas is introduced, and the temperature of the water bath is circulated. When the temperature is -5-30°C, start the ultrasonic instrument and carry out the polymerization reaction. The ultrasonic power adjustment range is 50-1500w, the frequency is 2×10 4 ～10 9 Hz, and the reaction time is 10 minutes to 5 hours, and the conductive polymer/nanocrystal is obtained oxide composite particles.
Description
本发明涉及一种导电聚合物/纳米晶氧化物复合粒子的制备方法。The invention relates to a preparation method of conductive polymer/nano crystal oxide composite particles.
导电聚合物与纳米晶氧化物粒子的复合可以结合两种材料的优点，发展具有特殊功能的新型纳米复合材料，近年来引起了人们广泛的关注。特别是导电聚合物/纳米晶氧化物粒子结构具有重要应用前景。但导电聚合物不易熔融，也难以溶解在通常的溶剂中，采用一般的溶液或熔融共混难以制备真正的纳米复合材料。制备导电聚合物/无机纳米粒子复合材料一般用溶胶法，模板法和原位生成法，然而这些方法在制备导电聚合物包覆纳米晶氧化物复合粒子时遇到困难，这主要有以下原因：(一)无机纳米晶氧化物粒子的形成必须经过高温烧结，如锐钛矿TiO2需400～600℃高温烧结。而金红石TiO2需600～800℃高温烧结。而有机导电聚合物不可能承受那么高的温度。溶胶或原位聚合仅局限于制备无定性的纳米粒子/导电聚合物复合材料。(二)由于无机纳米粒子表面能极高，极易凝聚成团，通过一般的溶液直接混合难以真正实现纳米分散和纳米复合。通过电化学沉积法可制备导电聚合物/纳米晶氧化物粒子复合材料，如Yoneyama等采用电化学沉积法将纳米二氧化钛粒子引入到聚苯胺薄膜中，成功地用光进行书写[Yoneyama H.Adv Mater；1993，5：394～396]。然而这一方法得到的仅仅是0-2型(纳米TiO2沉积在聚苯胺薄膜表面)纳米复合材料。制备0-3型(核壳型)导电聚合物/纳米晶氧化物粒子复合材料难度很大，需要新的技术。The combination of conductive polymers and nanocrystalline oxide particles can combine the advantages of the two materials to develop new nanocomposites with special functions, which has attracted widespread attention in recent years. In particular, the conductive polymer/nanocrystalline oxide particle structure has important application prospects. However, conductive polymers are not easy to melt, and are also difficult to dissolve in common solvents. It is difficult to prepare real nanocomposites by general solution or melt blending. The preparation of conductive polymer/inorganic nanoparticle composites generally uses the sol method, template method and in-situ generation method. However, these methods encounter difficulties in the preparation of conductive polymer-coated nanocrystalline oxide composite particles. This is mainly due to the following reasons: (1) The formation of inorganic nanocrystalline oxide particles must be sintered at high temperature, such as anatase TiO 2 needs to be sintered at a high temperature of 400-600 °C. Rutile TiO 2 needs to be sintered at a high temperature of 600-800°C. However, organic conductive polymers cannot withstand such high temperatures. Sol or in situ polymerization is limited to the preparation of amorphous nanoparticle/conducting polymer composites. (2) Due to the extremely high surface energy of inorganic nanoparticles, they are easily agglomerated into groups, and it is difficult to truly realize nano-dispersion and nano-composite through direct mixing of general solutions. Conductive polymer/nanocrystalline oxide particle composites can be prepared by electrochemical deposition. For example, Yoneyama et al. introduced nano-titanium dioxide particles into polyaniline films by electrochemical deposition, and successfully wrote with light [Yoneyama H. Adv Mater ; 1993, 5:394-396]. However, this method only obtains 0-2 type (nano-TiO 2 deposited on the surface of polyaniline film) nanocomposites. It is very difficult to prepare type 0-3 (core-shell) conductive polymer/nanocrystalline oxide particle composites and requires new technologies.
本发明的目的是针对现有技术的不足而提供一种导电聚合物/纳米晶氧化物复合粒子的制备方法，其特点是利用超声空化产生的分散、粉碎、乳化等多重作用，在实现纳米晶氧化物粒子在水相中纳米分散的同时进行单体的聚合，生成的导电聚合物吸附沉积在纳米晶氧化物粒子表面形成0-3型核壳结构复合粒子。在导电聚合物含量为90％时，电导率可为10-1～10S.cm-1数量级。制备的复合粒子兼具导电聚合物和纳米晶氧化物粒子的功能。The object of the present invention is to provide a kind of preparation method of conductive polymer/nanocrystalline oxide composite particles in view of the deficiencies in the prior art, which is characterized in that it utilizes multiple functions such as dispersion, pulverization and emulsification produced by ultrasonic cavitation, and realizes nanocrystalline The crystalline oxide particles are nano-dispersed in the water phase while the monomers are polymerized, and the generated conductive polymer is adsorbed and deposited on the surface of the nano-crystalline oxide particles to form 0-3 type core-shell structure composite particles. When the content of the conductive polymer is 90%, the electrical conductivity can be on the order of 10 −1 to 10 S.cm −1 . The prepared composite particles have the functions of conductive polymer and nanocrystalline oxide particles.
本发明的目的是由以下技术措施实现的，其中所述原料份数除特殊说明外，均为重量份数。The object of the present invention is achieved by the following technical measures, wherein the parts of raw materials are parts by weight unless otherwise specified.
导电聚合物/纳米晶氧化物复合粒子的配方组分为：The formula components of conductive polymer/nanocrystalline oxide composite particles are:
纳米晶氧化物粒径为1～100nm：0.5～20份The particle size of nanocrystalline oxide is 1-100nm: 0.5-20 parts
单体：0.1～20份Monomer: 0.1 to 20 parts
氧化剂：0.1～20份Oxidizing agent: 0.1 to 20 parts
掺杂剂：0.1～20份Doping agent: 0.1 to 20 parts
表面活性剂：0.1～10份Surfactant: 0.1 to 10 parts
溶剂：40～200份Solvent: 40~200 parts
纳米晶氧化物粒子为ZnO，ZrO2，TiO2，Co3O4，Sb2O5，Fe3O4，V2O5，NiO，MnO2和/或SnO2至少一种。The nanocrystalline oxide particles are at least one of ZnO, ZrO 2 , TiO 2 , Co 3 O 4 , Sb 2 O 5 , Fe 3 O 4 , V 2 O 5 , NiO, MnO 2 and/or SnO 2 .
单体为苯胺，吡咯，噻吩和/或3-甲基噻吩至少一种。The monomer is at least one of aniline, pyrrole, thiophene and/or 3-methylthiophene.
溶剂为水和/或与水任意比例混合的溶剂醇和/或酮，出于经济和环境方面的考虑，以水最为优选。The solvent is water and/or solvent alcohol and/or ketone mixed with water in any proportion, and water is the most preferred in terms of economy and environment.
本发明反应物中的氧化剂是现有技术公知的过硫酸铵，三氯化铁，掺杂剂是现有技术公知的盐酸，磷酸，硫酸和/或有机磺酸，表面活性剂是现有技术公知的阴离子，阳离子和和/或非离子乳化剂，这些都是这一领域技术人员公知的知识。Oxygenating agent in the reactant of the present invention is ammonium persulfate known in the prior art, iron trichloride, dopant is hydrochloric acid known in the prior art, phosphoric acid, sulfuric acid and/or organic sulfonic acid, surfactant is prior art Known anionic, cationic and/or nonionic emulsifiers are within the knowledge of those skilled in the art.
导电聚合物/纳米晶氧化物复合粒子的制备方法：Preparation method of conductive polymer/nanocrystalline oxide composite particles:
1.将1～100nm 0.5～20份，单体0.1～20份，氧化剂0.1～20份，掺杂剂0.1～20份，表面活性剂0.1～10份和溶剂40～200份加入超声辐照反应器中，再将超声波变幅杆插入反应器内，1. Add 0.5-20 parts of 1-100nm, 0.1-20 parts of monomer, 0.1-20 parts of oxidant, 0.1-20 parts of dopant, 0.1-10 parts of surfactant and 40-200 parts of solvent into ultrasonic irradiation reaction In the reactor, insert the ultrasonic horn into the reactor,
2.通入氮气约1～5分钟，通氮气速率为0.1～50毫升/分钟，通循环水浴温度为-5-30℃，2. Introduce nitrogen for about 1 to 5 minutes, the nitrogen rate is 0.1 to 50 ml/min, and the temperature of the circulating water bath is -5-30°C.
3.启动超声波仪，进行聚合反应，超声功率调节范围在50～1500w，频率为2×104～109Hz，反应时间10分钟～5小时。3. Start the ultrasonic instrument to carry out the polymerization reaction, the ultrasonic power adjustment range is 50-1500w, the frequency is 2×10 4 ～10 9 Hz, and the reaction time is 10 minutes-5 hours.
本发明制备的产物为导电聚合物/纳米晶氧化物复合粒子，经透射电镜测试结果如图1，图2所示，图1为导电聚苯胺/纳米晶TiO2复合粒子(加入的苯胺单体与纳米晶TiO2的比例为1∶2)，复合粒子尺寸为40～50nm；图2为导电聚苯胺/纳米晶TiO2复合粒子(加入的苯胺单体与纳米晶TiO2的比例为1∶3)，复合粒子尺寸为100～200nm。透射电镜测定的复合粒子尺寸可在纳米和亚微米级，尺寸大小与无机纳米粒子的含量及实验参数有关。纳米粒子呈良好分散，包裹层厚度为5～60nm。The product prepared by the present invention is conductive polymer/nanocrystalline oxide composite particle, through transmission electron microscope test result as shown in Figure 1, as shown in Figure 2, Fig. 1 is conductive polyaniline/nanocrystalline TiO 2 composite particle (aniline monomer added The ratio of nanocrystalline TiO2 to nanocrystalline TiO2 is 1:2), and the composite particle size is 40-50nm; Figure 2 shows the conductive polyaniline/nanocrystalline TiO2 composite particle (the ratio of added aniline monomer to nanocrystalline TiO2 is 1: 3), the composite particle size is 100-200nm. The size of the composite particles measured by the transmission electron microscope can be in the nanometer and submicron levels, and the size is related to the content of the inorganic nanoparticles and the experimental parameters. The nanoparticles are well dispersed, and the thickness of the coating layer is 5-60nm.
可用于导电涂层、静电屏蔽，特种填料，新型光学吸收，多波段吸收，传感器，光催化，光电转换，压敏和光致变色等领域。It can be used in conductive coatings, electrostatic shielding, special fillers, new optical absorption, multi-band absorption, sensors, photocatalysis, photoelectric conversion, pressure sensitivity and photochromism and other fields.
本发明具有如下优点：The present invention has the following advantages:
1.制备的粒子兼具导电聚合物和纳米晶粒子的功能，如纳米聚苯胺的近红外光吸收性能和纳米TiO2的紫外吸收，可提供一种新型的光学吸收材料，1. The prepared particles have both the functions of conductive polymers and nanocrystalline particles, such as the near-infrared light absorption properties of nano-polyaniline and the ultraviolet absorption of nano- TiO2 , which can provide a new type of optical absorption material,
2.解决了纳米晶氧化物粒子的分散、稳定和复合的问题，2. Solve the problems of dispersion, stability and recombination of nanocrystalline oxide particles,
3.工艺简单，操作方便，3. The process is simple and the operation is convenient,
4.可极大地提高无机纳米粒子的含量而电导率降低不多。4. It can greatly increase the content of inorganic nanoparticles without reducing the electrical conductivity much.
实施例：Example:
下面通过实施例对本发明进行具体描述。有必要在此指出的是以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的技术熟练人员可以根据上述本发明内容对本发明作出一些非本质的改进和调整。The present invention is specifically described below by way of examples. It is necessary to point out that the following examples are only used to further illustrate the present invention, and cannot be interpreted as limiting the protection scope of the present invention. Those skilled in the art can make some non-essential improvements and improvements to the present invention according to the above-mentioned content of the present invention. Adjustment.
1.将锐钛矿纳米晶TiO2粒子粒径为27nm 2g、苯胺1克，过硫酸铵2.5克，20克36.5％的浓盐酸，十二烷基硫酸钠8克，水180g加入到反应器中，通入氮气约2分钟，并控制水浴温度15℃。然后启动VC-1500超声波仪器(Sonic & Materials Co.，USA)，开始聚合反应，反应过程中超声波功率为600w，频率为20kHz，氮气速率为5毫升/分钟保持恒定。反应1小时完毕。得到的纳米复合粒子尺寸为40～50nm，粒径分布均匀，包裹层厚度为5～15nm，电导率为0.7S.cm-1。1. Anatase nanocrystalline TiO 2 particle size is 27nm 2g, 1 gram of aniline, 2.5 grams of ammonium persulfate, 20 grams of 36.5% concentrated hydrochloric acid, 8 grams of sodium lauryl sulfate, and 180 g of water are added to the reactor , nitrogen gas was passed through for about 2 minutes, and the temperature of the water bath was controlled at 15°C. Then start the VC-1500 ultrasonic instrument (Sonic & Materials Co., USA) to start the polymerization reaction. During the reaction, the ultrasonic power is 600w, the frequency is 20kHz, and the nitrogen gas rate is kept constant at 5 ml/min. The reaction was completed in 1 hour. The size of the obtained nanocomposite particles is 40-50 nm, the particle size distribution is uniform, the thickness of the coating layer is 5-15 nm, and the electrical conductivity is 0.7 S.cm -1 .
2.将纳米晶ZrO2粒子粒径为17nm 3g、吡咯1克，过硫酸铵3克，10克36.5％的浓盐酸，十二烷基硫酸钠6克，水180g加入到反应器中，通入氮气约2分钟，并控制水浴温度10℃。然后启动VC-1500超声波仪器(Sonic & Materials Co.，USA)，开始聚合反应，反应过程中超声波功率为500w，频率为20kHz，氮气速率为10毫升/分钟保持恒定。反应1.5小时完毕。得到的纳米复合粒子尺寸为30～60nm，包裹层厚度为5～30nm，电导率为0.4S.cm-1。2. with nanocrystalline ZrO Particle size is 17nm 3g , pyrrole 1 gram, ammonium persulfate 3 grams, the concentrated hydrochloric acid of 10 gram 36.5%, sodium lauryl sulfate 6 grams, water 180g joins in the reactor, pass Infuse nitrogen gas for about 2 minutes, and control the temperature of the water bath to 10°C. Then start the VC-1500 ultrasonic instrument (Sonic & Materials Co., USA) to start the polymerization reaction. During the reaction, the ultrasonic power is 500w, the frequency is 20kHz, and the nitrogen rate is kept constant at 10ml/min. The reaction was completed in 1.5 hours. The size of the obtained nanocomposite particles is 30-60nm, the thickness of the coating layer is 5-30nm, and the electrical conductivity is 0.4S.cm -1 .
3.将纳米晶ZnO粒子粒径为20nm 2g、噻吩1克，过硫酸铵3.5克，20克36.5％的浓盐酸，十二烷基硫酸钠4克，水180g加入到反应器中，通入氮气约2分钟，并控制水浴温度5℃。然后启动VC-1500超声波仪器(Sonic & Materials Co.，USA)，开始聚合反应，反应过程中超声波功率为400w，频率为20kHz，氮气速率为8毫升/分钟保持恒定。反应0.5小时完毕。得到的纳米复合粒子尺寸为40～60nm，包裹层厚度为10～20nm，电导率为0.5S.cm-1。3. 20nm 2g, 1 gram of thiophene, 3.5 grams of ammonium persulfate, 20 grams of 36.5% concentrated hydrochloric acid, 4 grams of sodium lauryl sulfate, and 180 g of water are added to the reactor, and 3. Nitrogen for about 2 minutes, and control the temperature of the water bath at 5°C. Then start the VC-1500 ultrasonic instrument (Sonic & Materials Co., USA) to start the polymerization reaction. During the reaction, the ultrasonic power is 400w, the frequency is 20kHz, and the nitrogen gas rate is kept constant at 8 ml/min. The reaction was completed in 0.5 hours. The size of the obtained nanocomposite particles is 40-60nm, the thickness of the coating layer is 10-20nm, and the electrical conductivity is 0.5S.cm -1 .
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| CN101864098A (en) * | 2010-06-03 | 2010-10-20 | 四川大学 | In situ reduction preparation method of polymer/graphene composites |
| CN107262156A (en) * | 2017-07-28 | 2017-10-20 | 赵丽 | A kind of Photocatalytic nano composite material and preparation method thereof |
| CN109385143A (en) * | 2017-08-08 | 2019-02-26 | Tcl集团股份有限公司 | A kind of conducting polymer ink and preparation method thereof and QLED device |
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| CN101864098A (en) * | 2010-06-03 | 2010-10-20 | 四川大学 | In situ reduction preparation method of polymer/graphene composites |
| CN107262156A (en) * | 2017-07-28 | 2017-10-20 | 赵丽 | A kind of Photocatalytic nano composite material and preparation method thereof |
| CN109385143A (en) * | 2017-08-08 | 2019-02-26 | Tcl集团股份有限公司 | A kind of conducting polymer ink and preparation method thereof and QLED device |
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