本文選題：毛細(xì)撞擊流反應(yīng)器　切入點(diǎn)：摻銻氧化錫(ATO)　出處：《北京化工大學(xué)》2015年碩士論文

【摘要】：二氧化錫作為一種典型的n型半導(dǎo)體材料,具有導(dǎo)電、抗腐蝕、熱穩(wěn)定性高等諸多優(yōu)良特性,銻的摻雜能夠大幅度降低其電阻率,并提高其透光率,因而摻銻氧化錫納米顆粒及其分散體被廣泛地應(yīng)用于半導(dǎo)體材料、電池、導(dǎo)電薄膜、透明隔熱玻璃、發(fā)光材料等諸多領(lǐng)域。毛細(xì)撞擊流反應(yīng)器作為一種新式的化工過(guò)程強(qiáng)化設(shè)備,具有高效的傳質(zhì)、傳熱和混合特性,在納米材料的制備方面擁有廣闊的應(yīng)用前景。本文以SnCl4·5H2O和SbCl3作為原材料,采用共沉淀法,首先探究了毛細(xì)撞擊流反應(yīng)器制備ATO納米顆粒的可行性。結(jié)果表明,毛細(xì)撞擊流反應(yīng)器能夠在較短的時(shí)間內(nèi)制備粒徑較小、分布均一、形貌規(guī)則,且結(jié)晶度較高的ATO納米顆粒。在可行性的基礎(chǔ)上,運(yùn)用毛細(xì)撞擊流反應(yīng)器制備ATO納米顆粒前驅(qū)體,然后通過(guò)煅燒法制備ATO納米顆粒。實(shí)驗(yàn)考察了摻雜度(Sb/Sn)、終點(diǎn)pH、體積流率和陳化方式等因素對(duì)ATO納米顆粒制備結(jié)果的影響。在前驅(qū)體制備基礎(chǔ)上引入水熱法替代煅燒制備得到ATO納米分散體,并探究了水熱時(shí)間、水熱溫度、水熱介質(zhì)以及水熱前洗滌操作對(duì)于分散體電性能和穩(wěn)定性的影響。本實(shí)驗(yàn)通過(guò)單一變量法得到了顆粒制備過(guò)程的優(yōu)化條件：Sb/Sn為1/10,終點(diǎn)pH范圍為2-3,體積流率范圍為90-120 mL·min-1,同時(shí),超聲陳化可極大縮短反應(yīng)時(shí)間。在該條件下制備得到的ATO納米顆粒粒徑較小,在10 nm左右,形貌規(guī)則、均一,結(jié)晶度較高,且電性能優(yōu)異,電阻率一般在100 Ω·cm以內(nèi)；水熱法制備ATO納米分散體的優(yōu)化條件：水熱前應(yīng)抽濾洗滌6次以上,水熱介質(zhì)以去離子水較佳,水熱溫度應(yīng)高于180℃,水熱時(shí)間不應(yīng)低于16 h。在該條件下制備的ATO納米分散體具有良好的穩(wěn)定性,可靜置較長(zhǎng)時(shí)間,且對(duì)應(yīng)顆粒電阻率較低,一般在200 Ω·cm左右。
[Abstract]:As a typical n-type semiconductor material, tin dioxide has many excellent properties, such as conductive, corrosion resistance, high thermal stability and so on. The doping of antimony can greatly reduce its resistivity and improve its transmittance.Therefore, antimony doped tin oxide nanoparticles and their dispersions are widely used in semiconductor materials, batteries, conductive films, transparent insulating glass, luminescent materials and so on.As a new type of chemical process strengthening equipment, capillary impinging flow reactor has high efficiency in mass transfer, heat transfer and mixing, and has a broad application prospect in the preparation of nanomaterials.In this paper, SnCl4 5H2O and SbCl3 were used as raw materials and coprecipitation method was used to investigate the feasibility of preparing ATO nanoparticles in capillary impingement flow reactor.The results show that the capillary impinging flow reactor can prepare ATO nanoparticles with small particle size, uniform distribution, regular morphology and high crystallinity in a short time.On the basis of feasibility, the precursor of ATO nanoparticles was prepared by capillary impinging flow reactor, and then ATO nanoparticles were prepared by calcination method.The effects of doping degree, pH, volume flow rate and aging mode on the preparation of ATO nanoparticles were investigated.Based on the preparation of precursor, hydrothermal method was introduced to prepare ATO nanocrystalline dispersion instead of calcination. The effects of hydrothermal time, hydrothermal temperature, hydrothermal medium and washing operation before hydrothermal treatment on the electrical properties and stability of the dispersion were investigated.In this experiment, the optimized conditions of particle preparation were obtained by single variable method: the ratio of SB / Sn was 1 / 10, the final pH was 2-3, and the volume flow rate was 90-120 mL min-1. At the same time, ultrasonic aging could greatly shorten the reaction time.The ATO nanoparticles prepared under these conditions are smaller in size, about 10 nm, regular in morphology, uniform in morphology, high in crystallinity, excellent in electrical properties, and the resistivity is generally within 100 惟 cm.The optimum conditions for the preparation of ATO nano-dispersion by hydrothermal method are as follows: before hydrothermal treatment, more than 6 times of filtration and washing should be carried out, the best hydrothermal medium should be deionized water, the hydrothermal temperature should be higher than 180 鈩，

本文編號(hào)：1723048