本文選題：間苯二酚-甲醛 + 反相懸浮法　； 參考：《哈爾濱工業(yè)大學(xué)》2010年博士論文

【摘要】： 本文以間苯二酚(R)-甲醛(F)為炭前驅(qū)體及模板,采用反相懸浮法和水熱法制備了炭空心微球,氧化物空心微球,及氧化物/炭復(fù)合微球。進(jìn)一步利用RF凝膠特性,結(jié)合模板技術(shù)制備了Sn-In_2O_3/炭(ITO/C)一維復(fù)合納米材料,驗(yàn)證了以RF為前驅(qū)體制備空心微納米材料的結(jié)構(gòu)可控性。采用X-射線衍射(XRD)、掃描電子顯微鏡(SEM)、透射電子顯微鏡(TEM、HRTEM)、傅立葉變換紅外光譜(FT-IR)、氮?dú)馕降确治鍪侄?系統(tǒng)研究了材料微觀組織結(jié)構(gòu),分析了結(jié)構(gòu)形成機(jī)理。探索了RF炭微球及ZnO/C復(fù)合微球在鋰離子電池和超級(jí)電容器材料方面的應(yīng)用,研究了RF炭微球結(jié)構(gòu)、形態(tài)對(duì)電性能的影響。討論了ITO/C一維復(fù)合納米材料在氣敏元件中的應(yīng)用。 首次以RF為炭前驅(qū)體,通過(guò)反相懸浮法,制備了形態(tài)可控的RF炭微球。實(shí)驗(yàn)結(jié)果表明,RF前驅(qū)體溶液的初始pH值、催化劑和表面活性劑類型是獲得RF炭空心球結(jié)構(gòu),“碗狀”結(jié)構(gòu)和膠囊等結(jié)構(gòu)的重要反應(yīng)參數(shù)。分析了不同形態(tài)的RF炭微球的形成機(jī)制,研究了RF炭微球的電學(xué)性能。電化學(xué)分析結(jié)果表明,以Na_2CO_3為催化劑所制備的RF炭微球電極材料具有理想的電容行為,循環(huán)伏安性能穩(wěn)定、可逆,適用于大電流下充放電。以K_2CO_3為催化劑制備的RF炭膠囊作為鋰離子電池陰極材料,充放電、循環(huán)特性測(cè)試結(jié)果表明,其初始放電電容量可達(dá)1059mAh/g,且電性能穩(wěn)定,循環(huán)效率可達(dá)99%,是理想的鋰離子電池陰極材料。 以表面功能化修飾的RF凝膠微球?yàn)槟０?制備了結(jié)構(gòu)完整、粒徑分布均勻的氧化物空心微球。研究了不同表面修飾劑對(duì)RF凝膠微球表面改性的作用機(jī)理,分析了RF表面改性對(duì)氧化物空心微球結(jié)構(gòu)的影響。通過(guò)炭化Zn~(2+)負(fù)載的RF凝膠微球,制備了ZnO/C復(fù)合微球。其穩(wěn)定的循環(huán)伏安特性和法拉第氧化-還原反應(yīng)效應(yīng)表明,ZnO/C復(fù)合微球可作為理想的超級(jí)電容器材料。 首次將ITO溶液和RF溶液組成復(fù)合前驅(qū)體,并結(jié)合多孔氧化鋁(AAO)模板技術(shù),制備了ITO/C一維復(fù)合納米材料。討論了ITO/RF復(fù)合前驅(qū)體中ITO濃度對(duì)ITO/C一維復(fù)合納米結(jié)構(gòu)的影響。結(jié)果表明,通過(guò)ITO與RF前驅(qū)體溶液的同步溶膠-凝膠化過(guò)程,有效地將ITO納米顆粒復(fù)合到RF凝膠網(wǎng)絡(luò)中形成一維納米復(fù)合材料。氣敏性測(cè)試表明,所制備的ITO/C一維復(fù)合納米材料具有較高氫氣靈敏度和較短的響應(yīng)時(shí)間,可作為氫氣氣敏材料。 以葡萄糖溶液為前驅(qū)體,利用水熱法制備了結(jié)構(gòu)完整、粒徑分布均勻的炭微球。通過(guò)加入不同添加劑可對(duì)炭微球結(jié)構(gòu)進(jìn)行有效控制。以所制備的炭微球?yàn)槟０?制備了多種氧化物空心微球。利用ZnCl_2/RF/葡萄糖復(fù)合體系的水熱反應(yīng)過(guò)程制備了結(jié)構(gòu)完整的Zn/炭復(fù)合前驅(qū)體微球,通過(guò)熱處理除去炭模板,并調(diào)控?zé)崽幚項(xiàng)l件,控制得到了多種形態(tài)的ZnO空心微球,為RF凝膠微球的水熱制備及其在生物單糖方面的應(yīng)用奠定了基礎(chǔ)。
[Abstract]:In this paper, carbon hollow microspheres, oxide hollow microspheres and oxide / carbon composite microspheres were prepared by reversed-phase suspension method and hydrothermal method using resorcinol (R) -formaldehyde (F) as carbon precursor and template. Furthermore, the one-dimensional composite nanocomposites of Sn-In_2O_3/ ITO / C were prepared by using RF gel characteristics and template technology. The structure controllability of hollow nanocomposites prepared with RF as precursor was verified. The microstructure and formation mechanism of the materials were systematically studied by means of X ray diffraction, scanning electron microscope (SEM), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FTIR), FT-IRT, nitrogen adsorption and so on. The microstructures of the materials were studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption. The applications of RF carbon microspheres and ZnO/C composite microspheres in lithium ion batteries and supercapacitor materials were investigated. The effects of the structure and morphology of RF carbon microspheres on the electrical properties were studied. The application of ITO/C one-dimensional composite nanomaterials in gas sensor is discussed. RF carbon microspheres with controllable morphology were prepared by reverse phase suspension with RF as precursor for the first time. The experimental results show that the initial pH value of RF precursor solution, the type of catalyst and surfactant are important reaction parameters for obtaining RF carbon hollow sphere structure, "bowl" structure and capsule structure. The formation mechanism of RF carbon microspheres with different morphology was analyzed and the electrical properties of RF carbon microspheres were studied. The results of electrochemical analysis show that the RF carbon microsphere electrode prepared with Na_2CO_3 as catalyst has ideal capacitance, stable cyclic voltammetry and reversible performance. It is suitable for charging and discharging at high current. RF carbon capsules prepared with K_2CO_3 as cathode material for lithium-ion batteries were tested for charge-discharge and cyclic characteristics. The results show that the initial discharge capacity of RF carbon capsules can reach 1059mAh / g, and its electrical properties are stable. The cycle efficiency can reach 99%. It is an ideal cathode material for lithium ion battery. The surface functionalized RF gel microspheres were used as templates to prepare hollow oxide microspheres with complete structure and uniform particle size distribution. The mechanism of surface modification of RF gel microspheres with different surface modifiers was studied, and the effect of RF surface modification on the structure of oxide hollow microspheres was analyzed. ZnO/C composite microspheres were prepared by carbonized Zn~(2 loaded RF gel microspheres. The stable cyclic voltammetry and Faraday redox effect indicate that ZnO / C composite microspheres can be used as ideal supercapacitor materials. For the first time, ITO/C one-dimensional composite nanomaterials were prepared by using ITO solution and RF solution as composite precursors and combined with porous alumina (AAO) template technology. The effect of ITO concentration in ITO/RF composite precursor on ITO/C one-dimensional composite nanostructures was discussed. The results show that ITO nanoparticles are effectively recombined into RF gel network to form one-dimensional nanocomposites through the synchronous sol-gel process of ITO and RF precursor solution. The gas sensitivity test showed that the ITO/C one-dimensional composite nanomaterials had higher hydrogen sensitivity and shorter response time and could be used as hydrogen gas sensing materials. Carbon microspheres with complete structure and uniform particle size distribution were prepared by hydrothermal method using glucose solution as precursor. The structure of carbon microspheres can be effectively controlled by adding different additives. A variety of oxide hollow microspheres were prepared using carbon microspheres as template. The Zn/ carbon composite precursor microspheres with intact structure were prepared by hydrothermal reaction of ZnCl_2/RF/ glucose composite system. The carbon template was removed by heat treatment, and various forms of ZnO hollow microspheres were obtained by controlling the heat treatment conditions. It lays a foundation for hydrothermal preparation of RF gel microspheres and its application in biological monosaccharide.
【學(xué)位授予單位】：哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2010
【分類號(hào)】：TB383.1

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