微波合成納米TiC粉體及分散性研究
發(fā)布時(shí)間:2018-04-25 00:10
本文選題:微波 + 合成; 參考:《西南科技大學(xué)》2016年碩士論文
【摘要】:本論文采用納米二氧化鈦和納米炭黑作為原料,在連續(xù)式微波窯中合成納米碳化鈦粉體,達(dá)到規(guī);a(chǎn)碳化鈦的目的。利用X射線衍射(XRD)、掃描電子顯微鏡(SEM)、激光粒度分布等分析手段,研究微波加熱時(shí)間、原料類型、摩爾比例等因素對(duì)TiC粉體合成的影響。結(jié)果表明:較佳微波加熱時(shí)間為100 min;采用銳鈦礦型納米TiO_2為原料有利于合成單相碳化鈦粉體;采用銳鈦礦型TiO_2和乙炔炭黑為原料,摩爾比例為1:3.5時(shí),合成碳化鈦粉體的平均晶粒尺寸為47.30 nm;碳黑的相對(duì)摻量越高,合成TiC的化學(xué)計(jì)量越接近TiC的理論化學(xué)計(jì)量。采用聚丙烯酸作為分散劑,無水乙醇作為分散介質(zhì),對(duì)原料進(jìn)行表面改性處理,處理后的原料通過濕磨混合,在間歇微波窯中合成碳化鈦粉體。利用Zeta電位測(cè)試、粘度測(cè)試、X射線衍射(XRD)、激光粒度分布等分析手段,研究pH值、分散劑、球磨等原料表面改性及混料工藝對(duì)微波合成TiC粉體的物相組成、化學(xué)計(jì)量、粒度分布的影響。結(jié)果表明:原料分散處理使微波合成TiC粉體的溫度降低了150℃,提高了TiC粉體的純度,減小了TiC的晶粒及平均晶粒尺寸,TiC粉體的化學(xué)計(jì)量更準(zhǔn)確;Ti O_2和乙炔炭黑的較佳改性pH值均為4,其較佳分散劑用量分別是2.4 wt.%和9.0 wt.%,TiO_2和碳黑的較佳分散濃度分別為4.67 wt.%和2 wt.%;TiO_2和碳黑混合原料懸浮液的較佳分散pH為4,較佳分散劑用量為4.38 wt.%,較佳分散濃度為6.67wt.%,較佳球磨混料時(shí)間為6 h;合成TiC粉體的較佳配方為TiO_2:炭黑=1:3(摩爾比),合成TiC粉體的平均晶粒為27.59 nm。采用聚丙烯酸作為分散劑,去離子水為分散介質(zhì),對(duì)合成碳化鈦粉體進(jìn)行超聲分散處理,利用激光粒度分布、Zeta電位測(cè)試、傅立葉變換紅外光譜(FTIR)、掃描電子顯微鏡(SEM)等分析手段,研究超聲時(shí)間、分散劑濃度、pH值對(duì)碳化鈦分散性的影響。結(jié)果表明:經(jīng)過分散處理能顯著降低納米TiC粉體的團(tuán)聚,分散性良好,平均粒徑為0.032μm;較佳超聲時(shí)間為4 min,較佳pH值為4,較佳分散劑(聚丙烯酸)用量為1.8 wt.%。
[Abstract]:In this paper, nanometer titanium carbide powder was synthesized in a continuous microwave kiln with nanometer titanium dioxide and nano carbon black as raw materials, and the purpose of producing titanium carbide on a large scale was achieved. By means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and laser particle size distribution, the effects of microwave heating time, type of raw materials and molar ratio on the synthesis of TiC powders were studied. The results show that the optimum microwave heating time is 100min, the anatase nanometer TiO_2 is used as the raw material to synthesize the single phase titanium carbide powder, the anatase type TiO_2 and acetylene carbon black are used as raw materials, the molar ratio is 1: 3.5. The average grain size of synthesized titanium carbide powder is 47.30 nm, and the higher the relative content of carbon black is, the closer the stoichiometry of synthetic TiC is to the theoretical stoichiometry of TiC. Using polyacrylic acid as dispersant and anhydrous ethanol as dispersing medium, the raw materials were treated by surface modification. The treated raw materials were mixed by wet grinding to synthesize titanium carbide powder in intermittent microwave kiln. By means of Zeta potential test, viscosity measurement, X-ray diffraction and laser particle size distribution, the phase composition and stoichiometry of TiC powder synthesized by microwave were studied by the surface modification of raw materials such as pH value, dispersant, ball milling and blending process. The effect of particle size distribution. The results showed that the temperature of TiC powder synthesized by microwave was reduced by 150 鈩,
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