分相铁红釉的研制及微观结构分析

采用钾长石、石英、苏州土、滑石、牛骨灰、氧化铁等原料制备出分相铁红釉,研究了釉料配方以及釉层厚度对分相铁红釉的影响,利用X射线衍射仪(XRD)、扫描电镜(SEM)和能谱分析仪(EDS)等手段,对铁红釉的微观结构进行了表征.结果表明:牛骨灰、氧化铁、滑石的添加量对铁红釉有显著的影响;釉表面红色区域Fe元素含量远远大于棕褐色区域,并富聚有大量的α-Fe2O3晶体;同时,在釉的断面也发现有大量晶体析出,呈上密下稀的分布规律;铁红釉最佳的釉层厚度应控制在0.8 ～1.0 mm范围之内.     

烧成制度对R2O-CaO-Al2O3-B2O3-SiO2分相乳浊釉的影响研究

用DSC、色度仪、XRD、SEM等仪器对R2O-CaO-Al2O3-B2O3-SiO2分相乳浊釉样品进行检测分析,探究烧成制度对釉面性状及显微结构的影响.结果表明,升温速率快慢影响釉中组分扩散和迁移的时间,致使釉中分相液滴的尺寸分布、平均粒径、体积分数产生变化,釉面呈现乳蓝、乳白等效果;提高烧成温度可促进釉层中组分的相互扩散,在1160～1220℃范围内可得到白度大于70;的光亮乳浊釉面,温度过高容易导致釉面出现针孔缺陷;降温冷却过程中釉熔体在热力学和动力学相互作用下发生分相现象,分相液滴的组分、形貌和尺寸是此过程中某一瞬时的平衡态,因此降温冷却过程对分相乳浊釉有重要影响.     

B2O3对中低温硅硼系分相乳浊釉性能的影响

本实验探究 B2O3组分对中低温(1200 ℃)K,NaO-CaO-Al2O3-B2O3-SiO2系分相乳浊釉性能的影响,通过SEM、XRD、FTIR、维氏硬度计、CIE L*a*b*等测试手段对样品釉面性能及显微结构进行测试分析.实验结果表明:随着B2O3引入量的增加,釉面乳浊度明显提高,白度随之增加,在B2O3为1.2 mol当量时可达最大值78.7;,但过量引入B2O3不利于乳浊度的提高,且易降低釉面平整度及硬度.SEM、XRD测试及CaO-B2O3-SiO2相图分析表明,分相釉的乳浊主要来源于釉层中分相液滴对入射光产生的散射效应.适当的B2O3含量有利于分相液滴的形成与长大,并提高两相折射率差值,从而有利于强化釉层对入射光的散射,提高釉面乳浊化程度.     

CaO-MgO-Al2O3-Fe2O3-B2O3-SiO2系微晶釉的制备

通过引入B2O3以降低烧成温度,利用赤泥中的Fe2O3为着色剂,在1150℃左右低温烧成制备了CaO-MgO-Al2O3-Fe2O3-B2O3-SiO2系微晶釉.赤泥的加入量为20;左右时,釉面具有良好的装饰效果和显微硬度.利用XRD、SEM研究了釉的物相及显微组织.结果表明,釉中析出的微晶是普通辉石,微晶的含量随MgO及CaO的含量增加而增加,而提高Al2O3含量则抑制微晶的析出.     

ZnO/B2O3对R2O-RO-B2O3-Al2O3-SiO2系统低温分相釉乳浊效果的影响

以K2O-CaO-Al2O3-SiO2系统为基础,通过添加氧化锌和硼酸钙,制备出了1120℃烧成的高白度无锆低硼低温分相乳浊釉,并借助TEM、XRD、FTIR和白度仪等测试手段研究了ZnO/B2 O3对乳浊釉分相结构和白度的影响,探讨了其乳浊机理.结果表明:随着ZnO/B2 O3的增大,釉面白度呈先增后降趋势,当ZnO/B2 O3为4.04时达最大值为80.5;.随着ZnO/B2 O3的增大,分相粒子尺寸逐渐减小,数量逐渐增多.ZnO/B2 O3过高,分相粒子尺寸太小,远小于可见光波长,不利于乳浊度的提高.     

银色金属光泽釉的研制及微观结构分析

通过在基础釉中添加金属氧化物MnO2 、CuO和V2O5,在随炉冷却的烧成制度下,成功制备了银色金属光泽釉.采用L9 (33)正交实验的方法研究了MnO2、CuO、V2O5加入量对釉面效果的影响.利用X射线衍射(XRD)和场发射扫描电子显微镜(FESEM)对釉层的微观结构进行了表征.研究表明:(1)CuO加入量对釉面金属光泽的产生显著影响,V2O5的影响不明显,当CuO加入量小于3;时,釉层为透明状.随着MnO2和CuO加入量的增大,釉面逐渐呈现无光及变色的趋势,MnO2、CuO、V2O5的推荐加入量分别为4;、3;和2;.(2)釉层中存在大量亚微米级甚至纳米级片状晶体.晶体尺寸均匀,表面平整光滑,并形成大面积平面网状排布.(3)釉层中大量沿坯体表面平行生长的片状晶体容易对光线造成强烈的镜面反射,是造成釉面出现高亮度银色金属光泽的重要原因之一.     

碱土金属氧化物对硼熔块釉的影响分析

针对碱土金属氧化物对陶瓷釉面质量影响显著、复杂的实际问题,以硼熔块釉为基础配方,适量氧化铜和氧化铁为离子着色剂,系统研究了钙、镁、钡、锌、锶碱土金属氧化物(RO)对釉面质量的影响.研究结果表明:(1)不同RO组成及比例的硼熔块釉效果差异显著,制备的复合碱土熔块釉较单一碱土能显著提高釉面质量、扩大发色范围及产生分相乳浊现象;(2)Ca碱土的加入有促使Na2 O-K2 O-CaO-RO-SiO2-B2 O3-Al2 O3系硼熔块釉产生较强釉面乳浊的特点,且使釉面颜色变淡变浅;(3)1180℃烧成温度下,当釉中RO为12;方解石和12;BaCO3,或者12;ZnO和12;SrCO3,同时添加3;氧化铜和1;氧化铁时,易使硼熔块釉呈现局部深蓝、附带流纹的花釉效果.     

Y2O3添加对Yb2Si2O7无压烧结致密化的影响

以Yb2O3粉末和溶胶-凝胶法制备的活性SiO2凝胶为原料,在1550℃保温4h合成了具有单斜结构的单相Yb2Si2O7粉体.采用无压烧结方法获得了Yb2Si2O7陶瓷.通过添加Y2O3烧结助剂,获得了气孔率为3.2;的致密Yb2Si2O7陶瓷.采用XRD、SEM方法对烧结体的结构、成分和形貌进行测试与表征.结果表明:烧结体均为单相的Yb2Si2O7,不含其它杂质相.Y2O3的添加大大降低了烧结体的气孔率,促进了烧结的致密化.所得致密Yb2Si2O7陶瓷的平均晶粒尺寸为1～2 μm,大部分晶粒为颗粒状晶粒.     

熔制坩埚对CaO-Al2O3-MgO-SiO2系矿渣微晶玻璃结构与性能的影响

以白云鄂博二次选后尾矿、高炉渣和粉煤灰为主要原料,采用熔融法分别在氧化铝坩埚和石墨坩埚熔制制得CaO-Al2O3-MgO-SiO2 (CAMS)系微晶玻璃,利用DSC、XRD、SEM、EDS、ICAP、XPS等测试手段,研究了不同坩埚熔制对微晶玻璃成分、显微结构及性能的影响.研究表明:高温玻璃熔液对氧化铝坩埚的侵蚀作用及石墨坩埚的还原作用,使基础玻璃中Al2O3和Fe2O3含量发生较大变化,氧化铝坩埚熔制制备的基础玻璃有一个析晶峰,温度为905 ℃,对应的微晶玻璃主晶相为含铁透辉石Ca(Mg,Al) (Si,Al)2O6,而石墨坩埚熔制制备的基础玻璃出现两个析晶峰,温度分别为866℃和805℃,对应的微晶玻璃主晶相透辉石Ca(Mg,Al) (Si,Al)2O6和次晶相柯石英SiO2,由于以上原因导致制备的微晶玻璃在显微结构及理化性能上也存在一定的差异.     

含MgO-Lu2O3-Re2O3三元添加剂Si3N4陶瓷摩擦磨损性能的研究

利用球盘式摩擦磨损试验机,研究了含MgO-Lu2O3-Re2O3(La2O3,Sm2O3,Gd2O3,Er2O3)三元添加剂Si3 N4陶瓷的摩擦磨损性能.结果表明:机械磨损和摩擦化学反应为主要磨损机理.在三元添加剂中,随着第二稀土离子Re3+半径的增加,粘附层增加,Si3N4摩擦系数降低.基于横向断裂理论模型,Si3N4陶瓷单位磨损率随着1/(KB1/2H5/8)的增加而增加,其中含有第二相Lu4Si2N2O7的样品SN-LuSm和SN-LuEr优于此线性关系,表现出更好的抗磨损性能.     

Pr2O3对含Cr2O3辉石系矿渣微晶玻璃晶化行为的影响

以白云鄂博西尾矿和粉煤灰为主要原料,分别制备了添加0,2.0wt;,4.0wt;和6.0wt; Pr2O3的辉石系矿渣微晶玻璃;综合采用基于DSC/DTA结果的析晶活化能Ek、Avrami指数以及粘流活化能Eη和背散射电子SEM显微形貌分析研究了Pr2O3对析晶的影响.结果表明在所研究范围内,Pr2O3含量的提高在整体上抑制了辉石相的析出.其原因除了与富Pr颗粒相对辉石相在析晶过程中的“钉扎”有关外,还与Pr2O3含量提高后使基础玻璃网络聚合程度加大,从而增大了辉石相形成所需离子扩散的阻力有关.     

Fe2O3-CO3O4共掺杂MgO-Al2O3-SiO2体系的红外辐射性能研究

采用固相反应法制备Fe2O3-Co3O4共掺杂MgO-Al2O3-SiO2体系的复合陶瓷材料,并通过XRD、SEM、XPS以及红外辐射测试等方法研究了样品的结晶行为与红外辐射性能.结果表明:Fe2 O3和Co3 O4共掺杂MgO-Al2 O3-SiO2体系后离子分布改变并生成混合尖晶石,从而引起品格畸变,从而有效提高材料的红外辐射性能.材料的红外发射率与其晶格畸变程度具有相同的变化趋势,并随Fe2 O3与Co3O4质量之比(R)的增加呈非线性变化.当R=3∶2时,材料在8 ～ 14 μm波段的辐射率可达0.92.     

EPR and magnetic susceptibility studies of B2O3–Bi2O3–Gd2O3 glasses

Glasses of the xGd₂O₃ · (100 − x)[B₂O₃ · Bi₂O₃] system with 0.5 ⩽ x ⩽ 10 mol% were studied by electron paramagnetic resonance (EPR) and magnetic susceptibility measurements. Data obtained show that for low gadolinium oxide contents of the samples (x ⩽ 3 mol%) the Gd³⁺ ions are randomly distributed in the host glass matrix and are present as isolated and dipole–dipole coupled species. For higher gadolinium oxide contents of the samples (x > 3 mol%) the Gd³⁺ ions appear as both isolated and antiferromagnetically coupled species. The EPR spectra of the glasses reveal resonance sites with an unexpected high crystalline field in addition to the ‘U’ spectrum, typical for Gd³⁺ ions in disordered systems. This absorption line is due to Gd³⁺ ions that replace Bi³⁺ ions from the host glass matrix and could play the network unconventional former role in the studied glasses.     

Yb2O3-Y2O3-Gd2O3-ZrO2热障涂层制备及性能研究

以Yb2O3、Y2O3 、Gd2O3稀土氧化物粉末和ZrOCl2·8H2O粉末为原料,采用化学共沉淀法制备了Yb2O3-Y2O3-Gd2O3-ZrO2 (YYGZO)热喷涂用粉末,采用大气等离子喷涂技术制备了YYGZO涂层,利用场发射扫描电镜(FESEM)、X射线衍射(XRD)研究了YYGZO粉末及涂层的微观组织形貌、相结构.结果表明,制备的热喷涂YYGZO粉末大部分呈规则实心球体状,且球形度良好,颗粒粒径均匀,大部分颗粒粒径分布为30～60μm,流动性能较好,满足大气等离子喷涂的要求.YYGZO涂层具有较好的高温相结构稳定性.所制备YYGZO热障涂层组织结构比较致密,涂层各个界面结合紧密,孔隙率约为9.23;,结合强度为35.2 MPa.     

Thermal expansion and transition temperature of glasses in the systems BeO–Al2O3–B2O3 and MgO–Al2O3–B2O3

Researches were conducted for glasses in the systems BeO–Al₂O₃–B₂O₃ and MgO–Al₂O₃–B₂O. The following characteristics have been determined: thermal expansion coefficient within 20–300 °C, structural thermal expansion coefficient (STEC) and glass transition temperature. The discussed properties of Be-aluminoborate and Mg-aluminoborate glasses have been compared with those of Ca-, Sr- and Ba-aluminoborate glasses. TEC of studied glasses gets higher going from Be-aluminoborate glasses to Ba-aluminoborate ones, but T_g decreases under the same succession. The dependence of STEC on the nature of a given cation is more complicated. The pattern of dependence of the properties on composition is due to changing the boron coordination number with respect to oxygen, which is the main network-former, and to competition between the aluminium and boron for the oxygen brought by an ion-modifier. The difference between the effect of one ion-modifier and that of another is determined by decreasing the radius of an ion and increasing its electric field strength in the succession from Ba²⁺ to Be²⁺. The ions of Be and Mg can also act as network-former to some extent.     

Structural properties of Cr2O3–Fe2O3–P2O5 glasses,Part I

The structural properties of xCr₂O₃–(40 − x)Fe₂O₃–60P₂O₅, 0 ⩽ x ⩽ 10 (mol%) glasses have been investigated by Raman and Mössbauer spectroscopies, X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The Raman spectra show that the addition of up to 5.3 mol% Cr₂O₃ does not produce any changes in the glass structure, which consists predominantly of pyrophosphate, Q¹, units. This is in accordance with O/P ≈ 3.5 for these glasses. The increase in glass density and T_g that occurs with increasing Cr₂O₃ suggests the strengthening of glass network. The Mössbauer spectra indicate that the Fe²⁺/Fe_tot ratio increases from 0.13 to 0.28 with increasing Cr₂O₃ content up to 5.3 mol%, which can be related to an increase in the melting temperature from 1423 to 1473 K. After annealing, the 10Cr₂O₃–30Fe₂O₃–60P₂O₅ (mol%) sample was partially crystallized and contained crystalline β-CrPO₄ and Fe₃(P₂O₇)₂. The SEM and AFM micrographs of the partially crystallized sample revealed randomly distributed crystals embedded in a homogeneous glass matrix. EDS analysis indicated that the glass matrix was rich in Fe₂O₃ (39.6 mol%) and P₂O₅ (54.9 mol%), but contained only 5.5 mol% of Cr₂O₃. These results suggest that the maximum solubility of chromium in these iron phosphate melts is 5.5 mol% Cr₂O₃.     

BaTiO3-Nb2O5-Fe2O3陶瓷介电性能的研究

利用传统方法制备了BaTiO3-Nb2O5-Fe2O3(BTNF)陶瓷,采用X射线衍射仪、电容测试仪、电滞回线测量仪等测试手段研究了不同添加剂(Fe2O3、Co2O3、Nb2O5)对陶瓷晶体结构、介电性能及铁电性的影响.结果表明:Nb2O5是施主掺杂,易引起晶格畸变,使四方率增大;而Fe2O3为受主掺杂,其可提高氧空位浓度,促进BaTiO3陶瓷晶粒生长.同时掺杂Fe2O3、Nb2O5时,可以相互补偿.当Fe2O3浓度约为0.15;摩尔分数,Nb2O5浓度为0.79;摩尔分数时,陶瓷的介电常数达到4443,温度特性≤±10;,可以满足Y5P瓷料的要求.     

In2O3 and tin-doped In2O3 nanocrystals prepared by glass crystallization

Glasses in the system Na₂O/B₂O₃/Al₂O₃/In₂O₃/(SnO₂) were melted and subsequently tempered in the range from 540 to 700 °C. This led to the crystallization of In₂O₃, besides also NaBO₂ and Na₂Al₂B₂O₇ were formed. The crystallite sizes were in the range from 12 to 34 nm, depending on the temperature of thermal treatment, as calculated from XRD-line broadening. Crystal sizes determined by TEM were in the same range. Particle size histograms show a narrow crystal size distribution. After crystallization, the glass matrices and the non indium-containing crystalline phases were dissolved in diluted acetic acid. Spectra of the obtained suspensions containing tin-doped In₂O₃ nanocrystals exhibited a sharp UV-cut off, high transmission in the visible range and strongly decreasing transmission at wavelengths >1000 nm.     

Semi-quantitative analysis for FTIR spectra of Al2O3-PbO-B2O3-SiO2 glasses

A series of glass of the molar formula xAl₂O₃-(50-x)PbO-25B₂O₃-25SiO₂ with x:2.5–17.5 with step of 2.5 mol.% was prepared and measured for, density, molar volume and infrared absorption. A semiquantitative analysis of the IR spectra was performed. It was found that each oxide would contribute in density with a specific factor. The density factor related to PbO is markedly higher than that of the other two oxides represent the glass skeleton which means that the content of PbO is the main factor affecting the density. The depolymerization of the whole glass skeleton increases with increasing the content of Al₂O₃. There is a competition between the role of PbO and Al₂O₃ in changing the value of N₄ and the crosslinking of the glass network. The silicate network tends to be distinguished from the reminder of the whole glass network with increasing alumina. The IR band located near 700 cm^? 1 was suggested to be due to the vibrations of bridging oxygens between trigonal boron atoms. An essential change in the role of PbO in these glasses from glass modifier to glass former occurred around 12 mol.% Al₂O₃.