基于光敏浆料的直写精细无模三维成型

配制了一种具有光敏特性的陶瓷浆料, 并用此浆料通过直写精细无模三维成型技术制备了线条直径为300μm的BaTiO3陶瓷基木堆结构. 系统地讨论了光敏浆料的配制方法、浆料直写无模成型的工作原理以及采用的烧结工艺. 制备过程中不同阶段的研究表明, 光敏浆料中的BaTiO₃纳米颗粒在烧结前未发生团聚, 从而保证挤压成型顺利进行; 烧结后样品成瓷效果好, 各向收缩均匀, 整体无变形、开裂. 该技术具有成型速度快、制造周期短、可用材料范围广等特点.     

无铅压电陶瓷KNN常压烧结及其电学性能

用常压烧结法制备K_0.5Na_0.5NbO₃陶瓷。研究烧结温度与陶瓷密度和电学性能的关系。研究表明在1065℃~1120℃范围内, 温度对陶瓷的密度有显著影响。当烧结温度为1100℃时, 密度达到4.35 g/cm³ (占理论密度的95%); 1100℃烧结的陶瓷表现出最好的电学性能, 压电常数最大118 pC/N, 相对介电常数最大达538, 介电损耗最小仅4.7%, 剩余极化强度为15.37 μC/cm², 矫顽场为13.16 kV/cm。陶瓷样品在206℃从正交结构转变到四方结构, 居里温度为410℃。     

陶瓷微球新型直接滴定成型工艺研究

以平均粒径为0.1~0.5μm的SnO₂粉为原料,通过凝胶注模成型制备SnO₂浆料,并使用滴定针筒将浆料直接滴定于旋转的金属基超疏水表面,使SnO₂液滴在不同条件下的旋转金属基超疏水表面固化成球。研究了液滴尺寸、成型时间、固含量等因素对微球成型的影响规律,结果表明:直接滴定成型的SnO₂陶瓷微球的球形度十分理想,球形度大于常规滴定成型法,并且可成型出直径0.1~0.5 mm的陶瓷微球;微球的球形度随固含量的增加而增大,随液滴尺寸的增加而减小,随固化时间的增加而减小;当液滴尺寸调整为0.05 mm时,使用凝胶注模工艺优化后的固含量为80%的SnO₂粉浆,在60℃时干燥固化30 min,该条件下获得的SnO₂陶瓷微球具有最高球形度,可达到99.5%;微球球坯烧结前后的表面微观组织结构较为均匀,烧结后可保持完整的球体形状。      

制备工艺对(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3无铅压电陶瓷结构与性能的影响

采用液相混合与固相烧结相结合的方法制备了(Ba_0.85Ca_0.15)(Ti_0.9Zr_0.1)O₃ (BCTZ) 无铅压电陶瓷, 系统研究了烧结保温时间对其相结构、介电、压电和铁电性能的影响以及电学性能随温度的变化。研究结果表明: 制备的陶瓷样品具有单一的四方钙钛矿结构。当烧结温度为1540℃时, 随着保温时间的延长, 样品晶粒尺寸变大, 居里温度(T_c)升高, 压电性能提高, 电致伸缩性能下降。当保温时间为24 h时, BCTZ陶瓷综合性能最为优异: T_c ~90℃, tanδ < 0.05, k_p ~ 0.46, d₃₃ ~ 540 pC/N, P_s ~17 μC/cm²。陶瓷电学性能随温度变化测试结果又表明, BCTZ陶瓷的电学性能具有很强的温度依赖性, 随着温度的升高其电学性能逐渐下降。     

直接凝固注模成型氮化硅陶瓷

直接凝固注模成型是一种新颖的原位凝固成型工艺,特别适合于复杂形状陶瓷部件的成型．通过粉体的表面改性、浆料ｐＨ值的调节以及引入高效分散剂等途径制备出了低粘度高固含量的氮化硅浆料,通过直接凝固注模成型可以获得适当的素坯密度和强度．坯体气孔分布均匀,为较窄的单峰分布,断口光滑平整,坯体各部位密度具有很好的均匀性．在相对较低的烧结温度下（１７５０℃）,成型坯体经过无压烧结可达到理论密度的９８％,基本实现致密化．烧结体结构均匀,晶粒均匀生长,发育良好．经１８００℃烧结２ｈ后,抗折强度达７５８．４ ＭＰａ,断裂韧性为６．３ＭＰａ·ｍ^１／２．     

Li补偿量对铌酸盐基无铅压电陶瓷结构和性能的影响

采用传统固相烧结工艺, 在1000℃成功制备了致密度较高、微观形貌较好的Li_0.05+x(Na_0.535K_0.48)_0.95NbO₃ (L_xNKN)压电陶瓷. 考察了Li补偿量对L_xNKN陶瓷致密度、微观结构、相结构、居里温度及电学性能的影响. 结果发现: 添加过量Li不仅促进陶瓷的烧结, 而且降低陶瓷的烧结温度. XRD图谱分析和相应的晶格常数计算表明, 在x=0.010~0.015范围内出现了四方-正交两相共存的多形态相界(PPT). 由于PPT的出现, 在最佳补偿量x=0.015处, 陶瓷的压电常数d₃₃、机电耦合系数k_p、介电常数ε_r和剩余极化强度P_r分别达到各自的最大值282 pC/N、44%、942和27 μC/cm². 与化学计量比的LNKN陶瓷相比, L_xNKN陶瓷的居里温度随Li补偿量的增加变化很小, 这可能是由于Li主要是起助烧作用而进入主相晶格很少的缘故. 研究工作为低温制备高性能铌酸盐系压电陶瓷提供了一种新的思路.     

MgF2助剂对MgAl1.9Ga0.1O4透明陶瓷的制备与光学性能的影响

MgAl_1.9Ga_0.1O₄透明陶瓷具有优异的光学性能,其制备依赖于高质量坯体的凝胶注模成型和长时间的无压预烧。本研究选择MgF2为烧结助剂,并通过瞬时液相调节无压预烧的致密化过程。采用干压成型、无压预烧和热等静压烧结制备了不同尺寸的MgAl_1.9Ga_0.1O₄透明陶瓷样品,并系统分析了MgF2对材料显微结构、光学和机械性能的影响。研究表明：MgF2在～1230℃熔化形成的液相促使陶瓷的致密度与晶粒尺寸增大,后续烧结过程中残留的MgF2氧化为MgO并固溶进入MgAl_1.9Ga_0.1O₄晶格。添加质量分数0.2%MgF2的2.04mm厚透明陶瓷样品在紫外和可见光区域具有76.5%～83.4%的直线透过率和较高的光学质量。此外,该陶瓷的特征抗弯强度为167.1MPa,与细晶MgAl2O4透明陶瓷相近,但是前者的Weibull模数(8.81±0.29)更高。本研究为制备光学性能良好的大尺寸MgAl...     

微波烧结对PLZT陶瓷电学性能的影响

采用部分共沉淀法制备锆钛酸铅镧(PLZT)粉体, 分别用普通马弗炉和微波马弗炉进行烧结成瓷, 对比分析不同烧结方法对PLZT陶瓷的晶体结构、微观形貌和电学性能的影响。结果表明: 微波烧结和常规烧结均成功制备出钙钛矿相PLZT陶瓷。采用微波烧结得到的PLZT陶瓷样品比常规烧结的晶粒细小, 尺寸更均匀, 孔洞较少; 在电学性能相近时, 微波烧结温度远低于常规烧结, 且保温时间远小于常规烧结。在1000℃进行微波烧结, 陶瓷的介电常数ε_r和压电常数d₃₃最大, ε_r为2512, d33为405 pC/N, 此时, 剩余极化强度为16.5 kV/cm, 矫顽场为8.2μC/cm²; 在1250℃常规烧结, 陶瓷的介电常数最大, 为2822, 压电常数最大, 为508 pC/N, 剩余极化强度为21.6 kV/cm, 矫顽场为9.6μC/cm²。     

利用浆料直写无模成型技术制备自支撑TiO2光降解器件

介绍了一种基于光敏特性陶瓷浆料的浆料直写无模三维成型技术制备的线条直径为270μm的TiO2木堆结构光降解器件.对光敏浆料的配制方法、浆料直写无模成型的工艺原理进行了研究;利用TEM和XRD表征光敏浆料中TiO2粉体的形貌和物相;对器件的光降解性能进行了分析与测试;利用光学显微镜和SEM对成型后的样品结构、尺寸及表面微观形貌进行了分析,并基于此分析给出了这种器件高催化效率的原因.实验结果显示,该器件具有完整的三维木堆结构,表面粗糙多孔,极大地增加了光催化的作用面积,从而使其具有较高的光降解效率.在紫外光照射10min后,初始浓度为4mg/L的亚甲基蓝溶液降解率达到76%,紫外光照射20min后,亚甲基蓝溶液降解率可达91%.     

无铅压电陶瓷K0.5Na0.5NbO3-BiFeO3的烧结工艺与压电性能研究

采用传统常压固相烧结工艺制备了掺杂0.8at%BiFeO₃(BF)的K_0.5Na_0.5NbO₃(KNN) 无铅压电陶瓷,着重研究了烧结温度与保温时间对陶瓷的晶体结构、相转变、致密度与压电、介电性能的影响. 研究结果表明, 所有陶瓷样品都为单一的钙钛矿结构, 烧结温度与保温时间对陶瓷样品的室温晶体结构与相转变温度几乎没有影响, 但对陶瓷的表面形貌、密度和压电性能有较大的影响. 当保温时间为3h,在1100℃至1150℃范围内, 随烧结温度的升高,陶瓷的压电常数d33、平面机电耦合系数Kp及机械品质因数Qm均一直升高, 介电损耗tanδ则显著降低. 当烧结温度为1150℃时, 随保温时间的增加, 陶瓷的压电性能先显著提高后基本保持不变. 1150℃保温2h烧结的陶瓷获得良好的性能：密度ρ=4.50g/cm³（致密度为95.63%）, d₃₃=132pC/N, K_p=45%, Q_m=333.73, tanδ=2.39%.     

镍基Ni-Ag复合纳米粒子直流电弧等离子体法制备及其烧结电学性能

采用直流电弧等离子体法,在氢/氩气氛下蒸发高Ni含量的Ni-Ag块体靶材,获得以Ni为主相的复合纳米粉体产物,Ni和Ag元素之间形成各自固溶体相,其中Ni含量为70.54%(质量分数),纳米粒子产物平均尺寸在30~70 nm范围。将纳米粉体压制成片,其室温电学性能测试结果表明:25 MPa压力下的样品电阻率为5.36×10^-5Ω·cm。利用纳米粉体作为导电组分,配制成液态导电墨水,在聚酰亚胺薄膜基体上绘制导电线路,在Ar气氛下完成烧结处理。烧结样品电学性能测试结果表明:在300℃以上温度,烧结体结构致密,导电性能良好。随温度提高,烧结样品的电阻率逐渐下降,450℃时烧结体的电阻率达1.83×10^-3Ω·cm,明显优于纯Ni纳米粉体墨水的烧结体电阻率。     

The densification and morphology of cordierite-based glass-ceramics

In this study, five different proportion of a borosilicate glass (from 30 to 70 wt.%) were added to stoichiometric cordierite to improve the densification behaviour of cordierite-based glass-ceramica. The phase and microstructural evolution of the samples were characterised by DTA and SEM. The results show that glass content plays an important role in the sintering of cordierite-based glass-ceramics. The sintered density increases as the glass content increases at low temperature (950°C). At high temperatures, the sintered density passes through a maximum value when the glass content is about 60 wt.%, followed by a decrease as the glass content further increases. DTA results show that densification is a non-reactive liquid phase sintering process. The microstructural evolution of the samples is in good agreement with the measurements of sintered densities. At the lower glass content, the sample shows more pores and a non-uniform pore size distribution. With the glass content increasing, the pore size becomes more uniform and sintered density increases.     

Characterization of printed pigment-based inks on ink-jet media using cross-sectional electron microscopy

This paper reports on the microscopic assessment of representative specimen cross-sections prepared by microtomy and ultramicrotomy with emphasis in structure–property information using optical, scanning and transmission electron microscopy, namely, the absolute optical density δ, the measured effective printing coverage , the averaged pigment-based ink layer thickness , and the morphology at 100% nominal printing coverage. This work shows that for different test patches printed at the same nominal printing coverage a number of different printing schemes yield a pre-defined absolute optical density δ which basically depends on the measured effective printing coverage and the type of pigment-based inks used (spectral absorptivity m≠∞) and therefore on the averaged pigment-based ink layer thickness . A method for estimating the spectral absorptivity m is presented which combines the absolute optical density δ of the test patch and the averaged pigment-based ink layer thickness as measured from cross-sectional electron microscopy.     

有机相脱酸体系对不同老化墨迹的影响

目的 为了评价古籍化学品的综合效果,完善其除纸张性能外的墨迹的评价指标,探究不同有机相脱酸体系对老旧书页墨迹的影响.方法 制备胶印、中性笔墨样和书法用墨样,并对墨样进行人工老化处理.选择氢氧化钡的甲醇溶液(质量浓度为20 g/L)、氢氧化钡的二乙二醇溶液(质量浓度为17 g/L)和碳酸镁的甲醛溶液(质量浓度为10 g/L)分别对老旧书页以及人工老化的墨样进行脱酸处理.通过扫描仪高分辨率扫描墨样进行图像观察,用分光光度计测量墨样色密度,对3种有机相脱酸剂处理后的墨迹效果进行主客观评价.结果 主客观评价结果显示,经氢氧化钡的甲醇溶液处理后的墨样变化轻微;经碳酸镁的甲醛溶液处理后,墨样表面覆有1层碳酸镁颗粒,墨迹颜色明显变浅,墨样色密度显著降低;经氢氧化钡的二乙二醇溶液处理后,墨迹颜色变深,墨样色密度和线宽均有所增加.结论 不同脱酸体系会对老化墨样字迹产生不同程度影响,研究从图文信息质量的角度为古籍脱酸化学品的综合效果与评价提供一定的参考和借鉴.     

Ca掺杂对Ni-Cu-Zn铁氧体烧结体强度的影响

采用微波水热法制备了(Ni0.30Cu0.20Zn0.50)Fe2O4·xCaO(x=0、0.02、0.04、0.1)纳米粉体,通过压制成型,研究了不同烧结条件下Ca掺量对铁氧体的物相组成、显微结构及维氏硬度的影响.结果表明,随Ca掺量的增加,晶胞参数增大、晶粒尺寸减小、材料密度减小、维氏硬度增大.因此,Ca的掺入可明显提高材料的烧结强度.     

脱脂预氧化对注射成形碳化硅显微组织的影响

为了揭示脱脂预氧化对粉末注射成形碳化硅显微组织的影响规律,制定最佳热脱脂工艺,采用空气热脱脂方法对碳化硅制品进行了脱脂(550～950℃).结果表明:随预氧化温度升高烧结制品气孔率先降低后增加,650℃预氧化脱脂坯烧结后气孔率最低;预氧化可以有效促进脱脂坯烧结收缩,但过高的预氧化温度易引起失重增加,650℃预氧化脱脂坯烧结后具有最高的真实密度(3.20 g/cm3),高于未经预氧化直接烧结制品(3.18 g/cm3);烧结后试样由固相碳化硅与晶间液相组成,XRD及TEM能谱分析表明试样内部无残余氧化硅;随预氧化温度的升高烧结试样液相逐渐减少,液相的减少影响了氧化铝与氧化钇的比率,因此烧结试样未见明显YAG衍射峰出现;晶间液相阻碍了碳化硅晶粒间的扩散长大,制品晶粒平均尺寸小于1μm.空气热脱脂可取代传统气氛保护热脱脂,预氧化温度应控制在550～750℃.     

Synthesis,microstructure and mechanical properties of Yttria Stabilized Zirconia (3YTZP) – Multi-Walled Nanotube (MWNTs) nanocomposite by direct in-situ growth of MWNTs on Zirconia particles

In this research, Yttria Stabilized Zirconia (3YTZP) – carbon nanotube (CNT) composites are fabricated by direct in-situ growth of CNTs on the Zirconia particles, followed by densification via the Spark Plasma Sintering (SPS) technique. Scanning electron microscopy analysis of the 3YTZP-CNT powders shows uniform distribution of CNTs without the formation of agglomerates frequently seen with the traditional ex-situ mixing of CNTs in ceramic compositions. The samples were sintered to nearly 100% theoretical density and with a finer grain size microstructure. High Resolution Transmission Electron Microscopy (HRTEM) and Raman Spectroscopy confirm CNT retention in the sintered nanocomposites up to 1600 °C. The flexural strength increases from ∼260 MPa for samples without CNTs sintered at 1600 °C to ∼312 MPa for samples with ∼4 wt.% CNTs sintered at the same temperature. A corresponding increase in the indentation fracture toughness is also observed for samples with ∼4 wt.% CNTs sintered at 1600 °C as compared to samples sintered at the same temperature without CNTs.     

胶印机周向墨色均匀性的控制研究

目的 通过建立一套印前控制与网点补偿的规范操作流程来减少单张纸胶印机在印刷时容易产生周向墨色不匀的现象。方法 首先设计可测试印刷机周向墨色均匀性的测试文件,然后测量样张的周向密度,并绘制密度分布曲线,利用密度分布进行数据拟合来确定网点补偿量的大小;最后在分色制版阶段利用补偿公式对网点进行补偿。结果 通过该方法得到网点周向的最大密度值和最小密度值之间的误差约为0.45,有效地控制了周向墨色的不匀性问题。结论 实验证明了采用文件预处理的网点补偿方法进行墨色补偿方案能有效控制印刷过程中油墨的转移,且补偿后的测试文件可用来记录设备的周向墨色不匀性特征。     

Study of micropart fabrication via 17-4 PH stainless nanopowder injection molding

Micropart fabrication via 17-4 PH stainless nanopowder injection molding was investigated. The nanopowder was mixed with a binder that was based on wax to produce a feedstock composed of 45% powder and binder (the powder load). Initially, the fit and proper test was done before the micropart was made by making some bars of green samples, which the properties were examined after the sintering process. The examination involved the mechanical properties such as the porosity, hardness, and some of metallurgical aspects, such as the second-phase formation and the final compound after the sintering. The results showed that utilizing 17-4 PH stainless nanopowder is promising for micropart fabrication since it can form a nearly full-density sintered sample with a low porosity and good toughness, and can provide a smooth surface finish. After this, the investigations followed with the injection of the feedstock into the PDMS micromold that was formed by the nickel pattern from the X-Ray LIGA process. The green samples successfully produced a high-aspect-ratio sample with a thickness of up to 1 mm and an aspect ratio of 15 in the microchannel part. Then the green samples were sintered at 1,300 degrees C for 2 h, since from the initial test, they showed optimum parameters with nearly full density, low porosity, and a high degree of hardness. The research shows the excellent results of the application of the 17-4 PH stainless nanopowder to micropart fabrication.     

Pressureless sintering of dense hydroxyapatite–zirconia composites

Hydroxyapatite (HA)–TZP (2.5 mol% Y₂O₃) containing 2, 5, 7.5 and 10 wt% TZP were prepared using calcium nitrate, diammonium hydrogen orthophosphate, zirconium oxychloride and yttrium nitrate. The composite powder was prepared by a reverse strike precipitation method at a pH of 10.5. The precipitates after aging and washing were calcined at 850°C to yield fine crystallites of HA and TZP. TEM study of the calcined powder revealed that while HA particles had both spherical and cuboidal morphology (∼50–100 nm) the TZP particles were only of spherical nature (∼50 nm). X-ray analysis showed that the calcined powder of all the four composition had only HA and t-ZrO₂. Uniaxially compacted samples were sintered in air in the temperature range 1,150–1,250°C. High sintered density (>95% of theoretical) was obtained for composites containing 2 and 5 wt% TZP, while it was 92% for 7.5 wt% and 90% for 10 wt% TZP compositions. X-ray analysis of sintered samples shows that with 2 wt% TZP, the retained phases were only HA and t-ZrO₂. However, for 5, 7.5 and 10 wt% TZP addition both TCP and CaZrO₃ were also observed along with HA and t-ZrO₂. Bending strength was measured by three point bending as well by diametral compression test. While in three point bending, the highest strength was 72 MPa, it was 35.5 MPa for diametral compression. The strength shows a decreasing trend at higher ZrO₂ content. SEM pictures show near uniform distribution of ZrO₂ in HA matrix. The reduction in sintered density at higher ZrO₂ content could be related to difference in the sintering behaviour of HA and ZrO₂.