Slip casting of highly concentrated ZnO suspensions: Rheological studies,two-step sintering and resistivity measurements

The paper presents research on elaboration of well dispersed and stable aqueous suspensions of ZnO fine powder. Within the work the influence of the type and concentration (0.2 wt% - 1.2 wt%) of selected dispersing agents (i.a. poly(acrylic acid)-based polyelectrolyte and tetramethylammonium hydroxide), solid loading (30 - 50 vol%) and milling time (1–3 h) on the rheological properties of the slurries was investigated. Two-step sintering (970/920 °C, 2 h) was applied to sinter the green bodies obtained by slip casting.The lowest viscosity of ZnO suspensions was obtained for the addition of 0.4 wt% of poly(acrylic acid)-based polyelectrolyte (PAA) and TMAH. ZnO suspension containing PAA had negative zeta potential in the whole pH range. The highest solid loading obtained in the study was 50 vol%. The applied two-step sintering allowed to obtain samples of high density (above 96% of TD) and homogeneous microstructure of average grain size of 640 nm. ZnO sintered bodies were characterized by different electric properties at the core part and outer part of the sample which was caused by the differences in concentration of oxygen vacancies.     

四甲基氢氧化铵的提纯实验研究

通过单因素实验考察了四甲基氢氧化铵的电解工艺。以钛基镀铱板为阳极,不锈钢为阴极,在电解槽中恒电流密度电解提纯四甲基氢氧化铵,主要考察了电解工艺中离子交换膜种类、原料浓度、电解温度和电流密度对电流效率的影响。当采用上海上化水处理厂3361为阳离子交换膜,在原料室四甲基氢氧化铵浓度25%、电解液温度50℃、电流密度8 ASD(A/dm2)时,电流效率可达66.74%,产品中金属离子杂质总含量从25×10-6降至0.8×10-6,氯离子浓度从0.65×10-6降至0.01×10-6。采用等离子体发射光谱仪(ICP-AES)、分光光度计对产品四甲基氢氧化铵进行表征。     

Experimental study and analysis of corner compensation structures for CMOS compatible bulk micromachining using 25 wt% TMAH

In the present work, most common compensation structures (〈1 1 0〉 squares and 〈1 0 0〉 bars) have been used for convex corner compensation with 25 wt% TMAH-water solution at 90±1 °C temperature. Etch flow morphology and self-align properties of the compensating structures have been investigated. For 25 wt% TMAH water solution {3 1 1} plane is found to be responsible for corner undercutting, which is the fast etch plane. Etch-front-attack angle is measured to be 24°. Generalized empirical formulas are also discussed for these compensation structures for TMAH-water solution. 〈1 1 0〉 square structure protects mesa and convex corner and is the most space efficient compared to other compensation structures, but unable to produce perfect convex corner as 〈1 0 0〉 bar type structures. Both the 〈1 0 0〉 bar structures provide perfect convex corners, but 〈1 0 0〉 wide bar structure is more space efficient than the 〈1 0 0〉 thin bar structure. Implications of these compensation structures with realization of accelerometer structure have also been discussed. A modified quad beam accelerometer structure has been realized with these compensation structures using 25 wt% TMAH.     

Thermally assisted in-line methylation and gas chromatography with statistical data analysis for determination of fatty acid distribution and fingerprinting of plant seeds and oils

Received: 11 October 1999 / Revised version: 7 December 1999     

通过添加表面活性剂和螯合剂改进硅片化学清洗工艺的研究

通过在传统RCA清洗法所用的SC-1液中,添加表面活性剂四甲基氢氧化铵(TMAH)和/或螯合剂乙二胺四乙酸(EDTA),实验比较了不同清洗方法对颗粒粘污、金属粘污的去除效率;并测试了其对硅片表面粗糙度的影响。用MOS电容结构的击穿电场强度Weibull分布,评价了不同清洗方法所得氧化层的质量。结果表明,上述改进能够显著提高对颗粒粘污和金属粘污的去除效果,同时能省去RCA的SC-2清洗步骤,具有节省工时、化学试剂消耗量小的优势。     

硅基热电堆真空传感器的制造技术

发展了一种与CMOS工艺完全兼容并可在商业化的1.2μm标准CMOS生产流水线上进行流片的硅基热电堆真空传感器的制造技术与流程.传感器为悬浮的多层复合薄膜结构,其上制作了n型多晶硅加热器和20对由p型多晶硅条和铝条构成的热电堆.利用标准制造工艺中铝层图形的掩蔽作用,使用干法刻蚀工艺一方面去除了传感器表面的SiNx层,使复合介质薄膜减至三层介质,即场氧化层、硼磷硅玻璃和层间介质,从而提高了传感器响应率;另一方面去除了传感器区域内腐蚀孔中的多层介质,将其中的硅衬底裸露,以便完成后续的四甲基氢氧化铵(TMAH)体硅各向异性腐蚀工艺,使传感器成为悬浮绝热结构,这种工艺具备铝保护性能,因此腐蚀中无需任何掩模.最终得到的器件尺寸为124 μm×100 μm,在空气压强为0.1 Pa～105 Pa之间的响应电压为26 mV～50 mV,响应时间为0.9 ms～1.3 ms.这种器件的制造技术具有工艺简单、成品率高、成本低、重复性好等特点.     

Bulk micromachining of silicon in TMAH-based etchants for aluminum passivation and smooth surface

The fabrication of silicon based micromechanical sensors often requires bulk silicon etching after aluminum metallization. All wet silicon etchants including ordinary undoped tetramethyl ammonium hydroxide (TMAH)-water solution attack the overlaying aluminum metal interconnect during the anisotropic etching of (100) silicon. This paper presents a TMAH-water based etching recipe to achieve high silicon etch rate, a smooth etched surface and almost total protection of the exposed aluminum metallization. The etch rate measurements of (100) silicon, silicon dioxide and aluminum along with the morphology studies of etched surfaces are performed on both n-type and p-type silicon wafers at different concentrations (2, 5, 10 and 15%) for undoped TMAH treated at various temperatures as well as for TMAH solution doped separately and simultaneously with silicic acid and ammonium peroxodisulphate (AP). It is established through a detailed study that 5% TMAH-water solution dual doped with 38 gm/l silicic acid and 7 gm/l AP yields a reasonably high (100) silicon etch rate of 70 μm/h at 80 °C, very small etch rates of SiO₂ and pure aluminum (around 80 Å/h and 50 Å/h, respectively), and a smooth surface (±7 nm) at a bath temperature of 80 °C. The etchant has been successfully used for fabricating several MEMS structures like piezoresistive accelerometer, vaporizing liquid micro-thruster and flow sensor. In all cases, the bulk micromachining is carried out after the formation of aluminum interconnects which is found to remain unaffected during the prolonged etching process at 80 °C. The TMAH based etchant may be attractive in industry due to its compatibility with standard CMOS process.     

Synthesis of tetramethyl ammonium hydroxide by cell diaphragm electrolytic method

Under the conditions of tetramethyl ammonia chloride (TMAC) used as starting material, Ti-based Dimensionally Stable Anode (DSA), stainless steel used as cathode and Nafion 900 cation membrane as cell diaphragm, this paper studies the synthesis of tetramethyl ammonium hydroxide (TMAH) by cell diaphragm electrolytic method, examining not only the effects of current density, concentration of starting material and cell temperature, on the product purity and current efficiency, but also the effects of electrolyte circulation rate on the service life of Ti-based DSA.The experiment puts forward an optimum processing condition, and experimental findings show that preparing TMAH by using this technique can obtain a current efficiency 74.7 , and get product with a purity greater than 99.9,.     

热释电薄膜单片式UFPA器件微桥单元结构研究

采用RF溅射制备出Ba_(0.65)Sr_(0.35)TiO_3薄膜,剥离法制备出UFPA器件单元所需的图形化金属电极,TMAH溶液进行体硅腐蚀,并且使用保护胶和独特的夹具保护硅片正面免受腐蚀液的腐蚀.总结了一套制作微桥的简便可行的工艺流程,并最终在厚度为300μm的硅基片上成功的制备了厚度小于3 μm的面积为100 μm×100 μm的微桥单元结构.该微桥单元可以满足制备热释电薄膜单片式UFPA器件的要求.     

单晶硅小金字塔绒面及其对太阳电池性能的影响

研究了TMAH(四甲基氢氧化铵)和NaOH腐蚀液在制作单晶硅片小绒面中的应用,制作出平均尺寸小于2μm的金字塔绒面;比较了不同硅片预处理(酸减薄、碱减薄、原片)对金字塔绒面尺寸、均匀性、覆盖率以及反射率的影响以及电池的I-V性能,分析了不同绒面结构对接触电阻的影响;指出单晶硅小金字塔绒面是使用激光制备高效晶体硅太阳电池的关键.