Degradative analysis of aquatic fulvic acid: CuO oxidation versus pyrolysis after tetramethylammonium hydroxide treatments in air and helium atmospheres

The structural composition of Nordic aquatic reference fulvic acid was investigated using chemical and thermal degradation methods: alkaline CuO oxidation and analytical pyrolysis after tetramethylammonium hydroxide (TMAH) pretreatment. Off-line procedures of the TMAH treatments were carried out under both air and helium atmospheres, with the aim of clarifying the effect of oxygen. Irrespective of the fact that the chemical and thermal degradation methods gave qualitatively quite similar basic products (mainly phenols and phenolic acids together with aromatic and aliphatic carboxylic acids), they also revealed their unique selectivity and efficiency for releasing different kinds of structural constituents. The results verify the formation of additional carboxyl functionality in the CuO oxidation. However, some similar oxidative reactions also appeared to take place during the pretreatment procedures of strongly basic TMAH, especially under an air atmosphere. The use of inert and protective atmosphere during the TMAH pretreatment is therefore recommended for producing more relevant structural information about the complex composition of humic substances.     

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.     

Use of an injection port for thermochemolysis–gas chromatography/mass spectrometry: Rapid profiling of biomaterials

A simple and direct approach was developed for thermochemolytic analysis of a wide range of biomolecules present in plant materials using an injection port of a gas chromatograph/mass spectrometer (GC/MS) and a novel solids injector consisting of a coiled stainless steel wire placed inside a modified needle syringe. Optimum thermochemolysis (or Thermally Assisted Hydrolysis/Methylation) was achieved by using a suitable methanolic solution of trimethylsulfonium hydroxide (TMSH) or tetramethylammonium hydroxide (TMAH) with an injection port temperature of 350 °C. Intact, methylated flavonoids, saccharides, phenolic and fatty acids, lignin dimers and diterpene resin acids were identified. Samples include tea leaves, hemicelluloses, lignin isolates and herbal medicines. Unexpected chromatographic results using TMAH reagent revealed the presence of intact methylated trisaccharides (658 Da) and structurally informative dimer lignin markers.     

Effects of textured morphology on the short circuit current of single crystalline silicon solar cells: Evaluation of alkaline wet-texture processes

The effect of different surface morphologies obtained by anisotropic etching on the light trapping and short circuit current of single crystalline silicon solar cells was investigated. The anisotropic texturing of a (1 0 0) silicon surface was performed using potassium hydroxide (KOH) solution and/or tetramethylammonium hydroxide (TMAH) solution including isopropyl alcohol (IPA) additive or tertiary butyl alcohol (TBA) additive. Texturing in TMAH solution formed smaller pyramids on the textured surface compared with texturing in KOH solution. Although the textured samples showed similar reflectances (except in the case of the TBA additive), they showed different short circuit currents. Texturing in KOH/TMAH solution led to a 9.6% increase in short circuit current compared with texturing in KOH/IPA solution, a typical etchant in commercial processes. Based on these results, the reflectivity has no simple proportionality relationship to the short circuit current, and the short circuit current of silicon solar cells should be the criterion used in evaluating texturing effects on reducing reflectance and forming a sound junction with high collection efficiency.     

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。     

Simple method for the determination of Cu and Fe by electrothermal atomic absorption spectrometry in biodiesel treated with tetramethylammonium hydroxide

A simple analytical procedure for the determination of Cu and Fe in biodiesel samples by electrothermal atomic absorption spectrometry is proposed. An aliquot of the sample is simply mixed with tetramethylammonium hydroxide (TMAH) and heated to 90 °C for 5 min. Pyrolysis and atomization temperatures were optimized through pyrolysis and atomization curves. The high pyrolysis temperature adopted, of 1000 °C, certainly helped minimizing potential interferences. Even though, calibration should be carried out with aqueous standard solutions in the presence of the TMAH. The detection limits (3 s, n = 10), in the sample, were quite low 15 ng g⁻¹ and 24 ng g⁻¹ for Cu and Fe, respectively. Seven biodiesel samples, produced from different raw materials, including vegetable seed, frying oil and animal fat were analyzed. Accuracy was validated by applying the recovery test to two samples, enriching the samples with two concentration levels (recoveries from 105% to 120%). The precision, expressed by the relative standard deviation was less than 3% for Cu and less than 7% for Fe. Copper could be quantified in two and Fe in three of the seven samples. The biodiesel sample from fodder turnip was especially rich in the analytes in comparison to the other samples.     

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.     

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.     

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.     

大体积直接进样离子色谱法检测四甲基氢氧化铵中痕量阳离子

以抑制型电导离子色谱法检测四甲基氢氧化铵溶液中痕量碱金属和碱土金属离子.色谱条件为:IonPac CS12A阳离子交换色谱柱,20mmol/L甲烷磺酸淋洗液等度淋洗,抑制型电导检测.稀释液样品通过Dionex OnGuardⅡ氢型聚苯乙烯基强酸性树脂柱和0.22μm微孔尼龙膜处理.该方法的检测限(S/N=3)在0.024μg/L～0.156μg/L之间,标准曲线在低ng/L到低μg/L范围内呈现良好线性,RSD在10%左右,回收率为88%～115%.