EDTA滴定法测定铟锡氧化物废靶粉中铟的含量

建立用EDTA滴定法测定铟锡氧化物(ITO)废靶粉中铟含量的方法。ITO废靶粉样品经盐酸和硝酸分解,用氢溴酸加热除锡,以冰乙酸做掩蔽剂,p H控制在2.5~3.0之间,在70~80℃下用EDTA直接滴定法测定铟的含量。该方法改进了除锡条件,优化了酸度、温度,讨论了络合掩蔽剂及其用量的选择过程。在最佳实验条件下,铟的回收率为99.4%~100.5%,测定结果的相对标准偏差小于1%(n=6)。该方法可以满足ITO靶材中常量铟的分析要求。     

锌粉-硼砂-硼酸熔融-碘酸钾滴定法测定高硅锡精矿中的锡

针对高硅锡精矿中锡的测定时通常用锌粉-氢氧化钠熔融,精密度差,不能满足分析要求的问题,建立了锌粉-硼砂-硼酸熔融,盐酸浸取,铝粒将锡还原,碘酸钾滴定法测定高硅锡精矿中锡的分析方法。方法结果稳定,精密度好,相对标准偏差在0.19%~0.55%,加标回收率在96.9%~105%。分析结果能够满足高硅锡精矿中锡的测定要求。     

吡柔比星在羧基离子注入氧化铟电极上的电化学还原及其测定

采用离子注入技术将羧基离子注入到氧化铟锡(ITO)表面,制备了羧基离子注入氧化铟锡电极(COOH/ITO).电极表面羧基的引入用X射线光电子能谱(XPS)进行表征.此电极被应用到了吡柔比星的电化学行为的研究及其测定当中.在COOH/ITO电极上,吡柔比星在5 nmmol/L磷酸盐缓冲溶液(pH 7.2)中,出现还原峰,...     

水基溶胶凝胶法制备纳米氧化铟锡粉末

氧化铟锡（ITO）;PEG辅助的溶胶 凝胶法;纳米粉末     

微波消解氢化物发生-原子荧光光谱法测定罐头食品中汞和锡

建立了一种微波消解、氢化物发生-原子荧光光谱法同时测定罐头食品中汞和锡的方法。研究了测定汞、锡时介质的酸度和硼氢化钾的用量对汞、锡测定的影响。优化了样品消解和测定的条件,采用硫脲-抗坏血酸为掩蔽剂,以酒石酸为载流,消除了影响锡测定的干扰因素。汞和锡的检出限、相对标准偏差、回收率分别为:0.005μg.L-1和0.20μg.L-1;5.0%~6.5%和4.0%~7.3%;93.0%~101.0%和92.5%~94.0%。     

不同介质对电感耦合等离子体发射光谱法测定水中锡元素的影响

选用电感耦合等离子体发射光谱法测定水中锡元素,讨论了硝酸、盐酸两种介质对锡溶液测定及保存的影响。结果表明,选用体积分数为1%~10%的HNO3介质配制质量浓度为0.250~10.0 mg/L的锡溶液,在1%的HNO3中锡溶液浓度仅能稳定5 d,当HNO3的体积分数大于5%时,锡溶液可稳定30 d。选用1%~10%的HCl介质配制质量浓度为0.500~10.0 mg/L的锡溶液,在近一个月的实验周期内浓度值稳定,测定结果的相对标准偏差在0.94%~3.04%之间。作为测定、保存水中锡元素的介质,盐酸比硝酸更为理想。     

Na2EDTA滴定法测定锡阳极泥中的铋量

研究了Na_2EDTA标准滴定溶液测定锡阳极泥中铋的方法。探讨了锡阳极泥的溶样方式、滴定溶液酸度、滴定溶液温度、共存元素干扰、加标回收、方法的准确度与精密度。方法适用于锡阳极泥中5%~20%铋量的测定,尤其是铟量在0.1%及以上时,方法相对标准偏差(RSD)为0.55%~1.4%,加标回收率为99.81%~101.3%。具有操作步骤简单、适用性广、分析结果重现性好与准确度高等优点。     

Na_2EDTA滴定法测定锡阳极泥中的铋量

研究了Na_2EDTA标准滴定溶液测定锡阳极泥中铋的方法。探讨了锡阳极泥的溶样方式、滴定溶液酸度、滴定溶液温度、共存元素干扰、加标回收、方法的准确度与精密度。方法适用于锡阳极泥中5%~20%铋量的测定,尤其是铟量在0.1%及以上时,方法相对标准偏差(RSD)为0.55%~1.4%,加标回收率为99.81%~101.3%。具有操作步骤简单、适用性广、分析结果重现性好与准确度高等优点。     

ITO成分分析标准物质的研制

研制3种掺杂铁、铜、铅、锌、钙、镁金属元素的氧化铟锡(ITO)成分分析标准物质。采用溶胶凝胶和共沉淀相结合的方法制备标准物质候选物,用电感耦合等离子体发射光谱法对其进行均匀性、稳定性检验及定值分析。采用8家具有资质的实验室对研制的标准物质进行协作定值,对定值结果的不确定度进行评定。结果表明:研制的ITO成分分析标准物质具有良好的均匀性和稳定性,3种标准物质中氧化锡含量在1%~10%之间,相对扩展不确定度为0.7%~6.6%(k=2);6种掺杂元素含量在0.05%~0.30%之间,相对扩展不确定度为3.4%~11%(k=2)。     

固体粉末进样交流电弧法测定区域地球化学调查样品中痕量银、硼、锡、铅

采用固体粉末进样交流电弧法测定区域地球化学调查样品中的痕量银、硼、锡、铅。对实验条件进行了优化,激发电流为14 A,曝光时间为40 s。选择内标元素为锗,银、硼、锡、铅的分析线波长分别为328.07,249.77,283.99,283.31 nm;内标线波长分别为303.91,270.96,270.96,270.96 nm。分别在含量0.05~3,10~140,1~50,10~100μg/g范围内,银、硼、锡、铅含量的对数与分析线、内标线的黑度差呈良好的线性关系,相关系数分别为0.998 2,0.998 8,0.999 6,0.999 0,检出限分别为0.01,1.1,0.2,0.7μg/g。用所建方法对土壤成分分析标准物质GBW07446,GBW 07453和水系沉积物成分分析标准物质GBW 07302a,GBW 07303a,GBW 07304a进行测试,银、硼、锡、铅的测定值与标准值的对数差分别为–0.007~0.024,–0.031~–0.013,0.000~0.029,0.002~0.028,测定结果的相对标准偏差分别为7.3%~9.3%,6.0%~9.9%,6.5%~9.0%,6.5%~9.9%(n=12)。该方法操作简单、快速,环境友好,适合于区域地球化学调查样品中痕量银、硼、锡、铅的分析。     

A novel precursor system and its application to produce tin doped indium oxide

A new type of precursor has been developed by molecular design and synthesised to produce tin doped indium oxide (ITO). The precursor consists of a newly developed bimetallic indium tin alkoxide, Me(2)In(O(t)Bu)(3)Sn (Me = CH(3), O(t)Bu = OC(CH(3))(3)), which is in equilibrium with an excess of Me(2)In(O(t)Bu). This quasi single-source precursor is applied in a sol-gel process to produce powders and coatings of ITO using a one-step heat treatment process under an inert atmosphere. The main advantage of this system is the simple heat treatment that leads to the disproportionation of the bivalent Sn(II) precursor into Sn(IV) and metallic tin, resulting in an overall reduced state of the metal in the final tin doped indium oxide (ITO) material, hence avoiding the usually necessary reduction step. Solid state (119)Sn-NMR measurements of powder samples confirm the appearance of Sn(II) in an amorphous gel state and of metallic tin after annealing under nitrogen. The corresponding preparation of ITO coatings by spin coating on glass leads to transparent conductive layers with a high transmittance of visible light and a low electrical resistivity without the necessity of a reduction step.     

氧化铟锡(ITO)自组装修饰及其对有机电致发光器件性能的影响

设计合成了一种新型的有机硅氧烷Cz-Si,并将其用于ITO自组装修饰。制备的Cz-Si具有较好的稳定性,可以在空气中对ITO进行自组装修饰,实验操作简单。为考察ITO自组装修饰对有机电致发光器件性能的影响,分别以修饰后的ITO(ITO/SAM)及不修饰的ITO(unmodified)作阳极,制备了一系列有机电致发光器件ITO/SAM(or unmodified)/NPB(40~50 nm)/Alq₃(60 nm)/LiF(1.0 nm)/Al。实验结果表明,ITO自组装修饰后器件性能可以得到显著提升,研究认为这与其调控ITO/有机层界面的电子能级、粗糙度以及界面一致性有关。     

氧化铟锡(ITO)自组装修饰及其对有机电致发光器件性能的影响

设计合成了一种新型的有机硅氧烷Cz-Si,并将其用于ITO自组装修饰。制备的Cz-Si具有较好的稳定性,可以在空气中对ITO进行自组装修饰,实验操作简单。为考察ITO自组装修饰对有机电致发光器件性能的影响,分别以修饰后的ITO(ITO/SAM)及不修饰的ITO(unmodified)作阳极,制备了一系列有机电致发光器件ITO/SAM(orunmodified)/NPB(40~50nm)/Alq₃(60nm)/LiF(1.0nm)/Al。实验结果表明,ITO自组装修饰后器件性能可以得到显著提升,研究认为这与其调控ITO/有机层界面的电子能级、粗糙度以及界面一致性有关。     

Calculation of the electronic and optical properties of indium tin oxide by density functional theory

Density functional theory (DFT) was used to calculate the bulk electronic and optical properties of indium tin oxide (ITO). The ITO model was constructed replacing indium atoms with tin atoms in the cubic unit cell of indium oxide. To allow more possibilities for tin atom substitution than afforded by the forty-atom primitive cell of indium oxide all eighty atoms of the unit cell were included in the stoichiometry (In_32−xSn_xO₄₈) using periodic boundary conditions. A number of properties of ITO were calculated including the optical band gap, charge carrier density and plasma frequency. The dependence of the electronic and optical properties of ITO on a variety of parameters such as the tin content, cubic lattice parameter and the distance between adjacent tin atoms was investigated. The electronic and optical properties agreed well with experimental data and allowed insight into the origin of the electronic and optical properties of ITO.     

X射线荧光光谱法测定锡矿石中锡

本文采用向样品中加入硼酸来降低基体效应,加入氧化镧来稳定样品总质量吸收系数,建立固体粉末压片制样-X射线荧光光谱法测定锡矿石中锡含量的方法。通过将标准物质按一定比例混合配制和选取部分自制标样来补充标准物质样品,以解决锡矿石标准物质样品缺乏的问题。实验优化了稀释比,确定了以最佳稀释比为m（矿物质样品）:m（硼酸）：m（氧化镧）=1.0:2.0:0.5。在最优的实验条件下,Sn的荧光强度（kcps）与Sn浓度CSn呈良好的线性关系,R2=0.9989。方法中锡元素的最低检出限为0.005 %,测定范围在0.015 %-4.47 %之间。样品的混合均匀性实验表明各元素测定结果的相对标准偏差（RSD,n=6）在1.0 %-2.64 %之间。对3个不同含量段的物质进行测定来验证方法的准确度和精密度,准确度分别为0.0082-0.0367,均小于0.04,精密度分别为0.39 %-1.18 %,均小于8.0 %,准确度和精密度均符合地质样品分析规范要求。测定值均在误差范围内,各组分测定结果的相对标准偏差（RSD,n=11）在1.20 %以下。粉末压片-X射线荧光光谱法测定锡矿石中锡含量具有分析范围广、分析时间短、重现性好、精度高且操作简单等特点。能应用于地质、环境、材料等领域。     

Use of a precursor solution to fill the gaps between indium tin oxide nanorods, for preparation of three-dimensional CuInGaS2 thin-film solar cells

We have fabricated a three-dimensional (3D) nanostructured indium tin oxide (ITO) film in which the spaces were filled by use of a Cu, In, and Ga precursor solution. This solution has potential for use in bulk heterojunction CuIn _x Ga_1?x S₂ (CIGS) thin-film solar cells. ITO nanorod films ~700 nm thick on glass substrates were synthesized by radio-frequency magnetron sputtering deposition. To ensure complete filling of the gaps in ITO nanorod films, a polymeric binder-free precursor solution was used. In addition, a two-step heating process (oxidation and sulfurization) was used after coating of the precursor solution to make a CIGS absorber film with a minimum of carbon impurities. Superstrate-type solar cell devices with 3D nanostructured films (CIGS–ITO) had a photovoltaic efficiency of 1.11 % despite the absence of a buffer layer (e.g. CdS) between the CIGS and ITO.     

等离子体聚合膜的电学性质研究——Ⅱ.腈类单体结构的影响

等离子体聚合膜多为具有高电阻的绝缘体。但是,近年来的研究结果表明,选择合适的单体及采取一些措施,可使等离子体聚合膜从绝缘体至半导体乃至导体的宽范围变化。本文将一些具有不同化学结构的腈类单体进行了等离子体聚合,研究了单体化学结构对所得聚合膜结构及电学性质的影响。聚合方法等同前报。     

等离子体聚合膜的电学性质研究：Ⅰ.TCNQ聚合膜的结构和电学性质

本文采用内部电极、电容耦合式钟罩型射频等离子体聚合装置,首次进行了四氰代对二次甲基苯醌(TCNQ)的等离子体聚合,得到了电导率为10~(-8)～10~(-6)Scm~(-1)的聚合物半导体薄膜。由这些聚合物薄膜制备的Al/聚合膜/ITO(铟锡氧化物透明电极)夹层元件显示出整流特性和光生伏打效应。这种聚合物薄膜还具有光电导性质。红外光谱(IR)、紫外光谱(UV)的研究结果表明,优良的半导体特性归因于聚合膜中存在有较大范围的π电子共轭结构。