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Indium tin oxide (ITO) target material and determination method for content of indium and tin during production process of ITO target material

A production process and measurement method technology, applied in the field of analysis, can solve problems such as inaccurate determination results of indium, inaccurate titration endpoints, and "tailing" of indicators, and achieve the effects of high accuracy, convenient operation, and simple reagents

Inactive Publication Date: 2012-10-10
SHAOGUAN SIGMA TECH
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, there have been reports on the determination method of indium content in ITO powder and target material, but the EDTA complexometric titration method is used to directly measure the indium content in the sample. This method has serious indicator "tailing" phenomenon, Inaccurate titration end point leads to inaccurate determination of indium (Wu Wenqi et al., Metallurgical Analysis, 2007, Vol.27, No.11)
In addition, although the masking agents tartaric acid and glacial acetic acid used in the existing test methods can mask tin ions, adding these reagents under selected pH conditions causes the end point to be difficult to identify (Zhang Hongmei et al., Rare Metals, 2003, Vol. 27, No.1)

Method used

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  • Indium tin oxide (ITO) target material and determination method for content of indium and tin during production process of ITO target material
  • Indium tin oxide (ITO) target material and determination method for content of indium and tin during production process of ITO target material
  • Indium tin oxide (ITO) target material and determination method for content of indium and tin during production process of ITO target material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0046] 1 reagent

[0047] 1.1 Hexamethylenetetramine: AR grade, solid.

[0048] 1.2 Potassium nitrate: AR grade, solid.

[0049] 1.3 Ammonium fluoride: AR grade, solid.

[0050] 1.4 EDTA standard solution: c(H 2 Y 2- )=0.02mol / L, weigh 15.04g of 99% EDTA, dissolve it in water, and set the volume to 2L, the content is close to 0.02mol / L.

[0051] 1.5 Zn 2+ Standard solution: c(Zn 2+ )=0.01mol / L, weigh 1.3106g99.8% zinc particles, dissolve with hydrochloric acid and set the volume to 2L, the content is 0.01mol / L.

[0052] 1.6 In 3+ Standard solution: c(In 3+ )=0.01g / ml, In 3+ Standard solution: Weigh 1g of indium and dissolve it with hydrochloric acid to 100ml, c(In 3+ )=0.01g / ml.

[0053] 1.7 Xylenol orange indicator: 2g / L.

[0054] 2 Titration of indium tin content

[0055] Dilute the sample with unknown content (indium tin hydroxide powder or indium tin oxide target) through microwave digestion to prepare indium tin solution, dilute it with 5% dilute hydrochloric...

example 1

[0068] Example 1: Accurately weigh 1.2g of indium tin oxide powder with sample numbers NPC and NPD, moisten with a little water, add 20ml of concentrated hydrochloric acid for microwave digestion, dilute the digested sample to 100ml, and operate according to the above test steps. The obtained test results are compared with the XRF test results as shown in Table 1, in which the indium and tin contents are calculated in the form of indium oxide and tin oxide, and the titration method and XRF test experimental data are shown in figure 1

example 2

[0069] Example 2: The number IZXG034 indium tin solution with unknown content is diluted to 100ml with 5% dilute hydrochloric acid; the number IZXG034F slurry is concentrated, heated and dissolved with concentrated hydrochloric acid, diluted to 100ml, and the indium content is about 10g / L; Take 1.5g of the hydroxide with the serial number W120511, dry it to remove moisture, add 20ml concentrated hydrochloric acid, heat and dissolve, and set the volume to 100ml; Grind the JP1 target until it passes through a 100-mesh sieve, and dry the sieved powder to remove moisture Finally, weigh 1.0 g and moisten it with a small amount of water, add 20 ml of concentrated hydrochloric acid for microwave digestion. According to the above test steps, the obtained test results are shown in figure 2 .

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Abstract

The invention relates to an indium tin oxide (ITO) target material and a determination method for content of indium and tin during a production process of the ITO target material, after a sample is dissolved by acid, potassium nitrate is added to liquid to be determined, excessive ethylene diamine tetraacetic acid (EDTA) is subjected to complexation with indium and tin, ammonia water is used for adjusting pH value, the solution is heated to a boiling state, and cooled to a room temperature; hexamethylene tetramine is added for adjusting pH value, indicator xylenol orange is added, titration of the solution is carried out by zinc standard liquid until the color is changed from yellow to red, and the total content of the indium and the tin in the sample is converted through a consumption volume of the zinc standard liquid; and ammonium fluoride masking tin is added, after ammonium fluoride is completely dissolved, the solution is heated to a requested temperature and cooled to the room temperature, and the solution presents yellow, finally the titration of the solution is carried out by the zinc standard liquid until the color becomes red which is a titration finishing point, and the content of indium oxide in the sample is converted through the consumption volume of the zinc standard liquid. According to the ITO target material and the determination method, continuous titration of the indium and the tin can be realized, the titration efficiency is high, and the test result has remarkable accuracy, stability and repeatability.

Description

technical field [0001] The invention relates to an analysis method, in particular to an ITO target material and a method for measuring the content of indium and tin in solutions, slurry, hydroxides and ITO powders during the production process of the ITO target material. Background technique [0002] ITO target is a very important optoelectronic material, mainly used to produce ITO transparent conductive film. ITO thin films are widely used in liquid crystal displays, plasma displays, OLED displays, light-emitting diodes, touch screens, thin-film solar power plants and other fields. The main component of ITO material is indium tin oxide, in which the content of indium oxide is about 90% to 98%, the content of tin oxide is about 10% to 2%, the purity is better than 99.99%, and the relative density is better than 99% TD. The ratio of indium and tin content in the ITO target not only has an important impact on the performance of the ITO target, but also affects the structure a...

Claims

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Application Information

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IPC IPC(8): G01N21/79
Inventor 周贤界郑子涛毛骏徐敏许积文林燕美
Owner SHAOGUAN SIGMA TECH
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