CN102798692A - Method for measuring contents of zinc oxide and aluminum oxide in AZO (aluminum-doped zinc oxide) ceramic target - Google Patents
Method for measuring contents of zinc oxide and aluminum oxide in AZO (aluminum-doped zinc oxide) ceramic target Download PDFInfo
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- CN102798692A CN102798692A CN2012102282380A CN201210228238A CN102798692A CN 102798692 A CN102798692 A CN 102798692A CN 2012102282380 A CN2012102282380 A CN 2012102282380A CN 201210228238 A CN201210228238 A CN 201210228238A CN 102798692 A CN102798692 A CN 102798692A
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Abstract
The invention relates to a method for measuring contents of zinc oxide and aluminum oxide in an AZO (aluminum-doped zinc oxide) ceramic target, which comprises the following steps: when using a first test solution to measure the content of zinc oxide, adding excessive EDTA (ethylene diamine tetraacetic acid) to be complexed with zinc ions, adding ammonium fluoride to shield aluminum ions, adding a sodium acetate buffer solution, adding a surfactant to increase the solubility of PAN which is used as an indicator, titrating the excessive EDTA with a Cu<2+> standard solution, and calculating the content of zinc oxide by using the titration volume of the Cu<2+> standard solution when reaching to the titration end point; and when using a second test solution to measure the content of aluminum oxide, adding excessive EDTA, boiling, regulating the pH value, completely complexing aluminum ions and zinc ions with the EDTA, adding a sodium acetate buffer solution, titrating the residual EDTA with a Cu<2+> standard solution, adding ammonium fluoride to shield the aluminum ion, replacing the EDTA complexed with the aluminum ions, carrying out replacement titration with the Cu<2+> standard solution to precipitate EDTA equivalent to the aluminum content, and calculating the content aluminum oxide by using the titration volume of the Cu<2+> standard solution when reaching to the titration end point. The invention has the advantages of accurate and stable result and favorable reproducibility.
Description
Technical field
The present invention relates to a kind of analytical approach of content of material, particularly relate to the assay method of zinc paste and alumina content in a kind of AZO ceramic target.
Background technology
The oxidic transparent conductive film is called for short TCO; Mainly contain oxide and the composite multi-component oxide film material thereof of In, Sb, Zn and Cd; Wherein mixing indium oxide film (ITO) with tin is representative, has that the forbidden band is wide, a comprehensive photoelectric properties such as visible range transmissivity height and resistivity are low.In recent years; Along with deepening continuously of the research of zinc-oxide film; Aluminium is mixed zinc-oxide film (AZO) and is had the photoelectricity that compares favourably with ito thin film at heart, and cost is low and in hydrogen plasma advantage such as stability be considered to one of TCO membraneous material that has most development potentiality.Wherein, the doping content of aluminium oxide is in 0～5wt% scope.
To the mensuration of zinc paste and alumina content in the AZO target, be the necessary means that AZO target manufacturing enterprise carries out production quality control.The mensuration of zinc paste and alumina content is except can analyzing with EDS, XRF instrument; The mensuration of zinc paste and aluminium oxide can adopt the EDTA compleximetry; And in former national standard electronic glass in the content assaying method of zinc paste and aluminium oxide; Because the phenomenon that ossifys in use can appear in PAN, the titration end-point sudden change is not obvious, causes the terminal point determining difficulty.In addition, the content of zinc paste and aluminium oxide differs greatly in the AZO target, uses the Continuous Titration method in the primary standard, accurately quantitative measurement.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art
,The present invention provides that a kind of less equipment investment, operating process are simple, accuracy height, the good reproducibility measured, can satisfy Quality Detection needs in the production of AZO target the AZO ceramic target in the assay method of zinc paste and alumina content.
The technical solution adopted for the present invention to solve the technical problems is: the assay method of zinc paste and alumina content in a kind of AZO ceramic target comprises the steps:
The one, the demarcation of standard solution:
Cu wherein
2+Mark liquid is demarcated: draw 5ml EDTA standard solution in the 250ml conical flask, adding 10ml pH value is 4.3 buffer solution, adds 5 PAN indicator, with Cu
2+The mark drop is fixed, and is green by xanthochromia to solution, adds 10ml ethanol, continues titration to aubergine, record reading V
1
Be calculated as follows Cu
2+Mark liquid is marked the reduction coefficient k of liquid to EDTA:
In the formula: V
1-Cu
2+The volume of mark liquid, ml;
K-Cu
2+Mark liquid is to the reduction coefficient of EDTA mark liquid;
Zn wherein
2+The demarcation of mark liquid: draw 5ml Zn
2+Mark liquid adds 10ml EDTA solution in the 250ml conical flask, add one of paranitrophenol indicator, transfers to yellow with 1+1 ammoniacal liquor earlier, transfers to colourless and excessive 3 with 1+1 hydrochloric acid again, adds 15ml buffer solution, adds 10 of PAN indicator, uses Cu
2+The mark drop is fixed, adds 10ml ethanol during nearly terminal point, continues titration to aubergine, record reading V
2Be calculated as follows titer:
In the formula: T
ZnO-EDTA standard solution is to the titer of zinc paste, mg/ml;
V
2-Zn
2+Consume Cu
2+Mark liquid is long-pending, ml;
Al wherein
3+The demarcation of mark liquid: draw 5ml Al
3+Mark liquid adds 10ml EDTA solution in the 250ml conical flask, add one of paranitrophenol indicator, drips to yellow with ammoniacal liquor, transfers to colourless and excessive 3 with hydrochloric acid again, and heated and boiled 3min adds 10ml buffer solution, and 10 PAN indicator are used Cu while hot
2+The fixed excessive EDTA of mark drop, nearly terminal point adds 10ml ethanol, continues titration to aubergine, disregards the volume number; Add the 1g ammonium fluoride, shake, heated and boiled 2min makes and Al
3+The EDTA of complexing discharges, and solution becomes green again, adds 5ml buffer solution and 3 PAN indicator, uses Cu again
2+The mark drop is fixed to aubergine, record reading V
3Be calculated as follows titer:
（2）
In the formula:
-EDTA standard solution is to the titer of aluminium oxide, mg/ml;
V
3-Al
3+Consume Cu
2+Mark liquid is long-pending, ml;
The 2nd, the mensuration of zinc paste and alumina content in the AZO ceramic target sample: AZO ceramic target sample is mixed with test solution behind the mixed acid solution micro-wave digestion of hydrochloric acid and nitric acid, adopts two parts of test solutions to separate the titrimetry that zinc paste and alumina content are carried out in titration; When first part of test solution is used for the zinc oxide content measurement, adding excessive EDTA and zinc ion complexing, shelter aluminium ion with ammonium fluoride, add buffer solution, is indicator with PAN, increases the solubleness of indicator PAN through adding surfactant, uses Cu
2+The fixed excessive EDTA of mark drop, Cu when using titration end-point
2+The mark drop is decided the content that the volume number calculates zinc paste; When second part of test solution is used for the alumina content measurement, adds excessive EDTA and boil processing, regulate the pH value, make the complete complexing of aluminium ion and zinc ion and EDTA, add buffer solution, use Cu
2+Behind the fixed remaining EDTA of mark drop, add ammonium fluoride and shelter aluminium ion, displace the EDTA with the aluminium ion complexing, use Cu again
2+The displacement titration of mark liquid is separated out the EDTA suitable with aluminium content, Cu when using titration end-point
2+The mark drop is decided the content that the volume number calculates aluminium oxide.
Described buffer solution is that the pH value is 4.3 sodium acetate solution.
The surfactant that adds in the described titrate indicator PAN solution is that in neopelex, TritonX-100, Tween 80, the OP emulsifying agent one or more are united the solubleness that makes indicator PAN and increased with the titration end-point variable color obvious.
The mol ratio of described copper mark liquid and EDTA mark liquid is M
Cu 2+: M
EDTA=1:4.
Said acid base indicator is a paranitrophenol.
Surfactant neopelex that adds in the said PAN indicator solution and TritonX-100 concentration are 10～50gL
-1, Tween 80 and OP emulsifying agent are 10%～30%.
Described PAN indicator solution uses ethanol and water mixed solvent, wherein V
Ethanol: V
Water=5～3:1.
The invention has the beneficial effects as follows: the present invention is on the basis of original standard; The actual conditions that differ greatly in conjunction with zinc paste and alumina content in the AZO target; Zinc paste in the target and alumina content are measured respectively, and adopted among surfactant neopelex, Tween 80, OP emulsifying agent, the TritonX-100 one or more to unite use, make that the indicator end point mutation is sharp, accuracy is high as enhanced sensitivity; It is accurately stable to measure the result, favorable reproducibility.
Description of drawings
Fig. 1 is a demonstration test tables of data according to the invention.
Fig. 2 is a repeated experiment tables of data according to the invention.
Fig. 3 is a Precision test result table according to the invention.
Fig. 4 is an operating process block scheme of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Referring to Fig. 4, the assay method of zinc paste and alumina content comprises the steps: in a kind of AZO ceramic target
The demarcation of standard solution:
Be calculated as follows Cu
2+Mark liquid is marked the reduction coefficient k of liquid to EDTA:
（1）
In the formula: V
1-Cu
2+The volume of mark liquid, ml;
K-Cu
2+Mark liquid is to the reduction coefficient of EDTA mark liquid;
（3）
In the formula: T
ZnO-EDTA standard solution is to the titer of zinc paste, mg/ml;
V
2-Zn
2+Consume Cu
2+Mark liquid is long-pending, ml;
In the formula:
-EDTA standard solution is to the titer of aluminium oxide, mg/ml;
V
3-Al
3+Consume Cu
2+Mark liquid is long-pending, ml;
The mensuration of zinc paste and alumina content in the AZO ceramic target sample: earlier AZO ceramic target sample is made into test solution through the mixed acid solution micro-wave digestion of hydrochloric acid and nitric acid; In first part of test solution, add excessive EDTA and zinc ion complexing, shelter aluminium ion with ammonium fluoride, add buffer solution, be indicator with PAN, increase the solubleness of PAN through adding surfactant, use Cu
2+The fixed excessive EDTA of mark drop; In second part of test solution, add excessive EDTA and boil processing, regulate the pH value, make the complete complexing of aluminium ion and zinc ion and EDTA, add buffer solution, use Cu
2+Behind the fixed remaining EDTA of mark drop, add ammonium fluoride and shelter aluminium ion, displace the EDTA with the aluminium ion complexing, use Cu again
2+The EDTA suitable with aluminium content separated out in the displacement titration of mark liquid, and the titration end-point color change is obvious.
Described buffer solution is that the pH value is acetate-sodium acetate of 4.3.
The surfactant that adds in the described PAN indicator solution is that among neopelex, Tween 80, OP emulsifying agent, the TritonX-100 one or more are united use as enhanced sensitivity.
The mol ratio of copper mark liquid of stating and EDTA mark liquid is M
Cu 2+: M
EDTA=1:4.
Surfactant neopelex that adds in the PAN indicator solution and TritonX-100 concentration are 10～50gL
-1, Tween 80 and OP emulsifying agent are 10%～30%.
The PAN indicator solution uses ethanol and water mixed solvent, wherein V
Ethanol: V
Water=5～3:1.
1, reagent
1.1 ammoniacal liquor (1+1): ammoniacal liquor: the volume ratio 1:1 of water
1.2 hydrochloric acid (1+1): hydrochloric acid: the volume ratio 1:1 of water
1.3 pH is 4.3 buffer solution: take by weighing anhydrous sodium acetate 60g, be dissolved in the suitable quantity of water, add glacial acetic acid 100ml, be diluted to 1000ml, mix, check with pH meter with water.
1.4 paranitrophenol: 0.1%
1.5 PAN [1-(2-pyridylazo)-beta naphthal]: take by weighing ethanol content that 0.2gPAN, 4g neopelex be dissolved in 100ml and be 60%～90% solution.
1.6 ammonium fluoride: AR level, solid
1.7 aluminum standard solution:
Accurately take by weighing metallic aluminium (more than 99.5%) 0.5318g in polytetrafluoroethylene beaker, add 1+1 hydrochloric acid (3.2) 50ml, be cooled to room temperature, be settled to 100ml with water to dissolving.
1.8 zinc standard solution:
Accurately take by weighing zinc granule (more than 99.8%) 0.8050g, be dissolved in the 80ml hydrochloric acid (3.2), after the dissolving fully, cool to room temperature is settled to 1L with water, shakes up.
1.9 copper sulphate standard solution: 0.005 M
Take by weighing copper sulphate (CuSO
45H
2O is more than 99%) 2.5221g is dissolved in the suitable quantity of water, is settled to 2L.
1.10 EDTA standard solution: 0.02 M
Accurately take by weighing disodium ethylene diamine tetraacetate (more than 99%) 15.0400g and be dissolved in the suitable quantity of water with 10% NaOH and regulate it, be settled to 2L to pH=5.
2 zinc-aluminium content titration
Accurately take by weighing 1.000g AZO sample and place beaker, add V
Hydrochloric acid: V
Nitric acid: V
WaterThe mixed acid solution 20ml of=1:2:3, the micro-wave digestion sample, the cooling back moves in the 250ml volumetric flask, is diluted to scale with water, shakes up.The micro-wave digestion specific procedure is following: 100 ℃, and 5min; 120 ℃, 5 min; 140 ℃, 5min; 200 ℃, 15 min.
2.1 the mensuration of standard sample
2.1.1 the mensuration of zinc oxide content
Pipette 25ml test solution to be measured with transfer pipet, move in the 100ml volumetric flask, be diluted to scale, mixing.Test solution to be measured after the absorption 10ml dilution adds excessive EDTA mark liquid 10ml in the 250ml conical flask.Add one of paranitrophenol indicator, drip to yellow, transfer to colourless and excessive 3 with hydrochloric acid again, add the 1g ammonium fluoride with ammoniacal liquor.Above-mentioned solution is heated to little boiling, and 10 of buffer solution, the PAN indicator of adding 10ml are used Cu
2+The mark drop is fixed, adds 10ml ethanol during nearly terminal point, and titration is to aubergine, and record titration volume is counted V
4
2.1.2 the mensuration of alumina content
Pipette 10ml test solution to be measured with transfer pipet, add EDTA mark liquid 30ml.Add one of paranitrophenol indicator, drip to yellow with ammoniacal liquor, transfer to colourless and excessive 3 with hydrochloric acid again, heated and boiled 3min adds 10ml buffer solution, and 10 PAN indicator are used Cu while hot
2+The fixed excessive EDTA of mark drop, nearly terminal point adds 10ml ethanol, continues titration to aubergine, disregards the volume number.Add the 1g ammonium fluoride, shake, heated and boiled 2min makes and Al
3+The EDTA of complexing discharges, and solution becomes green again, adds 5ml buffer solution and 3 PAN indicator, uses Cu again
2+The mark drop is fixed to aubergine, record reading V
5
Be calculated as follows out the content of zinc paste and aluminium oxide in the sample:
In the formula;
-EDTA mark liquid is to the titer of aluminium oxide, mg/ml;
T
ZnO-EDTA mark liquid is to the titer of zinc paste, mg/ml;
V
4-Zn
2+Consume Cu
2+Mark liquid product, ml;
V
5-Al
3+Consume Cu
2+Mark liquid is long-pending, ml;
K-Cu
2+Mark liquid is to the reduction coefficient of EDTA standard solution, ml;
M-sample quality;
3 test figures and checking
In the AZO ceramic target, the content of general aluminium oxide accounts for 0%～5wt% of zinc paste and aluminium oxide total content.Take by weighing the metallic zinc and the aluminium of required quality with analytical balance, be accurate to 0.0002g.With placing the 250ml beaker; Adding 1+1 hydrochloric acid solution is heated to solid and all dissolves; The cooling back all moves in the 1000ml volumetric flask; Be diluted to scale; Mixing is mixed with shown in the table 1 standard reagent in 3, and wherein S-1 is converted into
; S-2 is
; S-3 is
.By above-mentioned test method operation, test figure is seen Fig. 1.
Embodiment 2: materials and handle 6 parts, measure according to the method for assay, obtain the RSD% value, RSD% is not more than 2%.The repeated experiment data are referring to Fig. 2.
Embodiment 3: get same sample and survey 5 times continuously, obtain RSD%, RSD% is not more than 2%.Precision test result is referring to Fig. 3.
Prove that through above result the result of experimental data is in the permissible error scope, and repeatability is good with precision, so proves that this experimental technique is feasible, and has been applied in the production, result of use is good.
Claims (8)
1. the assay method of zinc paste and alumina content in the AZO ceramic target is characterized in that determination step is:
AZO ceramic target sample is mixed with test solution behind the mixed acid solution micro-wave digestion of hydrochloric acid and nitric acid, adopts two parts of test solutions to separate the titrimetry that zinc paste and alumina content are carried out in titration; When first part of test solution is used for the zinc oxide content measurement, adding excessive EDTA and zinc ion complexing, shelter aluminium ion with ammonium fluoride, add buffer solution, is indicator with PAN, increases the solubleness of indicator PAN through adding surfactant, uses Cu
2+The fixed excessive EDTA of mark drop, Cu when using titration end-point
2+The mark drop is decided the content that the volume number calculates zinc paste; When second part of test solution is used for the alumina content measurement, adds excessive EDTA and boil processing, regulate the pH value, make the complete complexing of aluminium ion and zinc ion and EDTA, add buffer solution, use Cu
2+Behind the fixed remaining EDTA of mark drop, add ammonium fluoride and shelter aluminium ion, displace the EDTA with the aluminium ion complexing, use Cu again
2+The displacement titration of mark liquid is separated out the EDTA suitable with aluminium content, Cu when using titration end-point
2+The mark drop is decided the content that the volume number calculates aluminium oxide.
2. the assay method of zinc paste and alumina content in the AZO ceramic target according to claim 1, it is characterized in that: described buffer solution is that the pH value is 4.3 sodium acetate solution.
3. the assay method of zinc paste and alumina content in the AZO ceramic target according to claim 1 is characterized in that: the surfactant that adds in the described titrate indicator PAN solution is that in neopelex, TritonX-100, Tween 80, the OP emulsifying agent one or more are united the solubleness that makes indicator PAN and increased with the titration end-point variable color obvious.
4. the assay method of zinc paste and alumina content in the AZO ceramic target according to claim 1, it is characterized in that: described copper mark liquid is M with the mol ratio that EDTA marks liquid
Cu 2+: M
EDTA=1:4.
5. the assay method of zinc paste and alumina content in the AZO ceramic target according to claim 1, it is characterized in that: acid base indicator is a paranitrophenol.
6. like the assay method of zinc paste and alumina content in claim 1 or the 3 said AZO ceramic targets, it is characterized in that: surfactant neopelex that adds in the PAN indicator solution and TritonX-100 concentration are 10～50gL
-1, Tween 80 and OP emulsifying agent are 10%～30%.
7. like the assay method of zinc paste and alumina content in claim 1 or the 3 said AZO ceramic targets, it is characterized in that: described PAN indicator solution uses ethanol and water mixed solvent, wherein V
Ethanol: V
Water=5～3:1.
8. like the assay method of zinc paste and alumina content in the said AZO ceramic target of claim 6, it is characterized in that: the PAN indicator solution uses ethanol and water mixed solvent, wherein V
Ethanol: V
Water=5～3:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203698A (en) * | 2015-10-22 | 2015-12-30 | 商洛天野高新材料有限公司 | Method for directly determining aluminum content in aluminum-niobium alloy |
| CN113866344A (en) * | 2021-08-31 | 2021-12-31 | 浙江方圆检测集团股份有限公司 | Method for measuring mass fraction of aluminum oxide in aluminum water treatment agent by potentiometric titration |
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| WO2011139245A1 (en) * | 2010-05-04 | 2011-11-10 | The Thailand Research Fund | A method and composition for quantifying magnesium ions |
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2012
- 2012-07-04 CN CN2012102282380A patent/CN102798692A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2011139245A1 (en) * | 2010-05-04 | 2011-11-10 | The Thailand Research Fund | A method and composition for quantifying magnesium ions |
Non-Patent Citations (2)
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| 涂小红: "EDTA容量法测定锌合金中的铝量", 《福建分析测试》, vol. 18, no. 3, 31 December 2009 (2009-12-31), pages 52 - 54 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203698A (en) * | 2015-10-22 | 2015-12-30 | 商洛天野高新材料有限公司 | Method for directly determining aluminum content in aluminum-niobium alloy |
| CN113866344A (en) * | 2021-08-31 | 2021-12-31 | 浙江方圆检测集团股份有限公司 | Method for measuring mass fraction of aluminum oxide in aluminum water treatment agent by potentiometric titration |
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Application publication date: 20121128 |