CN105424684A - Method for determining hydrochloric acid and ferric trichloride contents in ITO etching solution - Google Patents
Method for determining hydrochloric acid and ferric trichloride contents in ITO etching solution Download PDFInfo
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- CN105424684A CN105424684A CN201510732685.3A CN201510732685A CN105424684A CN 105424684 A CN105424684 A CN 105424684A CN 201510732685 A CN201510732685 A CN 201510732685A CN 105424684 A CN105424684 A CN 105424684A
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- hydrochloric acid
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention discloses a method for determining the hydrochloric acid and ferric trichloride contents in an ITO etching solution. Firstly, the ferric trichloride content is determined, and the mass fraction of ferric trichloride in a sample is calculated; then when the hydrochloric acid content is determined, a centrifugal machine is used for separating ferric hydroxide precipitate produced through reaction, the hydrochloric acid content in the ITO etching solution sample can be accurately measured by prejudging a titration end point in cooperation with a change curve of an electrode signal of a dynamic pH titrator, meanwhile the ITO etching solution sample can be online sampled in real time, titration of a titration experiment is performed by adopting an automatic titrator, sampling can be performed at any time, the detection speed is high, the hydrochloric acid concentration can be fed back, and the on-line detection and control requirements can be completely met.
Description
Technical field
The present invention relates to ITO etching solution field, be specially the assay method of hydrochloric acid and ferric trichloride content in a kind of ITO etching solution.
Background technology
ITO etching solution mainly refers to the chemicals for the etching of ITO layer.There are three classes at present: oxalic acid type, chloroazotic acid type and chlorination swage.Oxalic acid type etching solution can only be used for the etching of amorphous ITO layer, and the etching solution of chloroazotic acid type has very strong corrosivity, vigorous reaction instability of being heated, and the etching for crystalline state ITO layer mainly adopts the etching solution of chlorination swage.Because technological requirement is different, the etch-rate of different enterprise to ITO etching solution has different requirements, mainly controls etch-rate by the ratio of hydrochloric acid and ferric trichloride.
Be limited to detection method at present the preparation of ITO etching solution to be controlled mainly through process for preparation, and cannot do the content of hydrochloric acid in product and ferric trichloride and accurately measure.If this just causes occurring extremely in preparation, do not control by detecting, the undulatory property of product etch-rate is just larger.The current detection method for this product is there are no report.
Prior art cannot the content of each component in testing product, is just difficult to the stability controlling product etch-rate, also cannot carries out data analysis to abnormal article.This is because the normal detection method of acid uses standard solution of sodium hydroxide titration, but the existence of ferric trichloride and NaOH reaction can generate ferric hydroxide colloid, thus cannot judge titration end-point.
Summary of the invention
The technical problem to be solved in the present invention overcomes in prior art to do to the content of hydrochloric acid in product and ferric trichloride the defect accurately measured, and provides the assay method of hydrochloric acid and ferric trichloride content in a kind of ITO etching solution.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
An assay method for hydrochloric acid and ferric trichloride content in ITO etching solution, comprises the following steps:
1) mensuration of ferric trichloride content:
Take 1.5 ~ 2 grams, ITO etching solution sample, be accurate to 0.0001 gram, be placed in iodine flask, add 50 ml distilled waters, 3 milliliters of concentrated hydrochloric acids and 3 grams of potassium iodides, shake up, 30 minutes are placed in dark place, then add 50 ml distilled waters, be titrated to faint yellow with the sodium thiosulfate standard solution of 0.1N concentration, add the starch indicator solution of 2 milliliter of 10 grams per liter, continue to be titrated to solution blueness to disappear, do blank test simultaneously;
Ferric trichloride content X1 computing formula: X1=(V1-V2) * C*0.1622*100/M1
V1 is the consumption of sodium thiosulfate standard solution, and unit is milliliter;
V2 is the consumption of blank test sodium thiosulfate standard solution, and unit is milliliter;
C is the N of 0.1N sodium thiosulfate standard solution, and unit is N;
M1 is ITO etching solution example weight, and unit is gram;
0.1622 for being that 1.000mol/L sodium thiosulfate standard titration solution is suitable with 1.00mL concentration, with a gram quality for the iron chloride represented;
Gone out the massfraction of ferric trichloride in ITO etching solution sample by this formulae discovery, unit is %;
2) content of hydrochloric acid detects:
Take 4.5 ~ 5 grams, sample ITO etching solution sample, be accurate to 0.0001 gram, be placed in iodine flask, add 10 milliliters of 5N standard solution of sodium hydroxide, claim to obtain the gross weight M3 of sample hydro-oxidation sodium, be accurate to 0.0001 gram, shake 10 minutes, be placed in hydro-extractor rotating separation 10 minutes, get supernatant M4, be accurate to 0.0001 gram, add 2 instructions phenolphthalein solutions, the concentration of instructions phenolphthalein solution is 10 grams per liters, is titrated to solution redness disappears with 1N hydrochloric acid standard solution;
Content of hydrochloric acid X2 computing formula:
X2＝[10*C1-V*C2*(M3-M2*X1*0.006588)/M4-M2*X1*0.185]*3.646/M2
V is the consumption of hydrochloric acid standard solution, and unit is milliliter;
C1 is the N of 5N standard solution of sodium hydroxide, and unit is N;
C2 is the N of 1N hydrochloric acid standard solution, and unit is N;
X1 is the massfraction of ferric trichloride in ITO etching solution sample, and unit is %;
M2 is ITO etching solution example weight, gram;
M3 is the weight of ITO etching solution sample hydro-oxidation sodium standard solution, and unit is gram;
M4 is the weight of supernatant liquor, and unit is gram;
0.6588 generates for every gram of ferric trichloride and NaOH react, with a gram quality for the ferric hydroxide represented;
0.0185 consumes for every gram of ferric trichloride, the amount of the NaOH represented with molal quantity;
36.46 is suitable with every molar sodium hydroxide, with a gram quality for the hydrochloric acid represented;
Gone out the massfraction of hydrochloric acid in ITO etching solution sample by this formulae discovery, unit is %.
Preferably, in described step (1), the mass percent concentration of concentrated hydrochloric acid is 30 ~ 38%.
Preferably, to the online real time sample of ITO etching solution sample, titration experiments adopts autotitrator to carry out titration, can sample at any time, and detection speed is fast, and each acid concentration of energy Real-time Feedback, can meet the requirement of on-line checkingi and control completely.
Further, coordinate matching step 2 by the change curve of the electrode signal with dynamic ph titrator) in the judgement of titration end-point.When the electrode signal of dynamic ph titrator determines the real-time change of pH value, timely anticipation titration end-point terminal, then the situation that the redness paying close attention to solution disappears, there will not be the situation missing titration end-point, can accurately measure the content of hydrochloric acid in ITO etching solution sample.
The assay method of hydrochloric acid and ferric trichloride content in ITO etching solution of the present invention, when measuring the content of hydrochloric acid, hydro-extractor is used to carry out the ferric hydroxide precipitate of separating reaction generation, coordinate the change curve of the electrode signal of dynamic ph titrator to the anticipation of titration end-point, the content of hydrochloric acid in ITO etching solution sample can be accurately measured, simultaneously can to the online real time sample of ITO etching solution sample, titration experiments adopts autotitrator to carry out titration, can sample at any time, detection speed is fast, energy Real-time Feedback concentration of hydrochloric acid, the requirement of on-line checkingi and control can be met completely.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
An assay method for hydrochloric acid and ferric trichloride content in ITO etching solution, comprises the following steps:
1) mensuration of ferric trichloride content:
Take 1.8503 grams, ITO etching solution sample in real time online, be placed in iodine flask, add 50 ml distilled waters, 3 milliliters of mass percent concentrations be 30 ~ 38% hydrochloric acid and 3 grams of potassium iodides, shake up, place 30 minutes in dark place, then 50 ml distilled waters are added, adopt autotitrator, be titrated to faint yellow with the sodium thiosulfate standard solution of 0.1N concentration, add the starch indicator solution of 2 milliliter of 10 grams per liter, continue to be titrated to solution blueness to disappear, do blank test simultaneously;
Ferric trichloride content X1 computing formula: X1=(V1-V2) * C*0.1622*100/M1
V1 is the consumption 16.6mL of sodium thiosulfate standard solution;
V2 is the consumption 0.05mL of blank test sodium thiosulfate standard solution;
C is the N 0.1N of 0.1N sodium thiosulfate standard solution;
M1 is ITO etching solution example weight 1.8503g;
0.1622 for being that 1.000mol/L sodium thiosulfate standard titration solution is suitable with 1.00mL concentration, with a gram quality for the iron chloride represented;
Gone out the massfraction of ferric trichloride in ITO etching solution sample by this formulae discovery, unit is %;
X1＝(V1-V2)*C*0.1622*100/M1
X1＝(16.6-0.05)*0.1*0.1622*100/1.8503g＝14.51
2) content of hydrochloric acid detects:
Take sample ITO etching solution sample M24.6566g gram in real time online, be placed in iodine flask, add 10 milliliters of 5N standard solution of sodium hydroxide, claim to obtain the gross weight M316.5112g of sample hydro-oxidation sodium, shake 10 minutes, be placed in hydro-extractor rotating separation 10 minutes, get supernatant M4, be accurate to 0.0001 gram, add 2 instructions phenolphthalein solutions, the concentration of instructions phenolphthalein solution is 10 grams per liters, adopts autotitrator, coordinates matching step 2 by the change curve of the electrode signal with dynamic ph titrator) in the judgement of titration end-point.When the electrode signal of dynamic ph titrator determines the real-time change of pH value, timely anticipation titration end-point terminal, then the situation that the redness paying close attention to solution disappears, there will not be the situation missing titration end-point, is titrated to solution redness disappears with 1N hydrochloric acid standard solution;
Content of hydrochloric acid X2 computing formula:
X2＝[10*C1-V*C2*(M3-M2*X1*0.006588)/M4-M2*X1*0.185]*3.646/M2
V is the consumption of hydrochloric acid standard solution, and unit is milliliter;
C1 is the N of 5N standard solution of sodium hydroxide, and unit is N;
C2 is the N of 1N hydrochloric acid standard solution, and unit is N;
X1 is the massfraction of ferric trichloride in ITO etching solution sample, and unit is %;
M2 is ITO etching solution example weight, and unit is gram.
M3 is the weight 16.5112g of ITO etching solution sample hydro-oxidation sodium standard solution;
M4 is the weight 5.0256g of supernatant liquor;
X2＝[10*5-4.75*1*(16.5112-4.6566*14.51*0.006588)
/5.0256-4.6566*14.51*0.185]*3.646/4.6566＝17.47
After measured, the ferric trichloride in this ITO etching solution sample and the content of hydrochloric acid are all in the scope required, namely this ITO etching solution sample is qualified samples.
| Claimed range % | Measured value % | |
| Ferric trichloride | 14.0-15.0 | 14.51 |
| Hydrochloric acid | 17.0-18.0 | 17.47 |
The assay method of hydrochloric acid and ferric trichloride content in ITO etching solution of the present invention, when measuring the content of hydrochloric acid, hydro-extractor is used to carry out the ferric hydroxide precipitate of separating reaction generation, coordinate the change curve of the electrode signal of dynamic ph titrator to the anticipation of titration end-point, the content of hydrochloric acid in ITO etching solution sample can be accurately measured, simultaneously can to the online real time sample of ITO etching solution sample, titration experiments adopts autotitrator to carry out titration, can sample at any time, detection speed is fast, the each acid concentration of energy Real-time Feedback, the requirement of on-line checkingi and control can be met completely.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the assay method of hydrochloric acid and ferric trichloride content in ITO etching solution, is characterized in that, comprise the following steps:
1) mensuration of ferric trichloride content:
Take 1.5 ~ 2 grams, ITO etching solution sample, be accurate to 0.0001 gram, be placed in iodine flask, add 50 ml distilled waters, 3 milliliters of concentrated hydrochloric acids and 3 grams of potassium iodides, shake up, 30 minutes are placed in dark place, then add 50 ml distilled waters, be titrated to faint yellow with the sodium thiosulfate standard solution of 0.1N concentration, add the starch indicator solution of 2 milliliter of 10 grams per liter, continue to be titrated to solution blueness to disappear, do blank test simultaneously;
Ferric trichloride content X1 computing formula: X1=(V1-V2) * C*0.1622*100/M1
V1 is the consumption of sodium thiosulfate standard solution, and unit is milliliter;
V2 is the consumption of blank test sodium thiosulfate standard solution, and unit is milliliter;
C is the N of 0.1N sodium thiosulfate standard solution, and unit is N;
M1 is ITO etching solution example weight, and unit is gram;
0.1622 for being that 1.000 mol/L sodium thiosulfate standard titration solutions are suitable with 1.00 ml concns, with a gram quality for the iron chloride represented;
Gone out the massfraction of ferric trichloride in ITO etching solution sample by this formulae discovery, unit is %;
2) content of hydrochloric acid detects:
Take 4.5 ~ 5 grams, sample ITO etching solution sample, be accurate to 0.0001 gram, be placed in iodine flask, add 10 milliliters of 5N standard solution of sodium hydroxide, claim to obtain the gross weight M3 of sample hydro-oxidation sodium, be accurate to 0.0001 gram, shake 10 minutes, be placed in hydro-extractor rotating separation 10 minutes, get supernatant M4, be accurate to 0.0001 gram, add 2 instructions phenolphthalein solutions, the concentration of instructions phenolphthalein solution is 10 grams per liters, is titrated to solution redness disappears with 1N hydrochloric acid standard solution;
Content of hydrochloric acid X2 computing formula:
X2＝[10*C1/1000-V*C2/1000*(M3-M2*X1％*0.6588)
/M4-M2*X1％*0.0185]*36.46*100/M2
＝[10*C1-V*C2*(M3-M2*X1*0.006588)/M4-M2*X1*0.185]*3.646/M2
V is the consumption of hydrochloric acid standard solution, and unit is milliliter;
C1 is the N of 5N standard solution of sodium hydroxide, and unit is N;
C2 is the N of 1N hydrochloric acid standard solution, and unit is N;
X1 is the massfraction of ferric trichloride in ITO etching solution sample, and unit is %;
M2 is ITO etching solution example weight, gram;
M3 is the weight of ITO etching solution sample hydro-oxidation sodium standard solution, and unit is gram;
M4 is the weight of supernatant liquor, and unit is gram;
0.6588 generates for every gram of ferric trichloride and NaOH react, with a gram quality for the ferric hydroxide represented;
0.0185 consumes for every gram of ferric trichloride, the amount of the NaOH represented with molal quantity;
36.46 is suitable with every molar sodium hydroxide, with a gram quality for the hydrochloric acid represented;
Gone out the massfraction of hydrochloric acid in ITO etching solution sample by this formulae discovery, unit is %.
2. the assay method of hydrochloric acid and ferric trichloride content in a kind of ITO etching solution as claimed in claim 1, is characterized in that, in described step (1), the mass percent concentration of concentrated hydrochloric acid is 30 ~ 38%.
3. the assay method of hydrochloric acid and ferric trichloride content in a kind of ITO etching solution as claimed in claim 1, is characterized in that, to the online real time sample of ITO etching solution sample, titration experiments adopts autotitrator to carry out titration.
4. the assay method of hydrochloric acid and ferric trichloride content in a kind of ITO etching solution as claimed in claim 1, is characterized in that, the change curve matching step 2 by the electrode signal with dynamic ph titrator) in the judgement of titration end-point.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751491A (en) * | 2020-07-24 | 2020-10-09 | 苏州市晶协高新电子材料有限公司 | Method for analyzing concentration of mixed acid in silicon etching solution |
| CN112730735A (en) * | 2020-12-23 | 2021-04-30 | 四川通达惠金属制品有限公司 | Method for detecting acidity of hydrochloric acid containing iron salt |
| CN113252660A (en) * | 2021-05-13 | 2021-08-13 | 中航金属材料理化检测科技有限公司 | Method for analyzing chemical component content of high-temperature alloy corrosive liquid |
| CN113358813A (en) * | 2021-06-09 | 2021-09-07 | 合肥中聚合臣电子材料有限公司 | Method for detecting composition of hydrochloric acid and ferric trichloride ITO etching solution |
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- 2015-11-03 CN CN201510732685.3A patent/CN105424684B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751491A (en) * | 2020-07-24 | 2020-10-09 | 苏州市晶协高新电子材料有限公司 | Method for analyzing concentration of mixed acid in silicon etching solution |
| CN112730735A (en) * | 2020-12-23 | 2021-04-30 | 四川通达惠金属制品有限公司 | Method for detecting acidity of hydrochloric acid containing iron salt |
| CN113252660A (en) * | 2021-05-13 | 2021-08-13 | 中航金属材料理化检测科技有限公司 | Method for analyzing chemical component content of high-temperature alloy corrosive liquid |
| CN113358813A (en) * | 2021-06-09 | 2021-09-07 | 合肥中聚合臣电子材料有限公司 | Method for detecting composition of hydrochloric acid and ferric trichloride ITO etching solution |
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