CN107202831A - The assay method of copper ion concentration in a kind of copper acid etch liquid - Google Patents
The assay method of copper ion concentration in a kind of copper acid etch liquid Download PDFInfo
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- CN107202831A CN107202831A CN201710413128.4A CN201710413128A CN107202831A CN 107202831 A CN107202831 A CN 107202831A CN 201710413128 A CN201710413128 A CN 201710413128A CN 107202831 A CN107202831 A CN 107202831A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The present invention relates to the assay method of copper ion concentration in a kind of copper acid etch liquid in copper ion concentration determination techniques field in copper acid etch liquid.This method comprises the following steps：S1, pH cushioning liquid is added into copper acid etch liquid, weakly alkaline solution is obtained；S2, titrant is instilled in the weakly alkaline solution by automatical potentiometric titrimeter, and the current potential to the weakly alkaline solution is undergone mutation, and records the titrant volume V1 of consumption；S3, calculates the concentration C of copper ion in copper acid etch liquid.The assay method of copper ion concentration in copper acid etch liquid of the present invention, not only can rapidly and accurately detect the concentration of copper ion in copper acid etch liquid, improve the accuracy of detection, testing cost can be greatlyd save in addition, can be widelyd popularize in TFT industries.
Description
Technical field
The invention belongs to copper ion concentration determination techniques field in copper acid etch liquid, and in particular in a kind of copper acid etch liquid
The assay method of copper ion concentration.
Background technology
Thin film transistor (TFT) (TFT) technology is the large-scale semiconductive integrated circuit technique using new material and new technology, it
It is that on the on-monocrystalline piece such as glass or plastic base, atomic thin various films are constructed by multi-step process such as sputtering, chemical depositions,
And film is processed by etching, stripping etc., manufacture integrated circuit.
For the TFT generations line (i.e. G8.5) of current main flow, AL processing procedures can generally meet the demand of product.But
As Thin Film Transistor-LCD gradually develops toward in terms of oversize, high driving frequency, high-resolution, how effectively
Ground reduces panel conductor resistance and parasitic capacitance is increasingly important.Thin Film Transistor-LCD is high-quality to lead when making
Line process technique has become the key for dominating thin-film transistor component and panel characteristics.And copper conductor processing procedure have it is following excellent
Point：1. the influence of reduction driving signal delay.2. save the material cost of sputtered target material and lift production capacity.3. led compared to aluminium
Line, copper conductor processing procedure can effectively reduce line width, improve liquid crystal display penetration and the service efficiency of backlight.4. reduce gate
The usage amount of drive integrated circult, reduces cost.
In copper wiring, etching is a wherein the most key step.It is main and its used liquid etching composition is complex
To include hydrogen peroxide (about 18%), metal-chelator, various additives and fluorine compounds.The main function of hydrogen peroxide is etch copper
Film, its concentration directly affects the line width of copper conductor, thickness.And the copper ion dissolved in etching process can be catalyzed the decomposition of hydrogen peroxide
Reaction, influences hydrogen peroxide concentration, and then influences etch effect, finally influences product yield；And the decomposition reaction of hydrogen peroxide is
Exothermic reaction, if processing procedure do not control it is proper, it is easy to occur engineering safety unexpected.Simultaneously also containing big in waste water after the etching
The copper ion and hydrogen peroxide of amount, the catalytic decomposition of copper ion can cause liquid waste concentration to raise, and also result in waste water station or even transport
Defeated engineering safety is unexpected.Therefore, it is just aobvious outstanding to the monitoring of copper ion concentration in order to fundamentally suppress the decomposition of hydrogen peroxide
To be important.
At present determine Determined Copper in Aqueous Solution method have atomic absorption spectrophotometry, plasma emission spectrometry and
Titration (indicator colour developing).The Matrix effects of first two assay method are more complicated, detection speed relatively slow, expensive equipment and need
The test condition wanted is (dustless) relatively harsher., can be to instrument with first two method and copper ion concentration is higher in copper acid etch liquid
Device produces irreversible injury, and outcome measurement can be caused inaccurate if carrying out the dilution of big times of amount.In addition, first two
Method is required for preparing standard curve using expensive titer, considerably increases testing cost.And use indicator to develop the color and drip
When the method for determining is detected, artificial subjective judgement influence is big, causes larger resultant error.
The content of the invention
The required technical problem solved of the invention is to provide copper in a kind of copper acid etch liquid in view of the shortcomings of the prior art
The assay method of ion concentration, this method can rapidly and accurately detect the concentration of copper ion in copper acid etch liquid, for etching work
The prevention of the quality and engineering safety accident of skill has vital directive significance；Meanwhile, the cost of detection can be greatlyd save,
Improve the accuracy of detection.
Therefore, the invention provides a kind of assay method of copper ion concentration in copper acid etch liquid, it comprises the following steps：
S1, pH cushioning liquid is added into copper acid etch liquid, weakly alkaline solution is obtained；
S2, titrant is instilled in the weakly alkaline solution by automatical potentiometric titrimeter, molten to the alkalescent
The current potential of liquid is undergone mutation, and records the titrant volume V of consumption1；
S3, calculates the concentration C of copper ion in copper acid etch liquid.
According to the present invention, copper ion concentration C calculation formula is in described copper acid etch liquid：
Wherein, in C-copper acid etch liquid copper ion concentration, unit is mg/kg；
C1The concentration of-titrant, unit is mol/L；
V1The volume of the titrant of-consumption, unit is mL；
M1The molal weight of-copper ion, unit is g/mol；
m1The quality of-copper acid etch liquid, unit is g.
In certain embodiments of the present invention, the pH value of described weakly alkaline solution is 9-10.
In other embodiments of the present invention, described pH cushioning liquid is ammoniacal liquor-ammonium chloride buffer solution；Specifically
Ground, the pH value of the ammoniacal liquor-ammonium chloride buffer solution is 10 ± 0.5.
In certain embodiments of the present invention, described titrant is EDTA-Na2Solution；The present invention is to titration
The concentration of titer is not particularly limited, usually, the EDTA-Na2The concentration of solution is 0.1 ± 0.005mol/L.
In certain embodiments of the present invention, when potential jump occurs for described weakly alkaline solution, the change of current potential >=
5mv/s。
According to the present invention, the titrant volume V of the consumption1For 2-20mL.
According to the present invention, the copper ion concentration in described copper acid etch liquid is 1000-8000mg/kg.
Beneficial effects of the present invention are：The assay method of copper ion concentration in copper acid etch liquid of the present invention, can be quick
The concentration of copper ion in copper acid etch liquid is detected exactly, and the prevention of quality and engineering safety accident for etch process has
Vital directive significance；Meanwhile, need not be using expensive instrument and the standard liquid of copper ion in detection process, can
Greatly save testing cost.In addition, this method can improve the accuracy of detection, it can be widelyd popularize in TFT industries.
Embodiment
To be readily appreciated that the present invention, the present invention is described more detail below.
As it was previously stated, currently used for the method for determining Determined Copper in Aqueous Solution, either atomic absorption spectrophotometry
And plasma emission spectrometry, or titration (indicator colour developing), can not fast and accurately it detect in copper acid etch liquid
Copper ion concentration.
The application uses automatical potentiometric titrimeter, by titrimetric standard solution (EDTA-Na2Solution) it is automatic be added dropwise to be tuned into it is weak
In the copper acid etch liquid of alkalescence, due to EDTA-Na2With copper ion (Cu2+) complex reaction (shown in formula I), during titration end-point
Current potential in the alkalescent copper acid etch liquid can undergo mutation, and then judge titration end-point.The testing cost of this method is small, inspection
Survey result quick and precisely (one sample of 2-3 minutes), the concentration available for copper ion in laboratory and on-line monitoring copper acid etch liquid.
EDTA-Na2+Cu2+→EDTA-Cu+2Na+ (I)。
Therefore, in copper acid etch liquid involved in the present invention copper ion concentration assay method, available for detection copper ion
Concentration is copper ion concentration in 1000-8000mg/kg copper acid etch liquid, and it specifically includes following steps：
(1) ammoniacal liquor-ammonium chloride buffer solution is prepared：54g chloride solids are weighed to be dissolved in 350mL ammoniacal liquor, it is fixed with pure water
Hold to 1L, obtain ammoniacal liquor-ammonium chloride buffer solution, its pH is about 10.
(2) it is m accurately to weigh quality with electronics fraction analysis balance1G copper acid etch liquid is in measuring cup, right rearward measurement
A certain amount of above-mentioned ammoniacal liquor-ammonium chloride buffer solution is added in cup, jog makes it uniform, obtains mixed liquor；Pipetted with liquid-transfering gun
1uL mixed liquors, if it is not up to 9-10, continue ammonification water-ammonium chloride buffer in measuring pH on pH test paper, until its pH is
After 9-10,70-80mL is diluted with water to, weakly alkaline solution is obtained.
(3) measuring cup is put into the automatic rotating disk of automatical potentiometric titrimeter, current potential during titration end-point is set in software
Conductivity variations etc. judge when scope (- 200-200mv), the volume range (2-20mL) of required titrant and titration end-point
Canonical parameter；Then by EDTA-Na2Solution is instilled in the weakly alkaline solution by automatical potentiometric titrimeter, to the weak base
Property solution current potential undergo mutation, record consumption EDTA-Na2The volume V of solution1。
(4) concentration C of copper ion in copper acid etch liquid is calculated：Copper ion concentration C calculation formula is in copper acid etch liquid：
Wherein, in C-copper acid etch liquid copper ion concentration, unit is mg/kg；
C1The concentration of-titrant, unit is mol/L；
V1The volume of the titrant of-consumption, unit is mL；
M1The molal weight of-copper ion, unit is g/mol；
m1The quality of-copper acid etch liquid, unit is g.
Present inventor has found that, when the volume consumption of titrant is less than 2mL, electrode is easily sent out by studying
Raw erroneous judgement, causes experiment to terminate, therefore needed for setting during the volume range of titrant, by titration end-point regulation after 2mL.
20mL is the titrant consumption upper limit (purpose is cost-effective), if not occurring terminal during 20mL yet, reduces copper acid etch
Liquid sample weighting amount, is tested again.Therefore the volume range of the required titrant set in software is 2-20mL；Consume simultaneously
EDTA-Na2The volume V of solution1Also in the range of 2-20mL.
In the present invention, the quality of the copper acid etch liquid for weighing is not particularly limited.Usually, if in copper acid etch liquid
When the concentration of copper ion is in the range of 2000-3000mg/kg, the quality of the copper acid etch liquid weighed about 7-10g.If copper is sour
When the concentration of copper ion is in the range of 6000-8000mg/kg in etching liquid, the quality of the copper acid etch liquid weighed about 2-
3g.It is sample weighting amount typically with the general concentration agent of copper ion in 20000 divided by copper acid etch liquid.
Term " mg/kg " is equal with the implication of " ppm " in the present invention.
Embodiment
To make the present invention easier to understand, the present invention is further described in embodiment below, these embodiments
Only serve illustrative, it is not limited to application of the invention.If the raw material or component used in the present invention are without special
Illustrate be made by commercial sources or conventional method.
The automatical potentiometric titrimeter used in following embodiments is 888 automatical potentiometric titrimeter, and structure is logical from Switzerland ten thousand.
The pH buffer solutions used is ammoniacal liquor-ammonium chloride buffer solutions, and compound method is：54g chloride solids are weighed to be dissolved in
In 350mL ammoniacal liquor, 1L is settled to pure water, ammoniacal liquor-ammonium chloride buffer solution (pH=10) is obtained.
The EDTA-Na that the titrant used is 0.1mol/L for concentration2Solution.
The concentration of the copper ion standard liquid used for：5000ppm.
Embodiment 1
(1) analyse balance with electronics fraction and accurately weigh copper acid etch liquid that quality is 7.40494g in measuring cup, use ammonia
Water-ammonium chloride buffer solution adjusts its pH to 9-10, is then diluted with water to 70-80mL, obtains weakly alkaline solution.
(2) measuring cup is put into the automatic rotating disk of automatical potentiometric titrimeter, current potential during titration end-point is set in software
The criterion parameter such as conductivity variations when scope, the volume range of required titrant and titration end-point；Then by concentration
For 0.1mol/L EDTA-Na2Solution is instilled in the weakly alkaline solution, and the current potential to the weakly alkaline solution is undergone mutation,
Record the EDTA-Na of consumption2The volume of solution is 3.2424mL.
(3) according to the EDTA-Na of consumption2The concentration of copper ion is in the volume of solution, calculating copper acid etch liquid
2785.29mg/kg。
Embodiment 2：The degree of accuracy is tested.
It is the copper acid etch liquid in 5000ppm standard liquid alternate embodiment 1 from copper ion concentration, according to embodiment
The copper ion concentration in detection method bioassay standard solution in 1, parallel determination 3 times, experimental result is shown in Table 1.
Table 1：The degree of accuracy experimental result of detection method of the present invention.
| Standard sample | Standard value (mg/kg) | Measured value (mg/kg) | Average value (mg/kg) | Relative deviation |
| Standard liquid | 5000 | 4926/4988/4895 | 4936 | 1.28% |
From the above understand, the relative deviation of detection method of the present invention is smaller, the degree of accuracy can meet laboratory and
The analysis of copper ion concentration requires (relative deviation is within 5%) in on-line monitoring copper acid etch liquid, and molecular velocity is fast,
With higher application value.
It should be noted that embodiment described above is only used for explaining the present invention, do not constitute to any of the present invention
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that wherein word used is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it is related to
And specific method, material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, this hair
It is bright to can be extended to other all methods and applications with identical function.
Claims (9)
1. the assay method of copper ion concentration in a kind of copper acid etch liquid, it comprises the following steps：
S1, pH cushioning liquid is added into copper acid etch liquid, weakly alkaline solution is obtained；
S2, titrant is instilled in the weakly alkaline solution by automatical potentiometric titrimeter, to the weakly alkaline solution
Current potential is undergone mutation, and records the titrant volume V of consumption1；
S3, calculates the concentration C of copper ion in copper acid etch liquid.
2. assay method according to claim 1, it is characterised in that copper ion concentration C in described copper acid etch liquid
Calculation formula is：
<mrow>
<mi>C</mi>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>C</mi>
<mn>1</mn>
</msub>
<mo>&times;</mo>
<msub>
<mi>V</mi>
<mn>1</mn>
</msub>
<mo>&times;</mo>
<msub>
<mi>M</mi>
<mn>1</mn>
</msub>
<mo>&times;</mo>
<msup>
<mn>10</mn>
<mn>3</mn>
</msup>
</mrow>
<msub>
<mi>m</mi>
<mn>1</mn>
</msub>
</mfrac>
</mrow>
Wherein, in C-copper acid etch liquid copper ion concentration, unit is mg/kg；
C1The concentration of-titrant, unit is mol/L；
V1The volume of the titrant of-consumption, unit is mL；
M1The molal weight of-copper ion, unit is g/mol；
m1The quality of-copper acid etch liquid, unit is g.
3. assay method according to claim 1, it is characterised in that the pH value of described weakly alkaline solution is 9-10.
4. assay method according to claim 1, it is characterised in that described pH cushioning liquid is slow for ammoniacal liquor-ammonium chloride
Rush solution.
5. assay method according to claim 4, it is characterised in that the pH value of described ammoniacal liquor-ammonium chloride buffer solution
For 10 ± 0.5.
6. assay method according to claim 1, it is characterised in that described titrant is EDTA-Na2Solution.
7. assay method according to claim 1, it is characterised in that when potential jump occurs for described weakly alkaline solution,
Changing value >=5mv/s of current potential.
8. assay method according to claim 1, it is characterised in that the titrant volume V of the consumption1For 2-
20mL。
9. assay method according to claim 1, it is characterised in that the copper ion concentration in described copper acid etch liquid is
1000-8000mg/kg。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108562636A (en) * | 2018-03-01 | 2018-09-21 | 白银有色集团股份有限公司 | A kind of method that automatic potential titrator tests determine the content of copper in anode copper |
| CN109728098A (en) * | 2019-01-03 | 2019-05-07 | 合肥鑫晟光电科技有限公司 | Thin film transistor (TFT), sensor, detection method, detection device and detection system |
| CN110763749A (en) * | 2019-10-22 | 2020-02-07 | 湖北兴福电子材料有限公司 | Method for detecting fluorine ions in acid-containing etching solution |
| CN111579714A (en) * | 2020-06-28 | 2020-08-25 | 成都光明光电股份有限公司 | Method for measuring content of copper oxide in copper metaphosphate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108562636A (en) * | 2018-03-01 | 2018-09-21 | 白银有色集团股份有限公司 | A kind of method that automatic potential titrator tests determine the content of copper in anode copper |
| CN109728098A (en) * | 2019-01-03 | 2019-05-07 | 合肥鑫晟光电科技有限公司 | Thin film transistor (TFT), sensor, detection method, detection device and detection system |
| CN110763749A (en) * | 2019-10-22 | 2020-02-07 | 湖北兴福电子材料有限公司 | Method for detecting fluorine ions in acid-containing etching solution |
| CN110763749B (en) * | 2019-10-22 | 2022-05-06 | 湖北兴福电子材料有限公司 | Method for detecting fluorine ions in acid-containing etching solution |
| CN111579714A (en) * | 2020-06-28 | 2020-08-25 | 成都光明光电股份有限公司 | Method for measuring content of copper oxide in copper metaphosphate |
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