CN114486972B - Method for quickly measuring copper foil electroplating solution - Google Patents
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Abstract
The invention provides a method for rapidly determining copper foil electroplating solution, wherein in the anti-oxidation treatment of the production surface of a copper foil, substances such as zinc, nickel, potassium pyrophosphate and the like are frequently used in the electroplating solution, and the stability of the contents of the substances directly determines the appearance color, impurity content and oxidation resistance of the copper foil, so how to rapidly and accurately detect the contents of the substances in the production process becomes a key point for ensuring the quality; compared with the method for testing zinc-nickel potassium pyrophosphate in the electroplating solution by manual titration or spectrophotometry, the method has the advantages of high detection efficiency, no detection waste liquid and the like; by combining the analysis, the X-ray fluorescence spectrometry is used for measuring the contents of zinc, nickel and potassium pyrophosphate in the copper foil electroplating solution, the test result is accurate, the deviation is small, the detection requirement of the solution can be completely met, and the method can replace the measuring method of a titration method and a spectrophotometry method.
Description
Technical Field
The invention relates to the technical field of copper foil electroplating, in particular to a method for quickly measuring a copper foil electroplating solution.
Background
In the heat resistance treatment process of the copper foil surface, a method of electroplating other metals is generally adopted, and a layer of multi-element metal (such as zinc and nickel) is further plated on the copper foil surface to form multi-element alloy at high temperature so as to improve the heat resistance of the copper foil. In addition, the plating layers can not only prevent the attack of amine substances in the prepreg resin to the copper foil, but also contribute to improving the chemical affinity of the copper foil and the base material, and further improve the binding force of the copper foil and the base material; the potassium pyrophosphate in the electroplating solution plays a role in complexing, which is beneficial to improving the dispersing capacity and the covering capacity of the electroplating solution in the electroplating process, so that the plating layer is more uniform and fine.
In the common electroplating solution inspection, the analysis of the contents of zinc, nickel and potassium pyrophosphate can be carried out by a titration method and a spectrophotometry method, and some measurement and research are proposed by scholars. However, the method has the defects of long analysis time, complex operation, one-by-one analysis of each element and the like. Compared with titration analysis and spectrophotometry analysis, the fluorescence spectrometry can simultaneously and rapidly carry out qualitative and quantitative analysis on various elements, so that the analysis efficiency is higher in success.
Disclosure of Invention
The invention provides a method for rapidly measuring a copper foil electroplating solution, aiming at solving the technical problems of simultaneously and rapidly performing qualitative and quantitative analysis on various elements and enabling the analysis efficiency to be more productive in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for quickly measuring a copper foil electroplating solution,
s1, determining the optimal experimental conditions: analyzing the single reagent spectrogram structure so as to confirm the optimal test condition, and verifying and analyzing the mixed solution spectrogram structure;
s2, establishing a testing standard working curve: preparing a standard reagent required by a standard curve, testing the X-ray intensity of a standard solution, and establishing a standard curve for testing;
s3, verifying the accuracy of the determination: verifying the test result error of the prepared solution with the known concentration, verifying the error of multiple tests of the same electroplating solution with unknown concentration on a production field, and obtaining a measurement error according to the verification test result;
and S4, placing the electrolyte to be detected into equipment for determination, and comparing the electrolyte with the test standard working curve to obtain a determination result.
Further, the test instrument was an Shimadzu X fluorescence spectrometer, model EDX7000.
Further, the required standard reagent is nickel sulfate hexahydrate (NiSO) 4 ·6H 2 Grade O, AR), zinc sulfate heptahydrate (NiSO) 4 ·7H 2 Grade O, AR), potassium pyrophosphate trihydrate (K) 4 P 2 O 7 ·3H 2 O, AR grade).
Further, the analyzing the single reagent spectrogram structure in S1 includes:
establishing a quantitative blind scanning curve: in instrument system software, sequentially establishing a detection standard curve of zinc, nickel and potassium elements by referring to an operation instruction;
a. zinc sulfate spectrogram structure analysis: accurately weighing 0.8244g AR-grade ZnSO 4 ·7H 2 Preparing O into 100ml solution, and actually calculating theoretical value Zn 2+ =1.87g/L, and the intensity of each element in the standard curve is tested by using different filters;
b. and (3) nickel sulfate spectrogram structure analysis: accurately weighing 0.3427 gAR-level NiSO by using an analytical balance 4 ·6H 2 Preparing O into 100ml solution, and actually calculating theoretical value Ni 2+ =0.75g/L, using the newly established standard curve, the intensity of each element therein was tested by using different filters;
c. structural analysis of potassium pyrophosphate spectrogram: accurately weighing 9.3378gAR K by using an analytical balance 4 P 2 O 7 ·3H 2 Preparing O into 100ml solution, and actually calculating theoretical value K 4 P 2 O 7 =81.25g/L, and testing the intensity of each element by adjusting different filters by using a newly-built standard curve;
the best test conditions confirm: the conditions from a to c are tested: whether the X-ray intensity of each element is increased or decreased along with the increase and decrease of the atomic number of the element or not is determined along with the increase and decrease of the atomic number of the element, so that the selection and the use of the optical filter in the test process of the zinc content in zinc sulfate, the nickel content in nickel sulfate and the potassium content in potassium pyrophosphate are determined.
Further, the formula for calculating the concentration of the standard reagent in S2 is as follows:
in the formula: 65.41-relative atomic mass of zinc atoms,
287.57——ZnSO 4 ·7H 2 the relative molecular mass of O is the ratio of,
d-standard reagent ZnSO 4 ·7H 2 The content of O, unit%,
m-weighing ZnSO 4 ·7H 2 The mass of O, in units of g,
v is the preparation volume, unit L;
in the formula: 58.69-relative atomic mass of nickel atoms,
262.85——NiSO 4 ·6H 2 the relative molecular mass of O is the ratio of,
d-Standard reagent NiSO 4 ·6H 2 The content of O, unit%,
m-weighing NiSO 4 ·6H 2 The mass of O, in g,
v-volume of preparation, unit L;
in the formula: 398.06-K 4 P 2 O 7 With respect to the mass of the molecules,
446.06——K 4 P 2 O 7 ·3H 2 the relative molecular mass of O is,
d-Standard reagent K 4 P 2 O 7 ·3H 2 The content of O, unit%,
m-weighing K 4 P 2 O 7 ·3H 2 The mass of O, in g,
v-volume formulated, unit L.
Further, the standard reagent preparation concentration table in S2 is:
standard reagent preparation concentration table
Further, the standard solution X-ray intensity test in S2 comprises: the standard reagent samples were tested using the EDX7000 software to obtain standard solution radiation intensity values.
Further, a standard curve for testing is established in S2: and (3) inputting the theoretical concentration of each standard sample into a standard value in EDX7000 detection system software, and performing curve fitting to complete the establishment of a standard curve for testing.
Further, S3, verifying the error of the test result of preparing the solution with the known concentration, and accurately weighing the ZnSO with the preset amount by using an analytical balance 4 ·7H 2 O、NiSO 4 ·6H 2 O、K 4 P 2 O 7 ·3H 2 Preparing 100ml of O pure reagent, and calculating Zn, ni and K in the O pure reagent 4 P 2 O 7 The actual contents of the contents are respectively measured by the drawn standard curve, and the test results are compared to verify the test errorA range.
Further, the concentration of the standard solution used in the determination method must cover the lowest and highest concentration of the production line, and the concentration of the production solution can not exceed the concentration of the standard curve; the test sample must be guaranteed to be placed in the same position, and the test window must be completely covered by the sample; the standard curve calibration and test analysis must ensure the same condition, and avoid the test abnormity caused by the change of X-ray intensity due to the inconsistency of operating conditions.
Compared with the prior art, the invention has the beneficial effects that:
the content of zinc, nickel and potassium pyrophosphate in the copper foil surface treatment electroplating solution can be rapidly measured; compared with the method for testing zinc-nickel potassium pyrophosphate in the electroplating solution by manual titration or spectrophotometry, the method has the advantages of high detection efficiency, no detection waste liquid and the like; by combining the analysis, the X-ray fluorescence spectrometry is used for measuring the contents of zinc, nickel and potassium pyrophosphate in the copper foil electroplating solution, the test result is accurate, the deviation is small, the detection requirement of the solution can be completely met, and the method can replace the measuring method of a titration method and a spectrophotometry method.
Drawings
FIG. 1 shows XRF method for testing X-ray intensity of each element in zinc sulfate solution;
FIG. 2 is XRF method for testing the pattern of each element in zinc sulfate solution;
FIG. 3 is an XRF test for X-ray intensity of each element in nickel sulfate solution;
FIG. 4 is a XRF method for testing the spectrum of each element in nickel sulfate solution;
FIG. 5 shows XRF measurement of X-ray intensity of each element in potassium pyrophosphate solution;
FIG. 6 is a XRF test of the spectrum of each element in potassium pyrophosphate solution;
FIG. 7 is XRF test of the spectrum of each element in mixed solution of zinc-nickel-potassium pyrophosphate;
fig. 8 is an X-ray intensity value corresponding to each standard solution concentration.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which may be embodied in different forms and not limited to the embodiments described herein, but which are provided so as to provide a more thorough and complete disclosure of the invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may be present, and when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present, as the terms "vertical", "horizontal", "left", "right" and the like are used herein for descriptive purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the knowledge of the terms used herein in the specification of the present invention is for the purpose of describing particular embodiments and is not intended to limit the present invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Example, a method for rapidly measuring a copper foil plating solution,
s1, determining the optimal experimental conditions: analyzing the spectrogram structure of the single reagent so as to determine the optimal test condition, and verifying and analyzing the spectrogram structure of the mixed solution;
s2, establishing a testing standard working curve: preparing a standard reagent required by a standard curve, testing the X-ray intensity of a standard solution, and establishing a standard curve for testing;
s3, verifying the accuracy of determination: verifying the error of the test result of the prepared solution with the known concentration, verifying the error of multiple tests of the same electroplating solution with unknown concentration in the production field, and obtaining the measurement error according to the verification test result;
and S4, placing the electrolyte to be detected into equipment for determination, and comparing the electrolyte with the test standard working curve to obtain a determination result.
Example, the test instrument was an Shimadzu X fluorescence spectrometer, model EDX7000.
In the examples, the standard reagent required was nickel sulfate hexahydrate (NiSO) 4 ·6H 2 Grade O, AR), zinc sulfate heptahydrate (NiSO) 4 ·7H 2 Grade O, AR), potassium pyrophosphate trihydrate (K) 4 P 2 O 7 ·3H 2 O, AR grade).
Example, please refer to fig. 1-6, wherein the analysis of the single reagent spectrogram structure in S1 comprises:
establishing a quantitative blind scanning curve: in instrument system software, sequentially establishing a detection standard curve of zinc, nickel and potassium elements by referring to an operation instruction;
a. zinc sulfate spectrogram structure analysis: accurately weighing 0.8244g AR-grade ZnSO 4 ·7H 2 Preparing O into 100ml solution, and actually calculating theoretical value Zn 2+ And the new standard curve is used for testing the strength of each element by using different filters, as shown in figures 1 and 2, and the test strength of the zinc element is higher than that of the oxygen element and the sulfur element under the same concentration condition in the figures, so that the sensitivity is higher. Thus ZnSO 4 ·7H 2 O, analyzing and selecting zinc element; selecting 2# and 3# optical filter conditions according to the actual concentration of the solution and the change of the element X-ray intensity during testing;
b. and (3) nickel sulfate spectrogram structure analysis: accurately weighing 0.3427gAR NiSO by using an analytical balance 4 ·6H 2 Preparing O into 100ml solution, and actually calculating theoretical value Ni 2+ And the intensity of each element is tested by using different filters by using a newly-built standard curve, as shown in fig. 3 and 4, when the same concentration condition exists in the graph, the test intensity of the nickel element is obviously higher than that of the oxygen element and the sulfur element, and the sensitivity is higher. NiSO fixation 4 ·6H 2 O, analyzing and selecting nickel element; selecting 2# and 3# optical filter conditions according to the actual concentration of the solution and the change of the X-ray intensity of each element during testing;
c. structural analysis of potassium pyrophosphate spectrogram: accurately weighing 9.3378gAR K by using an analytical balance 4 P 2 O 7 ·3H 2 Preparing O into 100ml solution, and actually calculating theoretical value K 4 P 2 O 7 =81.25g/L, using newly created standard curve, passingThe intensity of each element in different optical filter tests is adjusted, as shown in fig. 5 and 6, when the same concentration in the graphs is the same, the test intensity of the potassium element is obviously higher than that of the phosphorus element and the oxygen element, and the sensitivity is higher. Solid K 4 P 2 O 7 ·3H 2 O, analyzing and selecting potassium element; selecting the condition without the optical filter according to the actual concentration of the solution and the change of the X-ray intensity of each element during testing;
the best test conditions confirm: the conditions a-c show that: along with the increase of the atomic number of the elements, the X-ray intensity of each element increases along with the increase of the atomic number, a No. 4 optical filter is selected for testing the zinc content in the solid zinc sulfate and the nickel content in the nickel sulfate, and a No. 4 optical filter is selected for testing the potassium content in the potassium pyrophosphate content, without using the optical filter.
In the examples, please refer to fig. 7, the mixed solution spectrogram structure is verified and analyzed.
In an embodiment, the calculation formula of the standard reagent concentration in S2 is:
in the formula: 65.41-relative atomic mass of zinc atoms,
287.57——ZnSO 4 ·7H 2 the relative molecular mass of O is,
d-standard reagent ZnSO 4 ·7H 2 The content of O, in units%,
m-weighing ZnSO 4 ·7H 2 The mass of O, in units of g,
v is the preparation volume, unit L;
in the formula: 58.69-relative atomic mass of nickel atoms,
262.85——NiSO 4 ·6H 2 the relative molecular mass of O is the ratio of,
d-Standard reagent NiSO 4 ·6H 2 The content of O, unit%,
m-weighing NiSO 4 ·6H 2 The mass of O, in g,
v-volume of preparation, unit L;
in the formula: 398.06-K 4 P 2 O 7 With respect to the mass of the molecules,
446.06——K 4 P 2 O 7 ·3H 2 the relative molecular mass of O is,
d-Standard reagent K 4 P 2 O 7 ·3H 2 The content of O, unit%,
m-weighing K 4 P 2 O 7 ·3H 2 The mass of O, in g,
v-volume formulated, unit L.
In the embodiment, the standard reagent preparation concentration table in S2 is as follows:
standard reagent preparation concentration table
Example, standard solution X-ray intensity test in S2: the standard reagent samples were tested using the EDX7000 software to obtain standard solution radiation intensity values.
In the embodiment, please refer to fig. 8, the standard curve for testing is established in S2: in the EDX7000 detection system software, the theoretical concentration of each standard sample is input into a standard value, which is shown in figure 8, and curve fitting is carried out to complete the establishment of the standard curve for testing.
In the example, the error of the test result of preparing the solution with the known concentration is verified in the S3, and 1.0428 g of ZnSO is accurately weighed by an analytical balance 4 ·7H 2 O, 0.3815 g NiSO 4 ·6H 2 O, 10.4454 g K 4 P 2 O 7 ·3H 2 O analytically pure reagent is prepared into 100ml,through calculation, the Zn content is 2.36g/L, the Ni content is 0.84g/L, and K 4 P 2 O 7 The content is 90.89g/L, and the actual content is tested by the drawn standard curve and is shown in the following table:
test results for solutions of known concentration
And (3) analyzing test values:
in 20 groups of data of the test, the average deviation of the test value of the potassium pyrophosphate content is 0.22%, the average deviation of the test value of the zinc content is 0.042%, and the average deviation of the test value of the nickel content is 0.36%.
In the example, the error of multiple tests of the same plating solution with unknown concentration in the production field is verified in the step S3, and the actual content is tested by using the drawn standard curve as follows:
test results of different times of solution with unknown concentration
And (3) analyzing a test result:
(1) Under the optimal condition, the spectrogram peak of each element in the mixed solution is obvious under specific energy, no other peak exists near the characteristic peak, and no influence peak appears, which shows that under the condition, the test method has strong selectivity and high accuracy.
(2) The method is characterized in that AR reagents are used for preparing standard samples with known concentrations in a verification test, the accuracy and the stability of a standard curve are verified, from 20 groups of results of the standard reagent test with the known concentrations, the content of each component of the standard samples is uniformly distributed on two sides of a theoretical value, the mean error of the test values is less than 1%, and the standard deviation of each content is less than 0.3.
(3) Continuously testing 20 groups of data by producing the same solution on site, wherein the range of potassium pyrophosphate is 0.78g/L, the range of zinc is 0.04g/L, and the range of nickel is 0.03g/L; the standard deviation of the potassium pyrophosphate content is 0.179, the standard deviation of the zinc content is 0.012, and the standard deviation of the nickel content is 0.008, which proves that the test data of the on-site production solution has high stability.
The invention is described above with reference to the accompanying drawings, it is obvious that the invention is not limited to the above-described embodiments, and it is within the scope of the invention to adopt such insubstantial modifications of the inventive method concept and solution, or to apply the inventive concept and solution directly to other applications without modification.
Claims (7)
1. A method for rapidly measuring a copper foil electroplating solution is characterized by comprising the following steps:
s1, determining the optimal experimental conditions: analyzing the spectrogram structure of the single reagent so as to determine the optimal test condition, and verifying and analyzing the spectrogram structure of the mixed solution;
s2, establishing a standard working curve: preparing a standard reagent required by a standard curve, testing the X-ray intensity of a standard solution, and establishing a standard curve for testing;
s3, verifying the accuracy of the determination: verifying the error of the test result of the prepared solution with the known concentration, verifying the error of multiple tests of the same electroplating solution with unknown concentration in the production field, and obtaining the measurement error according to the verification test result;
s4, placing the electrolyte to be detected into equipment for determination, and comparing the electrolyte with the test standard working curve to obtain a determination result;
the step of analyzing the spectrogram structure of the single reagent in the step S1 comprises the following steps:
establishing a quantitative blind scanning curve: in instrument system software, sequentially establishing a detection standard curve of zinc, nickel and potassium elements by referring to an operation instruction;
a. zinc sulfate spectrogram structure analysis: accurately weighing 0.8244g AR-grade ZnSO 4 ·7H 2 Preparing O into 100ml solution, and actually calculating theoretical value Zn 2+ =1.87g/L, using the newly established standard curve, the intensity of each element therein was tested by using different filters;
b. analyzing the structure of a nickel sulfate spectrogram: using analytical balancesAccurately weighing 0.3427 gAR-level NiSO 4 ·6H 2 Preparing O into 100ml solution, and actually calculating theoretical value Ni 2+ =0.75g/L, using the newly established standard curve, the intensity of each element therein was tested by using different filters;
c. structural analysis of potassium pyrophosphate spectrogram: accurately weighing 9.3378gAR K by using an analytical balance 4 P 2 O 7 ·3H 2 Preparing O into 100ml solution, and actually calculating theoretical value K 4 P 2 O 7 =81.25g/L, and testing the intensity of each element by adjusting different filters by using a newly-built standard curve;
the best test conditions confirm: the conditions a-c show that: whether the X-ray intensity of each element is increased or decreased along with the increase or decrease of the atomic number of the element so as to determine the selection and the use of the optical filter in the testing process of the zinc content in zinc sulfate, the nickel content in nickel sulfate and the potassium content in potassium pyrophosphate;
the calculation formula of the concentration of the standard reagent in the S2 is as follows:
in the formula: 65.41-relative atomic mass of zinc atoms,
287.57——ZnSO 4 ·7H 2 the relative molecular mass of O is the ratio of,
d-Standard reagent ZnSO 4 ·7H 2 The content of O, unit%,
m-weighing ZnSO 4 ·7H 2 The mass of O, in g,
v is the preparation volume, unit L;
in the formula: 58.69-relative atomic mass of nickel atoms,
262.85——NiSO 4 ·6H 2 the relative molecular mass of O is the ratio of,
d——standard reagent NiSO 4 ·6H 2 The content of O, unit%,
m-weighing NiSO 4 ·6H 2 The mass of O, in g,
v is the preparation volume, unit L;
in the formula: 398.06-K 4 P 2 O 7 With respect to the mass of the molecules,
446.06——K 4 P 2 O 7 ·3H 2 the relative molecular mass of O is the ratio of,
d-Standard reagent K 4 P 2 O 7 ·3H 2 The content of O, unit%,
m-weighing K 4 P 2 O 7 ·3H 2 The mass of O, in g,
v-volume of preparation, unit L;
s3, verifying the error of the test result of the prepared solution with the known concentration, and accurately weighing preset amount of ZnSO by using an analytical balance 4 ·7H 2 O、NiSO 4 ·6H 2 O、K 4 P 2 O 7 ·3H 2 Preparing 100ml of O pure reagent, and calculating Zn, ni and K in the O pure reagent 4 P 2 O 7 The actual content is tested by the drawn standard curve, and the test result is compared to verify the test error range.
2. The method for rapidly measuring a copper foil plating solution according to claim 1, wherein: the test instrument was an Shimadzu X fluorescence spectrometer, model EDX7000.
3. The method for rapidly measuring a copper foil plating solution according to claim 1, wherein: the required standard reagent is nickel sulfate hexahydrate (NiSO) 4 ·6H 2 Grade O, AR), zinc sulfate heptahydrate (NiSO) 4 ·7H 2 O, AR grade), triple water cokePotassium phosphate (K) 4 P 2 O 7 ·3H 2 O, AR grade).
4. The method for rapidly measuring a copper foil plating solution according to claim 1, wherein: the standard reagent preparation concentration table in the S2 is as follows:
standard reagent formulation concentration table.
5. The method for rapidly measuring a copper foil plating solution according to claim 1, wherein: and (3) testing the X-ray intensity of the standard solution in the S2: the standard reagent samples were tested using the EDX7000 software to obtain standard solution radiation intensity values.
6. The method for rapidly measuring a copper foil plating solution according to claim 1, wherein: and establishing a standard curve for testing in the S2: and (3) inputting the theoretical concentration of each standard sample into a standard value in EDX7000 detection system software, and performing curve fitting to complete the establishment of a standard curve for testing.
7. The method for rapidly measuring a copper foil plating solution according to any one of claims 1 to 6, wherein: the concentration of the standard solution used by the determination method must cover the lowest concentration and the highest concentration of the production line, and the concentration of the production solution can not exceed the concentration of a standard curve; the test sample must be guaranteed to be placed in the same position, and the test window must be completely covered by the sample; the calibration of the standard curve and the test analysis must ensure the same condition, and the abnormal test caused by the change of the X-ray intensity caused by the manual operation condition is avoided.
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