CN103018399A - Detection method for measuring silver content of silver paste for solar battery - Google Patents
Detection method for measuring silver content of silver paste for solar battery Download PDFInfo
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Abstract
The invention relates to a detection method for measuring silver content of silver paste for a solar battery. The detection method comprises the following steps of: firstly, weighing a right amount of a silver paste sample for the solar battery, adding nitric acid, and slowly heating to nitrify the solution through an electric hot plate until the solution is basically clear; then, adding a certain amount of nitric acid into a test solution subjected to primary nitration by nitric acid, sequentially heating to 150 DEG C by the electric hot plate for secondary nitration until the solution is completely clear, and finally taking ammonium ferric sulfate as an indicating agent, using a thiocyanate standard solution to titrate a test solution, and meanwhile, carrying out a blank test; and calculating the silver content of the sample according to test data and a formula. The result proves that the relative standard deviation (n=11) of the silver sample, measured according to the invention, is less than 1%, and the method is accurate and reliable. The detection method provided by the invention has the advantages that the operation is simple, the detection method is economical and practical, the measuring speed is rapid, the efficiency is high, the measuring result is accurate, and the applicability is good.
Description
Technical field
The present invention relates to a kind of detection method of measuring used for solar batteries silver slurry silver content, specifically a kind of sample is come the analytical approach of silver content in the quantitative determination used for solar batteries silver slurry with the titration of thiocyanate standard solution after with the nitric acid secondary digestion, belong to the detection technique field.
Background technology
Fossil energy (coal, oil, rock gas) is the main body of Present Global energy consumption structure.Along with the mankind's continuous exploitation, the exhaustion of fossil energy is inevitable.In addition, fossil energy in use can produce a large amount of greenhouse gases CO
2, causing global warming, polar glacier melts, and sea level rise waits day by day serious environmental problem.Therefore, the free of contamination regenerative resources such as exploitation sun power, wind energy, geothermal energy and water energy become developing direction from now on.But the reality of wind energy, geothermal energy and hydraulic power potentials can the exploitation amount can not satisfy human demand to the energy far away in the world at present, and only having sun power is unique energy source that can guarantee human energy demand.Therefore, national governments all pay much attention to the development of photovoltaic industry, and the photovoltaic generation industry of China starts to walk in 20 century 70s, has obtained in recent years fast development, and China has been the first producing country of world's solar cell at present.
The end-process of the epitaxial growth of the appropriate design of solar battery structure, solar cell material and battery is the basic link of solar cell make three in whole solar cell manufacturing process.Solar cell just, last procedure of making as solar battery cell of the serigraphy of backplate and ablating work procedure, the selection of its material and the control of condition will directly affect the properties of whole solar cell.Therefore, the silver electronic paste as the indispensable material of this procedure is that solar cell device is made one of required critical material.
Used for solar batteries silver slurry is comprised of conductive phase silver powder, inorganic binder frit, organic carrier and the trace mineral supplement that improves battery performance, wherein organic carrier comprises organic solvent and organic resin, it is undertaken the printing of at substrate surface by serigraphy or other spraying technologies, forms electrode behind the drying and forming-film.Require used for solar batteries silver slurry to possess and stablize good silver-silicon Ohmic contact; The high conductivity lower cost; The manufacturability of good weldability, adhesion, printing performance and suitable for mass production; Be connected firmly with silicon chip, the erosion of soda acid, steam etc. is had certain resistibility.These all produce in various degree impact to the efficient of photovoltaic cell.
The particulate of argent is the Main Ingredients and Appearance of conductive silver paste.The content of argent in slurry is directly relevant with electric conductivity.Say in a sense, the content of silver is high, useful to the electric conductivity that improves it, but when its content surpassed critical volume concentration, its electric conductivity can not improve, and general silver content is in the 80%-90%(weight ratio) time, electric conduction quantity has reached mxm., when silver content continuation increase, electric conductivity no longer improves, and resistance value is in rising trend; When silver content was lower than 60%, the variation of resistance was unstable.In concrete the application, silver-colored fraction of particle is too high in the silver slurry, is bonded the probability that resin wraps low, and the bonding force of silver conductor descends behind the film-forming, the danger that has silver granuel to come off.So the silver content in the silver slurry has a suitable scope, generally 60% ~ 70%.
The silver content of used for solar batteries silver slurry is the important quality index that affects electric conductivity, and Accurate Determining used for solar batteries silver slurry silver content is very important.Because the solar electrical energy generation industry is a new industry, do not find standard method or the bibliographical information of measuring used for solar batteries silver slurry silver content at present.The patent No. is 201110233626, and (open (bulletin) day: invention 2012.03.28) provides a kind of measuring method of silver element content of conductive silver paste material, may further comprise the steps: A, take by weighing a certain amount of silver-colored slurry samples, be designated as m1; B, the silver-colored slurry samples that will take by weighing are put into baking oven, take out after toasting 4 ~ 6 hours under 80 ℃ of conditions, weigh after the cooling and record; C, the silver-colored slurry samples that obtains among the step B being put into baking oven again, is under 150 ~ 200 ℃ of conditions at temperature conditions, toasts after 1 hour and takes out, and weighs after the cooling and record; D, the silver-colored slurry samples that obtains among the step C being put into baking oven again, is under 350 ℃ of conditions at temperature conditions, toasts after 1 hour and takes out, and weighs after the cooling and record; E, repeating step D until samples weighing no longer changes, are designated as m2 with the final weight of silver-colored slurry samples; F, obtain the content of silver element in the silver slurry according to formula.Owing to forming conductive phase silver powder, inorganic binder frit, the organic carrier (comprising organic solvent and organic resin) of used for solar batteries silver electronic paste and improving kind and the content of the components such as trace mineral supplement of battery performance different, we are through overtesting, be that the step of measuring method of silver element content of conductive silver paste materials of 201110233626 inventions is under 350 ℃ of conditions according to the patent No., toast after 1 hour, the organic component of used for solar batteries silver paste fails to destroy fully, can not accurately calculate the silver content of used for solar batteries silver slurry.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of detection method based on measure used for solar batteries silver slurry silver content with titrimetry behind the nitric acid secondary digestion is provided, its detection method is simple to operate, economical and practical, finding speed is fast, efficient is high, and measurement result is accurate, and applicability is good.
Another object of the present invention provides accurately and reliably a kind of and easy, can be applied to the analytical approach of the silver content mensuration of used for solar batteries silver slurry.
According to technical scheme of the present invention, a kind of detection method of measuring used for solar batteries silver slurry silver content comprises the steps:
(1) sample once digests: take by weighing an amount of used for solar batteries silver slurry samples in the iodine flask of 250mL, add a certain amount of nitric acid, place on the electric hot plate 150 ℃ of slow hot digestion to solution substantially to clarify;
(2) sample secondary digestion: in step (1) gained test solution, add a certain amount of nitric acid along a bottle wall, continue to place on the electric hot plate 150 ℃ of heating secondary digestion to solution to clarify fully;
(3) titrimetry: take ammonium ferric sulfate as indicator, with thiocyanate standard solution titration test solution, do simultaneously blank test;
(4) result calculates: the silver content that by formula calculates sample according to test figure.
The detection method of the silver content of described mensuration used for solar batteries silver slurry, concrete steps are:
(1) sample once digests:
Take by weighing the used for solar batteries silver slurry samples of 0.3 ~ 0.5g through mixing in the iodine flask of 250mL, weight is recorded as m accurately to 0.2mg, adds 5.0mL nitric acid, places 150 ℃ of slow hot digestions on the electric hot plate, substantially clarifies to solution;
(2) sample secondary digestion:
Step (1) test solution is added 3.0mL nitric acid along the bottle wall again, continue to place on the electric hot plate 150 ℃ of hot digestion to solution to clarify fully, iodine flask is moved on the electric furnace, heat little boiling, extremely a bottle inner volume is about 3 ~ 5mL, takes off and is cooled to room temperature, with the not carbonated deionized water rinsing bottle of 5mL wall, cover bottle cap, place the dark place cooling, treat titration;
(3) titrimetry:
Pipette the not carbonated deionized water of 50mL in the iodine flask that step (2) gained treatments of the sample liquid is housed with graduated cylinder, add 10mL 100g/L ammonium ferric sulfate solution, be that C=0.1mol/L thiocyanate standard solution is titrated to brick-red precipitation 30s and does not take off and be terminal point with concentration, record titration volume V, do simultaneously blank test, the titration volume V of record blank test
0
(4) result calculates:
The computing formula of sample silver (Ag) content:
Described thiocyanate standard solution is a kind of in ammonium thiocyanate standard solution, sodium thiocyanate standard solution or the potassium rhodanide standard solution.
The present invention has following advantage: the present invention has set up a kind of detection method based on measure used for solar batteries silver slurry silver content with titrimetry behind the nitric acid secondary digestion by experimental study.The present invention can be the lifting of one of critical material of solar cell device making used for solar batteries silver slurry quality determining method and quality standard and improves provides scientific basis and reference, thereby the quality that promotes China's photovoltaic cell product improves and is stable, standard photovoltaic cell market helps the sound development of China's emerging energy industry solar electrical energy generation industry better.
Embodiment
The present invention will be further described below in conjunction with embodiment, and following embodiment only is used for explanation the present invention but not limitation of the present invention.
The detection method research of used for solar batteries silver slurry silver content is measured in titrimetry behind the embodiment 1 usefulness nitric acid digestion
1, instrument, sample and reagent
1.1 sample
The used for solar batteries silver slurry of 2 batches of separate sources: gather by Wuxi City product quality supervision and inspection center;
1.2 reagent
Nitric acid: top grade pure (Chemical Reagent Co., Ltd., Sinopharm Group); Monoammonium ferric sulfate dodecahydrate: analyze pure (Chemical Reagent Co., Ltd., Sinopharm Group); Ammonium thiocyanate: analyze pure (Chemical Reagent Co., Ltd., Sinopharm Group); Sodium chloride (national grade ii standard material, GBW(E) 060024, State Standard Matter Research Centre, BeiJing, China); The 100g/L ammonium ferric sulfate solution: the 10g Monoammonium ferric sulfate dodecahydrate is dissolved in 90ML (1+10) salpeter solution; 0.1mol/L ammonium thiocyanate standard solution: according to GB/T 601-2002 " preparation of chemical reagent standard titration solution " metric system standby with demarcation.
1.3 instrument
CPA225D electronic balance (0.1mg) (Sai Duolisi scientific instrument Beijing company limited); Temp. controllable electric hot plate (Community of Jin Tan County city Jin Cheng Guoqiang test apparatus factory); Electric furnace (Jiangyin City Poly scientific research apparatus company limited); Muffle furnace (Shanghai, Nantong City leads to the pharmaceutical machine instrument factory); PH counts (sky, Shanghai reaches Instr Ltd.); 216 type silver electrodes (Changzhou auspicious silver-colored exact science Instr Ltd.); 232 type contrast electrodes (Changzhou auspicious silver-colored exact science Instr Ltd.); 79-1 magnetic force heating mixing platform (Community of Jin Tan County city Jin Cheng Guoqiang test apparatus factory); The brown buret of 50mL (East Platform welfare glass apparatus factory); 20mL transfer pipet (East Platform welfare glass apparatus factory); 5mL, 10mL pipette (East Platform welfare glass apparatus factory).
2, sample once digests:
Take by weighing 0.3 ~ 0.5g(accurately to 0.2mg, be recorded as m) used for solar batteries through mixing silver slurry samples in the iodine flask of 250mL, add 5.0mL nitric acid, place 150 ℃ of slow hot digestions on the electric hot plate, substantially clarify to solution.
3, sample secondary digestion:
Sample is once digested test solution add 3.0mL nitric acid along the bottle wall again, continue to place on the electric hot plate 150 ℃ of hot digestion to solution to clarify fully, iodine flask is moved on the electric furnace, heat little boiling, extremely a bottle inner volume is about 3 ~ 5mL, takes off and is cooled to room temperature, with the not carbonated deionized water rinsing bottle of 5mL wall, cover bottle cap, place the dark place cooling, treat titration.
4, titrimetry:
Pipette the not carbonated deionized water of 50mL in the iodine flask that step (2) gained treatments of the sample liquid is housed with graduated cylinder, add 10mL 100g/L ammonium ferric sulfate solution, being titrated to brick-red precipitation 30s with C=0.1mol/L ammonium thiocyanate standard solution does not take off and is terminal point, record titration volume V, do simultaneously blank test, the titration volume V of record blank test
0
5, the result calculates:
The computing formula of sample silver (Ag) content:
6, the experimental study of sample-pretreating method
2 used for solar batteries silver slurry samples are processed three kinds of different pre-treating methods and processed rear its silver contents of titrimetry with secondary digestion processing, three digestion process, high temperature sinterings respectively, and test figure sees Table 1.
The method of three digestion process is: the test solution of processing through secondary digestion is added 2.0mL nitric acid along the bottle wall again, continued to place on the electric hot plate 150 ℃ of hot digestions 5 minutes, bottle is moved on the electric furnace, heat little boiling, extremely a bottle inner volume is about about 5mL, take off slightly cold, with the not carbonated deionized water rinsing bottle of 5mL wall, cover bottle cap, place the dark place cooling, by 4, titration step carries out titrimetry, by 5, the formula that calculates of result calculates the silver content of sample.
The method that high temperature sintering is processed is: take by weighing 4.0g(accurately to 0.2mg, being recorded as m) silver-colored slurry samples through mixing is in the porcelain crucible of 50mL, place to be heated on the electric furnace and do not smolder, move in the muffle furnace, 850 ℃ of calcination 2hr, cooling, take out, add 8.0mL nitric acid, place on the electric hot plate 150 ℃ slowly to move on the electric furnace behind the heating 1hr and heat, remove unnecessary nitric acid (should avoid during heating spilling) as far as possible, take off when solids (silver nitrate) is closely dried to the crucible, put the dark place and let cool, after the cooling rapidly with the solids in the crucible (silver nitrate) with not carbonated deionized water dissolving, and in the brown volumetric flask of 250.0mL constant volume, shake up.Accurately pipette the 20.00mL test solution in the 250mL conical flask with transfer pipet, by 4, the titrimetry step carries out titrimetry.
The computing formula of high temperature sintering pre-treating method sample silver (Ag) content:
The comparative studies of table 1 pre-treating method
Test figure shows, secondary digestion pre-treatment and three digestion pre-treatments, for identical sample, test result is basically identical, illustrate through secondary digestion pre-treatment sample and digested fully, the secondary digestion pre-treatment is with respect to three digestion pre-treatments, and step can reduce, the time can reduce, reagent can be saved.The high temperature sintering pretreatment process, add at silver oxide that nitric acid reaction changes into the process of silver nitrate and silver nitrate that reaction generates is shifting in the process of constant volume, be very easy to loss, and cause Lower result, and whole operating process is more loaded down with trivial details than secondary digestion pre-treatment and three digestion pre-treatments.Therefore suitable sample-pretreating method is the secondary digestion pre-treating method.
7, the comparative studies of chemical titration and potentiometric titration
Adopt under the identical high temperature sintering disposition in sample pre-treatments, use respectively the silver content of ammonium thiocyanate standard solution chemical titration and potentiometric titration titrimetry sample, experimental data sees Table 2.
Potentiometric titration is: take by weighing 0.2g(accurately to 0.1mg, being recorded as m ') national grade ii standard material sodium chloride is in the 250mL conical flask, after the not carbonated deionized water dissolving of adding 50mL is complete, take silver electrode as indicator electrode, mercurous chloride electrode is contrast electrode, with the silver slurry test solution titration sodium chloride solution that is converted into silver nitrate, variation according to solution potential in the titration process, calculate titration volume V with secondary difference quotient method, by formula (1) calculates first the volumetric molar concentration of silver slurry test solution silver nitrate, and more by formula (2) calculate the silver content in the silver slurry.
The computing formula of potentiometric titration silver (Ag) content:
Formula (1): test solution silver nitrate volumetric molar concentration
Formula (2): sample silver (Ag) content
The comparison Ag of table 2 chemical titration and potentiometric titration, %
Above test shows, in the situation that the measurement result of sample pre-treatments identical ammonium thiocyanate standard solution chemical titration and potentiometric titration is substantially identical.Ammonium thiocyanate standard solution chemical titration, whole mensuration process operation is easier; Potentiometric titration is according to the variation of solution potential, calculates with secondary difference quotient method, and terminal point is clearer and more definite, but whole measurement operation process and computation process is all more loaded down with trivial details as a result.Determine to adopt simple and easy to do chemical titration.
8, the appropriate samples amount of taking by weighing determines
The amount of taking by weighing of sample is few, and the representativeness of sample is poor; The amount of taking by weighing of sample is many, because organism is faint yellow in the sample after digestion, to the certain interference of being determined with of titration end-point, and the amount of taking by weighing of sample is more, and color and luster is darker, and the interference that titration end-point is judged is also larger.Test figure shows, the amount of taking by weighing of sample is in 0.3 ~ 0.5g scope the time, the titer of ammonium thiocyanate standard solution is between 18 ~ 35mL, in 30% ~ 80% optimum range of 50mL buret full scale, and the color of treatments of the sample liquid is more shallow, substantially do not affect the judgement to titration end-point, therefore the suitable sample amount of taking by weighing is 0.3 ~ 0.5g.
9, the precision of method
To 2 used for solar batteries silver slurry samples with the nitric acid secondary digestion after the titrimetry of ammonium thiocyanate standard solution measure and do method precision 11 times and test, experimental data sees Table 3.
Table 3 precision test data (n=11) Ag, %
| ? | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | AVG | RSD |
| Sample 1 | 66.51 | 67.09 | 66.88 | 67.27 | 66.77 | 66.76 | 67.40 | 66.86 | 66.62 | 66.98 | 66.59 | 66.88 | 0.42% |
| Sample 2 | 62.80 | 62.90 | 62.53 | 62.71 | 63.03 | 62.72 | 62.93 | 62.51 | 62.98 | 62.57 | 63.15 | 62.80 | 0.35% |
Above test demonstration, the above-mentioned relative standard deviation of measuring the silver-colored silver content of starching of used for solar batteries with titrimetry behind the nitric acid digestion is less than 1%, and method is reliably accurate.
Claims (3)
1. a detection method of measuring used for solar batteries silver slurry silver content is characterized in that, comprises the steps:
(1) sample once digests: take by weighing an amount of used for solar batteries silver slurry samples in the iodine flask of 250mL, add a certain amount of nitric acid, place on the electric hot plate 150 ℃ of slow hot digestion to solution substantially to clarify;
(2) sample secondary digestion: in step (1) gained test solution, add a certain amount of nitric acid along a bottle wall, continue to place on the electric hot plate 150 ℃ of heating secondary digestion to solution to clarify fully;
(3) titrimetry: take ammonium ferric sulfate as indicator, with thiocyanate standard solution titration test solution, do simultaneously blank test;
(4) result calculates: the silver content that by formula calculates sample according to test figure.
2. measure as claimed in claim 1 the detection method of used for solar batteries silver slurry silver content, it is characterized in that, concrete steps are:
(1) sample once digests:
Take by weighing the used for solar batteries silver slurry samples of 0.3 ~ 0.5g through mixing in the iodine flask of 250mL, weight is recorded as m accurately to 0.2mg, adds 5.0mL nitric acid, places 150 ℃ of slow hot digestions on the electric hot plate, substantially clarifies to solution;
(2) sample secondary digestion:
Step (1) test solution is added 3.0mL nitric acid along the bottle wall again, continue to place on the electric hot plate 150 ℃ of hot digestion to solution to clarify fully, iodine flask is moved on the electric furnace, heat little boiling, extremely a bottle inner volume is about 3 ~ 5mL, takes off and is cooled to room temperature, with the not carbonated deionized water rinsing bottle of 5mL wall, cover bottle cap, place the dark place cooling, treat titration;
(3) titrimetry:
Pipette the not carbonated deionized water of 50mL in the iodine flask that step (2) gained treatments of the sample liquid is housed with graduated cylinder, add the 10mL100g/L ammonium ferric sulfate solution, be that C=0.1mol/L thiocyanate standard solution is titrated to brick-red precipitation 30s and does not take off and be terminal point with concentration, record titration volume V, do simultaneously blank test, the titration volume V of record blank test
0
(4) result calculates:
The computing formula of sample silver (Ag) content:
3. measure as claimed in claim 1 the detection method of used for solar batteries silver slurry silver content, it is characterized in that: described thiocyanate standard solution is a kind of in ammonium thiocyanate standard solution, sodium thiocyanate standard solution or the potassium rhodanide standard solution.
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| CN103760055A (en) * | 2013-11-30 | 2014-04-30 | 彩虹集团电子股份有限公司 | Method for measuring silver content in silver slurry |
| CN107991341A (en) * | 2017-11-23 | 2018-05-04 | 温州宏丰电工合金股份有限公司 | A kind of quantitative evaluation method of AgSn original washing powders body degree of oxidation |
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| CN103760055A (en) * | 2013-11-30 | 2014-04-30 | 彩虹集团电子股份有限公司 | Method for measuring silver content in silver slurry |
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| CN107991341A (en) * | 2017-11-23 | 2018-05-04 | 温州宏丰电工合金股份有限公司 | A kind of quantitative evaluation method of AgSn original washing powders body degree of oxidation |
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