CN106226288A - The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target - Google Patents
The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target Download PDFInfo
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Abstract
The invention discloses ICP AES method and measure gallium content in copper indium gallium selenium solar photovoltaic cell target, including preparing standard working solution, sample treatment, preparing in sample to be tested solution and blank solution, drafting standard working curve, the gallium content measured in sample to be tested solution and blank solution and sample six steps such as the calculating of the content of gallium, the inventive method simple and fast, result is accurate, and Repeatability and Reproducibility is good.
Description
Technical field
The invention belongs to technical field of measurement and test, relate to chemical composition quantitative analysis tech, be specifically related to ICP-AES method and measure
Gallium content in copper indium gallium selenium solar photovoltaic cell target.
Background technology
Solar energy is inexhaustible, nexhaustible Renewable resource, cleaning resource.Solar-energy photo-voltaic cell is exactly too
The light energy of sun radiation is converted into electric energy, and at present, solaode market major product is monocrystal silicon and polycrystalline silicon solar electricity
Pond, accounts for more than the 80% of total market.Due to high cost and the high pollution of production process of crystal silicon battery, cost is lower, production
The more environmentally-friendly thin-film solar cells of process is rapidly developed.Present stage, the thin-film solar cells of market prospect is had to have 3
Kind, it is non-crystalline silicon, cadmium telluride (CdTe) and CIGS (CuInGaSe2 is typically called for short CIGS) thin-film solar cells respectively.
As direct band gap compound semiconductor, CuInGaSe absorbed layer absorptance is up to 105cm-1, and transformation efficiency is all thin film
In solaode the highest, it has also become the whole world one of photovoltaic art study hotspot.CIGS target material is by copper, indium, gallium, selenium
The Chalkopyrite crystal formation material that four kinds of elements are constituted in proportion, is the core material producing thin-film solar cells, and the most each unit
The content of element, composition of proportions determine the quality of thin-film solar cells, therefore measure the content of each element in target and have great
Meaning.
Summary of the invention
For above-mentioned, it is an object of the invention to provide a kind of inductively coupled plasma atomic emission spectrum and (be called for short ICP-
AES) measuring the method for gallium content in copper indium gallium selenium solar photovoltaic cell target, sample, after nitric acid, dissolving with hydrochloric acid, with yttrium is
Internal standard inductively coupled plasma atomic emission spectrometer measures the intensity of elemental characteristic spectral line to be measured in sample solution, passes through
Internal standard curve method calculates gallium content in sample.
The concrete technical scheme that the present invention takes is:
The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target, its step includes:
(1) preparation of standard working solution:
Yttrium standard solution: weigh the high-purity yttrium oxide of 1.2699g first after 1000 DEG C of calcination 1h, be placed in exsiccator cold
But to room temperature, pour in 250mL beaker, add 20mL hydrochloric acid solution, cap upper surface ware, be heated to being completely dissolved, take off, with few
Amount water rinses surface plate, is cooled to room temperature, is transferred in 1000mL volumetric flask, and water is diluted to scale, shakes up；
Gallium standard solution: weigh 1.0000g gallium in 300mL beaker, adds 20mL hydrochloric acid solution, cap upper surface
Ware, low-temperature heat, to being completely dissolved, is taken off, and rinses surface plate with a small amount of water, adds 50mL hydrochloric acid solution, is cooled to room temperature, turns
Moving in 1000mL volumetric flask, water is diluted to scale, shakes up；
Gallium standard working solution: pipette gallium standard solution 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL,
5.00mL, in 6 50mL volumetric flasks, is separately added into 3mL salpeter solution and 0.50mL yttrium standard solution, makes after constant volume in solution
Containing yttrium 10 μ g/mL, water is diluted to scale, shakes up；This series standard solution 1mL containing gallium 0 μ g, 10.0 μ g, 20.0 μ g, 40.0 μ g,
80.0μg、100.0μg；
(2) sample treatment:
Sample is placed in 250ml beaker, little water moistening, addition nitric acid solution A, hydrochloric acid solution, cap upper surface ware, low
Temperature is heated to being completely dissolved, and takes off, and rinses surface plate with a small amount of water, adds nitric acid B solution, be cooled to room temperature, be transferred to by test solution
In 250mL volumetric flask, add 2.5mL yttrium standard solution, solution contains after making constant volume yttrium 10 μ g/mL, acid 5%, is diluted with water to
Scale, shakes up, and obtains sample to be tested solution, makees blank assay simultaneously；
(3) mensuration of standard working curve: according to the substantially concentration range of element to be measured in test solution, imports the work of gallium standard
Solution, by the intensity of spectral line of inductively coupled plasma atomic emission spectrometer metric works curve, with gallium element concentration
For abscissa, the intensity of spectral line is vertical coordinate, draws standard working curve；
(4) blank solution and the mensuration of sample to be tested solution: after standard working curve measures, first measure sample blank
Solution, then measure sample to be tested solution, if sample to be tested solution gallium content is beyond standard working curve scope, needs in addition dilute
Release, add after dilution into yttrium standard solution and salpeter solution, make in the dilute solution after constant volume containing yttrium 10 μ g/mL, salpeter solution
5%, calculate blank solution and the concentration of gallium element in sample to be tested solution by working curve；
(5) in sample, the content of gallium is calculated by formula:
In formula:
The content of gallium in W sample, unit is %；
Gallium concentration in the sample solution that ρ obtains from standard working curve, unit is μ g/mL；
ρ0Gallium concentration in the reagent blank liquid obtained from standard working curve, unit is μ g/mL；
V sample solution constant volume, unit is mL；
The quality of m sample, unit is g；
The multiple of k sample solution dilution.
In said determination method, sample granularity answers≤0.149mm.
In said determination method, sample need to carry out pretreatment: through 100 DEG C～110 DEG C of dry 1.5h, is placed in exsiccator cold
But to room temperature.
In said determination method, the mass fraction of gallium is between 3.00%～12.00%, and weighing sample quality is 0.2g,
It is accurate to 0.0001g.
In said determination method, yttrium oxide ω in step (1)Y2O3>=99.99%, the yttrium standard solution density of preparation
It is 1000 μ g/mL；Gallium ωGa>=99.99%, the gallium standard solution density of preparation is 1000 μ g/mL；
In said determination method, described salpeter solution density is 1.42g/mL, and hydrochloric acid solution density is 1.19g/mL；
In said determination method, the nitric acid solution A volume described in step (2) is 6ml, and the volume of hydrochloric acid solution is 2ml,
Nitric acid B solution volume is 7ml；
In said determination method, the analysis spectral line of described gallium element is: 417.206nm, and the analysis spectral line of yttrium is:
371.030nm。
In said determination method, the analysis spectral line of described gallium element is: 287.424nm, and the analysis spectral line of yttrium is:
324.228nm。
In said determination method, the detection of described gallium element is limited to 0.14 μ g.mL-1。
The invention has the beneficial effects as follows: the inventive method simple and fast, result is accurate, and Repeatability and Reproducibility is good.
Detailed description of the invention
Below embodiments of the invention are described in detail, so that advantages and features of the invention can be easier to by ability
Field technique personnel understand, thus protection scope of the present invention is made apparent clear and definite defining.
Instrument and equipment:
Electronic balance: sensibility reciprocal 0.1mg；
Adjustable temperature control electric hot plate；
Inductively coupled plasma atomic emission spectrometer: first start preheating 40min～60min before starting to measure, simultaneously
By argon purging light path to drive away the gas molecules such as light room air, to improve sensitivity and the stability of ultraviolet signal.
Material prepares:
Sample granularity≤0.149mm, sample, through 100 DEG C～110 DEG C of dry 1.5h, is placed in exsiccator and is cooled to room temperature.
Hydrochloric acid solution: density is 1.19g/mL；
Salpeter solution: density is 1.42g/mL；
High-purity yttrium oxide: ωY2O3>=99.99%；
Gallium: ωY2O3>=99.99%.
Embodiment
The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target, its step includes:
(1) preparation of standard working solution:
Yttrium standard solution: weigh the high-purity yttrium oxide of 1.2699g first after 1000 DEG C of calcination 1h, be placed in exsiccator cold
But to room temperature, pour in 250mL beaker, add 20mL hydrochloric acid solution, cap upper surface ware, be heated to being completely dissolved, take off, with few
Amount water rinses surface plate, is cooled to room temperature, is transferred in 1000mL volumetric flask, and water is diluted to scale, shakes up, and yttrium standard solution is close
Degree is 1000 μ g/mL；
Gallium standard solution: weigh 1.0000g gallium in 300mL beaker, adds 20mL hydrochloric acid solution, cap upper surface
Ware, low-temperature heat, to being completely dissolved, is taken off, and rinses surface plate with a small amount of water, adds 50mL hydrochloric acid solution, is cooled to room temperature, turns
Moving in 1000mL volumetric flask, water is diluted to scale, shakes up, and gallium standard solution density is 1000 μ g/mL；
Gallium standard working solution: pipette gallium standard solution 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL,
5.00mL, in 6 50mL volumetric flasks, is separately added into 3mL salpeter solution and 0.50mL yttrium standard solution, makes after constant volume in solution
Containing yttrium 10 μ g/mL, water is diluted to scale, shakes up；This series standard solution 1mL containing gallium 0 μ g, 10.0 μ g, 20.0 μ g, 40.0 μ g,
80.0μg、100.0μg；
(2) sample treatment:
Weigh 0.2g sample to be placed in 250ml beaker, little water moistening, add nitric acid 6mL, hydrochloric acid 2mL, cap upper surface
Ware, low-temperature heat, to being completely dissolved, is taken off, and rinses surface plate with a small amount of water, adds nitric acid 7mL, be cooled to room temperature, is shifted by test solution
Enter in 250mL volumetric flask, add 2.5mL yttrium standard solution, solution contains after making constant volume yttrium 10 μ g/mL, acid 5%, dilute with water
To scale, shake up, obtain sample to be tested solution, make blank assay simultaneously；
(3) mensuration of standard working curve: according to the substantially concentration range of element to be measured in test solution, imports the work of gallium standard
Solution, by the intensity of spectral line of inductively coupled plasma atomic emission spectrometer metric works curve, with gallium element concentration
For abscissa, the intensity of spectral line is vertical coordinate, draws standard working curve；
(4) blank solution and the mensuration of sample to be tested solution: after standard working curve measures, first measure sample blank
Solution, then measure sample to be tested solution, if sample to be tested solution gallium content is beyond standard working curve scope, needs in addition dilute
Release, add after dilution into yttrium standard solution and salpeter solution, make in the dilute solution after constant volume containing yttrium 10 μ g/mL, salpeter solution
5%, calculate blank solution and the concentration of gallium element in sample to be tested solution by working curve；
(5) in sample, the content of gallium is calculated by formula:
The measured value of the twice independent test result obtained under the conditions of repeatability, in average value ranges given below
In, the absolute difference of the two test result is less than repeatability limit (r), and the situation exceeding repeatability limit (r) is less than 5%,
Repeatability limit (r) is obtained by table 1 data acquisition linear interpolation:
Table 1 repeatability limit
| wGa/ % | 1.09 | 2.95 | 6.07 | 10.19 | 13.13 |
| R/% | 0.08 | 0.11 | 0.17 | 0.21 | 0.30 |
The absolute difference of the twice independent test result obtained under the conditions of repeatability is not more than repeatability limit (R), exceedes
The situation of repeatability limit (R) is less than 5%, and repeatability limit (R) is tried to achieve by table 2 data acquisition linear interpolation.
Table 2 repeatability limits
| wGa/ % | 1.09 | 2.95 | 6.07 | 10.19 | 13.13 |
| R/% | 0.09 | 0.14 | 0.19 | 0.21 | 0.32 |
Inductively coupled plasma atomic emission spectrometer operating reference condition
Claims (10)
1. the assay method of gallium content in a copper indium gallium selenium solar photovoltaic cell target, it is characterised in that its step includes:
(1) preparation of standard working solution:
Yttrium standard solution: weigh the high-purity yttrium oxide of 1.2699g first after 1000 DEG C of calcination 1h, be placed in exsiccator and be cooled to
Room temperature, pours in 250mL beaker, adds 20mL hydrochloric acid solution, cap upper surface ware, is heated to being completely dissolved, takes off, use a small amount of water
Rinsing surface plate, be cooled to room temperature, be transferred in 1000mL volumetric flask, water is diluted to scale, shakes up；
Gallium standard solution: weigh 1.0000g gallium in 300mL beaker, adds 20mL hydrochloric acid solution, and cap upper surface ware is low
Temperature is heated to being completely dissolved, and takes off, and rinses surface plate with a small amount of water, adds 50mL hydrochloric acid solution, is cooled to room temperature, is transferred to
In 1000mL volumetric flask, water is diluted to scale, shakes up；
Gallium standard working solution: pipette gallium standard solution 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 5.00mL in 6
In individual 50mL volumetric flask, it is separately added into 3mL salpeter solution and 0.50mL yttrium standard solution, makes after constant volume the μ g/ Han yttrium 10 in solution
ML, water is diluted to scale, shakes up；This series standard solution 1mL containing gallium 0 μ g, 10.0 μ g, 20.0 μ g, 40.0 μ g, 80.0 μ g,
100.0μg；
(2) sample treatment:
Being placed in by sample in 250ml beaker, little water moistening, add nitric acid solution A, hydrochloric acid solution, cap upper surface ware, low temperature adds
Heat, to being completely dissolved, is taken off, and rinses surface plate with a small amount of water, adds nitric acid B solution, be cooled to room temperature, test solution is transferred to 250mL
In volumetric flask, add 2.5mL yttrium standard solution, solution contain after making constant volume yttrium 10 μ g/mL, acid 5%, is diluted with water to scale,
Shake up, obtain sample to be tested solution, make blank assay simultaneously；
(3) mensuration of standard working curve: according to the substantially concentration range of element to be measured in test solution, imports the work of gallium standard molten
Liquid, by the intensity of spectral line of inductively coupled plasma atomic emission spectrometer metric works curve, with gallium element concentration be
Abscissa, the intensity of spectral line is vertical coordinate, draws standard working curve；
(4) blank solution and the mensuration of sample to be tested solution: after standard working curve measures, first measures sample blank molten
Liquid, then measure sample to be tested solution, if sample to be tested solution gallium content is beyond standard working curve scope, need to be diluted,
Add after dilution into yttrium standard solution and salpeter solution, make containing yttrium 10 μ g/mL, salpeter solution 5% in the dilute solution after constant volume,
Blank solution and the concentration of gallium element in sample to be tested solution is calculated by working curve；
(5) in sample, the content of gallium is calculated by formula:
In formula:
The content of gallium in W sample, unit is %；
Gallium concentration in the sample solution that ρ obtains from standard working curve, unit is μ g/mL；
ρ0Gallium concentration in the reagent blank liquid obtained from standard working curve, unit is μ g/mL；
V sample solution constant volume, unit is mL；
The quality of m sample, unit is g；
The multiple of k sample solution dilution.
Assay method the most according to claim 1, it is characterised in that sample granularity answers≤0.149mm.
Assay method the most according to claim 1, it is characterised in that sample need to carry out pretreatment: does through 100 DEG C～110 DEG C
Dry 1.5h, is placed in exsiccator and is cooled to room temperature.
Assay method the most according to claim 1, it is characterised in that the mass fraction of gallium 3.00%～12.00% it
Between, weighing sample quality is 0.2g, is accurate to 0.0001g.
Assay method the most according to claim 1, it is characterised in that yttrium oxide ω in step (1)Y2O3>=99.99%,
The yttrium standard solution density of preparation is 1000 μ g/mL；Gallium ωGa>=99.99%, the gallium standard solution density of preparation is 1000
μg/mL。
Assay method the most according to claim 1, it is characterised in that described salpeter solution density is 1.42g/mL, hydrochloric acid
Solution density is 1.19g/mL.
Assay method the most according to claim 6, it is characterised in that the nitric acid solution A volume described in step (2) is
6ml, the volume of hydrochloric acid solution is 2ml, and nitric acid B solution volume is 7ml.
Assay method the most according to claim 1, it is characterised in that the analysis spectral line of described gallium element is: 417.206nm,
The analysis spectral line of yttrium is: 371.030nm.
Assay method the most according to claim 1, it is characterised in that the analysis spectral line of described gallium element is: 287.424nm,
The analysis spectral line of yttrium is: 324.228nm.
Assay method the most according to claim 1, it is characterised in that the detection of described gallium element is limited to 0.14 μ g.mL-1。
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Application publication date: 20161214 |