CN115219535A - Method for detecting content of alpha-state crystalline silica in silica by powder polycrystal X-ray diffractometer - Google Patents
Method for detecting content of alpha-state crystalline silica in silica by powder polycrystal X-ray diffractometer Download PDFInfo
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- CN115219535A CN115219535A CN202110415143.9A CN202110415143A CN115219535A CN 115219535 A CN115219535 A CN 115219535A CN 202110415143 A CN202110415143 A CN 202110415143A CN 115219535 A CN115219535 A CN 115219535A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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Abstract
The invention discloses a method for detecting alpha-state crystalline silica content in silica by a powder polycrystal X-ray diffractometer, which comprises the following specific steps: setting reference values of parameters of a polycrystalline X-ray diffractometer, and crushing and grinding a sample into powder by using a ball mill; mixing the prepared alpha-state crystalline silica micro powder with amorphous silica micro powder according to a mass ratio, and collecting intensity data in a step scanning mode; collecting scattering intensity of amorphous silica micropowder and blank sample rack without sample, deducting scattering of blank sample, separating crystalline state from amorphous state by using amorphous silica micropowder scattering curve as standard, calculating integral area of amorphous silica and integral area of alpha-state crystalline silica micropowder, and calculating correction factor K of a sample α A value; subjecting the sample to be tested to determination K α Light path condition and step scanning range with same valueAnd collecting a scattering intensity curve of the sample to be measured, deducting the scattering of a blank frame, separating the scattering of the crystalline state and the amorphous state in the scattering curve by using peak separation software to obtain the integral area of amorphous silicon dioxide and the integral area of alpha-state crystalline silicon dioxide micropowder, and calculating the content of the state crystalline silicon dioxide.
Description
Technical Field
The invention relates to the field of physical and chemical analysis, in particular to a method for detecting alpha-state crystalline silica content in silica by a powder polycrystal X-ray diffractometer.
Background
The laboratory detection of the content of silica in quartz sand and quartz ore generally depends on the electronic industry standard SJ/T3228.4-2016 & high-purity quartz sand for electronic products part 4: measurement of silica. The standard principle is that three clean platinum crucibles are placed in a high-temperature muffle furnace at 1100 ℃ and are fired to be constant, a sample is fired in the high-temperature muffle furnace at 1000 ℃, an appropriate amount of the fired sample is weighed and is placed in the constant-weight platinum crucible, sulfuric acid and hydrofluoric acid are respectively added to dissolve the sample, the platinum crucibles which are completely dissolved and evaporated to dryness are fired in the muffle furnace at 1000 ℃, and then the content of silicon dioxide is calculated. The disadvantages of the method are: (1) the used acids are various in types and large in amount; a platinum crucible is used, so that the price is high and the loss is easy; (3) weighing for multiple times, and the error is large; (4) a muffle furnace is used, so that the power consumption is large and unsafe; (5) Too many analysis steps, at least three working days for the inspection period, and the problem of uncertainty of the result. This method is too labor intensive for laboratories dedicated to the field of silicon materials detection and too long for the customer to obtain results.
Disclosure of Invention
The invention aims to provide a method for detecting the content of alpha-state crystalline silica in silica by a powder polycrystalline X-ray diffractometer, which solves the technical problems of complexity and long time consumption of a traditional chemical method in the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
first, polycrystalline X-ray diffractometer parameter reference values were set: the copper target has a light pipe voltage of 40kV, a light pipe current of 40mA, an incident slit of 0.6mm, a receiving slit of 8mm, a set step length of 0.01 degrees, a scanning time of 0.05s and a diffraction angle range of 10-35 degrees.
Further, crushing and grinding the sample by using a ball mill, firstly, using a 600-mesh standard sieve to sieve the powder, and then, sieving the undersize materials by using a 10 mu m filter cloth sieve to obtain liquid with the particle size smaller than 10 mu m. Taking 10g of powder with the particle size of less than 10 mu m, placing the powder in a 600mL beaker, adding water, stirring, precipitating for about 2 hours, pouring out filtrate, precipitating the filtrate for about 16 hours, taking sediment of the filtrate, and testing the sediment by using a laser particle size analyzer, wherein the optimal particle size range is 2 mu m-10 mu m.
Furthermore, the prepared alpha-state crystalline silica micro powder and amorphous silica micro powder are taken to form six samples according to the mass ratio of 0.005.
Further, collecting the scattering intensity of the amorphous silica micropowder and a blank sample rack without a sample under the same experimental condition, deducting the scattering intensity of the blank sample, separating crystalline state from amorphous state by taking the scattering curve of the amorphous silica micropowder as a standard, and calculating the integral area S of the amorphous silica α Integral area S of fine powder of alpha-form crystalline silica c Then, the correction factor K of a sample is obtained α The value is obtained.
Further, K α The value is calculated according to equation (1):
further, the sample to be tested is tested for K α Light of the same valueCollecting scattering intensity curve of sample to be measured, deducting scattering of blank frame, utilizing peak-separating software to separate crystalline state from amorphous state in scattering curve to obtain integral area S of amorphous silicon dioxide ＇ α Integral area S of fine powder of alpha-form crystalline silica ＇ c 。
Further, the content (X) of crystalline silica in the alpha state c ) Calculating according to the formula (2):
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1
And (3) crushing and grinding by using a ball mill, firstly, taking powder by using a 600-mesh standard sieve, and then, taking liquid with the particle size smaller than 10 mu m by using a 10 mu m filter cloth sieve on the undersize. Taking 10g of powder with the particle size smaller than 10 mu m, placing the powder in a 600mL beaker, adding water, stirring, depositing for about 2 hours, pouring out filtrate, depositing the filtrate for about 16 hours, taking sediment, and testing the sediment by using a laser particle size analyzer, wherein the optimal particle size range is 2 mu m-10 mu m; taking prepared alpha-state crystalline silica micro powder and amorphous silica micro powder, forming six samples according to the mass ratio of 0.005; collecting the scattering intensity of amorphous silica micropowder and blank sample rack without sample under the same experimental condition, deducting blank sample scattering, separating crystalline state from amorphous state scattering by using amorphous silica micropowder scattering curve as standard, calculating integral area of amorphous silica and integral area of alpha state crystalline silica micropowder, and calculating correction factor K of a sample α A value; subjecting the sample to be tested to determination K α The light path conditions and the step scanning range with the same value are used for collecting the scattering intensity of the sample to be detectedAnd (3) deducting the scattering of a blank frame, separating the crystalline state from the amorphous state in the scattering curve by using peak separation software to obtain the integral area of amorphous silica and the integral area of silica micropowder, and finally calculating the content of alpha-state crystalline silica, wherein the result is shown in table 1.
TABLE 1
Through the analysis of the test data in the table 1, the relative deviation of the detection result obtained by the method compared with the standard sample is very small, and the result data obtained by the method is more stable and completely meets the test requirement.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (5)
1. A method for detecting the content of alpha-form crystalline silica in silica by a powder polycrystalline X-ray diffractometer, the method comprising the steps of:
a) The parameter setting reference value of the polycrystalline X-ray diffractometer is specified;
b) Crushing and grinding a sample by using a ball mill to prepare powder;
c) Mixing the prepared alpha-state crystalline silica micro powder and amorphous silica micro powder according to a mass ratio, and collecting intensity data in a step scanning mode;
d) Collecting scattering intensity of amorphous silica micropowder and blank sample rack without sample, deducting scattering of blank sample, separating crystalline state from amorphous state by using amorphous silica micropowder scattering curve as standard, calculating integral area of amorphous silica, and integral surface of alpha-state crystalline silica micropowderAfter the product, the correction factor K of a sample is obtained α A value;
e) Subjecting the sample to be tested to determination K α Collecting a scattering intensity curve of a sample to be detected under the same light path condition and step scanning range, deducting scattering of a blank frame, separating crystalline state and amorphous state scattering in the scattering curve by using peak separation software to obtain an integral area of amorphous silicon dioxide and an integral area of alpha state crystalline silicon dioxide micropowder, and calculating the content of the state crystalline silicon dioxide.
2. The method for detecting the content of alpha-form crystalline silica in silica by using a powder polycrystal X-ray diffractometer according to claim 1, wherein: reference value for parameter setting of polycrystalline X-ray diffractometer: the copper target, the light tube voltage 40kV, the light tube current 40mA, the incident slit 0.6mm, the receiving slit 8mm, the set step length 0.01 degrees, the scanning time 0.05s and the diffraction angle range 10-35 degrees.
3. The method for detecting the content of alpha-form crystalline silica in silica by using a powder polycrystal X-ray diffractometer according to claim 1, wherein: crushing and grinding a sample by using a ball mill, firstly, using a 600-mesh standard sieve to sieve and obtain powder, and then, using a 10-mu m filter cloth sieve to sieve and obtain liquid with the particle size smaller than 10 mu m.
4. The method for detecting the content of alpha-form crystalline silica in silica by using a powder polycrystal X-ray diffractometer according to claim 1, wherein: 10g of powder with the particle size smaller than 10 mu m is taken and placed in a 600mL beaker, water is added for stirring, the filtrate is poured out after 2 hours of sedimentation, the filtrate is precipitated for about 16 hours, sediment of the filtrate is taken, the sediment is tested by using a laser particle size analyzer, and the optimal particle size range is 2 mu m-10 mu m.
5. The method for detecting the content of alpha-form crystalline silica in silica by using a powder polycrystal X-ray diffractometer according to claim 1, wherein: the prepared alpha-state crystalline silica micro powder and amorphous silica micro powder are taken to form six samples according to the mass ratio of 0.005.
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