CN109324074A - The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content - Google Patents

The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content Download PDF

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Publication number
CN109324074A
CN109324074A CN201811279041.3A CN201811279041A CN109324074A CN 109324074 A CN109324074 A CN 109324074A CN 201811279041 A CN201811279041 A CN 201811279041A CN 109324074 A CN109324074 A CN 109324074A
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China
Prior art keywords
sample
component content
magnet ferrite
measurement
strontium permanent
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CN201811279041.3A
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邓兴民
王玉明
郑亮
刘超
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Hunan Aerospace Magnet and Magneto Co Ltd
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Hunan Aerospace Magnet and Magneto Co Ltd
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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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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content, comprising the following steps: (1) prepare standard sample of photo；(2) test condition, determination condition are set；(3) Spectrum Sample Curve is established；(4) sample constituents measure.The present invention is measured and is detected to ingredient in strontium permanent-magnet ferrite using x-ray fluorescence powder pressing method, it is horizontal that measurement accuracy can reach inductively coupled plasma atomic emission spectrometry measurement, the Spectrum Sample Curve established can be used for a long time, measurement sample detection cycle shortens within 10min, this method can go out Multiple components content in strontium permanent-magnet ferrite by rapid and accurate determination simultaneously, and it is easy to operate, accuracy is high, detection cycle is short, testing cost is low, environmental pollution is small.

Description

The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content
Technical field
The present invention relates to a kind of methods of component content in measurement strontium permanent-magnet ferrite, and in particular to a kind of x-ray fluorescence The method that spectrum powder pressing method measures component content in strontium permanent-magnet ferrite.
Background technique
Strontium permanent-magnet ferrite is with strontium carbonate (SrCO3) and di-iron trioxide (Fe2O3) it is main material, pass through ceramic process It is manufactured a kind of with wide hysteresis loop, high remanent magnetism, high-coercive force, magnetic basic function type can be kept constant once magnetization Material.The common additive of other in strontium permanent-magnet ferrite mainly has calcium carbonate (CaCO3), silica (SiO2), aluminium oxide (Al2O3), chromium oxide (Cr2O3), lanthana (La2O3), cobalt oxide (Co2O3) etc., major and minor component is to influence its performance height Key factor, rapidly and accurately carrying out composition measurement to material has positive effect for Instructing manufacture, promotion scientific research.
Currently, the common method of measurement strontium permanent-magnet ferrite ingredient is inductively coupled plasma atomic emission spectrometry, The method, which need to be chemically treated, dissolves sample sufficiently, and each element that measurement is directed to before measuring will prepare a series of gradients Standard solution, test sample element need to measure one by one, 8~10h of overall process time-consuming.In addition, utilizing inductively coupled plasma body Atomic emission spectrometry carry out strontium permanent-magnet ferrite material ingredient in the full measure workload of primary and secondary multielement it is big, it is time-consuming, heavy, Accuracy is lower.
Summary of the invention
The technical problem to be solved by the present invention is to, overcome above-mentioned prior art defect, provide a kind of sample preparation it is simple, Finding speed is fast, nondestructively measuring, multielement simultaneous determination, and measures precision, the higher X-ray fluorescence spectra of accuracy The method that method measures component content in strontium permanent-magnet ferrite.
The technical solution adopted by the present invention to solve the technical problems is as follows: x-ray fluorescence spectrometry strontium permanent magnet The method of component content in oxysome, comprising the following steps:
(1) it prepares standard sample of photo: using pressure-like after being handled with the strontium permanent magnetic ferrite powder drying sieving of each component content known Machine is pressed into the standard sample of photo that one group of each component content has gradient；
(2) test condition, determination condition are set: basic test condition, the determination condition of each ingredient corresponding element are set, it is described Basic test condition includes: measurement spectral line, analyzing crystal, electric current, voltage, time of measuring, peak position angle, the determination condition packet Include light pipe voltage, tube current, filter disc, attenuator；
(3) standard curve is established: using measurement step under the conditions of Xray fluorescence spectrometer basic test set by step (2) Suddenly the X-fluorescence intensity of each ingredient of (1) made standard sample of photo utilizes resulting each ingredient X-fluorescence intensity and known component content value Corresponding, after calibrated and deduction interference, linear Spectrum Sample Curve is established in linear regression, and is stored in Xray fluorescence spectrometer；
(4) sample constituents measure: will be pressed into sample print with pressure-like machine after sample to be tested powder drying sieving processing, use X-ray spectrometer measures each ingredient X-fluorescence intensity of sample, according to the Spectrum Sample Curve that step (3) are established, is gone out by instrument automatic measurement & calculation The content of each ingredient in sample to be tested.
Further, the chemical component of strontium permanent-magnet ferrite content to be detected includes Fe2O3、SrO、BaO、CaO、SiO2、 Al2O3、Cr2O3、La2O3And Co2O3。
Further, in step (1) and (4), it is all 105 DEG C~110 DEG C dry 2h, after 100 that drying sieving condition is identical ~300 meshes.
Further, in step (1) and (4), tablet press machine pressing conditions is identical, and pressure is all 20~50t, and the dwell time is all 30~60s.
Further, in step (1) and (4), it is 3~20 that one group of each component content, which has the standard sample of photo number of gradient,.
Further, in step (1) and (4), sample surface purging is clean, uniform ground, crack-free.
The method of the present invention the utility model has the advantages that measurement accuracy can reach inductively coupled plasma atomic emission spectrometry survey Fixed level, the Spectrum Sample Curve established can be used for a long time, and measurement sample detection cycle shortens to 10min, and this method can be simultaneously Rapid and accurate determination go out in strontium permanent-magnet ferrite Multiple components content and it is easy to operate, accuracy is high, detection cycle is short, detection at This is low, and environmental pollution is small.
Detailed description of the invention
Fig. 1 is Fe-K α calibration curve；
Fig. 2 is Sr-K α calibration curve；
Fig. 3 is Ba- L α calibration curve；
Fig. 4 is Ca-K α calibration curve；
Fig. 5 is Si-K α calibration curve；
Fig. 6 is Al-K α calibration curve；
Fig. 7 is Cr-K α calibration curve；
Fig. 8 is 1 calibration curve of La-L β；
Fig. 9 is Co-K α calibration curve.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Xray fluorescence spectrometer used in the embodiment of the present invention is instrument model Simultix14；Manufacturer is day This Neo-Confucianism Co., Ltd..
Embodiment
The present embodiment the following steps are included:
(1) it prepares standard sample of photo: using pressure-like after being handled with the strontium permanent magnetic ferrite powder drying sieving of each component content known Machine is pressed into the standard sample of photo that one group of each component content has gradient；Use the strontium known to 12 each component contents (referring to table 1) Permanent magnetic ferrite powder crosses 200 meshes after 105 DEG C of drying 2h, then is pressed into one group in pressure-like machine pressure 30t dwell time 30s Each component content has the standard sample of photo of gradient；
Each component content of 1 standard sample of table
(2) test condition, determination condition are set: basic test condition, the determination condition of each ingredient corresponding element are set, it is described Basic test condition includes: measurement spectral line, analyzing crystal, electric current, voltage, time of measuring, peak position angle, the determination condition packet Include light pipe voltage, tube current, filter disc, attenuator；Test condition and determination condition are referring to table 2；
1 adjusting instrument location parameter of table
(3) standard curve is established: using measurement step under the conditions of Xray fluorescence spectrometer basic test set by step (2) Suddenly the X-fluorescence intensity of each ingredient of (1) made standard sample of photo utilizes resulting each ingredient X-fluorescence intensity and known component content value Corresponding, after calibrated and deduction interference, the Spectrum Sample Curve that linear Spectrum Sample Curve is established is established in each element linear regression, is stored in In Xray fluorescence spectrometer, wherein Fe-K α calibration curve as shown in Figure 1, Sr-K α calibration curve as shown in Fig. 2, Ba-L α calibrate Curve as shown in figure 3, Ca-K α calibration curve as shown in figure 4, Si-K α calibration curve as shown in figure 5, Al-K α calibration curve as scheme Shown in 6, Cr-K α calibration curve as shown in fig. 7,1 calibration curve of La-L β as shown in figure 8, Co-K α calibration curve is as shown in Figure 9；
(4) sample constituents measure: will be pressed into sample print with pressure-like machine after sample to be tested powder drying sieving processing, use X-ray spectrometer measures each ingredient X-fluorescence intensity of sample, according to the Spectrum Sample Curve that step (3) are established, by the automatic band of instrument software Enter the component content for calculating each ingredient in sample to be tested.
The present embodiment is continuously measured 10 times using X-ray fluorescence spectra powder pressing method, the results are shown in Table 3.
3 X-ray fluorescence spectra powder pressing method measurement result of table
It can be seen from Table 3 that 10 measurement results are almost the same, illustrate that detection method stability is fine, accuracy is high.
Comparative example
Same strontium permanent-magnet ferrite sample is continuously measured 10 times using inductively coupled plasma atomic emission spectrometry, is as a result seen Table 4.
4 inductively coupled plasma atomic emission spectrometry measurement result of table
Table 3 and 4 measurement result of table are compared, it can be seen that in embodiment in X-ray fluorescence spectra powder pressing method and comparative example The result of inductively coupled plasma atomic emission spectrometry measurement is almost the same, but the result of embodiment 1 is more acurrate, and uses X-ray fluorescence spectra powder pressing method is easier quickly for the progress composition measurement of strontium permanent-magnet ferrite, and accuracy is high, is suitble to Applied to strontium permanent-magnet ferrite composition measurement.

Claims (6)

  1. The method of 1.X ray fluorescence measurement strontium permanent-magnet ferrite component content, which comprises the following steps:
    (1) it prepares standard sample of photo: using pressure-like after being handled with the strontium permanent magnetic ferrite powder drying sieving of each component content known Machine is pressed into the standard sample of photo that one group of each component content has gradient；
    (2) test condition, determination condition are set: basic test condition, the determination condition of each ingredient corresponding element are set, it is described Basic test condition includes: measurement spectral line, analyzing crystal, electric current, voltage, time of measuring, peak position angle, the determination condition packet Include light pipe voltage, tube current, filter disc, attenuator；
    (3) Spectrum Sample Curve is established: using measurement step under the conditions of Xray fluorescence spectrometer basic test set by step (2) Suddenly the X-fluorescence intensity of each ingredient of (1) made standard sample of photo utilizes resulting each ingredient X-fluorescence intensity and known component content value Corresponding, after calibrated and deduction interference, linear Spectrum Sample Curve is established in linear regression, is stored in Xray fluorescence spectrometer；
    (4) sample constituents measure: will be pressed into sample print with pressure-like machine after sample to be tested powder drying sieving processing, use X-ray spectrometer measures each ingredient X-fluorescence intensity of sample, according to the Spectrum Sample Curve that step (3) are established, is gone out by instrument automatic measurement & calculation The content of each ingredient in sample to be tested.
  2. 2. the method for the x-ray fluorescence method measurement strontium permanent-magnet ferrite component content according to claim 1, which is characterized in that The chemical component of the strontium permanent-magnet ferrite content to be detected includes Fe2O3、SrO、BaO、CaO、SiO2、Al2O3、Cr2O3、La2O3 And Co2O3。
  3. 3. the method for x-ray fluorescence method measurement strontium permanent-magnet ferrite component content according to claim 1 or claim 2, feature exist In step (1) is identical with the condition that (4) dry sieving processing, is all to cross 100~300 mesh after 105 DEG C~110 DEG C dry 2h Sieve.
  4. 4. the method that x-ray fluorescence method described according to claim 1~one of 3 measures strontium permanent-magnet ferrite component content, special Sign is that step (1) is identical with tablet press machine pressing conditions described in step (4), pressure be 20~50t, the dwell time be 30~ 60s。
  5. 5. the method that x-ray fluorescence method described according to claim 1~one of 4 measures strontium permanent-magnet ferrite component content, special Sign is that it is 3~20 that one group of each component content described in step (1) and step (4), which has the standard sample of photo number of gradient,.
  6. 6. the method that x-ray fluorescence method described according to claim 1~one of 5 measures strontium permanent-magnet ferrite component content, special Sign is that step (1) and (4) described sample surface purging are clean, uniform ground, crack-free.
CN201811279041.3A 2018-10-30 2018-10-30 The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content Pending CN109324074A (en)

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CN110715947A (en) * 2019-12-12 2020-01-21 湖南航天磁电有限责任公司 Method for measuring barium calcium in industrial strontium carbonate by adopting gel X-ray fluorescence spectrometry

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Application publication date: 20190212