SJ/T 10551-1994 Emission spectral analysis method for impurities in aluminum oxide for electronic ceramics SJ/T10551-1994 standard download decompression password: www.bzxz.net

Electronic Industry Standard of the People's Republic of China
SJ/T10551--94
Method of.emisson spectrochemical analysis of impurities inAlO3,TiOzand ZrO,for use in electron ceramicsPublished on August 8, 1994
Implementation on December 1, 1994
Published by the Ministry of Electronics Industry of the People's Republic of ChinaElectronic Industry Standard of the People's Republic of China
Method of emisson spectrochemical analysis of impuritiesinAl,O,foruseinelectronceramics1. Subject content and scope of application
1.1 Subject content
This standard specifies the method of emission spectrochemical analysis of impurities in aluminum oxide for electronic ceramics. 1.2 Scope of application
SJ/T10551—94
This standard applies to the determination of impurities such as silicon dioxide, iron oxide, magnesium oxide, and calcium oxide in aluminum oxide for electronic ceramics.
2 Summary of method
The aluminum oxide powder sample is calcined at 1000-1200℃ to convert it into α-type aluminum oxide. The sample is mixed with a carbon powder mixture (C:CuO=3:0.1) (sample: carbon powder mixture=1t3), and copper is used as the internal standard. The spectra of the tested sample and the standard sample are photographed on the same spectrum plate, and the impurity content is determined using the internal standard method. 3 Reagents or materialsbZxz.net
Aluminum oxide
Ferric oxide
Copper oxide
Magnesium oxide
Calcium oxide
Silicon dihydride
Spectral dry plate
Spectral pure:
Analytical pure;
Analytical pure;
Analytical pure;
Analytical pure;
Spectral pure;
Domestic Type I;
Metol-Hydelu developer and fixer (prepared according to the recipe in the instruction manual of the photosensitive plate); graphite electrode
Instruments or equipment
Medium-sized spectrograph;
Spectral pure, diameter 6+mm.
Approved by the Ministry of Electronics Industry of the People's Republic of China on August 8, 1994 and implemented on December 1, 1994
5 Test specimens
DC arc generator;
Microphotometer:
Spectrograph;
Analytical balance with a sensitivity of 10g;
High-temperature furnace above 1000℃;
High-alumina porcelain crucible or platinum;
SJ/T10551-94
Polytetrafluoroethylene mortar or plexiglass mortar; Stopwatch
Small lathe for turning graphite electrodes.
5.1 Preparation of standard samples
Put spectrally pure aluminum oxide powder in a high-alumina porcelain or platinum crucible, and sinter it in a high-temperature furnace at 1000-1200℃ for 2h. Put analytically pure iron oxide, silicon dioxide, magnesium oxide, and calcium oxide in the crucible respectively, and bake them in a high-temperature furnace at 300℃ for 2h. Take them out and cool them to room temperature. Use them within 30min. Prepare the main standard sample according to the determination content range, and gradually dilute it with the matrix spectrally pure aluminum oxide to prepare a set of standard samples containing 5 points. The content is shown in Table 1. Table 1
Analysis components
Standard sample No. 1
Standard sample No. 1
Standard sample No. 3
Standard sample No. 4
Standard sample No. 5
5.2 Sample treatment
Impurity content
Put the sample to be tested in a high-alumina porcelain or platinum crucible, move and burn it in a high-temperature furnace at 1000-1200℃ for 2h, take it out and cool it to room temperature, and use it within 30min.
6 Analysis steps
6.1 Mix the standard sample and the sample with the carbon powder mixture in a ratio of 1:3 respectively, put the mixture in a polytetrafluoroethylene or organic glass mortar and grind it evenly (grind the standard sample for more than 1h, and the sample for 30min), and use the filling method to install the lower electrode until it is filled, flattened and polished.
6.2 Use a three-lens illumination system to take a spectrum, DC arc anode excitation, voltage 220V, current intensity 8A, slit width 10um, shading plate 3.2mm, exposure 35s, and take a spectrum for each sample three times. Develop the type 1 photosensitive plate in Metol-Hydelu developer for 2-4min at a temperature of 18-20℃, then fix, wash and dry. 2
The stone circle electrode is shown in the figure below:
Calculation of analysis results
Upper electrode
SJ/T10551-94
Wall thickness 0.7
Lower electrode
On the microphotometer, measure the blackness of the analysis line pair, draw the AS-IgC working curve, and find out the content of impurities in the sample from the working curve.
△S(W) is the difference between the blackness of the analytical line and the blackness of the internal standard line, and IgC is the logarithm of the content of the analytical element in the standard sample. The analytical line pairs and the determination content range are shown in Table 2. Table 2
Analysis line pair wavelength
Measurement composition
8 Precision or allowable error
8.1 Precision
Analysis elements
Fe248.814
Si251.921
Ca317.983
Mg277.983
Comparison elements
Cu249.215
Cu249.215
Cu319.410
Cu249.215
Based on the calculation results of the measurement data of 11 photographic plates, the relative standard deviation is within 15%. 8.2 Accuracy
When the particle size and organizational structure of the standard sample are similar to those of the test sample, the accuracy is close to the precision measurement range
0.0100.016
0.020~0.32
0.030~0.18
0.010~0.16
Additional instructions
SJ/T10551-94
This standard is under the jurisdiction of the Standardization Research Institute of the Ministry of Electronics Industry. This standard is drafted by the Standardization Research Institute of the Ministry of Electronics Industry. The main drafters of this standard are: Wang Yugong, Liu Chengjun, Luo Shaotang, Wang Xiuwen, Li Guoxi4
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