Diffraction-fluorescence detection method for metal aluminum powder

Abstract

The invention discloses a diffraction-fluorescence detection method for metal aluminum powder, which comprises the following steps: firstly, judging whether the metal aluminum powder is doped by using a diffraction analyzer, and then, carrying out quantitative analysis by using a fluorescence tabletting method, and comprises the steps of preparing a sample, preparing a tabletting sample, carrying out primary screening measurement and carrying out rechecking measurement. The method has the advantages that the time is short, the whole detection process is completed for about 33 minutes, the operation is convenient and simple, batch analysis and detection can be carried out by one person, the whole-process operation is realized, the analysis and detection accuracy is high, whether the metal aluminum powder is adulterated or not can be quickly judged, the reproducibility of the analysis result is good, and the analysis result for detecting the aluminum content in the metal aluminum powder is accurate and stable; waste acid and waste liquid are not generated in the detection process, pollution to the environment is avoided, and the cost for treating the waste acid and waste liquid is greatly reduced.

Description

Technical Field

[0001] The invention relates to the technical field of metal analysis and detection, and in particular to a diffraction-fluorescence detection method for metal aluminum powder. Background Art

[0002] In the prior art, the metal aluminum content in the metal aluminum powder is usually analyzed by wet method. The wet method needs to be soaked in hydrochloric acid, heated in a water bath for four hours and filtered, and then the aluminum oxide content is determined by the fluoride salt replacement EDTA volumetric method. The metal aluminum content is calculated according to the aluminum oxide content, which takes a long time, about 6 to 7 hours to analyze a sample, the operation process is cumbersome, the calculation is complicated, the color change of the endpoint during the titration process is different for each person, and the titration consumption volume is too large, and the burette needs to be filled twice. After the two readings, the titration consumption volume is added, and the error becomes larger, causing deviation. On the other hand, the use of wet method to detect the aluminum content in the metal aluminum powder requires a large amount of acid and other related chemical reagents. The waste acid and waste liquid generated after the sample detection and analysis will cause pollution to the water and soil environment, and the collection and dilution and neutralization treatment will increase a certain cost. Therefore, it is necessary to develop a detection method that can reduce the detection cost and effectively improve the efficiency of metal aluminum powder analysis. Summary of the invention

[0003] The purpose of the present invention is to provide a diffraction-fluorescence detection method for metal aluminum powder in view of the deficiencies in the prior art.

[0004] To achieve the above object, the present invention is implemented by the following technical solution, including the following steps: S1. Sample preparation: first grind the metal aluminum to be tested to obtain metal aluminum powder, then divide the metal aluminum powder into four parts according to the quartering method and take samples; S2, preparation of tablet sample, take 1g of the aluminum powder sample obtained by grinding and sampling in step S1, put it on the groove of the glass sheet, and directly flatten it with a thin blade as a diffraction sample to be tested; then use a horn spoon to take a spoonful of the metal aluminum powder obtained by grinding in step S1 and put it into the tablet press mold, add boric acid around the tablet press mold, control the boric acid thickness to 4-4.5mm, use the tablet press to press to obtain the sample, and the sample thickness is 5mm; S3, preliminary screening measurement, using a diffraction analyzer to measure the diffraction sample prepared in step S2, scanning and performing phase retrieval analysis on the interplanar spacing, judging whether it is pure metal aluminum powder according to the scanning result, and if it is not pure metal aluminum powder, the detection and analysis is ended; if it is judged to be pure metal aluminum powder, proceed to the next step, using a fluorescence analyzer to perform quantitative analysis on the sample prepared in step S2, and detecting the Al content in the sample; S4. Review the measurement, select the QuantExpress curve on the fluorescence analyzer, adjust it to the oxide detection mode to analyze the sample, then evaluate the analysis results in the evaluation interface, select the non-existent oxides and set them as non-existent, change the molecular formula, that is, change Al2O3 to Al, and finally normalize and calculate the Al content, that is, the Al content in the metal aluminum powder sample.

[0005] The beneficial effects of the present invention are as follows: 1) It takes less time, and the entire detection process is completed in about 33 minutes. The operation is convenient and simple. A single person can perform batch analysis and detection, and realize the operation of the entire process. The analysis and detection accuracy is high, and it can quickly determine whether the metal aluminum powder is adulterated. The analysis results have good reproducibility and reproducibility, and the analysis results of the aluminum content in the metal aluminum powder are accurate and stable; 2) Improve and increase environmental benefits. Compared with the use of wet analysis to detect the aluminum content in metal aluminum powder, a large amount of acid and other related chemical reagents are required. Waste acid and waste liquid generated after sample detection and analysis will pollute the water and soil environment. The collection and dilution and neutralization treatment will increase certain costs. The diffraction-fluorescence detection method of the present application does not generate waste acid and waste liquid during the detection process, will not pollute the environment, and greatly reduce the cost of treating waste acid and waste liquid. DETAILED DESCRIPTION

[0006] The present invention will be further described below in conjunction with the embodiments, but is not limited to the contents of the description.

[0007] Example 1

[0008] A diffraction-fluorescence detection method for metallic aluminum powder comprises the following steps: S1. Sample preparation: first grind the metal aluminum to be tested that does not contain Al2O3 and β-Al2O3 to obtain the metal aluminum powder, and then divide the metal aluminum powder into four parts and take samples. The four-part division method can ensure the uniformity of the sample and make the analysis and detection sample more representative; S2, preparation of tablet sample, take 1g of the aluminum powder sample obtained by grinding and sampling in step S1, put it on the groove of the glass sheet, and directly flatten it with a thin blade as a diffraction sample to be tested; then use a horn spoon to take a spoonful of the metal aluminum powder obtained by grinding in step S1 and put it into the tablet press mold, add boric acid around the tablet press mold, and control the thickness of boric acid to 4-4.5mm, and use a tablet press to press to obtain a sample, and the total thickness of the sample is 5mm (metal aluminum powder cannot be melted in a platinum crucible for the glass sheet method, which will seriously damage the platinum crucible); boric acid is only used as a coagulant to promote the particles in the sample to stick together, so that the pressed sample is easy to form and not easy to loosen, ensuring that the sample will not scatter during the analysis process, thereby improving the accuracy and reliability of the analysis; S3, preliminary screening measurement, using an XRD diffraction analyzer to measure the diffraction sample prepared in step S2 (measurement conditions are detailed in Table 1), scanning and performing phase retrieval analysis on the interplanar spacing, judging whether it is pure metal aluminum powder according to the scanning result, if the Al content is less than 95%, it is judged that it is not pure metal aluminum powder, and the detection and analysis is ended; if the Al content is not less than 95%, it is judged that it is pure metal aluminum powder, and the next step is to use a fluorescence analyzer to perform quantitative analysis on the sample prepared in step S2 to detect the Al content in the sample; S4. Review the measurement, select the QuantExpress curve on the fluorescence analyzer, adjust it to the oxide detection mode to analyze the sample (see Table 2 for analysis conditions), then evaluate the analysis results on the evaluation interface, select the non-existent oxides and set them as non-existent, change the molecular formula, i.e. change Al2O3 to Al, and finally normalize and calculate the Al content to obtain the Al content of the metal aluminum powder sample. It should be noted that the diffraction-fluorescence detection method described in the present invention cannot directly use the fluorescence tablet method to quantitatively analyze the content of metallic aluminum in metallic aluminum powder. First, a diffraction analyzer is used to determine whether the metallic aluminum powder is doped, and then the fluorescence tablet method can be used for quantitative analysis. If the fluorescent tablet method is directly used for quantitative analysis, the metallic aluminum obtained may not be all the metallic aluminum content in the sample. Not only is the analysis inaccurate, but it can also lead to misjudgment of the Al content in the sample, and a sample with a low Al content is judged as having a high Al content.

[0009] Verification Example In this verification, samples were prepared using metal aluminum powder with an Al content of 99.86% and CL370 activated alumina powder with an Al content of 99.42%, and quantitative test analysis was performed using the diffraction-fluorescence detection operation mode of steps S1 to S4 in the above embodiment 1. The specific analysis results are shown in Table 3. From the analysis results in Table 3, it can be seen that the content of metallic aluminum in the samples is directly detected by the tablet pressing method, and the contents of metallic aluminum detected by SY1#, SY2#, SY3#, and SY4# are basically the same, about 99.60%; if the diffraction analysis is not performed but the fluorescent tablet pressing method is directly used for quantitative analysis, the SY1#, SY2#, SY3#, and SY4# samples will be judged as high-content metallic aluminum powders for use, but in fact, the theoretical content of metallic aluminum in SY1# we prepared is 33%, the theoretical content of metallic aluminum in SY2# is 50%, the theoretical content of metallic aluminum in SY3# is 67%, and the theoretical content of metallic aluminum in SY4# is 83%, which are basically consistent with the contents after phase analysis using an XRD diffraction analyzer.

[0010] In summary, before using the diffraction-fluorescence detection method to quantitatively analyze the metal aluminum content, the XRD diffraction analyzer in step S3 must be used to perform phase analysis to determine whether the metal aluminum powder is doped. If it is not doped, the tablet pressing method in step S4 is used to quantitatively analyze the metal aluminum content by fluorescence. If it is doped, no further analysis is required.

[0011] The experimental example uses the existing wet analysis detection method and the diffraction-fluorescence detection method of Example 1 of the present application to detect and analyze the metal aluminum powder.

[0012] Samples: metallic aluminum powder with an Al content of 99.86% and CL370 activated alumina powder with an Al content of 99.42%.

[0013] Metal aluminum powder with an Al content of 99.86% and CL370 activated alumina powder with an Al content of 99.42% were prepared as samples respectively, and the diffraction-fluorescence detection operation mode of steps S1 to S4 in the above embodiment 1 was used for testing. XRD diffraction analysis was used to directly determine whether high-purity Al2O3 was doped. If Al2O3 phase or β-Al2O3 phase was found in the phase analysis after detection, it was determined to be adulterated, and the subsequent metal aluminum analysis was not performed directly, thus eliminating unnecessary analysis operation steps. If there was only metal aluminum phase, the fluorescence analyzer was used to perform quantitative analysis of metal aluminum.

[0014] Finally, the results of the existing wet analysis test were compared with the results of the fluorescence tablet analysis test, (wet analysis results) - (diffraction-fluorescence detection method results) = E ± 0.4. The specific structure is shown in Table 4. From the analysis results in Table 4, it can be seen that the quantitative analysis of the metal aluminum content by wet analysis and diffraction-fluorescence detection method are both within the allowable error range, and the errors are all within 0.2. The analysis time of diffraction scanning detection is 13 minutes, and the metal aluminum powder is quantitatively analyzed by fluorescence tableting method, which takes 20 minutes. The entire analysis and detection process takes 33 minutes, which is significantly shorter than the 6-7 hours of wet analysis. This shows that the diffraction-fluorescence detection method of the present invention is feasible and effective for the metal aluminum powder detection and analysis method, and the error of the detection result is small. It can replace the existing detection and analysis technology and significantly improve the detection and analysis efficiency. In summary, the diffraction-fluorescence detection method has the following advantages over the existing wet analysis technology: 1. Improve the analysis efficiency and accuracy. After using XRD diffraction analysis, it can directly determine whether it is metal aluminum powder. If it is not metal aluminum powder, no further analysis is required. This greatly improves the analysis and detection efficiency. The operation process is simple, error is not likely to occur, and the final result has a small deviation. 2. First determine whether the metal aluminum powder is doped, and then use the fluorescent tablet method for analysis and detection. It takes about 33 minutes to complete a test analysis. Compared with the time spent on wet analysis of a batch of samples, the diffraction-fluorescence detection method can detect and analyze about 12 samples in the same time, which improves the analysis efficiency by 12 times. Compared with wet analysis, it has higher accuracy, repeatability and reproducibility, and significantly shortens the detection and analysis time.

Claims

1. A diffraction-fluorescence detection method for metallic aluminum powder, characterized in that: The following steps are involved: S1. Sample preparation: first grind the metal aluminum to be tested to obtain metal aluminum powder, then divide the metal aluminum powder into four parts according to the quartering method and take samples; S2, preparation of tablet sample, take 1g of the aluminum powder sample obtained by grinding and sampling in step S1, put it on the groove of the glass sheet, and directly flatten it with a thin blade as a diffraction sample to be tested; then use a horn spoon to take a spoonful of the metal aluminum powder obtained by grinding in step S1 and put it into the tablet press mold, add boric acid around the tablet press mold, control the boric acid thickness to 4-4.5mm, use the tablet press to press to obtain the sample, and the sample thickness is 5mm; S3, preliminary screening measurement, using a diffraction analyzer to measure the diffraction sample prepared in step S2, scanning and performing phase retrieval analysis on the interplanar spacing, judging whether it is pure metal aluminum powder according to the scanning result, and if it is not pure metal aluminum powder, the detection and analysis is ended; if it is judged to be pure metal aluminum powder, proceed to the next step, using a fluorescence analyzer to perform quantitative analysis on the sample prepared in step S2, and detecting the Al content in the sample; S4. Review the measurement, select the QuantExpress curve on the fluorescence analyzer, adjust it to the oxide detection mode to analyze the sample, then evaluate the analysis results in the evaluation interface, select the non-existent oxides and set them as non-existent, change the molecular formula, that is, change Al2O3 to Al, and finally normalize and calculate the Al content, that is, the Al content in the metal aluminum powder sample.

2. The diffraction-fluorescence detection method of metal aluminum powder according to claim 1, characterized in that: The pure metal aluminum powder in step S3 is metal aluminum powder having an Al content of not less than 95% measured by a diffraction analyzer.

3. The diffraction-fluorescence detection method of metal aluminum powder according to claim 1, characterized in that: The metal aluminum or metal aluminum powder refers to metal aluminum powder that does not contain Al2O3 and β-Al2O3.

4. The diffraction-fluorescence detection method of metal aluminum powder according to claim 1, characterized in that: The diffraction analyzer is an XRD diffraction analyzer.

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