A method for preparing a cobalt-iron-boron alloy and a method for analyzing and testing the same

Abstract

The application provides a sample preparation method and an analysis test method of a cobalt-iron-boron alloy. The sample preparation method comprises the following steps: performing acid pickling on the cobalt-iron-boron alloy for at least two times, and then performing cleaning and drying to obtain a sample to be tested; wherein the concentration of the acid pickling agent gradually decreases with the increase of the number of acid pickling. Through the step of acid pickling for at least two times, the pollutants on the surface of the cobalt-iron-boron alloy can be effectively removed, and the introduction of impurities is avoided as much as possible in the sample preparation process, so that a clean sample to be tested suitable for the detection of a glow discharge mass spectrometer is successfully prepared, and the test time of the glow discharge mass spectrometer can be shortened, and the test result has high accuracy.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of analytical testing technology, and relates to a cobalt-iron-boron alloy sample preparation method and an analytical testing method. BACKGROUND

[0002] The cobalt-iron-boron alloy is mainly an alloy with cobalt (Co), iron (Fe) and boron (B) as basic components. Among them, cobalt and iron are transition metal elements, and their atomic structure characteristics make the alloy have good magnetic and mechanical properties, and the addition of boron element can significantly improve the magnetic properties of the alloy. Generally speaking, the purity and impurity elements of the cobalt-iron-boron alloy have an important influence on its performance, so by testing the purity and impurity elements of the cobalt-iron-boron alloy, the performance of the alloy can be determined to a certain extent.

[0003] The glow discharge mass spectrometer (GDMS) belongs to the direct solid analysis technology, has the advantages of high sensitivity, high resolution, small matrix effect and full element analysis, and is the best means for analyzing high-purity metal solid samples. Generally, there are constant element contaminants on the surface of the cobalt-iron-boron alloy, such as Al, Si, P, S or Cl elements, etc., which cannot be directly tested by the glow discharge mass spectrometer, otherwise the test result will be low in accuracy and long in test time.

[0004] Therefore, it is urgent to provide a cobalt-iron-boron alloy sample preparation method, and the prepared sample is suitable for glow discharge mass spectrometer detection, can shorten the test time, and improve the accuracy of the test result. SUMMARY

[0005] In view of the deficiencies in the prior art, the purpose of the present application is to provide a cobalt-iron-boron alloy sample preparation method and an analytical testing method. The sample preparation method of the present application can effectively remove the pollutants on the surface of the cobalt-iron-boron alloy through at least two acid pickling steps, and the introduction of impurities is avoided as much as possible during the sample preparation process, so that a clean sample to be tested suitable for glow discharge mass spectrometer detection is successfully prepared, and the test time of the glow discharge mass spectrometer is shortened, and the test result is ensured to have high accuracy.

[0006] To achieve this purpose, the present application adopts the following technical solutions:

[0007] In a first aspect, the present application provides a cobalt-iron-boron alloy sample preparation method, which comprises:

[0008] The cobalt-iron-boron alloy is subjected to at least two acid pickling, and then is subjected to cleaning and drying to obtain a sample to be tested; wherein with the increase of the number of acid pickling, the concentration of the acid pickling agent is gradually reduced.

[0009] The at least two times may be 2 times, 3 times, 5 times or 6 times, etc., but is not limited to the listed values, and other values not listed in this range are also applicable.

[0010] The sample preparation method of the present application can effectively remove the contaminants on the surface of the cobalt-iron-boron alloy through the step of at least twice acid pickling, and the introduction of impurities is avoided as much as possible in the sample preparation process, so that a clean sample to be tested suitable for the detection of the glow discharge mass spectrometer is successfully prepared, and the test time of the glow discharge mass spectrometer can be shortened, and the test result has high accuracy.

[0011] In the sample preparation method of the present application, the concentration of the acid pickling agent gradually decreases with the increase of the number of acid pickling, which can avoid excessive corrosion of the cobalt-iron-boron alloy and save resources.

[0012] Preferably, the cobalt-iron-boron alloy is in a block shape, and the size is 20-35mm*20-35mm*10-20mm, for example, it can be 20mm*20mm*10mm, 30mm*30mm*15mm or 35mm*35mm*20mm, etc., but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0013] Preferably, the solid-liquid ratio of the cobalt-iron-boron alloy and the acid pickling agent is 1g:(3-5)mL, for example, it can be 1g:3mL, 1g:4mL or 1g:5mL, etc., but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0014] Preferably, the acid pickling agent used in each acid pickling is a composite acid, and the composite acid comprises nitric acid and hydrofluoric acid.

[0015] Preferably, the mass concentration of nitric acid in the composite acid is 10-20%, for example, it can be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%, etc.; the mass concentration of hydrofluoric acid in the composite acid is 10-20%, for example, it can be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%, etc., but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0016] In the present application, the combination of nitric acid and hydrofluoric acid can effectively remove the contaminants on the surface of the cobalt-iron-boron alloy. When the mass concentrations of nitric acid and hydrofluoric acid meet the above preferred range during each acid pickling, the effect of removing the contaminants is better.

[0017] Preferably, the mass concentration ratio of nitric acid to hydrofluoric acid in the composite acid is (1-3):(1-3), wherein the selection range (1-3) of nitric acid can be 1, 2 or 3, etc.; the selection range (1-3) of hydrofluoric acid can be 1, 2 or 3, etc., but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0018] Preferably, the mass concentration of nitric acid and hydrofluoric acid in the composite acid gradually decreases with the increase of the number of acid washing.

[0019] Preferably, the time of each acid washing ranges from 2 to 5 minutes, for example, can be 2 minutes, 3 minutes, 4 minutes or 5 minutes, etc., but not limited to the listed values, other values not listed in this range are also applicable.

[0020] Preferably, the ultrasonic power ranges from 120 to 180 W, for example, can be 120 W, 130 W, 140 W, 150 W, 160 W, 170 W or 180 W, etc., but not limited to the listed values, other values not listed in this range are also applicable.

[0021] Preferably, the water washing step is performed between adjacent two acid washings.

[0022] Preferably, the cleaning includes the steps of water washing and alcohol washing in sequence.

[0023] Preferably, the alcohol used in the alcohol washing includes ethanol.

[0024] Preferably, the water used in each water washing is deionized water or pure water.

[0025] Preferably, the alcohol washed material is dried by a baking lamp.

[0026] Preferably, the sample preparation method is performed in a fume hood.

[0027] In the present application, the sample preparation process is performed in a fume hood, the purity of the reagents used is above the premium grade, and the water is deionized water or pure water, which can minimize the introduction of pollution.

[0028] In a second aspect, the present application provides an analysis and testing method of cobalt-iron-boron alloy, which comprises:

[0029] The sample to be tested prepared by the sample preparation method of the first aspect is placed in a glow discharge mass spectrometer, and then the steps of refrigeration and sputtering are performed in sequence to obtain the test result.

[0030] In the present application, the sample to be tested prepared by the sample preparation method of the first aspect has its surface pollutants removed as much as possible and the introduction of impurities is minimized, so that the test and analysis time of the glow discharge mass spectrometer can be shortened and the accuracy of the data can be ensured.

[0031] Preferably, the sample to be tested is first loaded into the instrument sample chamber of the glow discharge mass spectrometer, then vacuumized, and then pushed into the discharge chamber of the glow discharge mass spectrometer, and then the steps of refrigeration and sputtering are performed in sequence.

[0032] Preferably, the refrigeration time is 10 min.

[0033] Preferably, the sputtering voltage is 1-1.1 kV.

[0034] Preferably, the sputtering current is 2-2.2 mA, for example, it can be 2 mA, 2.1 mA or 2.2 mA, etc., but is not limited to the listed values, and other values not listed in the range are also applicable.

[0035] Preferably, the resolution of the glow discharge mass spectrometer is 4000-5000.

[0036] In the present application, using the above-mentioned sputtering voltage and current and resolution for testing can obtain a strong signal and high sensitivity.

[0037] The numerical range of the present application includes not only the above-mentioned point values, but also any point values between the above-mentioned numerical ranges that are not listed, and the present application does not exhaustively list the specific point values included in the range for the sake of brevity and simplicity.

[0038] Compared with the prior art, the present application has the following beneficial effects:

[0039] The sample preparation method of the present application can effectively remove the pollutants on the surface of cobalt-iron-boron alloy through at least two acid washing steps, and the introduction of impurities is avoided as much as possible during the sample preparation process, thereby successfully preparing a clean sample to be tested suitable for detection by a glow discharge mass spectrometer, and the test time of the glow discharge mass spectrometer can be shortened, and the test result has high accuracy.

[0040] In the sample preparation method of the present application, the concentration of the acid washing agent gradually decreases with the increase of the number of acid washing, which can avoid excessive corrosion of cobalt-iron-boron alloy and save resources. DETAILED DESCRIPTION

[0041] The technical solutions of the present application will be further described through specific embodiments.

[0042] Example 1

[0043] The present embodiment provides a sample preparation method for cobalt-iron-boron alloy, which comprises the following steps:

[0044] (1) In a fume hood, the cobalt-iron-boron alloy material is mechanically processed to obtain a block-shaped cobalt-iron-boron alloy sample with a size of 20 mm x 20 mm x 10 mm.

[0045] (2) The nitric acid stock solution, the hydrofluoric acid stock solution and the deionized water are mixed in a volume ratio of 1:1:4 to obtain a first composite acid, and the mass concentration of nitric acid and hydrofluoric acid in the first composite acid is 16.67%; the nitric acid stock solution, the hydrofluoric acid stock solution and the deionized water are mixed in a volume ratio of 1:1:6 to obtain a second composite acid, and the mass concentration of nitric acid and hydrofluoric acid in the second composite acid is 12.5%.

[0046] (3) The blocky cobalt-iron-boron alloy sample is placed in a polytetrafluoroethylene cup, then the first composite acid is added, and the solid-liquid ratio is 1g:3mL, then the cup is placed in an ultrasonic cleaning machine for primary pickling for 2min, and the ultrasonic power is 150W; after the primary pickling is completed, the sample is rinsed with deionized water; then the sample is placed in a polytetrafluoroethylene cup, and the second composite acid is added, and the solid-liquid ratio is 1g:3mL, then the cup is placed in an ultrasonic cleaning machine for secondary pickling for 2min, and the ultrasonic power is 150W; after the secondary pickling is completed, the sample is rinsed with deionized water, then rinsed with anhydrous ethanol, dried with a baking lamp, and a sample to be tested is obtained.

[0047] The embodiment also provides an analysis and testing method of cobalt-iron-boron alloy, which comprises the following steps:

[0048] The sample to be tested prepared by the above method is loaded into the instrument sample chamber of a Nu Astrum glow discharge mass spectrometer, and then vacuumized to 10 -2 Pa, and then pushed into the discharge chamber of the glow discharge mass spectrometer; the sample is fully cooled for 10min, and then the sputtering is started, wherein the voltage of the sputtering is 1-1.1kV, the current is 2.0mA, the instrument resolution is 4000-5000, and the sputtering is performed for about two hours, and then the test result is obtained.

[0049] Example 2

[0050] The embodiment provides a sample preparation method of cobalt-iron-boron alloy, which comprises the following steps:

[0051] (1) In a fume hood, the cobalt-iron-boron alloy material is mechanically processed to obtain a blocky cobalt-iron-boron alloy sample, and the size is 20mm×20mm×10mm.

[0052] (2) The nitric acid stock solution, the hydrofluoric acid stock solution and the deionized water are mixed in a volume ratio of 1:1:4 to obtain a first composite acid, and the mass concentration of nitric acid and hydrofluoric acid in the first composite acid is 16.67%; the nitric acid stock solution, the hydrofluoric acid stock solution and the deionized water are mixed in a volume ratio of 1:1:6 to obtain a second composite acid, and the mass concentration of nitric acid and hydrofluoric acid in the second composite acid is 12.5%; the nitric acid stock solution, the hydrofluoric acid stock solution and the deionized water are mixed in a volume ratio of 1:1:8 to obtain a third composite acid, and the mass concentration of nitric acid and hydrofluoric acid in the third composite acid is 10%.

[0053] (3) Put the blocky cobalt-iron-boron alloy sample into a polytetrafluoroethylene cup, then add the first composite acid, the solid-liquid ratio is 1g:3mL, then put the cup into the ultrasonic cleaner for the first acid pickling for 2min, the ultrasonic power is 150W; after the first acid pickling, rinse the sample with deionized water; then put the sample into a polytetrafluoroethylene cup, then add the second composite acid, the solid-liquid ratio is 1g:3mL, then put the cup into the ultrasonic cleaner for the second acid pickling for 3min, the ultrasonic power is 150W; after the second acid pickling, rinse the sample with deionized water; then put the sample into a polytetrafluoroethylene cup, then add the third composite acid, the solid-liquid ratio is 1g:3mL, then put the cup into the ultrasonic cleaner for the third acid pickling for 5min, the ultrasonic power is 150W; after the third acid pickling, rinse the sample with deionized water, then rinse the sample with anhydrous ethanol, dry with a baking lamp, and obtain the sample to be tested.

[0054] The embodiment also provides an analysis and testing method of cobalt-iron-boron alloy, including the following steps:

[0055] Put the sample to be tested prepared by the above method into the instrument sample chamber of the Nu Astrum glow discharge mass spectrometer, then vacuumize to 10 -2 Pa, then push into the discharge chamber of the glow discharge mass spectrometer; fully cool the sample for 10min, then start sputtering, wherein the voltage of sputtering is 1-1.1kV, the current is 2.0mA, the instrument resolution is 4000-5000, and the sputtering is performed for about two hours, and the test result is obtained.

[0056] As can be seen from Examples 1-2, by using the sample preparation method of the present application, the pollutants on the surface of the cobalt-iron-boron alloy can be effectively removed, and the introduction of impurities is avoided as much as possible, and a clean sample to be tested is obtained; by using the glow discharge mass spectrometer to analyze and test the sample to be tested, the test time is short, the test result is accurate, and the purity analysis and impurity element analysis of the cobalt-iron-boron alloy are successfully performed.

[0057] Example 3

[0058] The difference between the present embodiment and Example 1 is that the mass concentrations of nitric acid and hydrofluoric acid in the first composite acid are both adjusted to 12.5%; and the mass concentrations of nitric acid and hydrofluoric acid in the second composite acid are both adjusted to 9%.

[0059] The remaining steps and parameters remain the same as those of Example 1.

[0060] Example 4

[0061] The difference between the present embodiment and Example 1 is that the mass concentrations of nitric acid and hydrofluoric acid in the first composite acid are both adjusted to 21%; and the mass concentrations of nitric acid and hydrofluoric acid in the second composite acid are both adjusted to 16.67%.

[0062] The remaining steps and parameters are consistent with example 1.

[0063] From example 1 and examples 3-4, it can be seen that, in the sample preparation process, if the mass concentration of nitric acid and hydrofluoric acid is too low, the sample surface will not be cleaned, more impurity elements will be left, and the data results will need a longer time to stabilize; if the mass concentration of nitric acid and hydrofluoric acid is too high, the sample will be over-cleaned, and each main component element will need a longer testing time to stabilize.

[0064] Comparative example 1

[0065] The difference between this comparative example and example 1 is that the second composite acid and the secondary acid washing are omitted.

[0066] The remaining steps and parameters are consistent with example 1.

[0067] From example 1 and comparative example 1, it can be seen that, in the sample preparation process, if only one acid washing is performed, the surface cleanliness of the sample to be tested will be slightly low, which will result in a longer testing time of the glow discharge mass spectrometer.

[0068] The above merely describes specific embodiments of the present application, but the protection scope of the present application is not limited thereto, and those skilled in the art should understand that any changes or replacements within the technical scope disclosed by the present application can be easily thought of by those skilled in the art, and all fall within the protection scope and disclosure scope of the present application.

Claims

1. A method of preparing a cobalt iron boron alloy, characterized by, The sample preparation method comprises: carrying out at least two times of acid pickling on the cobalt-iron-boron alloy, and then carrying out cleaning and drying to obtain a sample to be tested; the acid pickling agent used in each acid pickling is a composite acid, and the composite acid comprises nitric acid and hydrofluoric acid; the mass concentration of the nitric acid in the composite acid is 10-20%; and the mass concentration of the hydrofluoric acid in the composite acid is 10-20%; the mass concentration ratio of the nitric acid to the hydrofluoric acid in the composite acid is (1-3):(1-3); with the increase of the number of acid pickling, the mass concentrations of the nitric acid and the hydrofluoric acid in the composite acid are gradually reduced.

2. The sample preparation method of claim 1, wherein The cobalt-iron-boron alloy is in a block shape, and the size is 20-35mm*20-35mm*10-20mm.

3. The sample preparation method of claim 1, wherein The solid-liquid ratio of the cobalt-iron-boron alloy to the acid pickling agent is 1g:(3-5)mL.

4. The sample preparation method of claim 1, wherein The time range of each acid pickling is 2-5min.

5. The method of claim 1, wherein, The ultrasonic is used in each acid pickling, and the power range of the ultrasonic is 120-180W.

6. The sample preparation method of claim 1, wherein In the process of the at least two times of acid pickling, the water washing step is carried out between the adjacent two times of acid pickling.

7. The method of claim 1, wherein The cleaning comprises the steps of water washing and alcohol washing in sequence.

8. The sample preparation method of claim 7, wherein The material after the alcohol washing is dried by using a baking lamp.

9. A method for the analytical testing of a cobalt-iron-boron alloy, characterized in that The analysis test method comprises: the sample to be tested prepared by using the sample preparation method in any one of claims 1-8 is placed in a glow discharge mass spectrometer, and then the refrigeration and sputtering are carried out in sequence to obtain a test result.

10. The analytical test method according to claim 9, characterized in that, The voltage of the sputtering is 1-1.1kV.

11. The analytical test method according to claim 9, characterized in that, The current of the sputtering is 2-2.2mA.

12. The analytical test method according to claim 9, wherein, The resolution of the glow discharge mass spectrometer is 4000-5000.