CN111562280A - Method for testing carbon content distribution of neodymium iron boron blank - Google Patents
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Abstract
The invention discloses a method for testing the carbon content distribution of a neodymium iron boron blank, which relates to the technical field of analysis of neodymium iron boron components. Therefore, the defect that the conventional high-frequency infrared absorption method only aims at testing a random sampling area and cannot reflect the whole carbon content distribution of the neodymium iron boron blank from top to bottom can be avoided, and therefore an effective characterization means is provided for optimizing the demolding process of the neodymium iron boron, controlling the carbon content of the neodymium iron boron blank and improving the uniformity of the final neodymium iron boron product. The testing method also has the advantages that the number of the testing surfaces is controllable as required, the testing result of the carbon content distribution condition is visual, and the like.
Description
Technical Field
The invention relates to the technical field of neodymium iron boron component analysis, in particular to a method for testing the carbon content distribution of a neodymium iron boron blank.
Background
The neodymium iron boron magnetic material has wide application fields, has high requirements on comprehensive performance, and requires high coercive force and high magnetic energy product, high corrosion resistance and low weight loss. In the production process of high-performance products, the control of impurity elements is crucial, wherein the carbon content is the impurity element which is inevitably brought in during the use of the release agent during the molding of the sintered neodymium iron boron, and the influence on the product performance is great. The formula of the release agent contains various carbon-containing substances, the release agent is sprayed inside the die and slowly permeates from the surface of the neodymium iron boron blank to the inside, and under the action of gravity, more release agent exists on the lower surface of the neodymium iron boron blank, so that the carbon content is unevenly distributed. After the neodymium iron boron blank is demoulded, the neodymium iron boron blank is required to be cut into different sizes according to customer requirements, and the uniformity of the final product cannot be guaranteed due to the fact that the distribution of the carbon content of the neodymium iron boron blank is uneven. The carbon content is increased, a carbon-rich phase can be formed in the neodymium-rich phase of the magnet, the neodymium-rich phase of local tissues and even the main phase are damaged, and the intrinsic coercive force of the neodymium-iron-boron magnet is reduced; the destructive action loosens the matrix and also reduces the corrosion resistance. The reduction of the product performance greatly restricts the application range of the neodymium iron boron and influences the service life of related components.
The existing traditional testing methods such as the Nd-Fe-B industry standard mainly measure carbon by a high-frequency infrared absorption method, and after a sample is mechanically crushed, the test is only carried out on a random sampling area, so that the distribution condition of the whole carbon content of the Nd-Fe-B blank with non-uniform carbon content cannot be reflected from top to bottom. In order to optimize the demolding process of the neodymium iron boron, the demolding effect of the product is ensured, the carbon content of the neodymium iron boron blank is reduced, the uniformity of the product is improved, and a balance point of the demolding process and the carbon content is sought, so that the method for testing the carbon content distribution is especially important.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for testing the carbon content distribution of the neodymium iron boron blank, which has the advantages of controllable number of test surfaces as required, visual and visible test results and the like.
The technical problem of the invention is realized by the following technical scheme:
a method for testing the carbon content distribution of a neodymium iron boron blank comprises the following steps:
step one, selecting a rectangular neodymium iron boron blank after demolding, and removing oil stains and impurities on the surface;
step two, placing the neodymium iron boron blank subjected to the step one in an oven for low-temperature drying;
step three, averagely dividing the neodymium iron boron blank subjected to the step two into a plurality of layers of test surfaces, wherein each layer of test surface is a rectangular test surface, sequentially marking the plurality of layers of test surfaces in the order from top to bottom, and taking the pressed surface of the neodymium iron boron blank as a 1 st test surface, the lowest layer as the lower surface of the neodymium iron boron, namely the nth test surface, and the test surface closest to the nth test surface as an nth-1 test surface;
step four, starting the neodymium iron boron blank obtained in the step three from the 1 st test surface, and sequentially completing the carbon content test to the n-1 st test surface from top to bottom:
firstly, measuring the height from a 1 st test surface to a lower surface, selecting 5 test points on the 1 st test surface, and then taking the average value of the carbon content results of the 5 test points;
secondly, the No. 1 test surface after the carbon content test is downwards immersed into a nitric acid solution, and is etched and digested to the digital mark position of the No. 2 test surface;
thirdly, washing the neodymium iron boron blank processed in the second step by using deionized water, and polishing the 2 nd test surface to be flat;
fourthly, washing the neodymium iron boron blank treated by the third step with acetone or absolute ethyl alcohol and drying at low temperature;
measuring the height from the 2 nd test surface to the lower surface of the neodymium iron boron blank processed by the fourth step;
step five, repeating the operation processes from the first step to the fifth step, and sequentially testing the carbon content of the next testing surface until the carbon content of the n-1 testing surface is tested;
step six, turning over the neodymium iron boron blank subjected to the step five, directly testing the carbon content of the nth testing surface, firstly selecting 5 testing points on the nth testing surface, and then taking the average value of the carbon content results of the 5 testing points;
step seven, according to the carbon content test results of all the test surfaces obtained in the step five and the step six, making a distribution curve graph of the carbon content of the neodymium iron boron blank along with the height change;
and step eight, visually measuring the carbon content distribution in the neodymium iron boron blank according to the distribution curve chart obtained in the step seven.
In the production process of neodymium iron boron in the step one, the neodymium iron boron blank is prepared after being pressed and formed and being sintered and demoulded.
And in the first step, acetone or absolute ethyl alcohol is used for removing oil stains and impurities on the surface of the neodymium iron boron blank.
And in the second step, the low-temperature drying temperature is 80-100 ℃, and the time is 10-30 min, so that acetone or absolute ethyl alcohol is removed.
And the pressing surface in the third step is the upper surface formed by pressing in the production of the neodymium iron boron blank.
The carbon content test of each layer of test surface adopts a wavelength dispersion type X-ray fluorescence spectrometer (WDX) test, and the instrument is provided with a special crystal for carbon test to carry out nondestructive test on the test surface.
The 5 test points comprise 1 test point arranged at the position of the intersection of two diagonal lines of the rectangular test surface and 4 test points arranged at the positions of four middle points of the connecting lines of the four diagonal lines and the intersection.
In the fourth step, the nitric acid solution is prepared by concentrated nitric acid and deionized water according to the volume ratio of 1:1, and the depth of the nitric acid solution cannot exceed the digital mark of the next test surface.
And in the fourth step, deionized water is firstly used for washing away residual nitric acid solution, and then a metallographic polishing machine is used for polishing the test surface.
Compared with the prior art, the testing method has the advantages that the problem that the distribution of the carbon content on the surface and inside of the neodymium iron boron blank is uneven due to the use of the release agent in the neodymium iron boron production process is considered, the neodymium iron boron blank is uniformly divided into n layers of testing surfaces in the vertical direction of the pressing surface, the next testing surface is obtained after layer-by-layer testing and etching and digestion by nitric acid, each layer of testing surface adopts WDX to perform nondestructive carbon testing through a 5-point testing method, and the heights of the testing surface and the lower surface of each layer are measured simultaneously, so that the distribution relation between the carbon content and the height of the neodymium iron boron blank is obtained. Therefore, the defect that the conventional high-frequency infrared absorption method only aims at testing a random sampling area and cannot reflect the whole carbon content distribution of the neodymium iron boron blank from top to bottom can be avoided, and therefore an effective characterization means is provided for optimizing the demolding process of the neodymium iron boron, controlling the carbon content of the neodymium iron boron blank and improving the uniformity of the final neodymium iron boron product. The method for testing the carbon content distribution of the neodymium iron boron blank also has the advantages that the number of the testing surfaces is controllable as required, the testing result of the carbon content distribution condition is visual and visible, and the like.
Drawings
Fig. 1 is a schematic structural diagram of a neodymium iron boron blank pressing surface evenly divided into n layers of testing surfaces in the vertical direction.
Fig. 2 is a top view of fig. 1 (a schematic diagram of a structure of 5 test point locations).
Fig. 3 is a graph of the relationship between the distribution of the carbon content of the ndfeb blank and the height.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the above drawings.
As shown in fig. 1 to 3, 1 is a pressing surface, 2 is a lower surface, and 3 is a test point.
A method for testing the carbon content distribution of a neodymium iron boron blank comprises the following steps:
step one, selecting a rectangular neodymium iron boron blank after demolding, and removing oil stains and impurities on the surface by using acetone or absolute ethyl alcohol, wherein the neodymium iron boron blank is prepared by pressing and molding in a neodymium iron boron production process and sintering and demolding;
step two, placing the neodymium iron boron blank subjected to the step one in an oven for drying at a low temperature of 80-100 ℃ for 10-30 min to remove acetone or absolute ethyl alcohol;
step three, dividing the neodymium iron boron blank subjected to the step two into a plurality of layers of test surfaces according to the average shown in figure 1, wherein each layer of test surface is a rectangular test surface, sequentially marking the plurality of layers of test surfaces according to the vertical sequence from top to bottom, and taking the pressing surface 1 of the neodymium iron boron blank as the 1 st test surface, the lowest layer as the lower surface 2 of the neodymium iron boron, namely the nth test surface, and the test surface closest to the nth test surface as the nth-1 test surface; wherein the pressing surface 1 is the upper surface of the neodymium iron boron blank during pressing and forming;
step four, starting the neodymium iron boron blank obtained in the step three from the 1 st test surface, and sequentially completing the carbon content test to the n-1 st test surface from top to bottom:
firstly, measuring the height from a 1 st test surface to a lower surface 2 by using a vernier caliper, selecting 5 test points 3 on the 1 st test surface, and then taking the average value of the carbon content results of the 5 test points 3;
secondly, the No. 1 test surface after the carbon content test is downwards immersed into a nitric acid solution, and is etched and digested to the digital mark position of the No. 2 test surface;
thirdly, washing the neodymium iron boron blank treated in the second step by using deionized water to remove residual nitric acid solution, and polishing the 2 nd test surface by using a metallographic polishing machine to make the test surface smooth;
fourthly, washing the neodymium iron boron blank treated by the third step with acetone or absolute ethyl alcohol and drying at low temperature;
measuring the height from the 2 nd test surface to the lower surface 2 of the neodymium iron boron blank processed by the fourth step by using a vernier caliper;
step five, repeating the operation processes from the first to the fifth in the step four, sequentially testing the carbon content of the next testing surface until the carbon content of the n-1 testing surface is tested,
step six, turning over the neodymium iron boron blank subjected to the step five, directly testing the carbon content of the nth testing surface, firstly selecting 5 testing points 3 on the nth testing surface, and then taking the average value of the carbon content results of the 5 testing points 3;
step seven, according to the carbon content test results of all the test surfaces obtained in the step five and the step six, making a distribution curve graph of the carbon content of the neodymium iron boron blank along with the height change as shown in fig. 3;
and step eight, visually measuring the carbon content distribution in the neodymium iron boron blank according to the distribution curve chart obtained in the step seven.
Meanwhile, in the testing step, the carbon content of each layer of testing surface is tested by adopting a wavelength dispersion type X-ray fluorescence spectrometer (WDX), and the testing surface is subjected to nondestructive testing by using a special crystal for carbon testing.
The 5 test points 3 are shown in fig. 2, and include 1 test point 3 arranged at the intersection of two diagonal lines of the rectangular test surface, and 4 test points 3 arranged at four midpoint positions of the connecting lines of four diagonal lines and the intersection.
In addition, in the fourth step, the nitric acid solution is prepared by concentrated nitric acid and deionized water according to the volume ratio of 1:1, and the depth of the nitric acid solution cannot exceed the digital mark of the next test surface.
The invention is illustrated in detail by the following three specific examples:
example 1
Selecting a rectangular neodymium iron boron blank after demoulding, removing oil stains and impurities on the surface by using acetone, and then placing the blank in an oven for drying at low temperature, wherein the drying temperature is 80 ℃ for 20min to remove acetone on the surface; taking a pressing surface 1 of the neodymium iron boron blank as a 1 st testing surface, averagely dividing the neodymium iron boron blank into 5 layers according to testing requirements, sequentially marking 1-5 digital marks on the side surface according to the sequence from top to bottom, wherein the lowest layer is a lower surface 2 of the neodymium iron boron, namely the 5 th testing surface, and the closest to the 5 th testing surface is a 4 th testing surface; measuring the height from the 1 st test surface to the lower surface 2 by using a vernier caliper; adopting a wavelength dispersion type X-ray fluorescence spectrometer (WDX), sequentially testing the carbon content from a 1 st test surface, firstly taking 5 test points on the 1 st test surface, obtaining the carbon content result of the 1 st test surface, taking the average value of the result, then downwards immersing the 1 st test surface into a nitric acid solution, etching and digesting the solution until the solution depth can not exceed the digital mark of the 2 nd test surface, cleaning the solution to the digital mark of the 2 nd test surface by using deionized water to remove residual nitric acid, polishing the 2 nd test surface by using a metallographic grinding and polishing machine to flatten the 2 nd test surface, then cleaning the polished neodymium iron boron blank by using acetone, drying the blank at 80 ℃ for 20min, and finally measuring the height from the 2 nd test surface to a lower surface 2; in this way, the carbon content tests of the 3 rd test surface and the 4 th test surface can be sequentially carried out only by repeating the operation process, the carbon content test of the 5 th test surface is that after the carbon content test of the 4 th test surface is completed, the neodymium iron boron blank is turned over, the carbon content test of the 5 th test surface can be directly carried out, 5 test points 3 are selected on the 5 th test surface, and then the average value of the carbon content results of the 5 test points is taken; finally, a distribution curve graph of the carbon content of the neodymium iron boron blank along with the height change can be made.
Example 2
Selecting a rectangular neodymium iron boron blank after demoulding, removing oil stains and impurities on the surface by using acetone, and then placing the blank in an oven for drying at low temperature, wherein the drying temperature is 90 ℃ for 10min to remove the acetone on the surface; taking a pressing surface 1 of the neodymium iron boron blank as a 1 st testing surface, averagely dividing the neodymium iron boron blank into 6 layers according to testing requirements, sequentially marking the number of 1-6 on the side surface according to the sequence from top to bottom, wherein the lowest layer is a lower surface 2 of the neodymium iron boron, namely the 6 th testing surface, and the closest to the 6 th testing surface is a 5 th testing surface; measuring the height from the 1 st test surface to the lower surface 2 by using a vernier caliper; adopting a wavelength dispersion type X-ray fluorescence spectrometer (WDX), sequentially testing the carbon content from a 1 st test surface, firstly taking 5 test points on the 1 st test surface, obtaining the carbon content result of the 1 st test surface, taking the average value of the result, then downwards immersing the 1 st test surface into a nitric acid solution, etching and digesting the solution until the solution depth can not exceed the digital mark of the 2 nd test surface, cleaning the solution to the digital mark of the 2 nd test surface by using deionized water to remove residual nitric acid, polishing the 2 nd test surface by using a metallographic grinding and polishing machine to flatten the 2 nd test surface, then cleaning the polished neodymium iron boron blank by using acetone, drying the blank at 90 ℃ for 10min, and finally measuring the height from the 2 nd test surface to a lower surface 2; in this way, the carbon content tests of the 3 rd, the 4 th and the 5 th test surfaces can be sequentially carried out by only repeating the operation process, the carbon content test of the 6 th test surface is that after the carbon content test of the 5 th test surface is completed, the neodymium iron boron blank is turned over to directly carry out the carbon content test of the 6 th test surface, 5 test points 3 are selected on the 6 th test surface, and then the average value of the carbon content results of the 5 test points is taken; finally, a distribution curve graph of the carbon content of the neodymium iron boron blank along with the height change can be made.
Example 3
Selecting a rectangular neodymium iron boron blank after demoulding, removing oil stains and impurities on the surface by using absolute ethyl alcohol, and then placing the blank in an oven for drying at low temperature, wherein the drying temperature is 100 ℃, and the drying time is 30min, so as to remove the absolute ethyl alcohol on the surface; taking a pressing surface 1 of the neodymium iron boron blank as a test surface 1, averagely dividing the neodymium iron boron blank into 7 layers according to test requirements, sequentially marking the number of 1-7 on the side surface according to the sequence from top to bottom, wherein the lowest layer is a lower surface 2 of the neodymium iron boron, namely a test surface 7, and the test surface closest to the test surface 7 is a test surface 6; measuring the height from the 1 st test surface to the lower surface 2 by using a vernier caliper; adopting a wavelength dispersion type X-ray fluorescence spectrometer (WDX), sequentially testing the carbon content from a 1 st test surface, firstly taking 5 test points on the 1 st test surface, obtaining the carbon content result of the 1 st test surface, taking the average value of the result, then downwards immersing the 1 st test surface into a nitric acid solution, etching and digesting the solution until the solution depth can not exceed the digital mark of the 2 nd test surface, cleaning the solution to the digital mark of the 2 nd test surface by using deionized water to remove residual nitric acid, polishing the 2 nd test surface by using a metallographic grinder to flatten the test surface, then cleaning the polished neodymium iron boron blank by using absolute ethyl alcohol, drying the blank for 30min at 100 ℃, and finally measuring the height from the 2 nd test surface to the lower surface 2; in this way, the carbon content tests of the 3 rd, 4 th, 5 th and 6 th test surfaces can be sequentially carried out by only repeating the operation process, the carbon content test of the 7 th test surface is that after the carbon content test of the 6 th test surface is finished, the neodymium iron boron blank is turned over, the carbon content test of the 7 th test surface can be directly carried out, 5 test points 3 are selected on the 7 th test surface, and then the average value of the carbon content results of the 5 test points is taken; finally, a distribution curve graph of the carbon content of the neodymium iron boron blank along with the height change can be made.
The above description is only exemplary of the present invention, and it should be understood by those skilled in the art that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. It should also be understood that various changes or modifications to the method which may occur to those skilled in the art after reading the teachings herein, if they fall within the scope of the appended claims, should be considered to be equivalent forms.
Claims (9)
1. A method for testing the carbon content distribution of a neodymium iron boron blank is characterized by comprising the following steps:
step one, selecting a rectangular neodymium iron boron blank after demolding, and removing oil stains and impurities on the surface;
step two, placing the neodymium iron boron blank subjected to the step one in an oven for low-temperature drying;
step three, averagely dividing the neodymium iron boron blank subjected to the step two into a plurality of layers of test surfaces, wherein each layer of test surface is a rectangular test surface, sequentially marking the plurality of layers of test surfaces according to the sequence from top to bottom, and taking the pressed surface (1) of the neodymium iron boron blank as a 1 st test surface, the lowest layer as a lower surface (2) of the neodymium iron boron, namely the nth test surface, and the test surface closest to the nth test surface is an nth-1 test surface;
step four, starting the neodymium iron boron blank obtained in the step three from the 1 st test surface, and sequentially completing the carbon content test to the n-1 st test surface from top to bottom:
firstly, measuring the height from a 1 st test surface to a lower surface (2), selecting 5 test points (3) on the 1 st test surface, and then taking the average value of the carbon content results of the 5 test points (3);
secondly, the No. 1 test surface after the carbon content test is downwards immersed into a nitric acid solution, and is etched and digested to the digital mark position of the No. 2 test surface;
thirdly, washing the neodymium iron boron blank processed in the second step by using deionized water, and polishing the 2 nd test surface to be flat;
fourthly, washing the neodymium iron boron blank treated by the third step with acetone or absolute ethyl alcohol and drying at low temperature;
measuring the height from the 2 nd test surface to the lower surface (2) of the neodymium iron boron blank processed by the fourth step;
step five, repeating the operation processes from the first step to the fifth step, and sequentially testing the carbon content of the next testing surface until the carbon content of the n-1 testing surface is tested;
step six, turning over the neodymium iron boron blank subjected to the step five, directly testing the carbon content of the nth testing surface, firstly selecting 5 testing points (3) on the nth testing surface, and then taking the average value of the carbon content results of the 5 testing points (3);
step seven, according to the carbon content test results of all the test surfaces obtained in the step five and the step six, making a distribution curve graph of the carbon content of the neodymium iron boron blank along with the height change;
and step eight, visually measuring the carbon content distribution in the neodymium iron boron blank according to the distribution curve chart obtained in the step seven.
2. The method for testing the carbon content distribution of the neodymium-iron-boron blank according to claim 1, wherein in the step one, the neodymium-iron-boron blank is manufactured by pressing, sintering and demolding in a neodymium-iron-boron production process.
3. The method for testing the carbon content distribution of the neodymium iron boron blank according to claim 1, wherein in the step one, acetone or absolute ethyl alcohol is used for removing oil stains and impurities on the surface of the neodymium iron boron blank.
4. The method for testing the carbon content distribution of the neodymium iron boron blank according to claim 1, wherein the low temperature drying temperature in the second step is 80-100 ℃ for 10-30 min to remove acetone or absolute ethyl alcohol.
5. The method for testing the carbon content distribution of the neodymium iron boron blank according to claim 1, wherein the pressing surface (1) in the third step is the upper surface of the neodymium iron boron blank during pressing and forming.
6. The method for testing the carbon content distribution of the neodymium-iron-boron blank according to claim 1, wherein the carbon content test of each layer of the test surface is performed by using a wavelength dispersive X-ray fluorescence spectrometer (WDX), and the instrument is equipped with a crystal special for carbon testing to perform nondestructive testing on the test surface.
7. The method for testing the carbon content distribution of the neodymium-iron-boron blank according to claim 1, wherein the 5 test points (3) comprise 1 test point (3) arranged at the intersection of two diagonals of the rectangular test surface and 4 test points (3) arranged at four midpoint positions of the connecting lines of the four diagonals and the intersection respectively.
8. The method for testing the carbon content distribution of the neodymium-iron-boron blank according to claim 1, wherein the nitric acid solution in the fourth step is prepared from concentrated nitric acid and deionized water according to a volume ratio of 1:1, and the depth of the nitric acid solution cannot exceed the digital mark of the next test surface.
9. The method for testing the carbon content distribution of the neodymium-iron-boron blank according to claim 1, wherein in the fourth step, the residual nitric acid solution is washed away by deionized water, and then a metallographic polishing machine is used for polishing the test surface.
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