CN103335999A - Method for testing element distribution in alloy board - Google Patents

Method for testing element distribution in alloy board Download PDF

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CN103335999A
CN103335999A CN2013102635298A CN201310263529A CN103335999A CN 103335999 A CN103335999 A CN 103335999A CN 2013102635298 A CN2013102635298 A CN 2013102635298A CN 201310263529 A CN201310263529 A CN 201310263529A CN 103335999 A CN103335999 A CN 103335999A
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CN103335999B (en
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朱远志
赵超奇
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention relates to a method for testing the element distribution in an alloy board. The technical scheme comprises the following steps of: firstly, taking a board with the diameter of 10-20mm from the test boards as a test sample, except for one surface, sealing other surfaces of the test sample with an adhesion agent; then, mixing a strong acid solution with the concentration of 20-50% and mercuric chloride in a glass vessel according to the volume ratio of 1 to (0.003-0.01) to obtain the test solution; adding 10ml of the test solution into a first beaker, weighing the mass m0 of the test sample, adding the test sample into the first breaker, stirring for 30-240s under ultrasonic shaking, taking out the test sample, washing the test sample with distilled water, drying, and weighing the mass m1 of the dried test sample; testing the concentration of each element in the test solution in the breaker by using an inductively coupled plasma optical emission spectrometer, so as to sequentially obtain the thickness delta H1 etched off for the first time and the concentration of each element; repeating the testing process, until the test sample is etched off completely, then, acquiring the element distribution conditions in the alloy board. The method can accurately test the element distribution in the alloy board.

Description

The method that element distributes in a kind of beta alloy sheet material
Technical field:
The invention belongs to the metallurgical analysis technical field, be specifically related to the method that element distributes in a kind of beta alloy sheet material.
Background technology
Element distribution in the sheet alloy comes down to inhomogeneous.Particularly under as-cast condition, because the proportion of every kind of element is different, can cause gravity segregation.In addition, the precedence of alloy graining is different, also can cause the element skewness.Even homogenising is handled, also be difficult to make the element in the sheet material evenly to distribute.Thereby heterogeneity is ubiquitous problem in the sheet material.And exactly be exactly the performance of this unevenness many aspects such as mechanics, physics and chemistry that can badly influence sheet metal.In most cases, people often require the element in the sheet material to distribute more even.This just needs to understand the distribution situation of the element in the sheet material, for smelting and the Technology for Heating Processing improvement provides effective quantitative data, but will know more exactly that the distribution situation of element in sheet material is difficult.
Utilize metaloscope and scanning electron microscope energy disperse spectroscopy that (Li Yusheng is analyzed in the distribution of element at present, Zhai Hu, the horse bezoar people, Deng. high strength ZL205A alloy large-size foundry goods " white point " segregation research [J]. casting, 2007,56 (2): 185-187.), utilize metaloscope to carry out metallographic structure analysis, though can determine whether to exist the microstructure segregation intuitively, can analyze qualitatively the distribution of element, but can't quantitatively determine the distribution situation of element, and scanning electron microscope energy disperse spectroscopy can carry out qualitative and quantitative analysis to the distribution situation of element, but under the very little situation of alloying element content, scanning electron microscope energy disperse spectroscopy can't measure or measured deviation bigger, therefore all can not be for smelting and Technology for Heating Processing provides effective quantitative data.
Summary of the invention
The present invention is intended to overcome the prior art defective, and purpose provides the method that element distributes in a kind of sheet material of beta alloy accurately.
For achieving the above object, the step of the technical solution used in the present invention is:
Step 1, the intercepting diameter is 10～20mm sample identical with sheet material with thickness in sheet material to be tested, and except the upper surface or lower surface of sample, remaining surface employing tackifier seals, and makes specimen.
Step 2, get concentration be 20～50% strong acid solutions in glass container, add the mercuric chloride of strong acid solution volume 0.3～1% again in the glass container, make test solution.
Step 3, get 10ml test with solution in the 1st beaker, weighing and record specimen quality m 0, the specimen after the weighing is put into the 1st beaker, adopt ultrasonic oscillation to stir, the concussion mixing time is 30～240s, takes out and uses distilled water flushing, oven dry.Specimen quality m after weighing and record corrode for the 1st time again 1, according to the △ m of poor quality of specimen before and after the 1st corrosion 1=m 0-m 1, calculate the thickness △ H that erodes for the 1st time by reaction area and panel density to be tested 1Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 1st beaker with each element in the solution.
Step 4, get 10ml test with solution in the 2nd beaker, the specimen after the 1st corrosion is put into the 2nd beaker, adopt ultrasonic oscillation to stir, concussion mixing time is 30～240s, takes out and uses distilled water flushing, dries.Specimen quality m after weighing and record corrode for the 2nd time again 2, according to the △ m of poor quality of specimen before and after the 2nd corrosion 2=m 1-m 2, calculate the thickness △ H that erodes for the 2nd time by reaction area and panel density to be tested 2Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 2nd beaker with each element in the solution.
Step 5, repeating step four described methods, carry out the 3rd time ..., the n-1 time test.The n time method of testing is: namely get the 10ml test and use solution in the n beaker, specimen after the n-1 time corrosion is put into the n beaker, the employing ultrasonic oscillation stirs, the concussion mixing time is 30～240s, specimen is all corroded, take out the sealing test sample with epoxide resin AB glue distilled water flushing, dry.Sealing test sample epoxide resin AB glue m after weighing and record corrode for the n time again n, according to the △ m of poor quality of the specimen before the n time corrosion and the sealing test sample epoxide resin AB glue after the corrosion n=m N-1-m n, calculate the thickness △ H that erodes for the n time by reaction area and panel density to be tested nUse inductive coupling plasma emission spectrograph then, record the concentration of testing in the n beaker with each element in the solution.
Step 6, obtain the thickness △ H that erodes successively according to step 3～step 5 1, △ H 2..., △ H n, again according to the 1st beaker, the 2nd beaker ..., test obtains specimen along thickness △ H with the concentration of each element in the solution in the n beaker 1, △ H 2..., △ H nThe distribution situation of corresponding each element on the direction.
The tackifier of described sealed sample is epoxide resin AB glue.
Good effect of the present invention is to provide the method for elemental distribution in a kind of accurate beta alloy sheet material, overcoming metaloscope can only analyze qualitatively to the distribution of element, but can't quantitatively determine the shortcoming of the distribution situation of element, and improve scanning electron microscope energy disperse spectroscopy under the very little situation of alloying element content, can't measure in the scanning electron microscope energy disperse spectroscopy quantitative test or deficiency that measured deviation is bigger, for smelting and the Technology for Heating Processing improvement provides effective quantitative data, the improvement of technology more there is reference value.
Description of drawings
Fig. 1 tests a kind of Sb elemental distribution with steel board with the present invention;
Fig. 2 distribution situation of the Sn element of test pattern 1 described band steel board of the present invention;
Fig. 3 distribution situation of the W element of test pattern 1 described band steel board of the present invention;
Fig. 4 distribution situation of the Ni element of test pattern 1 described band steel board of the present invention;
Fig. 5 distribution situation of the Cu element of test pattern 1 described band steel board of the present invention;
Fig. 6 is the distribution situation of testing a kind of Si element of cast-rolling aluminum with the present invention;
Fig. 7 distribution situation of the Zn element of test pattern 6 described cast-rolling aluminums of the present invention;
Fig. 8 distribution situation of the Mg element of test pattern 6 described cast-rolling aluminums of the present invention;
Fig. 9 distribution situation of the Ti element of test pattern 6 described cast-rolling aluminums of the present invention;
Figure 10 distribution situation of the Mn element of test pattern 6 described cast-rolling aluminums of the present invention.
Specific embodiments
The invention will be further described below in conjunction with embodiment, is not limiting the scope of the invention.
Embodiment 1
The method that element distributes in a kind of beta alloy sheet material.The tested object of present embodiment is the band steel board, and thickness is 5mm, and purpose is the distribution in the band steel board of test Sb, Sn, W, Ni and Cu element.Concrete steps are:
Step 1, the intercepting diameter is that the 10mm band steel board identical with sheet material with thickness is specimen in band steel board to be tested, and except the upper surface of sample, remaining surface employing epoxide resin AB glue seals, and makes specimen.
Step 2, to get concentration be 20%HNO 3Solution adds HNO again in glass container in glass container 3The mercuric chloride of liquor capacity 0.3% makes test solution.
Step 3, get 10ml test with solution in the 1st beaker, weighing and record specimen quality m 0=3.620g puts into the 1st beaker with the specimen after the weighing, adopts ultrasonic oscillation to stir, and the concussion mixing time is 30s, takes out and uses distilled water flushing, oven dry.Specimen quality m after weighing and record corrode for the 1st time again 1=3.507g is according to the △ m of poor quality of specimen before and after the 1st corrosion 1=m 0-m 1=0.113g is by reaction area and band steel board density p=7.9g/cm 3Calculate the thickness △ H that erodes for the 1st time 1=0.183mm.Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 1st beaker with each element in the solution.See in the table 1 the 1st time test result for details.
Step 4, get 10ml test with solution in the 2nd beaker, the specimen after the 1st corrosion is put into the 2nd beaker, adopt ultrasonic oscillation to stir, concussion mixing time is 30s, takes out and uses distilled water flushing, dries.Specimen quality m after weighing and record corrode for the 2nd time again 2=3.401g is according to the △ m of poor quality of specimen before and after the 2nd corrosion 2=0.106g is by reaction area and band steel board density p=7.9g/cm 3Calculate the thickness △ H that erodes for the 2nd time 2=0.171mm.Use inductive coupling plasma emission spectrograph then, record in the 2nd beaker test with the concentration of each element in the solution, see in the table 1 the 2nd time test result for details.
Step 5, according to the described method of step 4, carry out the 3rd time ..., the 29th time test, see the 3rd～29 time test result in the table 1 for details.The 30th time method of testing is: get the 10ml test and use solution in the 30th beaker, specimen after the 29th corrosion is put into the 30th beaker, the employing ultrasonic oscillation stirs, the concussion mixing time is 30s, specimen is all corroded, take out the sealing test sample with epoxide resin AB glue distilled water flushing, dry.Sealing test sample epoxide resin AB glue m after weighing and record corrode for the 30th time again 30=0.52g is according to the △ m of poor quality of the specimen before the 30th corrosion and the sealing test sample epoxide resin AB glue after the corrosion n=0.106g is by reaction area and band steel board density p=7.9g/cm 3Calculate the thickness △ H that erodes for the 30th time n=0.171mm.Use inductive coupling plasma emission spectrograph then, record in the 30th beaker test with the concentration of each element in the solution, see in the table 1 the 30th time test result for details.
Step 6, obtain the thickness △ H that erodes successively according to step 3～step 5 1, △ H 2..., △ H 30Again according to the 1st beaker, the 2nd beaker ..., test obtains specimen along thickness △ H with the concentration of each element in the solution in the 30th beaker 1, △ H 2..., △ H 30The distribution situation of corresponding Sb, Sn, W, Ni and Cu element on the direction.The distribution situation of Sb, Sn, W, Ni and Cu element is followed successively by accompanying drawing 1～Fig. 5.
The table with test results of the band steel board of table 1 present embodiment
Figure BDA00003422731800051
Embodiment 2
The method that element distributes in a kind of beta alloy sheet material.
The step of the described method of present embodiment is: the tested object of present embodiment is cast-rolling aluminum sheet material, and thickness is 7.3mm, and purpose is test Si, Zn, Mg, Ti and the distribution of Mn element in cast-rolling aluminum.Concrete steps are:
Step 1, the intercepting diameter is the 20mm sample identical with sheet metal thickness with thickness in cast-rolling aluminum sheet material to be tested, and except the lower surface of sample, remaining surface employing epoxide resin AB glue seals, and makes specimen.
Step 2, get concentration be 50% strong acid solution HCL solution in glass container, add the mercuric chloride of HCL liquor capacity 0.3% again in the glass container, make test solution.
Step 3, get 10ml test with solution in the 1st beaker, weighing and record specimen quality m 0=7.079g puts into the 1st beaker with the specimen after the weighing, adopts ultrasonic oscillation to stir, and the concussion mixing time is 240s, takes out and uses distilled water flushing, oven dry.Specimen quality m after weighing and record corrode for the 1st time again 1=6.618g is according to the △ m of poor quality of specimen before and after the 1st corrosion 1=m 0-m 1=0.461g is by reaction area and cast-rolling aluminum panel density ρ=2.7g/cm 3Calculate the thickness △ H that erodes for the 1st time 1=0.544mm.Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 1st beaker with each element in the solution.See in the table 2 the 1st time test result for details.
Step 4, get 10ml test with solution in the 2nd beaker, the specimen after the 1st corrosion is put into the 2nd beaker, adopt ultrasonic oscillation to stir, concussion mixing time is 240s, takes out and uses distilled water flushing, dries.Specimen quality m after weighing and record corrode for the 2nd time again 2=6.260g is according to the △ m of poor quality of specimen before and after the 2nd corrosion 2=m 1-m 2=0.358g is by reaction area and cast-rolling aluminum panel density ρ=2.7g/cm 3Calculate the thickness △ H that erodes for the 2nd time 2=0.442mm.Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 2nd beaker with each element in the solution.See in the table 2 the 1st time test result for details.
Step 5, according to the described method of step 4, carry out the 3rd time ..., the 12nd time test, see the 3rd～12 time test result in the table 2 for details.The 13rd time method of testing is: get the 10ml test and use solution in the 13rd beaker, specimen after the 13rd corrosion is put into the 13rd beaker, the employing ultrasonic oscillation stirs, the concussion mixing time is 240s, specimen is all corroded, take out the sealing test sample with epoxide resin AB glue distilled water flushing, dry.Sealing test sample epoxide resin AB glue m after weighing and record corrode for the 13rd time again 30=0.89g is according to the △ m of poor quality of the specimen before the 13rd corrosion and the sealing test sample epoxide resin AB glue after the corrosion n=0.377g is by reaction area and cast-rolling aluminum panel density ρ=2.7g/cm 3Calculate the thickness △ H that erodes for the 13rd time n=0.445mm.Use inductive coupling plasma emission spectrograph then, record in the 13rd beaker test with the concentration of each element in the solution, see in the table 2 the 13rd time test result for details.
Step 6, obtain the thickness △ H that erodes successively according to step 3～step 5 1, △ H 2..., △ H 13Again according to the 1st beaker, the 2nd beaker ..., test obtains specimen along thickness △ H with the concentration of each element in the solution in the 13rd beaker 1, △ H 2..., △ H 13The distribution situation of corresponding Si, Zn, Mg, Ti and Mn element on the direction.The distribution situation of Si, Zn, Mg, Ti and Mn element sees annex map 6～Figure 10 for details.
The table with test results of the cast-rolling aluminum of this enforcement of table 2
Figure BDA00003422731800071
Execute example 3
The method that element distributes in a kind of beta alloy sheet material, the concrete steps of present embodiment are:
Step 1, the intercepting diameter is 10～20mm sample identical with sheet material with thickness in sheet material to be tested, and except the upper surface or lower surface of sample, remaining surface employing tackifier seals, and makes specimen.
Step 2, get concentration be 20～50% strong acid solutions in glass container, add the mercuric chloride of strong acid solution volume 0.3～1% again in the glass container, make test solution.
Step 3, get 10ml test with solution in the 1st beaker, weighing and record specimen quality m 0, the specimen after the weighing is put into the 1st beaker, adopt ultrasonic oscillation to stir, the concussion mixing time is 30～240s, takes out and uses distilled water flushing, oven dry.Specimen quality m after weighing and record corrode for the 1st time again 1, according to the △ m of poor quality of specimen before and after the 1st corrosion 1=m 0-m 1, calculate the thickness △ H that erodes for the 1st time by reaction area and panel density to be tested 1Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 1st beaker with each element in the solution.
Step 4, get 10ml test with solution in the 2nd beaker, the specimen after the 1st corrosion is put into the 2nd beaker, adopt ultrasonic oscillation to stir, concussion mixing time is 30～240s, takes out and uses distilled water flushing, dries.Specimen quality m after weighing and record corrode for the 2nd time again 2, according to the △ m of poor quality of specimen before and after the 2nd corrosion 2=m 1-m 2, calculate the thickness △ H that erodes for the 2nd time by reaction area and panel density to be tested 2Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 2nd beaker with each element in the solution.
Step 5, repeating step four described methods, carry out the 3rd time ..., the n-1 time test.The n time method of testing is: namely get the 10ml test and use solution in the n beaker, specimen after the n-1 corrosion is put into the n beaker, the employing ultrasonic oscillation stirs, the concussion mixing time is 30～240s, specimen is all corroded, take out the sealing test sample with epoxide resin AB glue distilled water flushing, dry.Sealing test sample epoxide resin AB glue m after weighing and record corrode for the n time again n△ m of poor quality according to the specimen before the n time corrosion and the sealing test sample epoxide resin AB glue after the corrosion n=m N-1-m n, calculate the thickness △ H that erodes for the n time by reaction area and panel density to be tested nUse inductive coupling plasma emission spectrograph then, record the concentration of testing in the n beaker with each element in the solution.
Step 6, obtain the thickness △ H that erodes successively according to step 3～step 5 1, △ H 2..., △ H nAgain according to the 1st beaker, the 2nd beaker ..., test obtains specimen along thickness △ H with the concentration of each element in the solution in the n beaker 1, △ H 2..., △ H nThe distribution situation of corresponding each element on the direction.
The tackifier of described sealed sample is epoxide resin AB glue.
The good effect of this embodiment is to provide the method for elemental distribution in a kind of accurate beta alloy sheet material, overcoming metaloscope can only analyze qualitatively to the distribution of element, but can't quantitatively determine the shortcoming of the distribution situation of element, and improve scanning electron microscope energy disperse spectroscopy under the very little situation of alloying element content, can't measure in the scanning electron microscope energy disperse spectroscopy quantitative test or deficiency that measured deviation is bigger, for smelting and the Technology for Heating Processing improvement provides effective quantitative data, the improvement of technology more there is reference value.

Claims (2)

1. the method that element distributes in the beta alloy sheet material is characterized in that the step of described method is:
Step 1, the intercepting diameter is 10 ~ 20mm sample identical with sheet material with thickness in sheet material to be tested, and except the upper surface or lower surface of sample, remaining surface employing tackifier seals, and makes specimen;
Step 2, get concentration be 20 ~ 50% strong acid solutions in glass container, add the mercuric chloride of strong acid solution volume 0.3 ~ 1% again in the glass container, make test solution;
Step 3, get 10ml test with solution in the 1st beaker, weighing and record specimen quality m 0, the specimen after the weighing is put into the 1st beaker, adopt ultrasonic oscillation to stir, the concussion mixing time is 30 ~ 240s, takes out and uses distilled water flushing, oven dry; Specimen quality m after weighing and record corrode for the 1st time again 1, according to the △ m of poor quality of specimen before and after the 1st corrosion 1=m 0-m 1, calculate the thickness △ H that erodes for the 1st time by reaction area and panel density to be tested 1Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 1st beaker with each element in the solution;
Step 4, get 10ml test with solution in the 2nd beaker, the specimen after the 1st corrosion is put into the 2nd beaker, adopt ultrasonic oscillation to stir, concussion mixing time is 30 ~ 240s, takes out and uses distilled water flushing, dries; Specimen quality m after weighing and record corrode for the 2nd time again 2, according to the △ m of poor quality of specimen before and after the 2nd corrosion 2=m 1-m 2, calculate the thickness △ H that erodes for the 2nd time by reaction area and panel density to be tested 2Use inductive coupling plasma emission spectrograph then, record the concentration of testing in the 2nd beaker with each element in the solution;
Step 5, repeating step four described methods, carry out the 3rd time ..., the n-1 time test; The n time method of testing is: namely get the 10ml test and use solution in the n beaker, specimen after the n-1 time corrosion is put into the n beaker, the employing ultrasonic oscillation stirs, the concussion mixing time is 30 ~ 240s, specimen is all corroded, take out the sealing test sample with epoxide resin AB glue distilled water flushing, dry; Sealing test sample epoxide resin AB glue m after weighing and record corrode for the n time again n, according to the △ m of poor quality of the specimen before the n time corrosion and the sealing test sample epoxide resin AB glue after the corrosion n=m N-1-m n, calculate the thickness △ H that erodes for the n time by reaction area and panel density to be tested nUse inductive coupling plasma emission spectrograph then, record the concentration of testing in the n beaker with each element in the solution;
Step 6, obtain the thickness △ H that erodes successively according to step 3 ~ step 5 1, △ H 2..., △ H n, again according to the 1st beaker, the 2nd beaker ..., test obtains specimen along thickness △ H with the concentration of each element in the solution in the n beaker 1, △ H 2..., △ H nThe distribution situation of corresponding each element on the direction.
2. the method that distributes according to element in the beta alloy sheet material described in the claim 1 is characterized in that described tackifier is epoxide resin AB glue.
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CN111487272A (en) * 2020-04-21 2020-08-04 中国航发沈阳发动机研究所 Analysis method for surface product layer of turbine blade of aero-engine

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