CN101029882A - Method for determining chemical ingredients in metal material matrix - Google Patents
Method for determining chemical ingredients in metal material matrix Download PDFInfo
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- CN101029882A CN101029882A CN 200710038729 CN200710038729A CN101029882A CN 101029882 A CN101029882 A CN 101029882A CN 200710038729 CN200710038729 CN 200710038729 CN 200710038729 A CN200710038729 A CN 200710038729A CN 101029882 A CN101029882 A CN 101029882A
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Abstract
A method for determining chemical composition in base body of metal material includes applying 3-D atomic probe and relevant computer software to carry out quantitative analysis on chemical composition of metal material base body, enabling to carry out quantitative analysis once on all elements contained in metal and enabling to carry out individual quantitative analysis on fine separated out particles.
Description
Technical field
The present invention relates to a kind of method of measuring chemical ingredients in metal material matrix, it is different from traditional chemical analysis method, belongs to modern novel atom-probe assay method technical field.
Background technology
The modern material science depends on the understanding to material property and its composition and microstructure relation to a great extent.The chemical composition analysis of material is except traditional chemical analysis technology, this includes mass spectrum, ultraviolet, visible light, Infrared spectroscopy, gas chromatography, liquid chromatography, nuclear magnetic resonance, X-ray fluorescence spectra, Auger and x-ray photoelectron spectroscopy, electron probe, laser probe etc.
For the metal that contains multiple element, the each test of traditional chemical analysis technology can only be determined a kind of accurate content of element, and is a kind of average content.Additive method then is that signal intensity is added up, and need to consider several factors and parameter, and the calculating by complexity just can obtain, its poor accuracy, and data deviation is big.
Summary of the invention
The purpose of this invention is to provide a kind of effective ways of measuring chemical ingredients in metal material matrix.
The present invention is a kind of method of measuring chemical ingredients in metal material matrix, it is characterized in that having following process and step:
A. the tip-like sample of usefulness is analyzed in preparation: earlier the metal material sample of desire test is processed into circular section or square section filament (φ＜0.5mm or＜0.5 * 0.5mm); Process with electrolytic polishing method then, its method is to inject skim electrolytic solution to swim on the bigger inert fluid of density in container, filament shape samples vertical is put into electrolytic solution carry out electropolishing, make filament produce thin neck until disconnection, obtain the tip-like sample at its length middle part; The radius-of-curvature of needle point is 10～100nm; Different metal materials adopts different electrolytic solution and voltage;
B. above-mentioned tip-like sample is put into the enterprising line data collection of three-dimensional atom probe; Pulse voltage is applied on the tip-like sample, and atom is from sample tip end surface evaporation, becomes ion and flies out and hit detector, by measuring the mass-to-charge ratio that the flight time can determine this ion, determines the element kind of flight ion; Atom is to evaporate one by one, surveys one by one, and carries out record with computing machine;
C. with computing machine all data are analyzed, tiny when separating out particle when not existing, can directly obtain in the metal material matrix all elements chemical constitution accurately, and make quantitative test.
Above-mentioned electropolishing process, different metal materials adopts different electrolytic solution and voltage:
(1) ferrous alloy, nickel-base alloy, niobium-base alloy, the used electrolytic solution of acieral are: the mixed liquor that the perchloric acid 10～25% of concentration 70% and glacial acetic acid 75～90% are formed; Its DC voltage is 10～25V;
(2) the used electrolytic solution of acid bronze alloy is: the mixed liquor that phosphatase 24 0%+ ethanol 20%+ sulfuric acid 5%+ thiocarbamide 5%+ water 30% is formed; Its DC voltage is 5～8V;
(3) the used electrolytic solution of tungsten-bast alloy is: the sodium hydrate aqueous solution of concentration 5%; Alternating voltage is 1～5V.
The characteristics of the inventive method are to utilize three-dimensional atom probe and computer software, can disposablely carry out quantitative test to all elements in the metal; Tiny when separating out particle when existing, can cause that composition rises and falls, but when analyzing, can not consider this part data, thereby can make quantitative test to the chemical constitution of material matrix separately.The inventive method analysis result is really accurate, good reproducibility.
Embodiment
After now the embodiment of the inventive method being described in.
Embodiment one: analyze the chemical constitution of certain steel grade with above-mentioned the inventive method, and compare with traditional chemical analytical approach result.Measurement results 1 (atomic percent) that see the following form:
The chemical constitution of certain steel grade of table 1 compares (at.%) with this method with the chemical method test result
| Alloying element | Si | Mn | Mo | Al | C | P | B | V | Nb | |
| This method | 1 | 0.65 | 1.08 | 0.16 | 0.17 | 0.047 | 0.015 | 0.016 | 0.133 | 0.015 |
| 2 | 0.75 | 1.256 | 0.17 | 0.14 | 0.036 | 0.016 | 0.013 | 0.1 | 0.019 | |
| 3 | 0.79 | 1.16 | 0.19 | 0.16 | 0.031 | 0.015 | 0.007 | 0.112 | 0.014 | |
| 4 | 0.59 | 1.048 | 0.12 | 0.20 | 0.029 | 0.007 | 0.020 | 0.123 | 0.029 | |
| Chemical method | 0.6 | 1.26 | 0.1 | 0.16 | 0.25 | 0.011 | 0.014 | 0.11 | 0.018 | |
As seen from Table 1, analyze the chemical constitution (atomic percent) of certain steel grade with the inventive method, except the C element, the result that other each elements and chemical method record is very approaching.Analyzed altogether in the present embodiment four times, repeatability is also fine.Because the C element can form carbide particle in steel, what obtain in the present embodiment is C constituent content in the matrix, so the result who obtains than chemical method is low.
Embodiment two: analyze the chemical constitution of certain aldary with above-mentioned the inventive method, and compare with the result of traditional chemical analytical approach gained.Measurement results 2 (atomic percents) that see the following form:
The chemical constitution of certain aldary of table 2 compares (at.%) with this method with the chemical method test result
| Alloying element | Fe | Ag | Cu | |
| This method | 1 | 0.87 | 0.63 | Surplus |
| 2 | 0.93 | 0.64 | Surplus | |
| 3 | 0.83 | 0.64 | Surplus | |
| 4 | 0.78 | 0.62 | Surplus | |
| 5 | 0.88 | 0.65 | Surplus | |
| Chemical method | 0.92 | 0.59 | Surplus | |
As seen from Table 2, analyze the chemical constitution (atomic percent) of certain aldary with the inventive method, very approaching with the result who records with chemical method.Analyzed altogether in the present embodiment five times, repeatability is also fine.
Claims (2)
1. method of measuring chemical ingredients in metal material matrix is characterized in that having following process and step:
A. the tip-like sample of usefulness is analyzed in preparation: earlier the metal material sample of desire test is processed into circular section or square section filament (φ＜0.5mm or＜0.5 * 0.5mm); Process with electrolytic polishing method then, its method is to inject skim electrolytic solution to swim on the bigger inert fluid of density in container, filament shape samples vertical is put into electrolytic solution carry out electropolishing, make filament produce thin neck until disconnection, obtain the tip-like sample at its length middle part; The radius-of-curvature of needle point is 10～100nm; Different metal materials adopts different electrolytic solution and voltage;
B. above-mentioned tip-like sample is put into the enterprising line data collection of three-dimensional atom probe; Pulse voltage is applied on the tip-like sample, and atom is from sample tip end surface evaporation, becomes ion and flies out and hit detector, by measuring the mass-to-charge ratio that the flight time can determine this ion, determines the element kind of flight ion; Atom is to evaporate one by one, surveys one by one, and carries out record with computing machine;
C. with computing machine all data are analyzed, when composition evenly constantly, can directly obtain in the metal material all elements chemical constitution accurately, tiny when separating out particle when existing, can obtain the interior all elements of metal material matrix chemical constitution accurately, and make quantitative test.
2. a kind of method of measuring chemical ingredients in metal material matrix according to claim 1 is characterized in that described electropolishing process, and different metal materials adopts different electrolytic solution and voltage:
(1) ferrous alloy, nickel-base alloy, niobium-base alloy, the used electrolytic solution of acieral are: the mixed liquor that the perchloric acid 10～25% of concentration 70% and glacial acetic acid 75～90% are formed; Its DC voltage is 10～25V;
(2) the used electrolytic solution of acid bronze alloy is: the mixed liquor that phosphatase 24 0%+ ethanol 20%+ sulfuric acid 5%+ thiocarbamide 5%+ water 30% is formed; Its DC voltage is 5～8V;
(3) the used electrolytic solution of tungsten-bast alloy is: the sodium hydrate aqueous solution of concentration 5%; Alternating voltage is 1～5V.
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| CN 200710038729 CN101029882A (en) | 2007-03-29 | 2007-03-29 | Method for determining chemical ingredients in metal material matrix |
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| CN 200710038729 CN101029882A (en) | 2007-03-29 | 2007-03-29 | Method for determining chemical ingredients in metal material matrix |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914628A (en) * | 2012-10-26 | 2013-02-06 | 江苏省沙钢钢铁研究院有限公司 | Method for representing center segregation of high-carbon steel wire rod |
| CN106289924A (en) * | 2015-06-29 | 2017-01-04 | 宁波江丰电子材料股份有限公司 | The display packing of metallographic structure of target |
| CN109001128A (en) * | 2018-06-29 | 2018-12-14 | 国网河南省电力公司电力科学研究院 | A kind of method of analysis of metallic materials matrix and precipitated phase Elemental partition |
| CN111044603A (en) * | 2020-01-14 | 2020-04-21 | 北京工业大学 | Method for analyzing non-metal impurity elements in high-purity molybdenum |
-
2007
- 2007-03-29 CN CN 200710038729 patent/CN101029882A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914628A (en) * | 2012-10-26 | 2013-02-06 | 江苏省沙钢钢铁研究院有限公司 | Method for representing center segregation of high-carbon steel wire rod |
| CN106289924A (en) * | 2015-06-29 | 2017-01-04 | 宁波江丰电子材料股份有限公司 | The display packing of metallographic structure of target |
| CN109001128A (en) * | 2018-06-29 | 2018-12-14 | 国网河南省电力公司电力科学研究院 | A kind of method of analysis of metallic materials matrix and precipitated phase Elemental partition |
| CN111044603A (en) * | 2020-01-14 | 2020-04-21 | 北京工业大学 | Method for analyzing non-metal impurity elements in high-purity molybdenum |
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