CN105606426A - Metallurgical analysis etching method of layered metal composite material - Google Patents
Metallurgical analysis etching method of layered metal composite material Download PDFInfo
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Abstract
The invention belongs to the technical field of metal material metallographic etching, and particularly relates to a metallurgical analysis etching method of layered metal composite material. The metallurgical analysis etching method employs electrolytic etching and chemical etching methods in order; and the microstructures of alloy components with different corrosion resistant performances in the layered metal composite material are displayed simultaneously, so as to analyze the phase composition, microstructure morphology, interface structure and grain size of components in each layer of the layered composite material.
Description
Technical field
The invention belongs to metal material etching pit technical field, particularly a kind of Metallographic Analysis corruption of laminated-metal compositeEtching method.
Background technology
Along with the appearance of scientific and technical development and various emerging technology and industry, more and more higher to the requirement of material property,The performance of single group element material is difficult to meet these demands. In recent decades, the production of laminated-metal composite, development and shouldWith the attention that is more and more subject to scientific and technological circle. Laminated-metal composite is to be formed by the metal composite of which floor different performance, with listThe alloy material of one constituent element is compared, through the material after appropriate design combination can obtain relatively high intensity, anti-corrosion, conduction,The combination property that heat conduction, magnetic conduction etc. are outstanding is also applied to the working environment of particular/special requirement. At present, laminated-metal compositeIn fields such as aerospace, oil, machinery, chemical industry, light industry, automobile, shipbuilding, building, electric power, electronics, nuclear energy and commodityObtain application.
In laminated-metal composite, the microstructure mechanics of each layer of metal material constituent element and decay resistance difference are comparativelyObviously, in detection analytic process, be difficult to demonstrate the metallographic microstructure of each layer of metal simultaneously.
Summary of the invention
The invention provides a kind of Metallographic Analysis caustic solution of laminated-metal composite, concrete technical scheme is as follows:
A Metallographic Analysis caustic solution for laminated-metal composite, adopts electrolytic etching and chemical corrosion method, successively by layerIn shape metallic composite, the discrepant alloy constituent element of decay resistance microscopic structure shows simultaneously.
Concrete steps are as follows:
(1) sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes,Machine glazed finish is to any surface finish no marking again;
(2) electrolytic etching: the sample after machine glazed finish is placed in to chromium trioxide-ethanolic solution, connects after respective electrode, carry outElectrolytic etching, adopts 1-15V voltage when corrosion, etching time 10-60s cleans and blows with clear water and absolute ethyl alcohol successively after corrosionDry;
(3) chemical attack: sample nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 10-60s, after corrosion, water and absolute ethyl alcohol clean and dry up successively.
When described electrolytic etching, in chromium trioxide-ethanolic solution used, the mass fraction of chromium trioxide is 10wt%; Chemical attackIn nitric acid-ethanolic solution of Shi Suoyong, the mass fraction of nitric acid is 4wt%-8wt%.
Layered metallic composite be austenitic stainless steel/carbon steel, martensitic stain less steel/carbon steel, ferritic stainless steel/carbon steel,Austenite-ferrite two phase stainless steel/carbon steel or nickel base superalloy/carbon steel.
General principle of the present invention is:
Low-alloy steel, carbon steel etc. belong to the poor constituent element of decay resistance, and stainless steel, titanium alloy, high temperature alloy etc. belong to corrosion resistantThe constituent element of erosion better performances, electrode potential when both corrosion resisting properties and electrolytic etching all has larger difference. When electrolytic etching,Under adopting compared with the condition of the electrolyte of strong oxidizing property and higher voltage, can realize for the group element material of good corrosion resistance equalEven corrosion and display organization, and for the poor constituent element of decay resistance, corrosion rate is exceedingly fast, can be simultaneously whole at itOn individual cross section, erode equably layer of metal, cannot display organization, form the effect that is similar to electrobrightening. Through this electricityAfter separating corrosion treatment, adopt nitric acid-ethanol to carry out chemical attack, the constituent element good for corrosion resisting property almost do not corrode work againWith, and can produce good corrosive effect for the poor metal of corrosion resisting property, and demonstrate its metallographic microstructure.
Beneficial effect of the present invention is:
Metallographic Analysis caustic solution of the present invention, combines the features of electrolytic etching and chemical attack, successively by compositeThe relatively better and poor alloy constituent element microscopic structure of middle decay resistance shows, thereby demonstrates decay resistance not simultaneouslyWith the metallographic microstructure of two kinds or more of metal group element materials, and then analyze each layer of group element material in laminar compositePhase composition, displaing micro tissue topography, interfacial structure and crystallite dimension etc.
Figure of description
Fig. 1 is the metallographic microstructure structure chart that in embodiment 2, composite obtains after electrolytic etching and chemical attack.
Fig. 2 is the metallographic microstructure structure chart that in embodiment 9, composite obtains after electrolytic etching and chemical attack.
Fig. 3 is the metallographic microstructure structure chart that in embodiment 10, composite obtains after electrolytic etching and chemical attack.
Detailed description of the invention
Embodiment 1:304 stainless steel/10# steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 2.5V voltage when corrosion, etching time 15s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of 304 stainless steel layers can be shown;
Chemical attack: sample 4wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 10s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 10# steel layer can be shown.
Embodiment 2:304 stainless steel/20G steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 2.5V voltage when corrosion, etching time 10s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of 304 stainless steel layers can be shown;
Chemical attack: sample 8wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 20s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 20G steel layer can be shown, and seeFig. 1.
Embodiment 3:316 steel/20G steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 3V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of 316 stainless steel layers can be shown;
Chemical attack: sample 8wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 20s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 20G steel layer can be shown.
Embodiment 4:GH625/10# steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 10V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of GH625 alloy-layer can be shown;
Chemical attack: sample 4wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 10s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 10# steel layer can be shown.
Embodiment 5:GH625/16Mn steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 10V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of GH625 alloy-layer can be shown;
Chemical attack: sample 6wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 30s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 16Mn steel layer can be shown;
Embodiment 6:GH625/13Cr steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 10V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of GH625 alloy-layer can be shown;
Chemical attack: sample 8wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 60s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 13Cr steel layer can be shown.
Embodiment 7:GH718/16Mn steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 5V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of GH718 alloy-layer can be shown;
Chemical attack: sample 6wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 30s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 16Mn steel layer can be shown.
Embodiment 8:GH600/16Mn steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 15V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of GH600 alloy-layer can be shown;
Chemical attack: sample 6wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 30s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 16Mn steel layer can be shown.
Embodiment 9:2205 two phase stainless steel/16Mn steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 5V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of 2205 stainless steel layers can be shown;
Chemical attack: sample 6wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 30s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 16Mn steel layer can be shown,See Fig. 2.
Embodiment 10:16Mn steel/2205 two phase stainless steel/16Mn steel laminated-metal composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 5V voltage when corrosion, etching time 50s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of 2205 stainless steel layers of centre can be shown;
Chemical attack: sample 6wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 20s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now can be by the microscopic structure of outer field two-layer 16Mn steel layerShow, see Fig. 3.
Stainless steel/316, embodiment 11:16Mn steel/304 stainless steel stratiform metallic composite
Sample preparation: sample surfaces is adopted the method processing such as line cutting, turning, milling smooth, then machinery polishes, then machineTool is polished to any surface finish no marking;
Electrolytic etching: the sample after machine glazed finish is placed in to 10wt% chromium trioxide-ethanolic solution, connects after respective electrode, enterRow electrolytic etching, adopts 4V voltage when corrosion, etching time 60s cleans and dries up with clear water and absolute ethyl alcohol successively after corrosion,Now the microscopic structure of 304 stainless steels and 316 stainless steel layers can be shown;
Chemical attack: sample 4wt% nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 30s, after corrosion, water and absolute ethyl alcohol clean and dry up successively, now the microscopic structure of 16Mn steel layer can be shown.
Claims (4)
1. a Metallographic Analysis caustic solution for laminated-metal composite, is characterized in that, adopts successively electrolytic etching and chemistryCaustic solution shows discrepant decay resistance in laminated-metal composite alloy constituent element microscopic structure simultaneously.
2. Metallographic Analysis caustic solution according to claim 1, is characterized in that, concrete steps are as follows:
(1) sample preparation: sample surfaces is processed smooth, then machinery polishes, then machine glazed finish is to any surface finish no marking;
(2) electrolytic etching: the sample after machine glazed finish is placed in to chromium trioxide-ethanolic solution, connects after respective electrode, carry outElectrolytic etching, adopts 1-15V voltage when corrosion, etching time 10-60s cleans and blows with clear water and absolute ethyl alcohol successively after corrosionDry;
(3) chemical attack: sample nitric acid-ethanolic solution that electrolytic etching is also cleaned after drying up carries out chemical attack, when corrosionBetween 10-60s, after corrosion, water and absolute ethyl alcohol clean and dry up successively.
3. Metallographic Analysis caustic solution according to claim 2, is characterized in that, chromium trioxide used when electrolytic etching-In ethanolic solution, the mass fraction of chromium trioxide is 10wt%; When chemical attack in nitric acid-ethanolic solution used, the matter of nitric acidAmount mark is 4wt%-8wt%.
4. Metallographic Analysis caustic solution according to claim 1, is characterized in that, layered metallic composite is OvshinskyBody stainless steel/carbon, martensitic stain less steel/carbon steel, ferritic stainless steel/carbon steel, austenite-ferrite two phase stainless steel/carbon steel orNickel base superalloy/carbon steel.
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| CN107389419A (en) * | 2017-06-21 | 2017-11-24 | 西安理工大学 | The corrosive liquid and deep etch method of deep etch are carried out to nickel Al-Cr-Mo eutectic lamellar |
| CN107462456A (en) * | 2016-06-03 | 2017-12-12 | 宁波江丰电子材料股份有限公司 | Method for displaying metallographic structure |
| CN109142793A (en) * | 2018-09-25 | 2019-01-04 | 天津大学 | A kind of lossless visible detection method of welding point interface microstructure |
| CN109505002A (en) * | 2018-12-10 | 2019-03-22 | 武汉工程大学 | A kind of electrochemical method controlling carbon steel crystal boundary active dissolution |
| CN109852895A (en) * | 2017-11-30 | 2019-06-07 | 中国科学院金属研究所 | A kind of high-strength and high ductility high magnetic characteristics metallic composite and its preparation |
| CN113325020A (en) * | 2021-06-24 | 2021-08-31 | 北京科技大学 | Metallographic erosion method for observing duplex stainless steel welded joint under SEM |
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| CN109852895A (en) * | 2017-11-30 | 2019-06-07 | 中国科学院金属研究所 | A kind of high-strength and high ductility high magnetic characteristics metallic composite and its preparation |
| CN109852895B (en) * | 2017-11-30 | 2021-07-02 | 中国科学院金属研究所 | High-strength high-toughness high-magnetic-performance metal composite material and preparation thereof |
| CN109142793A (en) * | 2018-09-25 | 2019-01-04 | 天津大学 | A kind of lossless visible detection method of welding point interface microstructure |
| CN109505002A (en) * | 2018-12-10 | 2019-03-22 | 武汉工程大学 | A kind of electrochemical method controlling carbon steel crystal boundary active dissolution |
| CN113325020A (en) * | 2021-06-24 | 2021-08-31 | 北京科技大学 | Metallographic erosion method for observing duplex stainless steel welded joint under SEM |
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Application publication date: 20160525 |