CN101655426A - Electrochemical metallographic etching method universal for nickel-based alloys - Google Patents
Electrochemical metallographic etching method universal for nickel-based alloys Download PDFInfo
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- CN101655426A CN101655426A CN200910092655A CN200910092655A CN101655426A CN 101655426 A CN101655426 A CN 101655426A CN 200910092655 A CN200910092655 A CN 200910092655A CN 200910092655 A CN200910092655 A CN 200910092655A CN 101655426 A CN101655426 A CN 101655426A
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- 238000005530 etching Methods 0.000 title claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 28
- 239000000956 alloy Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 6
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims abstract description 6
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011187 glycerol Nutrition 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 11
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000003486 chemical etching Methods 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 229910017060 Fe Cr Inorganic materials 0.000 abstract description 2
- 229910002544 Fe-Cr Inorganic materials 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 238000005498 polishing Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000002848 electrochemical method Methods 0.000 description 4
- 229910001026 inconel Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000010892 electric spark Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 235000013312 flour Nutrition 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000000059 patterning Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229910001293 incoloy Inorganic materials 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001040 Beta-titanium Inorganic materials 0.000 description 1
- 206010027146 Melanoderma Diseases 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
本发明公开了一种镍基合金普适的电化学金相浸蚀方法，涉及金属材料金相组织的电化学浸蚀。本发明采用电化学金相浸蚀法，以此浸蚀液为导电介质，以待观测金相试样为阳极，以铂电极为阴极，控制浸蚀条件为：浸蚀电压恒压：2V/cm2－8V/cm2，浸蚀时间：1min－5min，其浸蚀液按重量百分比计含有：磷酸65％－85％，硫酸5％－15％，铬酸8％－15％，甘油3％－8％，制得的G－3,825，X750等高温耐蚀镍基合金金相图片表面平整，晶界分明，晶粒清晰。相比化学浸蚀方法，本发明实验条件容易控制，实验重复性好，实验效率高，适用于Ni－Fe－Cr系合金。
The invention discloses a universal electrochemical metallographic etching method for nickel-based alloys, which relates to the electrochemical etching of the metallographic structure of metal materials. The present invention adopts the electrochemical metallographic etching method, with the etching solution as the conductive medium, the metallographic sample to be observed as the anode, and the platinum electrode as the cathode, and the control etching conditions are: etching voltage constant voltage: 2V/ cm 2 -8V/cm 2 , etching time: 1min-5min, the etching solution contains: phosphoric acid 65%-85%, sulfuric acid 5%-15%, chromic acid 8%-15%, glycerin 3 %-8%, the prepared G-3,825, X750 and other high-temperature corrosion-resistant nickel-based alloys have smooth surfaces, clear grain boundaries, and crystal grains. Compared with the chemical etching method, the present invention is easy to control the experimental conditions, has good experimental repeatability and high experimental efficiency, and is suitable for Ni-Fe-Cr alloys.
Description
Technical field
The present invention is a kind of electrochemical etching method that relates to the metal material metallographic structure.
Background technology
During electrochemical etching, processed sample as anode, is added the voltage of certain intensity between anode and cathode, anode sample dissolution then, crystal grain and grain boundary expose out, thereby can obtain the picture of metallographic structure.Its mechanism of generally acknowledging is to form one deck polarized film on the metal anode surface, make metallic ion pass through this layer film diffusion, the height point at lip-deep micro-and macroscopical salient point or coarse place and the current density specific surface remainder in burr district are big, and with fast speeds dissolving, thereby reach the purpose of leveling and deburring.Can regulate the crystal grain dissolution velocity by experiment conditions such as control polishing time, experimental temperature and current densities, obtain surface clean, crystal boundary is the metallographic structure photo clearly.
Nickel-base alloy is widely used in the deep-etching Service Environment such as oil and natural gas because of its excellent corrosion resistance and outstanding physical and mechanical properties.But the problem that incident its metallographic is difficult for making has brought a difficult problem for our the optimization research work of material.CN1167839 discloses a kind of patented claim of metallographic etching agent, is applicable to the etching pit of high copper-titanium alloy (C u content weight ratio is greater than 10%).CN101104935 discloses a kind of patented claim of metallographic etching agent, is done and water is formed by hydrofluorite, nitric acid, acetone, acetic acid.Adopt it can make metallographic observation face light, the metallographic structure crystal boundary is clear, tells α phase or other precipitated phase that disperse is separated out easily, is particularly suitable for the metallographic etching agent as the nearly β of aging state, metastable beta-titanium alloy.Yet adopt the chemical method etch for nickel-base alloy, its metallographic is often wayward because of the etch time, and causes gained metallographic readability not good enough, and prepared metallographic structure is difficult to differentiate; The research of the electrochemical etching aspect of nickel-base alloy rarely has report, therefore has a large amount of blank to remain to be filled in this field.
Summary of the invention
The object of the present invention is to provide a kind of electrochemical metallographic etching method of universal for nickel-based alloys, make the oxidation of nickel-base alloy corrosion-resistant easy, thereby obtain the metallographic structure of nickel-base alloy easily, sharpness is higher simultaneously.
Electrochemical metallographic etching method of the present invention is a conducting medium with metallographic etching liquid, is anode with the nickel-base alloy metallographic specimen, is negative electrode with the platinum electrode, and the etch condition is: etch voltage constant voltage 2V/cm
2-8V/cm
2, etch time 1min-5min.
Metallographic etching liquid involved in the present invention is by weight percentage: contain phosphoric acid 65%-85%, sulfuric acid 5%-15%, chromic acid 8%-15%, glycerine 3%-8%.
The G-3 that the present invention makes, 825, high temperature ni-resist base alloy metallograph surfacings such as X750, crystal boundary is clearly demarcated, and crystal grain is clear, is applicable to that Ni-Fe-Cr is an alloy.
The compound method of this electrochemical metallographic etching liquid is simple, and effect is remarkable.Compare chemical metallographic etching method, the easier control of electrochemical method condition, experimental repeatability is good, and the metallograph that makes is clear.
Description of drawings
The metallographic pattern that Fig. 1 etching solution chemical etching that to be nickel-base alloy INCONEL alloy G-3 form with 10g iron chloride+30ml concentrated hydrochloric acid+20ml water obtains.
The metallographic pattern that Fig. 2 etching solution chemical etching that to be nickel-base alloy INCONEL alloy G-3 form with 5ml nitric acid+25ml concentrated hydrochloric acid+30ml water obtains.
The metallographic pattern that Fig. 3 etching solution that to be nickel-base alloy INCONEL alloy G-3 form with 30ml sulfuric acid+20ml water obtains with the electrochemical etching method.
Fig. 4 is the metallographic pattern of embodiment 1.
Fig. 5 is the metallographic pattern of embodiment 2.
Fig. 6 is the metallographic pattern of embodiment 3.
Embodiment
With reference to the accompanying drawings and in conjunction with example the present invention and implementation result are further described below.
Embodiment 1: in the sampling of G-3 alloy oil pipe outside surface, it is carried out the experiment of electrochemical method etch metallographic
1, parallels to the axis at G-3 oil pipe outside surface with the electric spark patterning method that to cut area be 1x1cm to direction
2, thickness is the square sample of 2mm.
2, at sample back side welding lead, be panel with ethylenediamine-epoxy resin then, inlay sample.Encapsulation makes the cylindricality sample that radius is 20mm.
3, polish sample step by step to its smooth surface with waterproof abrasive paper, and remove the polishing scratch that stays by fine grinding on the metallographic specimen flour milling, become smooth flawless minute surface with mechanical polishing method.
4, metallographic etching liquid adopts prescription involved in the present invention to be: phosphoric acid 65%, sulfuric acid 15%, chromic acid 15%, glycerine 5% (percentage by weight).
5, adopting the constant voltage/constant current source is the decomposition voltage source.Experimental sample links to each other with positive source, and power cathode connects platinum electrode.With this metallographic etching liquid is conducting medium, connects electrochemical etching metallographic device.Control etch condition constant voltage is 4.5V/cm
2, the etch time is 2min.Make G-3 oil pipe outside surface metallograph as shown in Figure 4.
Embodiment 2: in the sampling of G-3 alloy pipe inner surface, it is carried out the experiment of electrochemical method etch metallographic
1, parallels to the axis at the G-3 pipe inner surface with the electric spark patterning method that to cut area be 1x1cm to direction
2, thickness is the square sample of 2mm.
2, at sample back side welding lead, be panel with ethylenediamine-epoxy resin then, inlay sample.Encapsulation makes the cylindricality sample that radius is 20mm.
3, polish sample step by step until its smooth surface with waterproof abrasive paper, and remove the polishing scratch that stays by fine grinding on the metallographic specimen flour milling, become smooth flawless minute surface with mechanical polishing method.
4, metallographic etching liquid adopts prescription involved in the present invention to be: phosphoric acid 84%, sulfuric acid 5%, chromic acid 8%, glycerine 3% (percentage by weight).
5, adopting the constant voltage/constant current source is the decomposition voltage source.Experimental sample links to each other with positive source, and power cathode connects platinum electrode.With this metallographic etching liquid is conducting medium, connects electrochemical etching metallographic device.Control etch condition constant voltage is 6V/cm
2, the etch time is 1.5min.Make G-3 oil pipe outside surface metallograph as shown in Figure 5.
Embodiment 3: in the sampling of Incoloy 825 alloy oil pipe outside surfaces, adopt the present invention that it is carried out the experiment of electrochemical method etch metallographic
1, parallel to the axis at Incoloy 825 oil pipe outside surfaces with the electric spark patterning method that to cut area be 1x1cm2 to direction, thickness is the square sample of 2mm.
2, at sample back side welding lead, be panel with ethylenediamine-epoxy resin then, inlay sample.Encapsulation makes the cylindricality sample that radius is 20mm.
3, polish sample step by step until its smooth surface with waterproof abrasive paper, and remove the polishing scratch that stays by fine grinding on the metallographic specimen flour milling, become smooth flawless minute surface with mechanical polishing method.
4, metallographic etching liquid adopts prescription involved in the present invention to be: phosphoric acid 65%, sulfuric acid 5%, chromic acid 15%, glycerine 15% (percentage by weight).
5, adopting the constant voltage/constant current source is the decomposition voltage source.Experimental sample links to each other with positive source, and power cathode connects platinum electrode.With this metallographic etching liquid is conducting medium, connects electrochemical etching metallographic device.Control etch condition constant voltage is 3.5V/cm
2, the etch time is 3min.Make G-3 oil pipe outside surface metallograph as shown in Figure 6.
For detecting the invention process effect, select etch nickel-base alloy Inconel Alloy G-3 metallographic to be the contrast experiment, condition is respectively 10g iron chloride+30ml concentrated hydrochloric acid+20ml water, chemical etching, as shown in Figure 1; 5ml nitric acid+25ml concentrated hydrochloric acid+30ml water, chemical etching, as shown in Figure 2; 30ml sulfuric acid+20ml water, electrochemical etching, as shown in Figure 3.
Fig. 4 that embodiment 1-3 obtains-Fig. 6 comparison diagram 1, Fig. 2, it is clear obviously to find out through grain boundary in the prepared metallograph of electrochemical etching method, tissue topography can be complete present, and eliminated simple chemical etching method because the etch time is difficult to grasp the defective of the peroxidating (stain, blackspot) that is occurred.Comparison diagram 3, the electrochemical etching liquor ratio sulfuric acid of being announced among the present invention as can be seen are that etching solution has more excellent metallographic and prepares effect.To sum up, the present invention a kind ofly has the electrochemical metallographic etching method that good metallographic structure prepares effect for nickel-base alloy.
Claims (1)
1, a kind of electrochemical metallographic etching method of universal for nickel-based alloys is characterized in that, adopts the electrochemical metallographic etching method, with metallographic etching liquid is conducting medium, with the nickel-base alloy metallographic specimen is anode, is negative electrode with the platinum electrode, and the etch condition is: etch voltage constant voltage 2V/cm
2-8V/cm
2, etch time 1min-5min.
Described metallographic etching liquid contains phosphoric acid 65%-85% by weight percentage, sulfuric acid 5%-15%, chromic acid 8%-15%, glycerine 3%-8%.
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| CN103196733A (en) * | 2013-04-01 | 2013-07-10 | 东方电气集团东方汽轮机有限公司 | Etchant for displaying metallographic structure of nickel-based high temperature alloy and method |
| CN103451714A (en) * | 2013-09-09 | 2013-12-18 | 昆山奥德鲁自动化技术有限公司 | Electrochemical renovation treatment technology for cutting tool |
| CN103808542A (en) * | 2012-11-10 | 2014-05-21 | 有研亿金新材料股份有限公司 | Method for preparing nickel-platinum alloy metallographic phase sample and displaying sample tissue |
| CN103822817A (en) * | 2014-02-28 | 2014-05-28 | 金川集团股份有限公司 | Pure nickel chemical polishing etching solution and application method |
| CN104977247A (en) * | 2015-06-15 | 2015-10-14 | 河南航天精工制造有限公司 | Metal streamline corrosion method |
| CN106757299A (en) * | 2016-12-15 | 2017-05-31 | 上海电气核电设备有限公司 | The electrobrightening corrosive agent and its application method of a kind of nickel-base alloy metallographic structure |
| CN108051441A (en) * | 2017-11-29 | 2018-05-18 | 西部金属材料股份有限公司 | A kind of observation procedure of Fe-Ni-Cr alloy microstructure |
| CN109540634A (en) * | 2018-11-20 | 2019-03-29 | 中国航发贵州黎阳航空动力有限公司 | A kind of detection method for GH4648 sheet coupon crystal grain and microscopic structure |
| CN110670115A (en) * | 2019-09-30 | 2020-01-10 | 飞而康快速制造科技有限责任公司 | Corrosive agent suitable for deposited GH3536 alloy and corrosion method thereof |
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| CN1080333A (en) * | 1992-10-06 | 1994-01-05 | 云南五环工业设计研究所 | A kind of electrolytic etching method of metal test-piece |
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| CN113758783A (en) * | 2021-08-11 | 2021-12-07 | 重庆材料研究院有限公司 | Method for displaying metallographic structure of platinum |
| CN113702379A (en) * | 2021-08-27 | 2021-11-26 | 华能国际电力股份有限公司 | Metallographic corrosion method for displaying homogenized structure of high-alloying nickel-based alloy |
| CN113702379B (en) * | 2021-08-27 | 2023-09-01 | 华能国际电力股份有限公司 | A Metallographic Corrosion Method for Displaying the Homogenized Microstructure of Highly Alloyed Nickel-Based Alloys |
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| CN113862677B (en) * | 2021-09-18 | 2023-11-14 | 北京星航机电装备有限公司 | GH4220 high-temperature alloy metallographic structure corrosive and corrosion method |
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