CN104404520A - Metallographic structure etching solution of high-nitrogen stainless steel and metallographic etching method - Google Patents
Metallographic structure etching solution of high-nitrogen stainless steel and metallographic etching method Download PDFInfo
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- CN104404520A CN104404520A CN201410656446.XA CN201410656446A CN104404520A CN 104404520 A CN104404520 A CN 104404520A CN 201410656446 A CN201410656446 A CN 201410656446A CN 104404520 A CN104404520 A CN 104404520A
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Abstract
The invention discloses metallographic structure etching solution of high-nitrogen stainless steel. The metallographic structure etching solution comprises the following constituents in percent by volume: 35 to 40 percent of hydrochloric acid, 25 to 30 percent of acetic acid, 25 to 30 percent of nitric acid, and 5 to 10 percent of glycerinum. An etching method comprises the following steps: firstly, preparing the etching solution, secondly, sanding and polishing an embedded sample, thirdly, immersing the polished sample into the etching solution to etch the sample till the surface of the sample becomes silver gray, or repeatedly wiping the surface of the sample with degreasing cotton dipped with the etching solution till the surface of the sample becomes silver gray; fourthly, washing the surface of the sample through deionized water immediately after etching, then washing the surface of the sample through absolute ethyl alcohol, finally drying the surface of the sample through compressed air, and observing a microstructure through a microscope. The etching solution is easy to prepare, nontoxic and harmless, good in etching effect and clear in crystal boundary; the etching method is simple to operate, the etching process is controllable, and the display effect of a metallographic structure is good.
Description
Technical field
The present invention relates to metallographic and detect analysis technical field, especially a kind of metallographic structure etchant solution of high nitrogen stainless steel and etching pit method.
Background technology
The effect of nitrogen in stainless steel in recent years causes the very large concern of people, and nitrogen can have a huge impact its performance adding in stainless steel, is mainly manifested in these several respects of stainless steel-based body tissue, mechanical property and corrosion resisting property.Research shows that nitrogen can be stablized and expand austenite phase field, thus has a huge impact stainless matrix.Therefore observe the metallographic structure of high nitrogen steel, the impact of research nitrogen element on its structure and properties is necessary.
The etchant solution of common steel grade is generally the nitric acid alcohol of 4%, but adopts this kind of etchant solution not reach the effect of the metallographic structure of corroding high nitrogen steel.And the etchant solution adopting the patent No. to be the common stainless steel described in the patent of invention of 200810042434.2 and method, adopt the mixing solutions of hydrofluoric acid, nitric acid and water as etchant solution, the border of metallographic structure is clear not, the effect of tissue display is bad, and easily causes environmental pollution.
Summary of the invention
The invention provides a kind of metallographic structure etchant solution of high nitrogen stainless steel, easily prepare, nontoxic, erosion effect is good, and crystal boundary is clear, and the corrosion product produced easily rinses, and can not remain in sample surfaces, sample surfaces is pollution-free.
The technical solution used in the present invention is:
A metallographic structure etchant solution for high nitrogen stainless steel, its volume proportion is as follows:
Hydrochloric acid 35 ~ 40%
Acetic acid 25 ~ 30%
Nitric acid 25 ~ 30%
Glycerine 5 ~ 10%
Preferably, hydrochloric acid, acetic acid, nitric acid and glycerine are analytical pure.
Present invention also offers the etching pit method utilizing above-mentioned metallographic structure etchant solution to carry out, simple to operate, corrosion process is controlled, and the display effect of metallographic structure is good.
Etching pit method comprises the steps:
(1) hydrochloric acid, acetic acid, nitric acid and glycerine are mixed in proportion, are made into etchant solution;
(2) by the sand papering respectively through 200#, 400#, 600#, 800#, 1000# of the sample inlayed, then with the silk cloth polishing being sprayed with 2.5 μm of diamond polishing agent;
(3) immersed in corrosive fluid by the sample after polishing, corrode 60 ~ 120 seconds, till sample surfaces becomes silver gray, or wipe samples is surperficial till surface becomes silver gray repeatedly to adopt absorbent cotton to dip in full etchant solution;
(4) use deionized water rinsing sample surfaces immediately after etching, then rinse sample surfaces with dehydrated alcohol, finally dry up with pressurized air, be i.e. its microtexture of available microscopic examination.
Preferably, in corrosive fluid, hydrochloric acid, acetic acid, nitric acid and glycerine are analytical pure.
Preferred further, adopt pointing machine to be embedded in resol by sample in step (2), inlay is: holding temperature is 130 DEG C, and soaking time is 500 seconds, adopts water cooling sample, after being down to room temperature, takes out sample stand-by.For some small samples or the sample needing observation edge, inlayed and be necessary, sample is conducive to the tissue that grinding and polishing is also conducive to observing its edge after inlaying.
The metallographic sample of the present invention to high nitrogen stainless steel is prepared, and utilizes above-mentioned corrosive fluid to process the sample handled well, finally with the metallographic structure that metallography microscope sem observation gained arrives.
The intercepting of sample is by standard GB/T13298-1991 operation.
Metallographic structure etchant solution of the present invention is applicable to the corrosion that nitrogen content is the metallographic structure of the high nitrogen stainless steel of 3% ~ 8%, and needs matching while using, and use temperature is best between 18 ~ 40 DEG C.
The beneficial effect adopting technique scheme to produce is:
Etchant solution of the present invention is easily prepared, nontoxic, and erosion effect is good, and crystal boundary is clear, and the corrosion product produced easily rinses, and can not remain in sample surfaces, sample surfaces is pollution-free.
Caustic solution of the present invention is simple to operate, and corrosion process is controlled, and the display effect of metallographic structure is good.
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Accompanying drawing explanation
Fig. 1 is the sample metallurgical tissue picture that embodiment 1 obtains, and magnification is 200 times;
Fig. 2 is the sample metallurgical tissue picture that embodiment 2 obtains, and magnification is 200 times;
Fig. 3 is the sample metallurgical tissue picture that embodiment 3 obtains, and magnification is 500 times;
Fig. 4 is the sample metallurgical tissue picture that comparative example 1 obtains, and magnification is 500 times.
Embodiment
In embodiment 1-3, the step of inlaying of sample is: adopt pointing machine to be embedded in resol by sample, inlay is: holding temperature is 130 DEG C, and soaking time is 500 seconds, adopts water cooling sample, after being down to room temperature, takes out sample stand-by.
Embodiment 1
(1) analytical reagent hydrochloric acid, acetic acid, nitric acid and glycerine is adopted to be raw material, according to the ratio mixed preparing solution of volume ratio 35:25:30:10, for subsequent use.
(2) by the sand papering respectively through 200#, 400#, 600#, 800#, 1000# of the sample inlayed, the silk cloth polishing being sprayed with 2.5 μm of diamond polishing agent is then adopted;
(3) sample after polishing to be immersed in corrosive fluid and to keep 120 seconds, until sample surfaces becomes silver gray;
(4) use deionized water rinsing sample surfaces immediately after etching, then rinse sample surfaces with dehydrated alcohol, finally dry up with pressurized air, then examine under a microscope, sample metallographic structure as shown in Figure 1.
Embodiment 2
(1) analytical reagent hydrochloric acid, acetic acid, nitric acid and glycerine is adopted to be raw material, according to the ratio mixed preparing solution of volume ratio 38:27:30:5, for subsequent use.
(2) by the sand papering respectively through 200#, 400#, 600#, 800#, 1000# of the sample inlayed, the silk cloth polishing being sprayed with 2.5 μm of diamond polishing agent is then adopted;
(3) sample after polishing to be immersed in corrosive fluid and to keep 60 seconds, until sample surfaces becomes silver gray;
(4) use deionized water rinsing sample surfaces immediately after etching, then rinse sample surfaces with dehydrated alcohol, finally dry up with pressurized air, then examine under a microscope, sample metallographic structure as shown in Figure 2.
Embodiment 3
(1) adopting analytical reagent hydrochloric acid, acetic acid, nitric acid and glycerine to be raw material, is the ratio mixed preparing solution of 40:30:25:5 according to volume ratio, for subsequent use.
(2) by the sand papering respectively through 200#, 400#, 600#, 800#, 1000# of the sample inlayed, the silk cloth polishing being sprayed with 2.5 μm of diamond polishing agent is then adopted;
(3) absorbent cotton is adopted to dip in the sample surfaces of full etchant solution repeatedly after wiping polishing till surface becomes silver gray;
(4) use deionized water rinsing sample surfaces immediately after etching, then rinse sample surfaces with dehydrated alcohol, finally dry up with pressurized air, then examine under a microscope, sample metallographic structure as shown in Figure 3.
Comparative example 1
The method of austenitic stainless steel is corroded to prepare sample in patent according to the patent No. 200810042434.2.Analytically pure hydrofluoric acid, nitric acid and water is adopted to be raw material, according to hydrofluoric acid: nitric acid: the volume ratio mixed preparing solution for standby of water=2:1:7, preparation and the corrosion process of sample are similar to Example 1, and the metallographic structure of sample as shown in Figure 4.
From Fig. 1-4, compared with the metallographic structure of corroding out in comparative example 1, the metallographic structure of high nitrogen steel corrodes out by method in embodiment 1-3 completely, and crystal boundary is more clear, and corrosive effect is better.
Claims (5)
1. a metallographic structure etchant solution for high nitrogen stainless steel, is characterized in that its volume proportion is as follows:
Hydrochloric acid 35 ~ 40%
Acetic acid 25 ~ 30%
Nitric acid 25 ~ 30%
Glycerine 5 ~ 10%.
2. the metallographic structure etchant solution of a kind of high nitrogen stainless steel according to claim 1, is characterized in that described hydrochloric acid, acetic acid, nitric acid and glycerine are analytical pure.
3. the etching pit method utilizing metallographic structure etchant solution described in claim 1 to carry out, is characterized in that comprising the steps:
(1) hydrochloric acid, acetic acid, nitric acid and glycerine are mixed in proportion, are made into etchant solution;
(2) by the sand papering respectively through 200#, 400#, 600#, 800#, 1000# of the sample inlayed, then with the silk cloth polishing being sprayed with 2.5 μm of diamond polishing agent;
(3) immersed in corrosive fluid by the sample after polishing, corrode 60 ~ 120 seconds, till sample surfaces becomes silver gray, or wipe samples is surperficial till surface becomes silver gray repeatedly to adopt absorbent cotton to dip in full etchant solution;
(4) use deionized water rinsing sample surfaces immediately after etching, then rinse sample surfaces with dehydrated alcohol, finally dry up with pressurized air, be i.e. its microtexture of available microscopic examination.
4. etching pit method according to claim 3, is characterized in that in described corrosive fluid, hydrochloric acid, acetic acid, nitric acid and glycerine are analytical pure.
5. etching pit method according to claim 3, it is characterized in that adopting pointing machine to be embedded in resol by sample in described step (2), inlay is: holding temperature is 130 DEG C, soaking time is 500 seconds, adopt water cooling sample, after being down to room temperature, take out sample stand-by.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513985A (en) * | 2014-12-10 | 2015-04-15 | 金川集团股份有限公司 | Nickel-chromium alloy metallographic corrosion solution and corrosion method |
| CN106596217A (en) * | 2016-11-16 | 2017-04-26 | 河钢股份有限公司 | Metallographic corrosive agent of high nitrogen stainless steel and metallographic structure display method |
| CN106872317A (en) * | 2017-02-20 | 2017-06-20 | 中国电子产品可靠性与环境试验研究所 | The preprocess method and measuring method of soft magnetic ferrite crystallite dimension measurement |
| CN108004549A (en) * | 2018-01-05 | 2018-05-08 | 华北电力科学研究院有限责任公司 | The metallographic etchant and caustic solution of ferrite/austenite Dissimilar Steel Welded Joint |
| CN108181308A (en) * | 2017-12-11 | 2018-06-19 | 崇义章源钨业股份有限公司 | The method for displaying metallographic structure of metal powder |
| CN109746771A (en) * | 2019-02-14 | 2019-05-14 | 南京航空航天大学 | A kind of CsPbX3The polishing method of inorganic perovskite crystalline material |
| CN110672397A (en) * | 2019-09-16 | 2020-01-10 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for aluminum-silicon coated steel plate |
| CN111024594A (en) * | 2019-11-20 | 2020-04-17 | 广州航海学院 | Observation method for metal material corroded by microorganism adhesion |
| CN112695323A (en) * | 2020-12-10 | 2021-04-23 | 广西北部湾新材料有限公司 | Metallographic etchant for austenitic stainless steel cold-rolled sheet and sample corrosion method |
| CN113588363A (en) * | 2021-07-23 | 2021-11-02 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for iron-aluminum-silicon layer of aluminum-silicon coated steel plate |
| CN113862677A (en) * | 2021-09-18 | 2021-12-31 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513985A (en) * | 2014-12-10 | 2015-04-15 | 金川集团股份有限公司 | Nickel-chromium alloy metallographic corrosion solution and corrosion method |
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| CN106872317A (en) * | 2017-02-20 | 2017-06-20 | 中国电子产品可靠性与环境试验研究所 | The preprocess method and measuring method of soft magnetic ferrite crystallite dimension measurement |
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| CN108004549A (en) * | 2018-01-05 | 2018-05-08 | 华北电力科学研究院有限责任公司 | The metallographic etchant and caustic solution of ferrite/austenite Dissimilar Steel Welded Joint |
| CN109746771A (en) * | 2019-02-14 | 2019-05-14 | 南京航空航天大学 | A kind of CsPbX3The polishing method of inorganic perovskite crystalline material |
| CN110672397A (en) * | 2019-09-16 | 2020-01-10 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for aluminum-silicon coated steel plate |
| CN111024594A (en) * | 2019-11-20 | 2020-04-17 | 广州航海学院 | Observation method for metal material corroded by microorganism adhesion |
| CN111024594B (en) * | 2019-11-20 | 2022-06-14 | 广州航海学院 | Observation method for metal material corroded by microorganism adhesion |
| CN112695323A (en) * | 2020-12-10 | 2021-04-23 | 广西北部湾新材料有限公司 | Metallographic etchant for austenitic stainless steel cold-rolled sheet and sample corrosion method |
| CN113588363A (en) * | 2021-07-23 | 2021-11-02 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for iron-aluminum-silicon layer of aluminum-silicon coated steel plate |
| CN113588363B (en) * | 2021-07-23 | 2023-10-31 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for iron-aluminum-silicon layer of aluminum-silicon coated steel plate |
| CN113862677A (en) * | 2021-09-18 | 2021-12-31 | 北京星航机电装备有限公司 | GH4220 high-temperature alloy metallographic structure corrosive and corrosion method |
| 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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