CN104404520B - 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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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 detection and analysis technical field, the metallographic structure etchant solution of especially a kind of high nitrogen stainless steel
And etching pit method.
Background technology
Effect in rustless steel for the nitrogen in recent years causes the very big concern of people, and addition in rustless steel for the nitrogen can be right
Its performance has a huge impact, and is mainly manifested in stainless steel base tissue, mechanical property and this several respect of corrosion resisting property.Grind
Study carefully and show that nitrogen can be stablized and expand austenite phase field, thus having a huge impact to stainless matrix.Therefore see
Examine the metallographic structure of high nitrogen steel, it is organized research nitrogen and the impact of performance is necessary.
The nitric acid ethanol of the etchant solution generally 4% of common steel grade, but it is high not reach corrosion using this kind of etchant solution
The effect of the metallographic structure of nitrogen steel.And adopt the common stainless steel described in the patent of invention of Patent No. 200810042434.2
Etchant solution and method, using Fluohydric acid., nitric acid and water mixed solution as etchant solution, the border of metallographic structure is inadequate
Clearly, the effect of tissue display is bad, and easily causes environmental pollution.
Content of the invention
The present invention provides a kind of metallographic structure etchant solution of high nitrogen stainless steel, easily prepares, nontoxic, erosion effect
Good, crystal boundary is clear, and the corrosion product producing easily rinses, and will not remain in sample surfaces, sample surfaces are pollution-free.
The technical solution used in the present invention is：
A kind of metallographic structure etchant solution of high nitrogen stainless steel, its volume proportion is as follows：
Hydrochloric acid 35 ~ 40%
Acetic acid 25 ~ 30%
Nitric acid 25 ~ 30%
Glycerol 5 ~ 10%
Preferably, hydrochloric acid, acetic acid, nitric acid and glycerol be analysis pure.
Present invention also offers the etching pit method being carried out using above-mentioned metallographic structure etchant solution, simple to operate, rotten
Erosion process control, the display effect of metallographic structure is good.
Etching pit method comprises the steps：
（1）Hydrochloric acid, acetic acid, nitric acid and glycerol are mixed in proportion, are made into etchant solution；
（2）By the sample inlayed respectively through 200#, the sand papering of 400#, 600#, 800#, 1000#, then with spray
There is the silk cloth polishing of 2.5 μm of diamond polishing agent；
（3）By in the sample immersion corrosive liquid after polishing, corrode 60～120 seconds, until sample surfaces become silver gray and are
Only, or full etchant solution is dipped in using absorbent cotton and be wiped repeatedly sample surfaces till surface becomes silver gray；
（4）After etching, deionized water rinses sample surfaces immediately, then rinses sample surfaces with dehydrated alcohol,
Dried up with compressed air afterwards, you can with its microstructure of micro- sem observation.
Preferably, in corrosive liquid hydrochloric acid, acetic acid, nitric acid and glycerol be analysis pure.
It is further preferred that step（2）Middle using pointing machine, sample is embedded in phenolic resin, mosaic technology is：Protect
Temperature is 130 DEG C, and temperature retention time is 500 seconds, using water cooling sample, after being down to room temperature, takes out sample stand-by.For some
Small sample or the sample needing observation edge, are inlayed and are necessary, and sample is conducive to after inlaying grinding
Throw the tissue being also beneficial to observe its edge.
The present invention is prepared to the metallographic sample of high nitrogen stainless steel, and using above-mentioned corrosive liquid, the sample handled well is entered
Row is processed, and finally uses the metallographic structure obtained by metallography microscope sem observation.
The intercepting of sample is pressed standard GB/T13298-1991 and is operated.
The metallographic structure etchant solution of the present invention is applied to the metallographic structure of the high nitrogen stainless steel that nitrogen content is 3%～8%
Corrosion, and need matching while using, optimal between 18～40 DEG C using temperature.
Have the beneficial effects that using produced by technique scheme：
The etchant solution of the present invention is easily prepared, nontoxic, and erosion effect is good, and crystal boundary is clear, and the corrosion producing is produced
Thing easily rinses, and will not remain in sample surfaces, and sample surfaces are pollution-free.
The caustic solution of the present invention is simple to operate, and corrosion process is controlled, and the display effect of metallographic structure is good.
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Brief description
The sample metallurgical tissue picture that Fig. 1 obtains for embodiment 1, amplification is 200 times；
The sample metallurgical tissue picture that Fig. 2 obtains for embodiment 2, amplification is 200 times；
The sample metallurgical tissue picture that Fig. 3 obtains for embodiment 3, amplification is 500 times；
The sample metallurgical tissue picture that Fig. 4 obtains for comparative example 1, amplification is 500 times.
Specific embodiment
In embodiment 1-3, the step of inlaying of sample is：Using pointing machine, sample is embedded in phenolic resin, bed setter
Skill is：Holding temperature is 130 DEG C, and temperature retention time is 500 seconds, using water cooling sample, after being down to room temperature, takes out sample stand-by.
Embodiment 1
（1）It is raw material using analytical reagent hydrochloric acid, acetic acid, nitric acid and glycerol, according to volume ratio 35：25：30：10
Ratio mixed preparing solution, standby.
（2）By the sample inlayed respectively through 200#, the sand papering of 400#, 600#, 800#, 1000#, then adopt
It is sprayed with the silk cloth polishing of 2.5 μm of diamond polishing agent；
（3）Sample after polishing is immersed in corrosive liquid and keeps 120 seconds, until sample surfaces become silver gray；
（4）After etching, deionized water rinses sample surfaces immediately, then rinses sample surfaces with dehydrated alcohol,
Dried up with compressed air afterwards, then examine under a microscope, sample metallographic structure is as shown in Figure 1.
Embodiment 2
（1）It is raw material using analytical reagent hydrochloric acid, acetic acid, nitric acid and glycerol, according to volume ratio 38：27：30：5 ratio
Example mixed preparing solution, standby.
（2）By the sample inlayed respectively through 200#, the sand papering of 400#, 600#, 800#, 1000#, then adopt
It is sprayed with the silk cloth polishing of 2.5 μm of diamond polishing agent；
（3）Sample after polishing is immersed in corrosive liquid and keeps 60 seconds, until sample surfaces become silver gray；
（4）After etching, deionized water rinses sample surfaces immediately, then rinses sample surfaces with dehydrated alcohol,
Dried up with compressed air afterwards, then examine under a microscope, sample metallographic structure is as shown in Figure 2.
Embodiment 3
（1）It is raw material using analytical reagent hydrochloric acid, acetic acid, nitric acid and glycerol, be 40 according to volume ratio：30：25：5
Ratio mixed preparing solution, standby.
（2）By the sample inlayed respectively through 200#, the sand papering of 400#, 600#, 800#, 1000#, then adopt
It is sprayed with the silk cloth polishing of 2.5 μm of diamond polishing agent；
（3）Full etchant solution is dipped in using absorbent cotton and is wiped repeatedly the sample surfaces after polishing until surface becomes silver gray and is
Only；
（4）After etching, deionized water rinses sample surfaces immediately, then rinses sample surfaces with dehydrated alcohol,
Dried up with compressed air afterwards, then examine under a microscope, sample metallographic structure is as shown in Figure 3.
Comparative example 1
Method according to corroding austenitic stainless steel in the patent of the patent No. 200810042434.2 to prepare sample.Using
Analytically pure Fluohydric acid., nitric acid and water are raw material, according to Fluohydric acid.：Nitric acid：Water=2：1：7 volume ratio mixed preparing solution
Standby, the preparation of sample is similar to Example 1 with corrosion process, and the metallographic structure of sample is as shown in Figure 4.
From Fig. 1-4, compared with the metallographic structure corroding out in comparative example 1, method in embodiment 1-3 is by high nitrogen
The metallographic structure of steel corrodes out completely, and crystal boundary is relatively sharp, and corrosive effect is more preferable.
Claims (3)
1. a kind of metallographic structure etchant solution of high nitrogen stainless steel is it is characterised in that its volume proportion is as follows：
Hydrochloric acid 35-40%
Acetic acid 25-30%
Nitric acid 25-30%
Glycerol 5-10%；
It is pure that described hydrochloric acid, acetic acid, nitric acid and glycerol are analysis.
2. a kind of etching pit method that metallographic structure etchant solution using high nitrogen stainless steel described in claim 1 is carried out, its
It is characterised by comprising the steps：
（1）Hydrochloric acid, acetic acid, nitric acid and glycerol are mixed in proportion, are made into etchant solution；
（2）By the sample inlayed respectively through 200#, the sand papering of 400#, 600#, 800#, 1000#, then with being sprayed with
The silk cloth polishing of 2.5 μm of diamond polishing agent；
（3）By in the sample immersion corrosive liquid after polishing, corrode 60～120 seconds, till sample surfaces become silver gray, or
Person dips in full etchant solution using absorbent cotton and is wiped repeatedly sample surfaces till surface becomes silver gray；
（4）After etching, deionized water rinses sample surfaces immediately, then rinses sample surfaces with dehydrated alcohol, finally uses
Compressed air dries up, you can with its microstructure of micro- sem observation；
Described high nitrogen stainless steel is the high nitrogen stainless steel that nitrogen content is 3%～8%, metallographic structure etchant solution matching while using, uses
Temperature is between 18～40 DEG C.
3. etching pit method according to claim 2 is it is characterised in that described step（2）Middle employing pointing machine is by sample
It is embedded in phenolic resin, mosaic technology is：Holding temperature is 130 DEG C, and temperature retention time is 500 seconds, using water cooling sample, drops
To room temperature, take out sample stand-by.
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| 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 |
| 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 |
| CN108004549B (en) * | 2018-01-05 | 2020-07-10 | 华北电力科学研究院有限责任公司 | Metallographic etchant and etching method for ferrite/austenite dissimilar steel welded joint |
| CN109746771B (en) * | 2019-02-14 | 2020-11-20 | 南京航空航天大学 | CsPbX3Polishing method of inorganic perovskite crystal material |
| CN110672397B (en) * | 2019-09-16 | 2022-05-27 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for aluminum-silicon coated steel plate |
| CN111024594B (en) * | 2019-11-20 | 2022-06-14 | 广州航海学院 | Observation method for metal material corroded by microorganism adhesion |
| CN112695323B (en) * | 2020-12-10 | 2023-06-02 | 广西北港新材料有限公司 | Metallographic etching solution for austenitic stainless steel cold-rolled sheet and sample etching method |
| 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 |
| 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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| US3753817A (en) * | 1971-07-16 | 1973-08-21 | Driver Co W | Method for processing wire |
| CN101034044A (en) * | 2007-04-06 | 2007-09-12 | 王训宏 | Preparation method for metallic phase sample of 1060 aluminium plate and MB3 magnesium alloy palate join |
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