CN103712844A - Corrosion method for displaying Cr13-type martensitic stainless steel grain size - Google Patents
Corrosion method for displaying Cr13-type martensitic stainless steel grain size Download PDFInfo
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- CN103712844A CN103712844A CN201310689268.6A CN201310689268A CN103712844A CN 103712844 A CN103712844 A CN 103712844A CN 201310689268 A CN201310689268 A CN 201310689268A CN 103712844 A CN103712844 A CN 103712844A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a corrosion method for displaying a Cr13-type martensitic stainless steel grain size. The method comprises the following steps of firslyt preparing a corrosive by utilizing 100ml of saturated bitter acid solution and 0.2 to 1.5ml of HCl solution, washing and drying a ground and polished Cr13-type martensitic stainless steel sample, immersing the washed and dried Cr13-type martensitic stainless steel sample into the corrosive with the detection surface of the sample facing upwards for 20s to 40s, and taking out the sample when the detection surface is dark yellow; washing the detection surface by utilizing 10% oxalic acid aqueous solution, and washing the entire sample and drying the sample by utilizing flowing water when the detection surface is grey white. The corrosion method is mainly used for corroding the Cr13-type martensitic stainless steel. By adopting the corrosion method, the grain size of the Cr13-type martensitic stainless steel can be clearly observed under the optical microscope.
Description
Technical field
The present invention relates to a kind of caustic solution that shows stainless steel grain size, particularly related to a kind of caustic solution of the Cr13 of demonstration type martensitic stain less steel grain size.
Background technology
Martensitic stain less steel is stainless a kind of, different according to condition of heat treatment, under use state, be generally tempered martensite, tempered sorbite, ferrite, carbonide and/or retained austenite etc., it contains 12%～17% chromium, makes steel have good corrosion resistance and inoxidizability.In the present invention, by chromium content, the stainless steel such as the 1Cr13 between 12%～14%, 2Cr13 is called Cr13 type martensitic stain less steel.Because stainless steel can not fully show its tissue signature and organize details because of its fine corrosion resistance, general mordant, and the crystal boundary of Cr13 martensitic stain less steel and intracrystalline martensitic stucture corrosivity more approaching, be difficult to by its grain size of the clear demonstration of simple caustic solution.
At present, be mainly to adopt metallography microscope sem observation martensitic phase position to judge the grain size of Cr13 type martensitic stain less steel.But in check, adopt said method precision not high at the scene, cannot use resection in GB/T6394 to remove to evaluate accurately grain size number.Therefore, demand provides a kind of mordant and caustic solution that can show clearly martensitic stucture crystal boundary, makes can observe the grain size of Cr13 type martensitic stain less steel under optical microscope.
On January 23rd, 2013, disclosed Chinese invention patent instructions CN102888608A disclosed a kind of mordant that shows fine grained austenite stainless steel crystal boundary and preparation method thereof, and this mordant comprises: H
2o:80～150ml; Hydrochloric acid: 10～20ml; FeCl
3: 15～25g; CuCl
22H
2o:10～15g; Glacial acetic acid: 2.0～7.0ml; New gill goes out: 1～5.Preparation method is: first by CuCl
22H
2o is placed in beaker, then adds FeCl
3, then add hydrochloric acid, H
2after O, stir; Finally add glacial acetic acid and new gill to go out, mix.This mordant has very strong corrosive attack to austenite crystal, simultaneously because new gill goes out adding of this surfactant and delayed the corrosion of mordant to matrix, make it reach balance, make this mordant can corrode austenite grain boundary, and don't can erode to austenitic matrix tissue, thereby can clearly show former primary state and condition of heat treatment fine grained austenite stainless steel crystal boundary.But to martensitic stain less steel, because the corrosive nature of its crystal boundary and intergranular structure is close, when adopting this mordant to corrode it, martensite crystal boundary and intergranular structure are all corroded, and can not show clearly the grain size of martensitic stain less steel.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of reasonable in design, method is simple, corrosion process is steady, corrosive effect is good, corrosion after sample organize clear display, handling safety to show reliably the caustic solution of Cr13 type martensitic stain less steel grain size.
For solving the problems of the technologies described above, the caustic solution of demonstration Cr13 type martensitic stain less steel grain size of the present invention, comprises and comprising the following steps:
First according to the ratio preparation mordant of the HCl solution of the saturated picric acid solution of 100ml and 0.2～1.5ml; Then get polishing and polished Cr13 type martensitic stain less steel sample, clean and dry up in rear immersion mordant, the detection faces of sample, is soaked 20～40s upward, when detection faces is dark yellow, takes out; Then with 10% oxalic acid aqueous solution, clean detection faces, when detection faces is canescence, then uses flowing water instead and clean whole sample and dry up.
Preferably, the mass concentration of HCl is 36.0%～38.0%.
Compared with prior art, beneficial effect of the present invention is as follows:
The caustic solution of demonstration Cr13 type martensitic stain less steel grain size of the present invention, it is main additive that its mordant mainly adopts picric acid, it is well corrosion Cr13 type martensitic stain less steel crystal boundary of corrosion, and select HCl as auxiliary additive, can regulate the corrosive effect of different tissues, can well distinguish martensitic stain less steel crystal boundary and intergranular structure.
The caustic solution of Cr13 type martensitic stain less steel grain size provided by the invention can just can clearly be observed the grain size of Cr13 type martensitic stain less steel under optical microscope.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 amplifies the metallograph of 100 times after the mordant of preparation in embodiment 1 corrodes 1Cr13 martensitic stain less steel
Fig. 2 amplifies the metallograph of 100 times after the mordant of preparation in embodiment 2 corrodes 2Cr13 martensitic stain less steel
Fig. 3 amplifies the metallograph of 100 times after mordant corrosion 1Cr13 martensitic stain less steel used in the prior art
Embodiment
Below by specific embodiment, the caustic solution of demonstration Cr13 type martensitic stain less steel grain size of the present invention is described in further detail.
Embodiment 1
It is 1Cr13 that the present embodiment adopts the material of Cr13 type martensitic stain less steel sample, and its main chemical elements content (percentage by weight) is: C content 0.08%～0.15%, containing Mn amount≤0.60%, si content≤0.60%, containing Cr amount 12.00%～14.00%, ni content≤0.60%, containing S amount≤0.030%, P content≤0.030%, surplus, be Fe.
The saturated picric acid solution of the formula of mordant: 100ml; The HCl saturated aqueous solution of 0.5ml.
The preparation of mordant: first the saturated picric acid solution of 100ml is placed in to water-bath and is incubated a period of time, picric acid can be fully dissolved in water, bath temperature is constant 60; The HCl saturated aqueous solution that ℃ adds again 0.5ml, stirs follow-up continuation of insurance temperature a period of time, and picric acid and hydrochloric acid are fully also evenly mixed mutually with water.
Caustic solution: prepare first according to the method described above mordant; Then get polishing and polished 1Cr13 martensitic stain less steel sample, clean and dry up in rear immersion mordant, the detection faces of sample, is soaked 30s upward, when detection faces is dark yellow, takes out; Then with 10% oxalic acid aqueous solution, clean detection faces, when detection faces is canescence, then uses flowing water instead and clean whole sample and dry up.With metaloscope, carry out the metallographic structure of 1Cr13 martensitic stain less steel and observe, as shown in Figure 1.
Embodiment 2
It is 2Cr13 that the present embodiment adopts the material of Cr13 type martensitic stain less steel sample, and its main chemical elements content (percentage by weight) is: C content 0.16%～0.24%, containing Mn amount≤0.60%, si content≤0.60%, containing Cr amount 12.00%～14.00%, ni content≤0.60%, containing S amount≤0.030%, P content≤0.030%, surplus, be Fe.
The saturated picric acid solution of the formula of mordant: 100ml; The HCl saturated aqueous solution of 0.5ml.
The preparation of mordant: first the saturated picric acid solution of 100ml is placed in to water-bath and is incubated a period of time, picric acid can be fully dissolved in water, bath temperature is constant 60; The HCl saturated aqueous solution that ℃ adds again 0.5ml, stirs follow-up continuation of insurance temperature a period of time, and picric acid and hydrochloric acid are fully also evenly mixed mutually with water.
Caustic solution: prepare first according to the method described above mordant; Then get polishing and polished 2Cr13 martensitic stain less steel sample, clean and dry up in rear immersion mordant, the detection faces of sample, is soaked 30s upward, when detection faces is dark yellow, takes out; Then with 10% oxalic acid aqueous solution, clean detection faces, when detection faces is canescence, then uses flowing water instead and clean whole sample and dry up.With metaloscope, carry out the metallographic structure of 2Cr13 martensitic stain less steel and observe, as shown in Figure 2.
Fig. 3 amplifies the metallograph of 100 times after mordant corrosion 1Cr13 martensitic stain less steel used in the prior art.By Fig. 1 and Fig. 2 and Fig. 3, contrast, obviously can find that martensite crystal boundary is obvious in Fig. 1 and Fig. 2, can observe clearly the grain size of Cr13 type martensitic stain less steel, and martensite crystal boundary and martensite interior tissue are distinguished not obviously in Fig. 3, can not observe the grain size of observing clearly Cr13 type martensitic stain less steel.
Claims (2)
1. a caustic solution that shows Cr13 type martensitic stain less steel grain size, is characterized in that, comprises the following steps:
First according to the ratio preparation mordant of the HCl solution of the saturated picric acid solution of 100ml and 0.2～1.5ml, then get polishing and polished Cr13 type martensitic stain less steel sample, cleaning dries up in rear immersion mordant, the detection faces of sample upward, soak 20～40s, when detection faces is dark yellow, take out; Then with 10% oxalic acid aqueous solution, clean detection faces, when detection faces is canescence, then uses flowing water instead and clean whole sample and dry up.
2. the caustic solution that shows according to claim 1 Cr13 type martensitic stain less steel grain size, is characterized in that, the mass concentration of described HCl solution is 36.0%～38.0%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699137A (en) * | 2014-11-25 | 2016-06-22 | 宁波江丰电子材料股份有限公司 | Displaying method for structure of metal chromium |
| CN106498400A (en) * | 2016-12-14 | 2017-03-15 | 陕西宏远航空锻造有限责任公司 | 17 4PH steel grain size caustic |
| CN107014661A (en) * | 2017-04-27 | 2017-08-04 | 东北大学 | A kind of caustic solution for showing high nitrogen martensitic stain less steel original austenite crystal boundary |
| CN115613033A (en) * | 2022-10-31 | 2023-01-17 | 宝武特冶航研科技有限公司 | Corrosive for treating grain boundary of 4Cr14Ni14W2Mo heat-resistant steel and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699137A (en) * | 2014-11-25 | 2016-06-22 | 宁波江丰电子材料股份有限公司 | Displaying method for structure of metal chromium |
| CN106498400A (en) * | 2016-12-14 | 2017-03-15 | 陕西宏远航空锻造有限责任公司 | 17 4PH steel grain size caustic |
| CN107014661A (en) * | 2017-04-27 | 2017-08-04 | 东北大学 | A kind of caustic solution for showing high nitrogen martensitic stain less steel original austenite crystal boundary |
| CN107014661B (en) * | 2017-04-27 | 2019-08-23 | 东北大学 | A kind of caustic solution showing high nitrogen martensitic stain less steel original austenite crystal boundary |
| CN115613033A (en) * | 2022-10-31 | 2023-01-17 | 宝武特冶航研科技有限公司 | Corrosive for treating grain boundary of 4Cr14Ni14W2Mo heat-resistant steel and application thereof |
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Application publication date: 20140409 |