CN103695907A - Corrosive agent for displaying grain size of Cr13 martensite stainless steel and preparation method thereof - Google Patents
Corrosive agent for displaying grain size of Cr13 martensite stainless steel and preparation method thereof Download PDFInfo
- Publication number
- CN103695907A CN103695907A CN201310689277.5A CN201310689277A CN103695907A CN 103695907 A CN103695907 A CN 103695907A CN 201310689277 A CN201310689277 A CN 201310689277A CN 103695907 A CN103695907 A CN 103695907A
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- Prior art keywords
- stainless steel
- martensite stainless
- picric acid
- etching reagent
- water
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- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 46
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 42
- 239000010935 stainless steel Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000003518 caustics Substances 0.000 title abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical class OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 33
- 238000005530 etching Methods 0.000 claims description 33
- 238000004321 preservation Methods 0.000 abstract 2
- 230000003287 optical effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 239000013078 crystal Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 229910001566 austenite Inorganic materials 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052729 chemical element Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005088 metallography Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002271 resection Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Classifications
-
- 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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention discloses a corrosive agent for displaying the grain size of Cr13 martensite stainless steel and a preparation method thereof. The method comprises the steps of putting 100ml of saturated picric acid solution in a water bath, and carrying out heat preservation for a period of time, so as to thoroughly dissolve picric acid into water, wherein the temperature of the water bath is constant and is 60 DEG C; adding 0.2-1.5ml HCl solution, stirring, and then, continuing to carry out heat preservation for a period of time, so as to enable picric acid and hydrochloric acid to be thoroughly and uniformly mixed with water. The corrosive agent is mainly used for corroding the Cr13 martensite stainless steel, and the grain size of the Cr13 martensite stainless steel can be clearly observed by an optical microscope.
Description
Technical field
The present invention relates to a kind of etching reagent that shows stainless steel grain fineness number and preparation method thereof, particularly related to etching reagent of a kind of Cr13 type Martensite Stainless Steel grain fineness number and preparation method thereof.
Background technology
Martensite Stainless Steel is stainless a kind of, different according to as-heat-treated condition, under use state, be generally tempered martensite, tempered sorbite, ferrite, carbide and/or residual austenite etc., it contains 12%～17% chromium, makes steel have good erosion resistance and oxidation-resistance.In the present invention, by chromium content, the stainless steel such as the 1Cr13 between 12%～14%, 2Cr13 is called Cr13 type Martensite Stainless Steel.Because stainless steel can not fully show its tissue signature and organize details because of its fine corrosion resistance, general etching reagent, and the crystal boundary of Cr13 Martensite Stainless Steel and intracrystalline martensitic stucture corrodibility more approaching, be difficult to by its grain fineness number 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 fineness number of Cr13 type Martensite Stainless Steel.But in check, adopt aforesaid 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 etching reagent and caustic solution that can show clearly martensitic stucture crystal boundary, makes can observe the grain fineness number of Cr13 type Martensite Stainless Steel under opticmicroscope.
On January 23rd, 2013, disclosed Chinese invention patent specification sheets CN102888608A disclosed a kind of etching reagent that shows fine grained austenite stainless steel crystal boundary and preparation method thereof, and this etching reagent 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 etching reagent has very strong corrosive nature to austenite crystal, simultaneously because new gill goes out adding of this tensio-active agent and delayed the corrosion of etching reagent to matrix, make it reach balance, make this etching reagent can corrode austenite grain boundary, and don't can erode to austenitic matrix tissue, thereby can clearly show former primary state and as-heat-treated condition fine grained austenite stainless steel crystal boundary.But to Martensite Stainless Steel, because the corrosive nature of its crystal boundary and intergranular structure is close, when adopting this etching reagent to corrode it, martensite crystal boundary and intergranular structure are all corroded, and can not show clearly the grain fineness number of Martensite Stainless Steel.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of etching reagent that can show clearly martensite grain fineness number, makes can observe the grain fineness number of Cr13 type Martensite Stainless Steel under opticmicroscope.
For solving the problems of the technologies described above, the etching reagent of demonstration Cr13 type Martensite Stainless Steel grain fineness number of the present invention, comprising: the saturated picric acid solution of 100ml; The HCl solution of 0.2～1.5ml.
The preparation method of the etching reagent of described demonstration Cr13 type Martensite Stainless Steel grain fineness number, its step is as follows:
First the saturated picric acid solution of 100ml is placed in water-bath and is incubated for some time, and picric acid can be fully dissolved in water, and bath temperature is constant 60; ℃ add again 0.2～1.5ml HCl solution, stir follow-up continuation of insurance temperature for some time, picric acid and hydrochloric acid are fully also evenly mixed mutually with water.
Preferably, the mass concentration of HCl solution is 36.0%～38.0%.
Compared with prior art, beneficial effect of the present invention is as follows:
Etching reagent of demonstration Cr13 type Martensite Stainless Steel grain fineness number of the present invention and preparation method thereof, employing picric acid is main additive, it is well corrosion Cr13 type Martensite Stainless Steel crystal boundary of corrosion, and select HCl as supplementary additive, can regulate the corrosive effect of different tissues, can well distinguish Martensite Stainless Steel crystal boundary and intergranular structure.
Etching reagent of Cr13 type Martensite Stainless Steel grain fineness number provided by the invention and preparation method thereof, can provide a kind of etching reagent, makes Cr13 type Martensite Stainless Steel just can clearly observe its grain fineness number under opticmicroscope.
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 etching reagent of preparation in embodiment 1 corrodes 1Cr13 Martensite Stainless Steel
Fig. 2 amplifies the metallograph of 100 times after the etching reagent of preparation in embodiment 2 corrodes 2Cr13 Martensite Stainless Steel
Fig. 3 amplifies the metallograph of 100 times after etching reagent corrosion 1Cr13 Martensite Stainless Steel used in the prior art
Embodiment
Below by specific embodiment, etching reagent of Cr13 type Martensite Stainless Steel grain fineness number of the present invention and preparation method thereof is described in further detail.
Embodiment 1
It is 1Cr13 that the present embodiment adopts the material of Cr13 type Martensite Stainless Steel sample, and its main chemical elements content (weight percent) 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 etching reagent: 100ml; The HCl solution of 0.5ml.
The preparation of etching reagent: first the saturated picric acid solution of 100ml is placed in to water-bath and is incubated for some time, picric acid can be fully dissolved in water, bath temperature is constant 60; The HCl solution that ℃ adds again 0.5ml, stirs follow-up continuation of insurance temperature for some 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 etching reagent; Then get polishing and polished 1Cr13 Martensite Stainless Steel sample, clean and dry up in rear immersion etching reagent, 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 Martensite Stainless Steel and observe, as shown in Figure 1.
Embodiment 2
It is 2Cr13 that the present embodiment adopts the material of Cr13 type Martensite Stainless Steel sample, and its main chemical elements content (weight percent) 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 etching reagent: 100ml; The HCl solution of 0.5ml.
The preparation of etching reagent: first the saturated picric acid solution of 100ml is placed in to water-bath and is incubated for some time, picric acid can be fully dissolved in water, bath temperature is constant 60; The HCl solution that ℃ adds again 0.5ml, stirs follow-up continuation of insurance temperature for some 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 etching reagent; Then get polishing and polished 2Cr13 Martensite Stainless Steel sample, clean and dry up in rear immersion etching reagent, 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 Martensite Stainless Steel and observe, as shown in Figure 2.
Fig. 3 amplifies the metallograph of 100 times after etching reagent corrosion 1Cr13 Martensite Stainless 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 fineness number of Cr13 type Martensite Stainless Steel, and martensite crystal boundary and martensite interior tissue are distinguished not obviously in Fig. 3, can not observe the grain fineness number of observing clearly Cr13 type Martensite Stainless Steel.
Claims (3)
1. an etching reagent that shows Cr13 type Martensite Stainless Steel grain fineness number, is characterized in that, comprises the saturated picric acid solution of 100ml and the HCl solution of 0.2～1.5ml.
2. the etching reagent that shows according to claim 1 Cr13 type Martensite Stainless Steel grain fineness number, is characterized in that, the mass concentration of described HCl solution is 36.0%～38.0%.
3. prepare the method that shows the etching reagent of Cr13 type Martensite Stainless Steel grain fineness number described in claim 1 for one kind, it is characterized in that, first the saturated picric acid solution of 100ml is placed in water-bath and is incubated for some time, and picric acid can be fully dissolved in water, and bath temperature is constant 60 ℃; Add again 0.2～1.5ml HCl solution, stir follow-up continuation of insurance temperature for some time, picric acid and hydrochloric acid are fully also evenly mixed mutually with water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310689277.5A CN103695907A (en) | 2013-12-16 | 2013-12-16 | Corrosive agent for displaying grain size of Cr13 martensite stainless steel and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310689277.5A CN103695907A (en) | 2013-12-16 | 2013-12-16 | Corrosive agent for displaying grain size of Cr13 martensite stainless steel and preparation method thereof |
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| CN103695907A true CN103695907A (en) | 2014-04-02 |
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| CN201310689277.5A Pending CN103695907A (en) | 2013-12-16 | 2013-12-16 | Corrosive agent for displaying grain size of Cr13 martensite stainless steel and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420731A (en) * | 2015-12-29 | 2016-03-23 | 南京科润工业介质股份有限公司 | Metallographic corrosion liquid suitable for displaying quenching state grain boundaries of multiple types of steel workpieces and preparation method thereof |
| CN105908186A (en) * | 2016-05-06 | 2016-08-31 | 江西昌河航空工业有限公司 | Stainless steel corrosive agent and stainless steel grain size display method |
| 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 |
| CN107523833A (en) * | 2017-08-22 | 2017-12-29 | 河南科技大学 | A kind of metallographic etching agent and its application in terms of carbide, crystal boundary in showing steel |
| CN113218736A (en) * | 2021-05-07 | 2021-08-06 | 大唐锅炉压力容器检验中心有限公司 | Original austenite grain boundary corrosion method of martensitic stainless steel for steam turbine bolt |
Citations (2)
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| JP2005164340A (en) * | 2003-12-01 | 2005-06-23 | Sanyo Special Steel Co Ltd | Corrosion method due to corrosive liquid for microscopically detecting metal texture of martensite stainless steel or alloy tool steel |
| CN103234801A (en) * | 2013-04-25 | 2013-08-07 | 北京科技大学 | Method for displaying and treating Cr12 type martensitic heat-resistant steel primary austenite grain boundary |
-
2013
- 2013-12-16 CN CN201310689277.5A patent/CN103695907A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005164340A (en) * | 2003-12-01 | 2005-06-23 | Sanyo Special Steel Co Ltd | Corrosion method due to corrosive liquid for microscopically detecting metal texture of martensite stainless steel or alloy tool steel |
| CN103234801A (en) * | 2013-04-25 | 2013-08-07 | 北京科技大学 | Method for displaying and treating Cr12 type martensitic heat-resistant steel primary austenite grain boundary |
Non-Patent Citations (2)
| Title |
|---|
| 刘建华等: "新型耐蚀塑料模具钢的组织和性能", 《钢铁研究学报》, vol. 20, no. 4, 15 April 2008 (2008-04-15) * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420731A (en) * | 2015-12-29 | 2016-03-23 | 南京科润工业介质股份有限公司 | Metallographic corrosion liquid suitable for displaying quenching state grain boundaries of multiple types of steel workpieces and preparation method thereof |
| CN105420731B (en) * | 2015-12-29 | 2018-07-27 | 南京科润工业介质股份有限公司 | A kind of metallographic etchant and preparation method thereof being suitable for showing multiple types steel workpiece quenching state crystal boundary |
| CN105908186A (en) * | 2016-05-06 | 2016-08-31 | 江西昌河航空工业有限公司 | Stainless steel corrosive agent and stainless steel grain size display method |
| 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 |
| CN107523833A (en) * | 2017-08-22 | 2017-12-29 | 河南科技大学 | A kind of metallographic etching agent and its application in terms of carbide, crystal boundary in showing steel |
| CN107523833B (en) * | 2017-08-22 | 2019-06-14 | 河南科技大学 | A metallographic etchant and its application in displaying carbides and grain boundaries in steel |
| CN113218736A (en) * | 2021-05-07 | 2021-08-06 | 大唐锅炉压力容器检验中心有限公司 | Original austenite grain boundary corrosion method of martensitic stainless steel for steam turbine bolt |
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Application publication date: 20140402 |