CN102888608A - Corrosive for displaying austenitic stainless steel grain boundary of fine grains and method for preparing corrosive - Google Patents
Corrosive for displaying austenitic stainless steel grain boundary of fine grains and method for preparing corrosive Download PDFInfo
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- CN102888608A CN102888608A CN2012104350984A CN201210435098A CN102888608A CN 102888608 A CN102888608 A CN 102888608A CN 2012104350984 A CN2012104350984 A CN 2012104350984A CN 201210435098 A CN201210435098 A CN 201210435098A CN 102888608 A CN102888608 A CN 102888608A
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Abstract
The invention discloses a corrosive for displaying austenitic stainless steel grain boundaries of fine grains and a method for preparing the corrosive. The corrosive is characterized by comprising the following components by weight: 80-150ml of H2O, 10-20ml of HCl, 15-25g of FeCl3, 10-15g of CuCl2/H2O, 2.0-7.0ml of glacial acetic acid and 1-5 drops of benzalkonium bromide. The method comprises the steps of: placing CuCl2.H2O in a beaker; then adding FeCl3, and uniformly stirring after adding HCl and H2O; and uniformly mixing after adding glacial acetic acid and benzalkonium bromide finally. According to the corrosive for the austenitic stainless steel of the fine grains, the grain boundaries of the austenitic stainless steel of the fine grains in the original state and the thermal treatment state can be clearly displayed, the 100 times of rating on grain size can be easily performed, the grain boundaries are clear, the interference of a texture to the grain boundaries is small, and the corrosion effect is good.
Description
Technical field
The present invention relates to a kind of etching reagent that shows fine grained austenite stainless steel crystal boundary and preparation method thereof, belong to austenite stainless steel making field.
Background technology
The size of metal grain has conclusive impact to its mechanical property under room temperature and high temperature.The size of metal grain size is directly connected to mechanics and the mechanical property of material, so in metallographic structure analysis, the evaluation of grain-size is very important.
The high-temperature bearing parts of super (super-) critical unit (overheated hot arc pipeline, reheating hot pipe etc.) mainly adopt the manufacturing of fine grained austenite stainless steel, and if the materials such as the fine grained austenite primary stainless steel TP347HFG stainless steel that these high-temperature bearing parts are commonly used, Super304H stainless steel.Wherein, requiring TP347HFG stainless steel grain fineness number among the ASME SA213 is 7～10 grades.But when the fine grained austenite stainless steel after former primary state and the thermal treatment being carried out the metallographic detection, existing often crystal boundary is smudgy with etching reagent, and intracrystalline is seriously polluted, has a strong impact on the grading of grain fineness number.This phenomenon fine grained austenite stainless steel after thermal treatment is more outstanding in detecting, and has brought many inconvenience for the material property analytical work.Therefore need to seek a kind of etching reagent that under the different heat treatment state, can show preferably fine grained austenite stainless steel crystal boundary.
Consult documents and materials and the patent published at present, have no the correlative study report of the etching reagent that shows fine grained austenite stainless steel crystal boundary, and the Grain size analysis of material plays an important role to research and the failure analysis of metallic substance, therefore the invention solves the problem of the fine grained austenite stainless steel crystal boundary that shows former primary state and as-heat-treated condition, the performance analysis work of material is had important improved action and realistic meaning.
Summary of the invention
Technical problem to be solved by this invention is: the quality of improving the grain fineness number evaluation, improve the effect of the observation of metallographic structure, a kind of etching reagent that can show preferably former primary state and as-heat-treated condition fine grained austenite stainless steel crystal boundary is provided, and this etching reagent is applicable to TP347HFG stainless steel and the Super304H stainless steel of former primary state and as-heat-treated condition.
In order to achieve the above object, the invention provides a kind of etching reagent that shows the fine grained austenite stainless steel crystal boundary of former primary state and as-heat-treated condition, it is characterized in that, comprise the component that forms in following ratio:
H
2O：80-150mL；
Hydrochloric acid: 10-20mL;
FeCl
3：15-25g；
CuCl
2·2H
2O：10-15g；
Glacial acetic acid: 2.0-7.0mL;
New gill goes out and (calls: Morpan BB/Benzalkonium Bromide; Chemical name: dodecyl dimethyl benzyl ammonium bromide): 1-5 drips.
Preferably, the mass concentration of described hydrochloric acid is 36%.
Preferably, the described new gill mass concentration of going out is 0.2%.
The present invention also provides the preparation method of above-mentioned etching reagent, it is characterized in that, first with CuCl
22H
2O places beaker, then adds FeCl
3, add again hydrochloric acid, H
2After the O, stir; Add at last Glacial acetic acid and new gill goes out, mix to get final product.
H among the present invention
2O is solvent, CuCl
2, HCl and FeCl
3Be oxygenant; Glacial acetic acid is a kind of weak acid, corrodibility that on the one hand can Contrast agent, the on the other hand also acid base equilibrium of easier control reagent; It is a kind of tensio-active agent that new gill goes out, and delays etching reagent to the corrosion of matrix.
Fine grained austenite Corrosion of Stainless Steel provided by the invention agent can clearly show the stainless crystal boundary of fine grained austenite of former primary state and as-heat-treated condition, under 100 times, carry out easily the grain fineness number grading, crystal boundary is clear, organizes littlely to the interference of crystal boundary, and corrosive effect is good.
Description of drawings
Fig. 1 amplifies 100 times photo after the etching reagent of embodiment 1 preparation corrodes former primary state TP347HFG stainless steel;
Fig. 2 amplifies 100 times photo after the etching reagent of embodiment 2 preparations corrodes former primary state TP347HFG stainless steel;
Fig. 3 is that the etching reagent corrosion of embodiment 2 preparations was amplified 100 times photo through 10 minutes behind the heat treated TP347HFG stainless steel;
Fig. 4 is that the etching reagent corrosion of embodiment 2 preparations was amplified 100 times photo through 20 minutes behind the heat treated TP347HFG stainless steel;
Fig. 5 amplifies 100 times photo after the etching reagent of embodiment 3 preparations corrodes former primary state TP347HFG stainless steel;
Fig. 6 amplifies 100 times after the etching reagent of embodiment 4 preparations corrodes former primary state Super304H stainless steel
Photo;
Fig. 7 is CuSO
4Amplify 100 times photo after corroding former primary state TP347HFG stainless steel;
Fig. 8 is CuSO
4Corrosion was amplified 100 times photo through 10 minutes behind the heat treated TP347HFG stainless steel;
Fig. 9 is CuSO
4Corrosion was amplified 100 times photo through 20 minutes behind the heat treated TP347HFG stainless steel;
Figure 10 is FeCl
3Amplify 100 times photo after corroding former primary state TP347HFG stainless steel;
Figure 11 is CuSO
4Etching reagent amplifies 100 times photo after corroding former primary state Super304H stainless steel.
Embodiment
For the present invention is become apparent, hereby with preferred embodiment, and cooperate accompanying drawing to be described in detail below.
The TP347HFG Stainless Steel Alloy composition that adopts among embodiment 1-3 and the Comparative Examples 1-2 is as shown in table 1:
Table 1 test TP347HFG stainless steel composition (wt%)
The Super304H Stainless Steel Alloy composition that adopts in embodiment 4 and the Comparative Examples 3 is as shown in table 2:
Table 2 test Super304H stainless steel composition (wt%)
| C | Si | Mn | P | S | Ni | B |
| 0.07～0.13 | ≤0.30 | ≤1.00 | ≤0.040 | ≤0.010 | 7.5～10.5 | 0.001～0.01 |
| Cr | N | Nb | Al | Cu | Fe | |
| 17.0～19.0 | 0.05～0.12 | 0.30～0.60 | 0.003～0.03 | 2.5～3.50 | More than |
Embodiment 1
Prescription: as shown in table 3
Table 3
| H 2O | Hydrochloric acid | FeCl 3 | CuCl 2·2H 20 | Glacial acetic acid | New gill goes out |
| 80mL | 10mL | 15g | 10g | 2mL | 2 |
The preparation method:
First with 10g CuCl
22H
2O places beaker, then adds 15g FeCl
3, add again the 10mL mass concentration and be after 36% hydrochloric acid, the 80mL distilled water, stir; Add at last the 2mL Glacial acetic acid and 2 new gills go out, mix to get final product.
Test method:
Former primary state fine grained austenite TP347HFG stainless steel is processed into metallographic specimen, after the polishing sample is immersed above-mentioned etching reagent etch 35 seconds, when the surface is light grey, water cleans up, with drying up with blower after the alcohol flushing, carry out metallographic structure with metaloscope and observe, as shown in Figure 1.
Embodiment 2
Prescription: as shown in table 4
Table 4
| H 2O | Hydrochloric acid | FeCl 3 | CuCl 2·2H 2O | Glacial acetic acid | New gill goes out |
| 100mL | 15mL | 18g | 12g | 5mL | 4 |
The preparation method:
First with 12g CuCl
22H
2O places beaker, then adds 18g FeCl
3, add again the 15mL mass concentration and be after 36% hydrochloric acid, the 100mL distilled water, stir; Add at last the 5mL Glacial acetic acid and 4 new gills go out, mix to get final product.
Test method:
With former primary state, through thermal treatment in 10 minutes (heat treatment mode: be incubated 10 minutes after being warming up to 950 ℃, air cooling is to room temperature), thermal treatment in 20 minutes (heat treatment mode: after being warming up to 950 ℃ the insulation 20 minutes, air cooling is to room temperature) fine grained austenite TP347HFG stainless steel be processed into metallographic specimen, after the polishing sample immersed above-mentioned etching reagent etch 25 seconds, when the surface is light grey, water cleans up, with drying up with blower after the alcohol flushing, carry out metallographic structure with metaloscope and observe, respectively such as Fig. 2, Fig. 3, shown in Figure 4.
Embodiment 3
Prescription: as shown in table 5
Table 5
| H 2O | Hydrochloric acid | FeCl 3 | CuCl 2·2H 2O | Glacial acetic acid | New gill goes out |
| 150mL | 20mL | 20g | 15g | 5mL | 5 |
The preparation method:
First with 15g CuCl
22H
2O places beaker, then adds 20g FeCl
3, add again the 20mL mass concentration and be after 36% hydrochloric acid, the 150mL distilled water, stir; Add at last the 5mL Glacial acetic acid and 5 new gills go out, mix to get final product.
Test method:
Former primary state fine grained austenite TP347HFG stainless steel is processed into metallographic specimen, after the polishing sample is immersed above-mentioned etching reagent etch 20 seconds, when the surface is light grey, water cleans up, with drying up with blower after the alcohol flushing, carry out metallographic structure with metaloscope and observe, as shown in Figure 5.
Embodiment 4
Prescription: as shown in table 6
Table 6
| H 2O | Hydrochloric acid | FeCl 3 | CuCl 2·2H 2O | Glacial acetic acid | New gill goes out |
| 100mL | 20mL | 15g | 15g | 4mL | 5 |
The preparation method:
First with 105CuCl
22H
2O places beaker, then adds 15g FeCl
3, add again the 20mL mass concentration and be after 36% hydrochloric acid, the 100mL distilled water, stir; Add at last the 4mL Glacial acetic acid and 5 new gills go out, mix to get final product.
Test method:
Former primary state fine grained austenite Super304H stainless steel is processed into metallographic specimen, after the polishing sample is immersed above-mentioned etching reagent etch 28 seconds, when the surface is light grey, water cleans up, with drying up with blower after the alcohol flushing, carry out metallographic structure with metaloscope and observe, as shown in Figure 6.
Comparative Examples 1
With former primary state, through thermal treatment in 10 minutes (heat treatment mode: be incubated 10 minutes after being warming up to 950 ℃, air cooling is to room temperature), thermal treatment in 20 minutes (heat treatment mode: after being warming up to 950 ℃ the insulation 20 minutes, air cooling is to room temperature) fine grained austenite TP347HFG stainless steel be processed into metallographic specimen, after the polishing sample is immersed CuSO
4Solution is (by CuSO
420g, HCl100mL, H
2O100mL is formulated) etch 25 seconds, when the surface is light grey, water cleans up, and with drying up with blower after the alcohol flushing, carries out metallographic structure with metaloscope and observes, respectively such as Fig. 7, Fig. 8, shown in Figure 9.
Comparative Examples 2
Former primary state fine grained austenite TP347HFG stainless steel is processed into metallographic specimen, after the polishing sample is immersed FeCl
3Solution is (by CuSO
420g, HCl30mL, H
2O100mL is formulated) etch 20 seconds, when the surface is light grey, water cleans up, and with drying up with blower after the alcohol flushing, carries out metallographic structure with metaloscope and observes, as shown in figure 10.
Comparative Examples 3
Former primary state fine grained austenite Super304H stainless steel is processed into metallographic specimen, after the polishing sample is immersed CuSO
4Solution is (by CuSO
420g, HCl30mL, H
2O100mL is formulated) etch 30 seconds, when the surface is light grey, water cleans up, and with drying up with blower after the alcohol flushing, carries out metallographic structure with metaloscope and observes, as shown in figure 11.
Comparison diagram 1-5 and Fig. 7-10 as can be known, same fine grained austenite TP347HFG stainless steel uses conventional reagent, such as CuSO
4Reagent or FeCl
3After the reagent corrosion, the bad grasp of etching time, easily excessive erosion, and the corrosion sample crystal boundary is unintelligible, the color is too dark in intergranular structure, and the evaluation of grain fineness number is had interference effect; After using the special-purpose etching reagent corrosion of embodiment 1-3 preparation, crystal boundary is clear, and intergranular structure is less or not obvious.
Comparison diagram 6 and Figure 11 as can be known, same fine grained austenite Super304H stainless steel uses conventional reagent, such as CuSO
4After the reagent corrosion, the bad grasp of etching time, easily excessive erosion, and the corrosion sample crystal boundary is unintelligible, the color is too dark in intergranular structure, and the evaluation of grain fineness number is had interference effect; After using the special-purpose etching reagent corrosion of embodiment 4 preparations, crystal boundary is clear, and intergranular structure is less or not obvious.
Claims (4)
1. an etching reagent that shows fine grained austenite stainless steel crystal boundary is characterized in that, comprises the component that forms in following ratio:
H
2O：80-150mL；
Hydrochloric acid: 10-20mL;
FeCl
3：15-25g；
CuCl
2·2H
2O：10-15g；
Glacial acetic acid: 2.0-7.0mL;
New gill goes out: 1-5 drips.
2. a kind of etching reagent that shows fine grained austenite stainless steel crystal boundary according to claim 1 is characterized in that, the mass concentration of described hydrochloric acid is 36%.
3. a kind of etching reagent that shows fine grained austenite stainless steel crystal boundary according to claim 1 is characterized in that, the mass concentration that described new gill goes out is 0.2%.
4. a kind of preparation method who shows the etching reagent of fine grained austenite stainless steel crystal boundary claimed in claim 1 is characterized in that, first with CuCl
22H
2O places beaker, then adds FeCl
3, add again hydrochloric acid, H
2After the O, stir; Add at last Glacial acetic acid and new gill goes out, mix to get final product.
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| CN103074630A (en) * | 2013-02-06 | 2013-05-01 | 东方电气集团东方锅炉股份有限公司 | Metallographic corrosive liquid for bimetal composite pipe with transition layer and etching method of metallographic corrosive liquid |
| CN103628062A (en) * | 2013-08-22 | 2014-03-12 | 中国重汽集团济南动力有限公司 | Metallographic corrosive for showing grain boundaries of steels |
| CN103698192A (en) * | 2013-12-21 | 2014-04-02 | 哈尔滨锅炉厂有限责任公司 | Chemical etching liquid and method for displaying raw stainless steel austenite grain boundary |
| CN104020033A (en) * | 2014-05-28 | 2014-09-03 | 天津诚信达金属检测技术有限公司 | Normal temperature 9Cr-1Mo classification steel grain boundary display corrosive agent |
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| CN105603430A (en) * | 2016-03-01 | 2016-05-25 | 上海锅炉厂有限公司 | Corrosive agent for displaying slip band tissue of shot blasting layer |
| CN106350820A (en) * | 2016-08-30 | 2017-01-25 | 东方电气集团东方锅炉股份有限公司 | Etching agent for displaying shot-blasted layer of inner wall of austenitic heat-resistant steel pipe, and use method of etching agent |
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