CN106245029B - Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, preparation method and application method - Google Patents
Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, preparation method and application method Download PDFInfo
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- CN106245029B CN106245029B CN201610537629.9A CN201610537629A CN106245029B CN 106245029 B CN106245029 B CN 106245029B CN 201610537629 A CN201610537629 A CN 201610537629A CN 106245029 B CN106245029 B CN 106245029B
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Abstract
Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, preparation method and application method, the aggressive agent includes: the distilled water that volume fraction is 30-40%, volume fraction is the pure dehydrated alcohol of analysis of 35-45%, volume fraction is that 10-15% analyzes pure hydrofluoric acid, fraction is that 10-15% analyzes pure hydrochloric acid and mass fraction 3-5% ferric trichloride；The volume fraction is the percentage that each component accounts for aggressive agent total volume, and mass fraction is the percentage that solid accounts for aggressive agent gross mass；The invention also discloses the preparation method and application methods of the aggressive agent；The present invention solves the problems, such as that existing Super304H austenitic stainless steel aggressive agent is difficult to show precipitated phase and crystal boundary in lasting sample tissue.
Description
Technical field
The invention belongs to the aggressive agents of metal material metallographic test method, and in particular to arrive Super304H austenite stainless
Aggressive agent that the lasting sample tissue of steel is shown, preparation method and application method.
Background technique
Currently, the most common chemical erosion agent of Super304H austenitic stainless steel metal lographic examination be mainly chloroazotic acid (hydrochloric acid and
Nitric acid volume ratio is 3:1) and ferric trichloride aqueous hydrochloric acid solution (5 grams of+100 milliliters of hydrochloric acid of+50 milliliters of ferric trichloride water).Newly match
Chloroazotic acid need to use after 24h, be mainly used in Super304H austenite stainless steel raw material, and ferric trichloride aqueous hydrochloric acid solution
Can be ready-to-use, suitable for the Super304H austenitic stainless steel after being on active service.
Under the action of temperature and stress, microscopic structure changes the lasting sample of Super304H austenitic stainless steel, more
Different degrees of precipitation can occur for kind precipitated phase.Aggressive agent using chloroazotic acid and ferric trichloride aqueous hydrochloric acid solution as this sample
Have the defects that in use certain, effect is undesirable in terms of showing the precipitation phase morphology in lasting sample tissue.By
In the corrosion rate that the strong oxidizing property and ferric trichloride hydrochloride alcohol solution of chloroazotic acid are too fast, it is easy to corrode in erosion process
It crosses, causes precipitated phase because excessive erosion is fallen off, and crystal boundary is difficult completely to clearly indicate out, to influence subsequent microcosmic
The accuracy of structure observation and analysis influences the judgement of the lasting sample tissue Aging Damage analysis of Super304H.
Summary of the invention
It is complete, clear it is an object of the invention to overcome existing Super304H austenite stainless structure of steel aggressive agent to be difficult to
The shortcomings that showing the lasting sample crystal boundary of Super304H and precipitated phase guarantees the lasting sample high temperature ageing damage point of Super304H
The accuracy of analysis provides a kind of crystal boundary that can clearly show the lasting sample microstructure of Super304H austenitic stainless steel
Aggressive agent, preparation method and application method with precipitated phase.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
The aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, the aggressive agent include volume fraction
For 30-40% distilled water, volume fraction be 35-45% the pure dehydrated alcohol of analysis, volume fraction be 10-15% the pure salt of analysis
The pure hydrofluoric acid of analysis and mass fraction that acid, volume fraction are 10-15% are 3-5% ferric trichloride；The volume fraction is equal
The percentage of aggressive agent total volume is accounted for for each component, the mass fraction is the percentage that ferric trichloride accounts for aggressive agent gross mass.
The aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, including volume fraction is
Analysis pure hydrochloric acid that the pure dehydrated alcohol of analysis that 36% distilled water, volume fraction are 36%, volume fraction are 14%, volume fraction
It is 4% ferric trichloride for the 14% pure hydrofluoric acid of analysis and mass fraction.
The aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, including volume fraction is
Analysis pure hydrochloric acid that the pure dehydrated alcohol of analysis that 33% distilled water, volume fraction are 41%, volume fraction are 13%, volume fraction
The ferric trichloride that the pure hydrofluoric acid of analysis and mass fraction for 13% are 3%.
The aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, including volume fraction is
Analysis pure hydrochloric acid that the pure dehydrated alcohol of analysis that 31% distilled water, volume fraction are 43%, volume fraction are 13%, volume fraction
The ferric trichloride that the pure hydrofluoric acid of analysis and mass fraction for 13% are 4%.
The preparation method for the aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel described above is shown measures
It accounts for aggressive agent total volume fraction to be added in beaker for 30-40% distilled water, 35-45% dehydrated alcohol, then successively measures and account for respectively
Aggressive agent total volume fraction is that 10-15% analyzes pure hydrofluoric acid, 10-15% analyzes pure hydrochloric acid, is slowly added into burning along beaker inner wall
It in cup, and is constantly stirred with glass bar, adds and account for aggressive agent total mass fraction 3-5% ferric trichloride, be uniformly mixed and invaded
Lose agent.
The aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel described above is shown is used for Super304H steel
The method that lasting sample microstructure is shown, includes the following steps:
Step 1: intercepting metallographic test block on the lasting sample of Super304H, its surface is polished and mechanically polished, use
Washes of absolute alcohol is clean, is then dried up with hair dryer；
Step 2: aggressive agent of the present invention is poured into the glassware for being placed with absorbent cotton, it will be polished
The metallographic test block of the lasting sample of Super304H is corroded immerses down, and erosion time is 1-3 minutes；Until specimen surface is in white
It takes out, is rinsed with water when grey, the corrosion product of specimen surface is wiped with clean rayon balls；
Step 3: the metallographic test block surface by the lasting sample of Super304H corroded is cleaned with dehydrated alcohol,
It is dried up, carry out metallographic structure observation under the microscope and is taken pictures with hair dryer again.
Compared to the prior art compared with, the present invention has the advantage that
The present invention, by adjusting the ratio of hydrochloric acid, is added certain on the basis of common ferric trichloride aqueous hydrochloric acid solution is formulated
Hydrofluoric acid is measured, while by adjusting solvent, dehydrated alcohol is added and configures.In order to reduce corrosion rate, on the one hand pass through tune
The volatility for having changed aggressive agent since whole solvent, improves its stability；On the other hand, by reducing the content of acid, or use
A kind of weak acid slows down its erosion performance.The present invention has selected to reduce the content of hydrochloric acid, hydrofluoric acid has been added, using dehydrated alcohol
Slow down the corrosive nature of matched aggressive agent and increases its stability.Using aggressive agent of the present invention to Super304H austenite stainless
The lasting sample of steel erodes, and tissue display effect is good, and precipitated phase and Display of Grain Boundary are clear；Erosive velocity is easily controllable；It corrodes
Agent reusability is strong.
Detailed description of the invention
Fig. 1 is with the lasting sample metallographic structure (200 ×) of chloroazotic acid aggressive agent Super304H austenitic stainless steel.
Fig. 2 is with the lasting sample metallographic structure (500 ×) of chloroazotic acid aggressive agent Super304H austenitic stainless steel.
Fig. 3 is with the lasting sample metallographic structure of ferric trichloride aqueous hydrochloric acid solution aggressive agent Super304H austenitic stainless steel
(500×)。
Fig. 4 is with the lasting sample metallographic structure (200 ×) of aggressive agent Super304H austenitic stainless steel of the present invention.
Fig. 5 is with the lasting sample metallographic structure (500 ×) of aggressive agent Super304H austenitic stainless steel of the present invention.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Embodiment 1: taking 50 milliliters of distilled water and 50 milliliters of dehydrated alcohol to mix in beaker, measures 20 milliliters respectively
Pure hydrochloric acid and the 20 pure hydrofluoric acid of analysis are analyzed, is successively slowly added into beaker, is stirred continuously along beaker inner wall, be eventually adding and weigh
5 grams of ferric trichloride, be stirred continuously be uniformly mixed obtain aggressive agent.
Embodiment 2: taking 45 milliliters of distilled water and 56 milliliters of dehydrated alcohol to mix in beaker, measures 18 milliliters respectively
Pure hydrochloric acid and the 18 pure hydrofluoric acid of analysis are analyzed, is successively slowly added into beaker, is stirred continuously along beaker inner wall, be eventually adding and weigh
4.5 gram ferric trichloride, be stirred continuously be uniformly mixed obtain aggressive agent.
Embodiment 3: taking 45 milliliters of water and 62 milliliters of dehydrated alcohol to mix in beaker, measures 19 milliliters of analyses respectively
Pure hydrochloric acid and the 19 pure hydrofluoric acid of analysis, are successively slowly added into beaker along beaker inner wall, are stirred continuously, be eventually adding and weigh 5.5
Gram ferric trichloride, be stirred continuously be uniformly mixed obtain aggressive agent.
The application method of aggressive agent of the present invention is as follows:
1) metallographic test block is intercepted on the lasting sample of Super304H, its surface is polished and mechanically polished, use is anhydrous
Ethyl alcohol cleans up, and is then dried up with hair dryer；
2) aggressive agent of the present invention is poured into the glassware for being placed with absorbent cotton, by polished Super304H
The metallographic test block of lasting sample is corroded immerses down, and erosion time is 1-3 minutes.Until specimen surface is gone when being in lime color
Place, is rinsed with water, the corrosion product of specimen surface is wiped with clean rayon balls；
3) the metallographic specimen surface by corroding the lasting sample of Super304H is cleaned with dehydrated alcohol, then with blowing
Blower is dried up, and is carried out metallographic structure observation under the microscope and is taken pictures.
Fig. 1-2 is the metallographic structure after being corroded using chloroazotic acid aggressive agent the lasting sample of Super304H, and Fig. 1 is times magnification
Number 200 ×, Fig. 2 be amplification factor 500 ×, Display of Grain Boundary is deeper in figure, and precipitated phase is unobvious, and part precipitated phase has fallen off.
Fig. 3 is the metallographic structure after being corroded using ferric trichloride aqueous hydrochloric acid solution aggressive agent the lasting sample of Super304H,
Crystal boundary and precipitated phase are shown smudgy in figure.
Fig. 4-5 is the metallographic structure after being corroded using aggressive agent in the present invention the lasting sample of Super304H, and Fig. 4 is to put
Big multiple 200 ×, Fig. 5 be amplification factor 500 ×, Display of Grain Boundary is complete in figure, and transgranular tiny precipitated phase is shown clearly.
Claims (6)
- The aggressive agent that the lasting sample tissue of 1.Super304H austenitic stainless steel is shown, it is characterised in that: the aggressive agent includes Volume fraction is 30-40% distilled water, volume fraction is 35-45% the pure dehydrated alcohol of analysis, volume fraction are 10-15%'s Analyzing pure hydrochloric acid, the pure hydrofluoric acid of analysis that volume fraction is 10-15% and mass fraction is 3-5% ferric trichloride；The body Fraction is the percentage that each component accounts for aggressive agent total volume, and the mass fraction is that ferric trichloride accounts for aggressive agent gross mass Percentage.
- 2. the aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel according to claim 1 is shown, feature Be: the aggressive agent includes the pure dehydrated alcohol of analysis that volume fraction is 36% distilled water, volume fraction is 36%, volume point Counting the analysis pure hydrochloric acid for 14%, the pure hydrofluoric acid of analysis that volume fraction is 14% and mass fraction is 4% ferric trichloride.
- 3. the aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel according to claim 1 is shown, feature Be: the aggressive agent includes the pure dehydrated alcohol of analysis that volume fraction is 33% distilled water, volume fraction is 41%, volume point Count the analysis pure hydrochloric acid for being 13%, the ferric trichloride that the pure hydrofluoric acid of analysis that volume fraction is 13% and mass fraction are 3%.
- 4. the aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel according to claim 1 is shown, feature Be: the aggressive agent includes the pure dehydrated alcohol of analysis that volume fraction is 31% distilled water, volume fraction is 43%, volume point Count the analysis pure hydrochloric acid for being 13%, the ferric trichloride that the pure hydrofluoric acid of analysis that volume fraction is 13% and mass fraction are 4%.
- 5. the preparation method for the aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown described in claim 1, Be characterized in that: it is 30-40% distilled water, the pure dehydrated alcohol addition beaker of 35-45% analysis that measurement, which accounts for aggressive agent total volume fraction, In, then successively measure respectively and account for aggressive agent total volume fraction as the pure hydrofluoric acid of 10-15% analysis, 10-15% analysis pure hydrochloric acid, edge Beaker inner wall is slowly added into beaker, and is constantly stirred with glass bar, is added and is accounted for aggressive agent total mass fraction 3-5% tri-chlorination Iron is uniformly mixed and obtains aggressive agent.
- 6. the aggressive agent that any one of Claims 1-4 lasting sample tissue of Super304H austenitic stainless steel is shown is used for The method that the lasting sample tissue of Super304H is shown, characterized by the following steps:Step 1: intercepting metallographic test block on the lasting sample of Super304H, its surface is polished and mechanically polished, use is anhydrous Ethyl alcohol cleans up, and is then dried up with hair dryer；Step 2: the aggressive agent being poured into the glassware for being placed with absorbent cotton, polished Super304H is persistently tried The metallographic test block of sample is corroded immerses down, and erosion time is 1-3 minutes；It takes out when specimen surface is in lime color, is rushed with water It washes, the corrosion product of specimen surface is wiped with clean rayon balls；Step 3: the metallographic test block surface by the lasting sample of Super304H corroded being cleaned with dehydrated alcohol, then is used Hair dryer is dried up, and is carried out metallographic structure observation under the microscope and is taken pictures.
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| CN108004548B (en) * | 2017-12-06 | 2020-02-21 | 国网山东省电力公司电力科学研究院 | Preparation method and application of HR3C steel microstructure corrosive liquid after being in service for 5 ten thousand hours |
| CN111607794B (en) * | 2020-06-17 | 2022-05-27 | 宁波福至新材料有限公司 | Method for improving etching quality of metal product |
| CN112284860B (en) * | 2020-09-11 | 2023-05-12 | 河钢股份有限公司 | Corrosion agent for displaying austenitic structure of heat-resistant steel for air valve and use method thereof |
| CN115078680A (en) * | 2022-06-24 | 2022-09-20 | 武汉钢铁有限公司 | Metallographic analysis method and sample |
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| CA2714829C (en) * | 2004-03-18 | 2016-02-09 | Jfe Steel Corporation | Metallic material for conductive member, separator for fuel cell using the same, and fuel cell using the separator |
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