CN106908301A - A kind of etching pit method of clear display nickel-base alloy austenite grain boundary - Google Patents
A kind of etching pit method of clear display nickel-base alloy austenite grain boundary Download PDFInfo
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- CN106908301A CN106908301A CN201510980066.6A CN201510980066A CN106908301A CN 106908301 A CN106908301 A CN 106908301A CN 201510980066 A CN201510980066 A CN 201510980066A CN 106908301 A CN106908301 A CN 106908301A
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- base alloy
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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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
- 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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Abstract
The present invention relates to field of metallographic sample preparation, more particularly to a kind of etching pit method of clear display nickel-base alloy austenite grain boundary.The present invention provides a kind of etching pit method of clear display nickel-base alloy austenite grain boundary, comprises the following steps：a）Grinding；b）Polishing；c）Corrosion；d）Cleaning.A kind of etching pit method of clear display nickel-base alloy austenite grain boundary provided by the present invention, can be observed clearly austenite grain boundary under an optical microscope, can not only preferably show nickel-base alloy austenite crystal, and implementation is simple, be easy to implementation.
Description
Technical field
The present invention relates to field of metallographic sample preparation, more particularly to a kind of metallographic of clear display nickel-base alloy austenite grain boundary is rotten
Etching method.
Background technology
Nickel-base alloy refers to have intensity and good anti-oxidant, fire-resistant higher in the range of 650 DEG C~1000 DEG C by matrix of nickel
The high temperature alloy of gas corrosion ability.Refractoloy, abros, nickel-base antiwear can be subdivided into according to main performance to close
Golden, Ni-based Precise Alloy and Ni-based marmem etc..Wherein, it is most widely used with Refractoloy.Nickel-base high-temperature
More alloying element is can dissolve in alloy, preferable structure stability can be kept；It is orderly that nickel base superalloy can form coherence
Hardening constituent, can obtain the elevated temperature strength higher than ferrous alloy and cobalt-base alloys；Additionally, the nickel-base alloy containing chromium has than iron-based
The more preferable anti-oxidant and resistance to combustion gas corrosion ability of high temperature alloy.
There is austenite structure, the austenite grain size and uniformity of nickel-base alloy not only influence alloy mechanical property nickel-base alloy more
Can, the also nondestructive inspection sensitivity to material has a great impact.Therefore the austenite crystal of accurate display nickel-base alloy has ten
Divide important meaning.
Showing that the caustic solution of nickel-base alloy austenite crystal is conventional has：(1) copper sulphate aqueous hydrochloric acid solution (4g copper sulphate+20ml
Hydrochloric acid+20ml pure water)；(2) copper chloride hydrochloride alcohol solution (5g copper chloride+100ml hydrochloric acid+100ml alcohol).But above-mentioned two
The corrosive effect of person is all general, can not well highlight the austenite grain boundary of nickel-base alloy.
The content of the invention
The shortcoming of prior art, nickel-base alloy austenite crystal is clearly shown it is an object of the invention to provide a kind of in view of the above
The etching pit method on boundary, for solving the problems, such as that the display of nickel-base alloy austenite crystal is difficult in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a kind of metallographic of clear display nickel-base alloy austenite grain boundary
Caustic solution, comprises the following steps：
A) grind：The metallographic specimen of well cutting is treated that erosional surface is ground treatment, the metallographic specimen is nickel-base alloy；
B) polish：Step a gained samples are treated into erosional surface cleaning, polishing；
C) corrode：Treating step b gained samples that erosional surface is put into corrosive liquid and corrode, the corrosive liquid include hydrogen peroxide,
Hydrochloric acid and methyl alcohol；
D) clean：By the cleaning of step c gained samples, dry, and observe the austenite grain boundary of sample.
Nickel-base alloy generally refers to the alloy material with nickel as matrix, wherein the content of nickel it is general >=50wt%.
Preferably, the nickel content >=50wt% of the nickel-base alloy, chromium >=10wt%, molybdenum content >=5wt%, aluminium+titanium >=0.5wt%,
Iron≤20wt%, carbon content≤0.5wt%.
Preferably, the nickel-base alloy is the nickel-base alloy of cobalt content >=5wt%, and further, the nickel-base alloy is cobalt content
The nickel-base alloy of 5~25wt%.
In an embodiment of the present invention, the nickel-base alloy is the nickel-base alloys of Inconel 617.
Preferably, in the step a, the specific method of milled processed is：First erosional surface is treated using emery wheel to be polished, then
Erosional surface is treated using sand paper to be ground.
In the step a, treated during erosional surface polished using emery wheel, it is thick that emery wheel will treat that erosional surface is polishing to surface
Slightly polish, those skilled in the art can rule of thumb judge to treat whether erosional surface surface polishes roughly, and further use sand paper pair
Treat that erosional surface is ground.
In the step a, treat erosional surface using sand paper and be ground, to treating on erosional surface without substantially thick cut, ability
Field technique personnel can rule of thumb judge to treat on erosional surface with the presence or absence of thick cut, be walked with terminating grinding steps and entering polishing
Suddenly.Treated during erosional surface is ground using sand paper, the sand paper that usable mesh number gradually increases is treated erosional surface and ground
Mill treatment.In an embodiment of the present invention, the sand paper of 200 mesh, 400 mesh, 600 mesh, 800 mesh and 1000 mesh is used successively
Erosional surface is treated to be ground.
In the step a, treat erosional surface using emery wheel and polished and treated during erosional surface is ground using sand paper,
Treatment surface need to be often observed to ensure all of cut all along the grinding direction of the treatment passage and without substantially thick cut.
In the step b, those skilled in the art may be selected the various cleaning methods in this area and treat that erosional surface is cleaned to sample.
Preferably, in the step b, the specific method of cleaning is：Erosional surface is cleaned to be treated to sample with water.
In the step b, those skilled in the art may be selected the suitable polishing method in this area and treat that erosional surface is polished to sample.
Preferably, in the step b, the specific method of polishing is：Erosional surface is polished to be treated to sample using polishing cloth, is polished
Agent uses 2.0-3.0 μm of diamond polishing cream, and water wash away debris are used in polishing process.
Preferably, in the step b, that sample is further cleaned and dried up after polishing treats erosional surface.
It is furthermore preferred that in the step b, after polishing further with alcohol washes and dry up the sample after polishing treat erosional surface.
It is further preferred that percentage by volume >=84% of the alcohol.In an embodiment of the present invention, the alcohol for using is body
The alcohol of product percentage 84%-96%.
In the step b, sample treats that erosional surface is polished to and treats erosional surface (generally multiplication factor is more than 50 times in microscope
Light microscope) under observe without obvious cut, those skilled in the art can rule of thumb judge to treat on erosional surface with the presence or absence of draw
Trace, to judge whether polishing program completes.
Preferably, in the step c, the volume ratio of hydrogen peroxide, hydrochloric acid and methyl alcohol is 5~15 in the corrosive liquid：80~120：
200~400.
It is furthermore preferred that in the step c, the volume ratio of hydrogen peroxide, hydrochloric acid and methyl alcohol is 8~12 in the corrosive liquid：80~120：
250~350.
It is furthermore preferred that in the step c, the corrosive liquid is made up of hydrogen peroxide, hydrochloric acid and methyl alcohol.
Preferably, in the step c, sample treats that erosional surface submerges in corrosive liquid completely, keeps 5~60min, preferably keeps
15~25min, then takes out sample.
In the step d, those skilled in the art may be selected the various cleanings in this area and drying means is cleaned and done to sample
It is dry.Preferably, in the step d, sample cleaning, dry specific method are：Sample is cleaned with water first, then is used
Alcohol washes are simultaneously dried up.
It is furthermore preferred that the percentage by volume 84-96% of the alcohol.In an embodiment of the present invention, the alcohol for using is volume hundred
The alcohol of fraction 84%-96%.
In the step d, those skilled in the art may be selected the Ovshinsky that the various austenite grain boundary observational techniques in this area observe sample
Body crystal boundary, in an embodiment of the present invention, austenite grain boundary observational technique is：The austenite of sample is observed under an optical microscope
Crystal boundary.The general austenite grain boundary that sample can be observed under light microscope of the multiplication factor more than 50 times, is preferably amplifying
Multiple be 100~500 multiples light microscope under observed.
As described above, a kind of etching pit method of clear display nickel-base alloy austenite grain boundary provided by the present invention, in optics
Clearly austenite grain boundary can be observed under microscope.Specifically, nickel-base alloy, especially chromium and cobalt content nickel higher
Based alloy, with good decay resistance, the effect of general corrosion liquid is not obvious.Contrast existing caustic solution (sulfuric acid mantoquita
Aqueous acid and copper chloride hydrochloride alcohol solution), the corrosive effect of (hydrogen peroxide methanol hydrochloride solution) of the invention is optimal, can obtain
It is obvious with transgranular contrast to clear-cut austenite grain boundary, and crystal boundary.It can be seen that, caustic solution provided by the present invention can not only
It is enough preferably to show nickel-base alloy austenite crystal, and implementation is simple, be easy to implementation.
Brief description of the drawings
Fig. 1 is shown as the austenite crystal figure of the nickel-based alloy samples of Inconel 617 that the present invention shows, and with use copper sulphate
The corrosive effect of aqueous hydrochloric acid solution and copper chloride hydrochloride alcohol solution is contrasted.
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be as disclosed by this specification
Content understand other advantages of the invention and effect easily.The present invention can also add by way of a different and different embodiment
To implement or apply, the various details in this specification can also be based on different viewpoints and application, without departing from essence of the invention
Various modifications or alterations are carried out under god.
It should be clear that not specific dated process equipment or device use conventional equipment or device in the art in the following example.
In addition, it is to be understood that one or more method and steps mentioned in the present invention do not repel before and after the combination step can be with
There is other method step or other method step can also be inserted between the step of these are specifically mentioned, unless otherwise indicated；
It should also be understood that the combination annexation between one or more the equipment/devices mentioned in the present invention is not repelled being set in the combination
Can also there is other equipment/device before and after standby/device or can also insert it between these two equipment/devices for specifically mentioning
His equipment/device, unless otherwise indicated.And, unless otherwise indicated, the numbering of various method steps is only discriminating various method steps
Convenient tool, rather than to limit the ordering of various method steps or limiting enforceable scope of the invention, its relativeness
It is altered or modified, in the case of without essence change technology contents, when being also considered as enforceable category of the invention.
Embodiment 1
The technical process and step of this embodiment are (if without specified otherwise, each step is carried out at room temperature) as described below：
A grinds：The nickel-base alloy metallographic specimens of Inconel 617 of well cutting are placed on emery wheel and are polished, polished roughly, will
The sample polished is successively placed on the sand paper of 200 mesh, 400 mesh, 600 mesh, 800 mesh and 1000 mesh and is ground.Grind
During, need to often observe grinding direction (the i.e. passage ensured without substantially thick cut and all of cut all along the passage
Cut is completely covered the cut of a time), grinding is further continued for after should being rotated by 90 ° sample when grinding of lower a time is carried out.
B is polished：Ground sample is cleaned up, is polished on polishing cloth (commercially available), with water as lubricant,
Polishing agent uses 2.5 μm of diamond polishing cream.By the sample after polishing with 95% alcohol washes and dry up, be placed on optics show
Observed without obvious cut under 50 times of micro mirror.
C corrodes：Polished sample is respectively put into hydrogen peroxide methanol hydrochloride solution (10ml hydrogen peroxide+100ml hydrochloric acid
+ 300ml methyl alcohol), copper sulphate aqueous hydrochloric acid solution (4g copper sulphate+20ml hydrochloric acid+20ml pure water) and copper chloride hydrochloride alcohol solution
In (5g copper chloride+100ml hydrochloric acid+100ml alcohol), sample is treated that corrosion surface is completely immersed in corrosive liquid, keeps 20min,
Then take out sample.
D is cleaned：The sample of taking-up is rinsed well using flowing water, then with the alcohol washes that volume fraction is 95% and is dried up；
More clearly austenite grain boundary can be observed under 50x light microscopes, and experimental result is shot under 200x light microscopes.
Fig. 1 is respectively adopted corrosive liquid of the present invention, copper sulphate aqueous hydrochloric acid solution and copper chloride hydrochloride alcohol solution and shows
Alloy austenite crystal grain figure (200x) of Inconel 617, lower right corner black region is the position mark done using hardometer in figure, with
Ensure unification before and after metallograph position.
As can be seen from the figure：Copper sulphate aqueous hydrochloric acid solution corrosive effect is worst, and corrosive liquid can corrode out austenite grain boundary substantially；
Copper chloride hydrochloride alcohol solution corrodes and twin boundary, but austenite grain boundary corrosive effect is general；The method of the present invention can be more clear
Austenite grain boundary is shown clearly, and twin boundary corrosion is not obvious, austenite grain boundary is obvious with twin boundary contrast, easily judges Austria
Family name's body crystal boundary.Therefore, the method for the present invention corrodes the best results of the austenite grain boundaries of Inconel 617.
Embodiment 2
The technical process and step of this embodiment are (if without specified otherwise, each step is carried out at room temperature) as described below：
A grinds：Nickel-base alloys metallographic specimen (sample 2-5) of Inconel 617 of multiple well cuttings are individually placed to emery wheel enterprising
Row polishing, is polished roughly, and the sample polished is successively placed on into 200 mesh, 400 mesh, 600 mesh, 800 mesh and 1000 purposes
It is ground on sand paper.In grinding process, need to often observe ensures without substantially thick cut and all of cut all along the road
Secondary grinding direction (i.e. the passage cut is completely covered the cut of a time), should be by sample when grinding carry out lower a time
Grinding is further continued for after being rotated by 90 °.
B is polished：Ground sample is cleaned up, is polished on polishing cloth (commercially available), with water as lubricant,
Polishing agent uses 2.0 μm of diamond polishing cream.By the sample after polishing with 95% alcohol washes and dry up, be placed on optics show
Observed without obvious cut under 50 times of micro mirror.
C corrodes：Polished sample is respectively put into the hydrogen peroxide methanol hydrochloride solution of different formulations, sample is waited to corrode
Surface is completely immersed in corrosive liquid, is kept for a period of time, then takes out sample (Ju Ti Pei Fang and process time are shown in Table 1).
D is cleaned：The sample of taking-up is rinsed well using flowing water, then with the alcohol washes that volume fraction is 95% and is dried up, seen
Examine the austenite grain boundary of sample tested surface.
Observation result is as shown in table 1：
Table 1
In sum, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any to be familiar with this skill
The personage of art all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Therefore, such as
Those of ordinary skill in the art completed under without departing from disclosed spirit and technological thought all etc.
Effect modifications and changes, should be covered by claim of the invention.
Claims (10)
1. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary, comprises the following steps：
A) grind：The metallographic specimen of well cutting is treated that erosional surface is ground treatment, the metallographic specimen is nickel-base alloy；
B) polish：Step a gained samples are treated into erosional surface cleaning, polishing；
C) corrode：Treating step b gained samples that erosional surface is put into corrosive liquid and corrode, the corrosive liquid include hydrogen peroxide,
Hydrochloric acid and methyl alcohol；
D) clean：By the cleaning of step c gained samples, dry, and observe the austenite grain boundary of sample.
2. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
State the nickel content >=50wt% of nickel-base alloy, chromium >=10wt%, molybdenum content >=5wt%, aluminium+titanium >=0.5wt%, iron≤20wt%,
Carbon content≤0.5wt%.
3. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
The nickel-base alloy that nickel-base alloy is cobalt content >=5wt% is stated, further, the nickel-base alloy is 5~25wt%'s of cobalt content
Nickel-base alloy.
4. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
State in step a, the specific method of milled processed is：First erosional surface is treated using emery wheel to be polished, reuse sand paper and treat
Erosional surface is ground.
5. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
State in step b, the specific method of cleaning is：Erosional surface is cleaned to be treated to sample with water.
6. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
State in step b, the specific method of polishing is：Erosional surface is polished to be treated to sample using polishing cloth, polishing agent is used
2.0-3.0 μm of diamond polishing cream, uses water wash away debris in polishing process.
7. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
State in step b, that sample is further cleaned and dried up after polishing treats erosional surface.
8. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
State in step c, the volume ratio of hydrogen peroxide, hydrochloric acid and methyl alcohol is 5~15 in the corrosive liquid：80~120：200~400.
9. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, it is characterised in that institute
In stating step c, sample treats that erosional surface submerges in corrosive liquid completely, keeps 5~60min, then takes out sample.
10. a kind of etching pit method of clear display nickel-base alloy austenite grain boundary as claimed in claim 1, its feature exists
In, in the step d, sample is cleaned with water first, then with alcohol washes and dry up, and see under an optical microscope
Examine the austenite grain boundary of sample.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760452A (en) * | 2018-05-30 | 2018-11-06 | 山东大学 | Nickel base superalloy γ ' phases show and quantitative evaluation method |
| CN109975207A (en) * | 2019-03-30 | 2019-07-05 | 西北有色金属研究院 | A kind of observation method of 2 kirsite metallurgical structure of Zamak |
| CN110455605A (en) * | 2019-08-23 | 2019-11-15 | 中国航发北京航空材料研究院 | A kind of clear metallographic etching agent and application method for showing δ phase in GH4169 alloy |
| CN112284860A (en) * | 2020-09-11 | 2021-01-29 | 河钢股份有限公司 | Etching agent for displaying austenitic structure of heat-resistant steel for air valve and using method |
| CN112981406A (en) * | 2021-02-03 | 2021-06-18 | 安徽应流航源动力科技有限公司 | Surface grain corrosion method of IN718C nickel-based superalloy aviation bearing seat |
| CN113005456A (en) * | 2021-02-23 | 2021-06-22 | 西安热工研究院有限公司 | Metallographic corrosive agent and corrosion method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760452A (en) * | 2018-05-30 | 2018-11-06 | 山东大学 | Nickel base superalloy γ ' phases show and quantitative evaluation method |
| CN109975207A (en) * | 2019-03-30 | 2019-07-05 | 西北有色金属研究院 | A kind of observation method of 2 kirsite metallurgical structure of Zamak |
| CN110455605A (en) * | 2019-08-23 | 2019-11-15 | 中国航发北京航空材料研究院 | A kind of clear metallographic etching agent and application method for showing δ phase in GH4169 alloy |
| CN112284860A (en) * | 2020-09-11 | 2021-01-29 | 河钢股份有限公司 | Etching agent for displaying austenitic structure of heat-resistant steel for air valve and using method |
| CN112981406A (en) * | 2021-02-03 | 2021-06-18 | 安徽应流航源动力科技有限公司 | Surface grain corrosion method of IN718C nickel-based superalloy aviation bearing seat |
| CN113005456A (en) * | 2021-02-23 | 2021-06-22 | 西安热工研究院有限公司 | Metallographic corrosive agent and corrosion method |
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