CN106191981A - A kind of caustic solution of high-temperature alloy blades surface depleted layer - Google Patents
A kind of caustic solution of high-temperature alloy blades surface depleted layer Download PDFInfo
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- CN106191981A CN106191981A CN201610742538.9A CN201610742538A CN106191981A CN 106191981 A CN106191981 A CN 106191981A CN 201610742538 A CN201610742538 A CN 201610742538A CN 106191981 A CN106191981 A CN 106191981A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/32—Polishing; Etching
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Abstract
The invention discloses the caustic solution of a kind of high-temperature alloy blades surface depleted layer, purpose is, high-temperature alloy material surface depleted layer is carried out high power corrosion, preferably show the high-temperature alloy blades surface depleted layer after using and the element dilution phenomenon that piece surface produces in heat treatment process, the form of high-temperature alloy blades surface depleted layer can be reflected objectively, distribution and the degree of depth, thus correct blade situation is passed judgment on, reflect the state on high-temperature alloy blades surface further, the technical scheme used is: after surface 1) occurs that the metallographic specimen of the high-temperature alloy material of alloying element dilution carry out heat treatment, it is ground successively and polishes；2) burnishing surface of metallographic specimen is carried out electrochemical corrosion, the mixture that caustic is oxalic acid and pure water used in electrochemical corrosion, the volume ratio of caustic mesoxalic acid and pure water is (1～2): (8～9), thus corrodes the depleted layer high-temperature alloy material surface.
Description
Technical field
The present invention relates to metallographic microstructure detection field in high-temperature alloy blades physico-chemical examination technique, be specifically related to one
The caustic solution of high-temperature alloy blades surface depleted layer.
Background technology
High temperature alloy level of development is as weighing aero-engine and an important mark of industry gas turbine level of development
Will, causes the great attention of countries in the world, and numerous and confused input substantial amounts of man power and material research and develop high temperature alloy.
Although the research of high temperature alloy has been achieved for the biggest progress, it is thus achieved that many gratifying achievements in research, but high temperature alloy material
Material production, the course of processing still also exist many problems, such as: high-temperature alloy material, in it smelts heat treatment process, holds
It is easily generated the phenomenon of surface alloy element dilution.It is extremely hazardous that high-temperature alloy blades surface exists dilution phenomenon, because having
The dilution of element, can cause the dilution that γ ' phase occurs near superalloy grain boundary.The appearance of crystal boundary γ ' phase stripping section, or lead
Cause creep resistance reduces, or the stress caused during lax Grain Boundary Sliding is concentrated, thus affects the strengthening effect of crystal boundary.
Depletion of alloying element is exactly briefly that the alloying element in matrix solid solution disappears or partial disappearance, to materials microstructure
Performance creates impact.Complicated point is said and is exactly matrix solid solution kind solvent alloy element and C, N, B, O react generating
Compound, and arrived on crystal boundary or phase boundary most of assembly, cause the performance of material matrix to there occurs huge change.
Researcher has put into substantial amounts of time and efforts, for the inspection of engine high-temperature alloy vane surface depleted layer
Testing work, wherein the detection of physics metallographic method is exactly one detection method the most intuitively, but this method can only be to high temperature alloy
Material surface could use when having obvious dilution phenomenon.Therefore, unconspicuous for high-temperature alloy material surface dilution phenomenon
For sample, will seem helpless, especially by the physics metallographic method detection high-temperature alloy material surface depleted layer degree of depth
The reliability of value is poor.But, manifesting of high-temperature alloy material surface depleted layer mainly relies on corrosion technology to support, institute
With, the research for this depleted layer caustic is also the most necessary.
Summary of the invention
In order to solve the problems of the prior art, the present invention proposes the corrosion side of a kind of high-temperature alloy blades surface depleted layer
Method, it is possible to high-temperature alloy material surface depleted layer is carried out high power corrosion, the high-temperature alloy blades after preferably display uses
Surface depleted layer and the element dilution phenomenon that piece surface produces in heat treatment process, it is possible to reflect high temperature alloy objectively
The form of blade surface depleted layer, distribution and the degree of depth, thus correct pass judgment on blade situation, reflection high temperature closes further
The state of gold blade surface.
In order to realize object above, the technical solution adopted in the present invention is:
The caustic solution of a kind of high-temperature alloy blades surface depleted layer, comprises the following steps:
1), after the metallographic specimen that surface occurs the high-temperature alloy material of alloying element dilution carries out heat treatment, carry out successively
Grind and polishing；
2) burnishing surface of metallographic specimen being carried out electrochemical corrosion, the caustic used in electrochemical corrosion is oxalic acid and pure
The mixture of water, the volume ratio of caustic mesoxalic acid and pure water is (1～2): (8～9), thus corrodes and high-temperature alloy material table
The depleted layer in face.
Described step 2) in the electrolytic etching time be 5～10s.
Described step 2) in electrolytic etching voltage be 1.5V.
Described step 2) in electrolytic etching electric current be 0.3～0.4A.
Described step 2) in caustic mesoxalic acid and the preferred 1:9 of volume ratio of pure water.
Described step 1) in high-temperature alloy material be DZ125 high temperature alloy or K417G high temperature alloy.
A kind of caustic for corroding high-temperature alloy blades surface depleted layer, is (1～2) including volume ratio: (8～9)
Oxalic acid and pure water.
Described caustic includes oxalic acid and the pure water that volume ratio is 1:9.
Compared with prior art, after the present invention carries out heat treatment and grinding and polishing to metallographic specimen, use oxalic acid and pure water
The caustic mixed carry out electrochemical corrosion, the oxalic acid in caustic is faintly acid, by the way of electrolytic etching, energy
Enough well corrode out by the depleted layer of high-temperature alloy surface, reach to divide effect clearly with basal body interface.Compared to mesh
Front usual Nimonic caustic, the oxidisability of this caustic is relatively strong, after being corroded by this caustic, at metallographic optical microphotograph
Microscopic observation, high-temperature alloy material surface depleted layer feature shows the fuzzyyest, and material matrix is unclear with depleted layer boundary division
Clear.The caustic solution that the present invention provides is able to observe that more visible obvious depleted layer feature, the dilution of high-temperature alloy material surface
Layer belongs to one of defect affecting high-temperature alloy blades serviceability, objectively demonstrates high-temperature alloy blades surface depleted layer
Pattern, distribution and the degree of depth, it is possible to be estimated the combination property of high-temperature alloy blades, by high-temperature alloy blades surface
The analysis of depleted layer form, it is possible to detection feedback blade process rationality in the fabrication process, thus become adjusting process ginseng
The foundation of number, optimizes the Fabrication parameter of high-temperature alloy blades, improves blade surface structure property level further.
Scientific and reasonable detection high-temperature alloy blades surface depleted layer is to ensure that high-temperature alloy blades class product meets and uses
Requiring and the Main Means of steady operation, solution selected in the employing present invention is as caustic, to high-temperature alloy material surface
Depleted layer carries out electrolytic etching, then carries out microexamination by metallographic optical microscope, it is possible to conclude this blade surface clearly
The dilution phenomenon characteristic existed, can be verified by the detection method of aura.The present invention is lean to high-temperature alloy blades surface
That changes layer manifests the effect having uniqueness, carries out the depleted layer inspection of high-temperature alloy material surface by this caustic solution, it is possible to rotten
Lose high-temperature alloy material surface depleted layer clearly, provide intuitive and reliable Detection results for metallographic method detection depleted layer, can
To realize the science examination of high-temperature alloy blades quality, the manufacturing process to such blade is improved and is proposed to instruct simultaneously.
Accompanying drawing explanation
Fig. 1 is the corrosive effect metallograph of embodiment one；
Fig. 2 is the corrosive effect metallograph of embodiment two；
Fig. 3 is the corrosive effect metallograph of embodiment three；
Fig. 4 is the corrosive effect metallograph of the comparative example of embodiment three；
Fig. 5 is the corrosive effect metallograph of embodiment four；
Fig. 6 is the corrosive effect metallograph of the comparative example of embodiment four.
Detailed description of the invention
Below in conjunction with specific embodiment and Figure of description, the present invention is further explained.
The method of the present invention comprises the following steps:
1), after the metallographic specimen that surface occurs the high-temperature alloy material of alloying element dilution carries out heat treatment, carry out successively
Grinding and polishing, high-temperature alloy material is DZ125 high temperature alloy or K417G high temperature alloy；
2) burnishing surface to metallographic specimen carries out electrochemical corrosion, and the electrolytic etching time is 5～10s, electrolytic etching voltage
For 1.5V, electrolytic etching electric current is 0.3～0.4A, the mixture that caustic is oxalic acid and pure water used in electrochemical corrosion,
The volume ratio of caustic mesoxalic acid and pure water is (1～2): (8～9), the preferred 1:9 of volume ratio of oxalic acid and pure water, thus corrodes
Go out the depleted layer on high-temperature alloy material surface.
The inventive method is to use electrochemical etching method, and high-temperature alloy material surface occurs the gold of alloying element dilution
Phase sample is ground, carry out electrochemical corrosion, electrolytic etching voltage: 1.5V after polishing；Electrolytic etching electric current: 0.3～0.4A；Electricity
Solution etching time: 5～10s, has carried out substantial amounts of test by changing the proportioning of electrolytic etching solvent, etch time etc., has found
The volume proportion of more satisfactory caustic composition；Work as oxalic acid: H2O is (1～2): corrodes time (8～9) and high-temperature alloy blades surface
Depleted layer metallographic microstructure effect is ideal, but the proportioning that volume ratio is outside this scope all can not the most effectively be seen
Observe the depleted layer in high-temperature alloy blades surface.Wherein in preferred caustic, the volume relationship of each composition is: 10% oxalic acid+
90%H2O。
Oxalic acid in caustic is faintly acid, by the way of electrolytic etching, and can well be by high-temperature alloy surface
Depleted layer corrodes out, reaches to divide effect clearly with basal body interface.
Everybody the most usual Nimonic caustic carries out wiping corrosion at present, and the oxidisability of this caustic is relatively strong, passes through
After the corrosion of this caustic, at metallographic optical microphotograph Microscopic observation, high-temperature alloy material surface depleted layer feature shows the fuzzyyest,
Material matrix is unintelligible with depleted layer boundary division.
The caustic solution that the present invention provides is able to observe that more visible obvious depleted layer feature, high-temperature alloy material surface
Depleted layer belongs to one of defect affecting high-temperature alloy blades serviceability, objectively demonstrates the dilution of high-temperature alloy blades surface
Pattern, distribution and the degree of depth of layer, can be estimated the combination property of high-temperature alloy blades.By to high-temperature alloy blades
The analysis of surface depleted layer form, it is possible to detection feedback blade process rationality in the fabrication process, thus become adjustment work
The foundation of skill parameter, optimizes the Fabrication parameter of high-temperature alloy blades, improves blade surface structure property level further.
Scientific and reasonable detection high-temperature alloy blades surface depleted layer is to ensure that high-temperature alloy blades class product meets and uses
Require and the Main Means of steady operation.Solution selected in the employing present invention is as caustic, to high-temperature alloy material surface
Depleted layer carries out electrolytic etching, then carries out microexamination by metallographic optical microscope, can conclude this blade surface clearly
The dilution phenomenon characteristic existed, this result can be verified by the detection method of aura.
Caustic solution of the present invention manifests the effect having uniqueness to high-temperature alloy blades surface depleted layer, by this corrosion
Method carries out the depleted layer inspection of high-temperature alloy material surface, it is possible to achieve the science of high-temperature alloy blades quality is checked and accepted, the most right
The manufacturing process of such blade is improved and is proposed to instruct.By the caustic solution of the present invention, it is possible to corrode and high temperature alloy clearly
Material surface depleted layer, provides intuitive and reliable Detection results for metallographic method detection depleted layer.
Embodiment one:
By DZ125 high-temperature alloy blades after Overheating Treatment, the middle part choosing blade carries out the detection of surface depleted layer, will
Detected face, after Mechanical polishing, is put into equipped with in the solution of caustic, caustic mesoxalic acid and volume ratio=10 of pure water:
90, carry out electrolytic etching, corrosion parameter: voltage is 1.5V, electric current is 0.5A, and the time is 10s.See under metallographic optical microscope
Examining, corrosive effect is shown in Fig. 1, finds that the depleted layer on DZ125 high-temperature alloy blades surface is high-visible, and corrosive effect is obvious.
Embodiment two:
By DZ125 high-temperature alloy blades after Overheating Treatment, the middle part choosing blade carries out the detection of surface depleted layer, will
Detected face, after Mechanical polishing, is put into equipped with in the solution of caustic, caustic mesoxalic acid and volume ratio=20 of pure water:
80, carry out electrolytic etching, corrosion parameter: voltage is 1.5V, electric current is 0.5A, and the time is 10s.See under metallographic optical microscope
Examining, corrosive effect is shown in Fig. 2, finds that the depleted layer on DZ125 high-temperature alloy blades surface is high-visible, and corrosive effect is obvious.
Embodiment three:
By DZ125 high-temperature alloy blades after Overheating Treatment, the middle part choosing blade carries out the detection of surface depleted layer, will
Detected face, after Mechanical polishing, is put into equipped with in the solution of caustic, caustic mesoxalic acid: H2O volume ratio=10:90,
Carrying out electrolytic etching, corrosion parameter: voltage is 1.5V, electric current is 0.5A, and the time is 5s.At metallographic optical microphotograph Microscopic observation,
Corrosive effect is shown in Fig. 3, finds that the depleted layer on DZ125 high-temperature alloy blades surface is high-visible, and corrosive effect is obvious.
Comparative example: by DZ125 high-temperature alloy blades after Overheating Treatment, the middle part choosing blade carries out the inspection of depleted layer
Surveying, by detected face after Mechanical polishing, select caustic to carry out wiping erosion, the proportioning of caustic is 100ml HNO3+500ml
HCl+25g FeCl3+25g CuCl2Adding water to 1000ml, corrosive effect is shown in Fig. 4, and metallographic optical microphotograph Microscopic observation finds
The depleted layer on DZ125 high-temperature alloy blades surface is fuzzy with matrix boundary, and corrosive effect is inconspicuous.
Embodiment four:
By K417G high-temperature alloy blades after Overheating Treatment, the middle part choosing blade carries out the detection of depleted layer, by tested
Survey face, after Mechanical polishing, is put into and is carried out electrolytic etching, caustic mesoxalic acid: H in the solution equipped with caustic proportioning2O's
Volume ratio=10:90, corrosion parameter: voltage is 1.5V, electric current is 0.5A, and the time is 5s.Corrosive effect is shown in Fig. 5, at metallographic light
Learning basis of microscopic observation and find that the depleted layer on DZ125 high-temperature alloy blades surface is high-visible, corrosive effect is obvious.
Comparative example:
By K417G high-temperature alloy blades after Overheating Treatment, the middle part choosing blade carries out the detection of depleted layer, by tested
Survey face, after Mechanical polishing, selects caustic to carry out wiping erosion, and caustic proportioning is 100ml HNO3+500ml HCl+25g
FeCl3+25g CuCl2Add water to 1000ml.Corrosive effect is shown in Fig. 6, finds DZ125 high temperature at metallographic optical microphotograph Microscopic observation
The depleted layer on alloy vane surface is fuzzy with matrix boundary, and corrosive effect is inconspicuous.
Corrosive effect of the present invention is good, is the effective ways of detection high-temperature alloy blades surface depleted layer, does not interferes with lean
Change the measurement of layer depth, by high-temperature alloy material surface depleted layer is carried out high power etching detection, can preferably show and make
With high-temperature alloy blades surface depleted layer later and in heat treatment process piece surface produce element dilution phenomenon, it is possible to
Reflect the form of high-temperature alloy blades surface depleted layer, distribution and the degree of depth objectively, thus correct blade situation is carried out
Pass judgment on, reflect the state on high-temperature alloy blades surface further.
Claims (8)
1. the caustic solution of a high-temperature alloy blades surface depleted layer, it is characterised in that comprise the following steps:
1), after the metallographic specimen that surface occurs the high-temperature alloy material of alloying element dilution carries out heat treatment, it is ground successively
And polishing；
2) burnishing surface of metallographic specimen being carried out electrochemical corrosion, the caustic used in electrochemical corrosion is oxalic acid and pure water
Mixture, the volume ratio of caustic mesoxalic acid and pure water is (1～2): (8～9), thus corrodes and high-temperature alloy material surface
Depleted layer.
The caustic solution of a kind of high-temperature alloy blades surface the most according to claim 1 depleted layer, it is characterised in that described
Step 2) in the electrolytic etching time be 5～10s.
The caustic solution of a kind of high-temperature alloy blades surface the most according to claim 1 depleted layer, it is characterised in that described
Step 2) in electrolytic etching voltage be 1.5V.
The caustic solution of a kind of high-temperature alloy blades surface the most according to claim 1 depleted layer, it is characterised in that described
Step 2) in electrolytic etching electric current be 0.3～0.4A.
The caustic solution of a kind of high-temperature alloy blades surface the most according to claim 1 depleted layer, it is characterised in that described
Step 2) in caustic mesoxalic acid and the preferred 1:9 of volume ratio of pure water.
The caustic solution of a kind of high-temperature alloy blades surface the most according to claim 1 depleted layer, it is characterised in that described
Step 1) in high-temperature alloy material be DZ125 high temperature alloy or K417G high temperature alloy.
7. one kind for corroding the caustic of high-temperature alloy blades surface depleted layer, it is characterised in that include volume ratio be (1～
2): the oxalic acid of (8～9) and pure water.
A kind of caustic for corroding high-temperature alloy blades surface depleted layer the most according to claim 7, its feature exists
In, described caustic includes oxalic acid and the pure water that volume ratio is 1:9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109827830A (en) * | 2019-01-22 | 2019-05-31 | 上海理工大学 | A kind of twin boundary of super stainless steel and the display methods of precipitate |
| CN111504753A (en) * | 2020-06-11 | 2020-08-07 | 中国航发成都发动机有限公司 | General corrosive agent and corrosion method for gamma' phase and depletion layer metallographic structure of corrosion-resistant high-temperature alloy |
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| CN102759475A (en) * | 2012-06-23 | 2012-10-31 | 西安航空动力股份有限公司 | Method for surface peeling of powder superalloy |
| CN103695809A (en) * | 2013-12-15 | 2014-04-02 | 中广核工程有限公司 | Travel sleeve of control rod drive mechanism for nuclear power plant and preparation method thereof |
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| CN102759475A (en) * | 2012-06-23 | 2012-10-31 | 西安航空动力股份有限公司 | Method for surface peeling of powder superalloy |
| CN104634639A (en) * | 2013-11-13 | 2015-05-20 | 中国科学院金属研究所 | Coupled type metallographic corrosion method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109827830A (en) * | 2019-01-22 | 2019-05-31 | 上海理工大学 | A kind of twin boundary of super stainless steel and the display methods of precipitate |
| CN111504753A (en) * | 2020-06-11 | 2020-08-07 | 中国航发成都发动机有限公司 | General corrosive agent and corrosion method for gamma' phase and depletion layer metallographic structure of corrosion-resistant high-temperature alloy |
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Application publication date: 20161207 |