CN107389419B - The corrosive liquid and deep etch method of deep etch are carried out to nickel Al-Cr-Mo eutectic lamellar - Google Patents
The corrosive liquid and deep etch method of deep etch are carried out to nickel Al-Cr-Mo eutectic lamellar Download PDFInfo
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Abstract
The invention discloses the corrosive liquids that a kind of pair of nickel Al-Cr-Mo eutectic lamellar carries out deep etch, it is formulated by chromium oxide, concentrated hydrochloric acid and deionized water, wherein, the chromium oxide quality being added in every 10mL concentrated hydrochloric acid is 2.5~3.5g, and the volume ratio of the deionized water and concentrated hydrochloric acid is 4~5:1.Can not directly accurately tissue be judged by solving the problems, such as that existing caustic solution is directed to when NiAl-Cr (Mo) lamellar eutectic alloy with the single direction of growth is corroded and analyzed.The invention also discloses the methods for carrying out deep etch to nickel Al-Cr-Mo eutectic lamellar using corrosive liquid, are specifically implemented according to the following steps: step 1, configuring corrosive liquid；Step 2, it prepares sample to be corroded and is pre-processed；Step 3, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, etching time be 5~for 24 hours；Step 4, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Description
Technical field
The invention belongs to the Metallographic Analysis technical field of alloy, it is related to carrying out nickel Al-Cr-Mo eutectic lamellar the corruption of deep etch
Liquid is lost, the invention further relates to the methods for carrying out deep etch using the corrosive liquid.
Background technique
NiAl-Cr (Mo) eutectic alloy is expected to replace Ni based high-temperature alloy, is applied to aero engine turbine blades material,
Belong to high-end applications field.Engine turbine blade material usually requires to use for a long time under high temperature environment, this just needs material
Material has good and stable high-temperature behavior.In general, microstructure stabilization just most possibly guarantees excellent performance under high temperature.Cause
This, the thermal stability of research NiAl-Cr (Mo) eutectic alloy microstructure is particularly important.In microstructure thermal stability
In research process, judge that the real change of tissue is one of its difficult point, this is just needed using a kind of more reasonable Metallographic Analysis skill
Art solves this problem.
In the microstructure research to NiAl-Cr (Mo) eutectic alloy, the metallographic analysing method shallowly corroded is generallyd use
To judge microstructure evolution caused by synusia spacing, unit cell dimension, tissue defects and the high temperature of alloy microstructure etc..But in height
Temperature causes in the research process of microstructure evolution, carries out control point to using the cross section and longitudinal section of alloy prepared by directional solidification
Analysis predicts that shallow corrosion analysis (two dimension observation) can not the objective real change for comprehensively reflecting the alloy microstructure.If
Its matrix phase (three dimensional viewing) is removed using the method for deep etch, then intuitively can comprehensively judge the true change of microstructure
Change.
Currently, the shallow corrosion research data of metallographic for NiAl-Cr (Mo) eutectic alloy sample is more, chloroazotic acid is generallyd use
It is shallowly corroded.If still using the corrosive agent, extends etching time and deep etch is carried out to the alloy, corrosive effect is not
Good, tissue corrosion is uneven, and some regions are easy excessive erosion, and go matrix effect not significant.
Summary of the invention
The object of the present invention is to provide the corrosive liquids that a kind of pair of nickel Al-Cr-Mo eutectic lamellar carries out deep etch, solve existing
Caustic solution is directed to can not be direct when NiAl-Cr (Mo) lamellar eutectic alloy with the single direction of growth is corroded and analyzed
The problem of accurately tissue is judged.
The technical scheme adopted by the invention is that the corrosive liquid of deep etch is carried out to nickel Al-Cr-Mo eutectic lamellar, by aoxidizing
Chromium, concentrated hydrochloric acid and deionized water are formulated, wherein the chromium oxide quality being added in every 10mL concentrated hydrochloric acid is 2.5~3.5g, institute
The volume ratio of the deionized water and concentrated hydrochloric acid stated is 4~5:1.
The features of the present invention also characterized in that
The chromium oxide is CrO3, mass fraction >=99%.
The mass fraction of the concentrated hydrochloric acid is 36%~38%.
It is a further object of the present invention to provide the methods that a kind of pair of nickel Al-Cr-Mo eutectic lamellar carries out deep etch.
Another technical solution of the invention is the method for carrying out deep etch to nickel Al-Cr-Mo eutectic lamellar using corrosive liquid,
It is specifically implemented according to the following steps:
Step 1, corrosive liquid is configured；
Step 2, it prepares sample to be corroded and is pre-processed；
Step 3, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, etching time be 5~for 24 hours；
Step 4, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
It is of the invention to be further characterized in that,
The step 1 specifically: the ratio for being 2.5~3.5g according to the chromium oxide quality being added in every 10mL concentrated hydrochloric acid
Weigh chromium oxide；It is that 4~5:1 measures concentrated hydrochloric acid and deionized water according to deionized water and the volume ratio of concentrated hydrochloric acid, by concentrated hydrochloric acid
It pours into deionized water, is uniformly mixed, add chromium oxide, and stir and be completely dissolved to chromium oxide, the depth can be obtained
Corrosive liquid.
The step 2 is specifically implemented according to the following steps:
Step 2.1, the alloy after high-temperature process is subjected to Wire EDM, when cutting along and tissue growth direction be in 0 °
~90 ° of direction carries out, if obtaining section dry sample different from tissue growth orientation angle；The alloy is directional solidification side
Method preparation, the high-temperature process temperature are 1100~1250 DEG C, and the high-temperature process time is 50~400h；
Step 2.2, the sample cut in step 2.1 is polished with sand paper；The detailed process of polishing is sample
Waterproof abrasive paper successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh is polished；
Step 2.3, the sample polished is polished on polishing machine using diamond polishing cream；Using 3.5 granularities
Or 5.0 granularity diamond polishing cream.
Etching time in the step 3 is specifically, different from tissue growth orientation angle for section, described
Etching time specifically:
It is in 90 ° of cross section sample for section and the direction of growth, etching time is 12~for 24 hours；
Angle for section and the direction of growth is the oblique section sample of x (0 ° of 90 ° of < x <), etching time is 12~
24h；
The longitudinal section sample that angle for section and the direction of growth is 0 °, etching time are 5~12h.
The invention has the advantages that use prepared with directional freeze method it is a kind of with the single direction of growth
NiAl-Cr (Mo) lamellar eutectic alloy is research object, provides a kind of judgement NiAl-Cr (Mo) lamellar eutectic alloy in high temperature
The method that real change is organized after processing, specifically includes a kind of preparation of NiAl-Cr (Mo) lamellar eutectic microstructure of the alloy corrosive liquid
Method；It further include a kind of deep etch method of NiAl-Cr (Mo) lamellar eutectic alloy.
Detailed description of the invention
Fig. 1 is that the tissue after deep etch is carried out to sample 1 using corrosive liquid and caustic solution of the invention；
Fig. 2 is that the tissue after deep etch is carried out to sample 2 using corrosive liquid and caustic solution of the invention；
Fig. 3 is that the tissue after deep etch is carried out to sample 3 using corrosive liquid and caustic solution of the invention；
Fig. 4 is that the tissue after deep etch is carried out to sample 4 using corrosive liquid and caustic solution of the invention；
Fig. 5 is that the tissue after deep etch is carried out to sample 5 using corrosive liquid and caustic solution of the invention；
Fig. 6 is the tissue for carrying out shallow corrosion front and back using the prior art to sample 1；
Fig. 7 is the tissue for carrying out shallow corrosion front and back using the prior art to sample 2；
Fig. 8 is the tissue for carrying out shallow corrosion front and back using the prior art to sample 3；
Fig. 9 is the tissue for carrying out shallow corrosion front and back using the prior art to sample 4；
Figure 10 is the tissue for carrying out shallow corrosion front and back using the prior art to sample 5.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of pair of nickel Al-Cr-Mo eutectic lamellar carries out the corrosive liquid of deep etch, is matched by chromium oxide, concentrated hydrochloric acid and deionized water
It makes, wherein the chromium oxide quality being added in every 10mL concentrated hydrochloric acid is 2.5~3.5g, the deionized water and concentrated hydrochloric acid
Volume ratio be 4~5:1；
Preferably, the chromium oxide is CrO3, mass fraction >=99%；
Preferably, the mass fraction of the concentrated hydrochloric acid is 36%~38%.
The method that a kind of pair of nickel Al-Cr-Mo eutectic lamellar carries out deep etch, is specifically implemented according to the following steps:
Step 1, corrosive liquid is configured, the ratio for being 2.5~3.5g according to the chromium oxide quality being added in every 10mL concentrated hydrochloric acid
Weigh chromium oxide；It is that 4~5:1 measures concentrated hydrochloric acid and deionized water according to deionized water and the volume ratio of concentrated hydrochloric acid, by concentrated hydrochloric acid
It pours into deionized water, is uniformly mixed, add chromium oxide, and stir and be completely dissolved to chromium oxide, the depth can be obtained
Corrosive liquid.
Step 2, it prepares sample to be corroded and is pre-processed,
Step 2.1, the alloy after high-temperature process is subjected to Wire EDM, when cutting along and tissue growth direction be in 0 °
~90 ° of direction carries out, if obtaining section dry sample different from tissue growth orientation angle；The alloy is directional solidification side
Method preparation, the high-temperature process temperature are 1100~1250 DEG C, and the high-temperature process time is 50~400h；
Step 2.2, the sample cut in step 2.1 is polished with sand paper；The detailed process of polishing is sample
Waterproof abrasive paper successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh is polished；
Step 2.3, the sample polished is polished on polishing machine using diamond polishing cream；Using 3.5 granularities
Or 5.0 granularity diamond polishing cream.
Step 3, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, etching time be 5~for 24 hours.
The etching time different from tissue growth orientation angle, described for section specifically:
It is in 90 ° of cross section sample for section and the direction of growth, etching time is 12~for 24 hours；
Angle for section and the direction of growth is the oblique section sample of x (0 ° of 90 ° of < x <), etching time is 12~
24h；
The longitudinal section sample that angle for section and the direction of growth is 0 °, etching time are 5~12h.
Step 4, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Sample after deep etch is subjected to observation analysis using scanning electron microscope, utilizes deep etch of the invention
After method handles sample, organization internal structure can be more clearly told, in observation, if observing cross section
There is not molten lamellar microstructure in (90 °) tissue and longitudinal section (0 °) tissue depth, then show synusia group after alloy high-temp processing
It knits and is not fully disconnected, and shallowly corrode conclusion and show that lamellar microstructure disconnects, real change is local dissolution；
If observing there is not molten lamellar microstructure in cross section (90 °) tissue and longitudinal section (0 °) tissue depth, and horizontal
Cr (Mo) phase morphology is mainly circle in section (90 °) tissue, and Cr (Mo) synusia in oblique section (x °) tissue is rendered as U-shaped circle
Column then organizes not nodularization (shallow corrosion conclusion shows tissue nodularization) after alloy high-temp processing, real change is tissue
It is cylindricity.
Embodiment 1
The corrosion liquid making method of this NiAl-Cr (Mo) lamellar eutectic microstructure of the alloy deep etch and the following institute of deep etch method
It states.
The preparation method of metallographic etchant: at room temperature, 40mL deionized water is measured with graduated cylinder, is poured into beaker.Dosage again
Cylinder measures concentrated hydrochloric acid 10mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.2.5g is then weighed on an electronic balance
Chromium oxide pours into beaker, and stirring is completely dissolved to chromium oxide, and the metallographic etchant, set aside for use can be obtained.
The method for carrying out deep etch using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy of directional solidification preparation is carried out to the high-temperature process of 1250 DEG C/50h
Afterwards, sample to be tested is intercepted using Wire EDM, in 90 ° and 0 ° of direction progress, is obtained along with tissue growth direction when cutting
To cross section tissue's sample and longitudinal section tissue sample；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, cross section sample, etching time
For 12h, longitudinal section sample, etching time 5.0h.
Step 3, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Step 4, the sample after deep etch is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after deep etch observed obtained by shown in cross section tissue such as Fig. 1 (a),
Longitudinal section tissue is as shown in Fig. 1 (b).As seen from Figure 1, cross section (90 °) tissue and longitudinal section (0 °) tissue depth presence be not molten
Lamellar microstructure, lamellar microstructure is not fully disconnected (shallow corrosion conclusion shows that lamellar microstructure disconnects) after alloy high-temp processing,
Therefore, real change is local dissolution.
Embodiment 2
The corrosion liquid making method of this NiAl-Cr (Mo) lamellar eutectic microstructure of the alloy deep etch and the following institute of deep etch method
It states.
The preparation method of metallographic etchant: at room temperature, 44mL deionized water is measured with graduated cylinder, is poured into beaker.Dosage again
Cylinder measures concentrated hydrochloric acid 10mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.2.8g is then weighed on an electronic balance
Chromium oxide pours into beaker, and stirring is completely dissolved to chromium oxide, and the metallographic etchant, set aside for use can be obtained.
The method for carrying out deep etch using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy of directional solidification preparation is carried out to the high-temperature process of 1150 DEG C/50h
Afterwards, sample to be tested is intercepted using Wire EDM, in 90 ° and 0 ° of direction progress, is obtained along with tissue growth direction when cutting
To cross section tissue's sample and longitudinal section tissue sample；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 3.5.
Step 2, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, cross section sample, etching time
For 12h, longitudinal section sample, etching time 12h.
Step 3, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Step 4, the sample after deep etch is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after deep etch observed obtained by shown in cross section tissue such as Fig. 2 (a),
Longitudinal section tissue is as shown in Fig. 2 (b).From Figure 2 it can be seen that cross section (90 °) tissue and longitudinal section (0 °) tissue depth presence be not molten
Lamellar microstructure, lamellar microstructure is not fully disconnected (shallow corrosion conclusion shows that lamellar microstructure disconnects) after alloy high-temp processing,
Therefore, real change is local dissolution.
Embodiment 3
The corrosion liquid making method of this NiAl-Cr (Mo) lamellar eutectic microstructure of the alloy deep etch and the following institute of deep etch method
It states.
The preparation method of metallographic etchant: at room temperature, 46mL deionized water is measured with graduated cylinder, is poured into beaker.Dosage again
Cylinder measures concentrated hydrochloric acid 10mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.3.0g is then weighed on an electronic balance
Chromium oxide pours into beaker, and stirring is completely dissolved to chromium oxide, and the metallographic etchant, set aside for use can be obtained.
The method for carrying out deep etch using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy by directional solidification preparation carries out at the high temperature of 1150 DEG C/100h
After reason, sample to be tested is intercepted using Wire EDM, when cutting along with tissue growth direction in 90 ° and 0 ° of direction progress,
Obtain cross section tissue's sample and longitudinal section tissue sample；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 3.5.
Step 2, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, cross section sample, etching time
For 18h, longitudinal section sample, etching time 8h.
Step 3, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Step 4, the sample after deep etch is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after deep etch observed obtained by shown in cross section tissue such as Fig. 3 (a),
Longitudinal section tissue is as shown in Fig. 3 (b).As seen from Figure 3, cross section (90 °) tissue and longitudinal section (0 °) tissue depth presence be not molten
Lamellar microstructure, lamellar microstructure is not fully disconnected (shallow corrosion conclusion shows that lamellar microstructure disconnects) after alloy high-temp processing,
Therefore, real change is local dissolution.
Embodiment 4
The corrosion liquid making method of this NiAl-Cr (Mo) lamellar eutectic microstructure of the alloy deep etch and the following institute of deep etch method
It states.
The preparation method of metallographic etchant: at room temperature, 48mL deionized water is measured with graduated cylinder, is poured into beaker.Dosage again
Cylinder measures concentrated hydrochloric acid 10mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.3.2g is then weighed on an electronic balance
Chromium oxide pours into beaker, and stirring is completely dissolved to chromium oxide, and the metallographic etchant, set aside for use can be obtained.
The method for carrying out deep etch using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy by directional solidification preparation carries out at the high temperature of 1150 DEG C/400h
After reason, sample to be tested is intercepted using Wire EDM, when cutting along with tissue growth direction in 90 °, 45 ° and 0 ° direction into
Row, obtains cross section tissue's sample, oblique section tissue sample and longitudinal section tissue sample；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, cross section sample etching time is
For 24 hours, sample etching time in oblique section is 18h, and longitudinal section sample etching time is 12h.
Step 3, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Step 4, the sample after deep etch is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after deep etch observed obtained by cross section tissue according to such as Fig. 4 (a) institute
Show, longitudinal section tissue is as shown in Fig. 4 (b), shown in bevel covering weave such as Fig. 4 (c).From fig. 4, it can be seen that cross section (90 °) tissue and
There is not molten lamellar microstructure in longitudinal section (0 °) tissue depth, and Cr (Mo) phase morphology is mainly in cross section (90 °) tissue
Circle, it is cylindric that Cr (Mo) synusia in oblique section (x °) tissue is rendered as U-shaped, therefore, organizes simultaneously after alloy high-temp processing
Non- nodularization (shallow corrosion conclusion shows tissue nodularization), real change is organizing cylindrical.
Embodiment 5
The corrosion liquid making method of this NiAl-Cr (Mo) lamellar eutectic microstructure of the alloy deep etch and the following institute of deep etch method
It states.
The preparation method of metallographic etchant: at room temperature, 50mL deionized water is measured with graduated cylinder, is poured into beaker.Dosage again
Cylinder measures concentrated hydrochloric acid 10mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.3.5g is then weighed on an electronic balance
Chromium oxide pours into beaker, and stirring is completely dissolved to chromium oxide, and the metallographic etchant, set aside for use can be obtained.
The method for carrying out deep etch using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy by directional solidification preparation carries out at the high temperature of 1100 DEG C/400h
After reason, sample to be tested is intercepted using Wire EDM, when cutting along with tissue growth direction in 90 °, 45 ° and 0 ° direction into
Row, obtains cross section tissue's sample, oblique section tissue sample and longitudinal section tissue sample；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, cross section sample etching time is
12h, oblique section sample etching time are 18h, and longitudinal section sample etching time is 12h.
Step 3, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
Step 4, the sample after deep etch is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after deep etch observed obtained by shown in cross section tissue such as Fig. 5 (a),
Longitudinal section tissue is as shown in Fig. 5 (b), shown in bevel covering weave such as Fig. 5 (c).As seen from Figure 5, it cross section (90 °) tissue and vertical cuts
There is not molten lamellar microstructure in face (0 °) tissue depth, and Cr (Mo) phase morphology is mainly circle in cross section (90 °) tissue,
It is cylindric that Cr (Mo) synusia in oblique section (x °) tissue is rendered as U-shaped, therefore, organizes not nodularization after alloy high-temp processing
(shallow corrosion conclusion shows tissue nodularization), real change is organizing cylindrical.
Comparative example 1
The corrosion liquid making method and caustic solution that this NiAl-Cr (Mo) lamellar eutectic alloy shallowly corrodes are as described below.
The preparation method of metallographic etchant: at room temperature, 25mL deionized water is measured with graduated cylinder, is poured into volumetric flask.It uses again
Graduated cylinder measures concentrated hydrochloric acid 40mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.Concentrated nitric acid is measured with graduated cylinder again
10mL is slowly poured into and is stirred continuously with glass bar, is uniformly mixed, the metallographic etchant, set aside for use can be obtained.
The method shallowly corroded using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy of directional solidification preparation is carried out to the high-temperature process of 1250 DEG C/50h
Afterwards, the sample before and after high-temperature process is intercepted using Wire EDM, when cutting along with tissue growth direction in 90 ° direction into
Row, obtains cross section tissue's sample before and after high-temperature process；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 3.5.
Step 2, after soaking absorbent cotton with above-mentioned metallographic etchant, nuzzled up rapidly polished specimen surface with absorbent cotton,
And water and alcohol rinse are used immediately, finally specimen surface is dried up.
Step 3, the sample after shallow corrosion is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after shallow corrosion observed obtained by cast alloy cross section tissue such as
Shown in Fig. 6 (a), after high-temperature process shown in cross section tissue such as Fig. 6 (b), it is only capable of seeing Cr (Mo) layer on surface layer from Fig. 6 (b)
Piece disconnects, and can not see that (deep etch conclusion shows Cr (Mo) phase that deep layer can be observed, i.e. Cr (Mo) for Cr (Mo) phase of deep layer
Local dissolution mutually has occurred), the shallow corrosion of this explanation cannot characterize the real change of lamellar microstructure.
Comparative example 2
The corrosion liquid making method and caustic solution that this NiAl-Cr (Mo) lamellar eutectic alloy shallowly corrodes are as described below.
The preparation method of metallographic etchant: at room temperature, 25mL deionized water is measured with graduated cylinder, is poured into volumetric flask.It uses again
Graduated cylinder measures concentrated hydrochloric acid 40mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.Concentrated nitric acid is measured with graduated cylinder again
10mL is slowly poured into and is stirred continuously with glass bar, is uniformly mixed, the metallographic etchant, set aside for use can be obtained.
The method shallowly corroded using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy of directional solidification preparation is carried out to the high-temperature process of 1150 DEG C/50h
Afterwards, the sample before and after high-temperature process is intercepted using Wire EDM, when cutting along with tissue growth direction in 90 ° direction into
Row, obtains cross section tissue's sample before and after high-temperature process；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, after soaking absorbent cotton with above-mentioned metallographic etchant, nuzzled up rapidly polished specimen surface with absorbent cotton,
And water and alcohol rinse are used immediately, finally specimen surface is dried up.
Step 3, the sample after shallow corrosion is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after shallow corrosion observed obtained by cast alloy cross section tissue such as
Shown in Fig. 7 (a), after high-temperature process shown in cross section tissue such as Fig. 7 (b), it is only capable of seeing Cr (Mo) layer on surface layer from Fig. 7 (b)
Piece disconnects, and can not see that (deep etch conclusion shows Cr (Mo) phase that deep layer can be observed, i.e. Cr (Mo) for Cr (Mo) phase of deep layer
Local dissolution mutually has occurred), the shallow corrosion of this explanation cannot characterize the real change of lamellar microstructure.
Comparative example 3
The corrosion liquid making method and caustic solution that this NiAl-Cr (Mo) lamellar eutectic alloy shallowly corrodes are as described below.
The preparation method of metallographic etchant: at room temperature, 25mL deionized water is measured with graduated cylinder, is poured into volumetric flask.It uses again
Graduated cylinder measures concentrated hydrochloric acid 40mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.Concentrated nitric acid is measured with graduated cylinder again
10mL is slowly poured into and is stirred continuously with glass bar, is uniformly mixed, the metallographic etchant, set aside for use can be obtained.
The method shallowly corroded using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy by directional solidification preparation carries out at the high temperature of 1150 DEG C/100h
After reason, the sample before and after high-temperature process is intercepted using Wire EDM, along the direction for tissue growth direction being in 90 ° when cutting
It carries out, obtains cross section tissue's sample before and after high-temperature process；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, after soaking absorbent cotton with above-mentioned metallographic etchant, nuzzled up rapidly polished specimen surface with absorbent cotton,
And water and alcohol rinse are used immediately, finally specimen surface is dried up.
Step 3, the sample after shallow corrosion is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after shallow corrosion observed obtained by cast alloy cross section tissue such as
Shown in Fig. 8 (a), after high-temperature process shown in cross section tissue such as Fig. 8 (b), it is only capable of seeing Cr (Mo) layer on surface layer from Fig. 8 (b)
Piece disconnects, and can not see that (deep etch conclusion shows Cr (Mo) phase that deep layer can be observed, i.e. Cr (Mo) for Cr (Mo) phase of deep layer
Local dissolution mutually has occurred), the shallow corrosion of this explanation cannot characterize the real change of lamellar microstructure.
Comparative example 4
The corrosion liquid making method and caustic solution that this NiAl-Cr (Mo) lamellar eutectic alloy shallowly corrodes are as described below.
The preparation method of metallographic etchant: at room temperature, 25mL deionized water is measured with graduated cylinder, is poured into volumetric flask.It uses again
Graduated cylinder measures concentrated hydrochloric acid 40mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.Concentrated nitric acid is measured with graduated cylinder again
10mL is slowly poured into and is stirred continuously with glass bar, is uniformly mixed, the metallographic etchant, set aside for use can be obtained.
The method shallowly corroded using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy by directional solidification preparation carries out at the high temperature of 1150 DEG C/400h
After reason, the sample before and after high-temperature process is intercepted using Wire EDM, along the direction for tissue growth direction being in 90 ° when cutting
It carries out, obtains cross section tissue's sample before and after high-temperature process；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, after soaking absorbent cotton with above-mentioned metallographic etchant, nuzzled up rapidly polished specimen surface with absorbent cotton,
And water and alcohol rinse are used immediately, finally specimen surface is dried up.
Step 3, the sample after shallow corrosion is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after shallow corrosion observed obtained by cast alloy cross section tissue such as
Shown in Fig. 9 (a), after high-temperature process shown in cross section tissue such as Fig. 9 (b), it is only capable of seeing surface layer Cr (Mo) phase shape from Fig. 9 (b)
Circle is mainly presented in looks, i.e. nodularization mutually has occurred in Cr (Mo), and cannot see that Cr (Mo) phase of deep layer (deep etch conclusion is shown can
Observe Cr (Mo) phase of deep layer, nodularization mutually not occurs for Cr (Mo) but cylindricity), the shallow corrosion of this explanation cannot characterize synusia
The real change of tissue.
Comparative example 5
The corrosion liquid making method and caustic solution that this NiAl-Cr (Mo) lamellar eutectic alloy shallowly corrodes are as described below.
The preparation method of metallographic etchant: at room temperature, 25mL deionized water is measured with graduated cylinder, is poured into volumetric flask.It uses again
Graduated cylinder measures concentrated hydrochloric acid 40mL, slowly pours into and is stirred continuously with glass bar, is uniformly mixed.Concentrated nitric acid is measured with graduated cylinder again
10mL is slowly poured into and is stirred continuously with glass bar, is uniformly mixed, the metallographic etchant, set aside for use can be obtained.
The method shallowly corroded using above-mentioned corrosive liquid, is specifically implemented according to the following steps:
Step 1, it prepares sample to be corroded and is pre-processed,
Step 1.1, the NiAl-28Cr-6Mo eutectic alloy by directional solidification preparation carries out at the high temperature of 1100 DEG C/400h
After reason, the sample before and after high-temperature process is intercepted using Wire EDM, along the direction for tissue growth direction being in 90 ° when cutting
It carries out, obtains cross section tissue's sample before and after high-temperature process；
Step 1.2, by the sample cut in step 1.1 successively through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500
Mesh, 2000 mesh waterproof abrasive paper polish；
Step 1.3, the sample polished is polished on polishing machine using the diamond polishing cream that granularity is 5.0.
Step 2, after soaking absorbent cotton with above-mentioned metallographic etchant, nuzzled up rapidly polished specimen surface with absorbent cotton,
And water and alcohol rinse are used immediately, finally specimen surface is dried up.
Step 3, the sample after shallow corrosion is subjected to observation analysis using scanning electron microscope.
Using scanning electron microscope to the sample after shallow corrosion observed obtained by cast alloy cross section tissue such as
Shown in Figure 10 (a), after high-temperature process shown in cross section tissue such as Figure 10 (b), it is only capable of seeing surface layer Cr (Mo) phase from Figure 10 (b)
Circle is presented in pattern more, i.e. nodularization mutually has occurred in Cr (Mo), and cannot see that Cr (Mo) phase of deep layer (deep etch conclusion is shown can
Observe Cr (Mo) phase of deep layer, nodularization mutually not occurs for Cr (Mo) but cylindricity), the shallow corrosion of this explanation cannot characterize synusia
The real change of tissue.
Claims (5)
1. the method that pair nickel Al-Cr-Mo eutectic lamellar carries out deep etch, which is characterized in that be specifically implemented according to the following steps:
Step 1, corrosive liquid is configured, corrosive liquid is formulated by chromium oxide, concentrated hydrochloric acid and deionized water, wherein every dense salt of 10mL
The chromium oxide quality being added in acid is 2.5~3.5g, and the volume ratio of deionized water and concentrated hydrochloric acid is 4~5:1；
Step 2, it prepares sample to be corroded and is pre-processed；
Step 3, polished sample is put into above-mentioned corrosive liquid and carries out deep etch, etching time be 5~for 24 hours, for cut
Face is different from tissue growth orientation angle, the etching time specifically:
It is in 90 ° of cross section sample for section and the direction of growth, etching time is 12~for 24 hours；
The oblique section sample that angle for section and the direction of growth is x, wherein 0 ° of 90 ° of < x <, etching time is 12~for 24 hours；
The longitudinal section sample that angle for section and the direction of growth is 0 °, etching time are 5~12h；
Step 4, water and alcohol rinse are used after taking out sample, finally dries up specimen surface.
2. the method according to claim 1 for carrying out deep etch to nickel Al-Cr-Mo eutectic lamellar, which is characterized in that the step
Chromium oxide is CrO3, mass fraction >=99% in rapid 1.
3. the method according to claim 1 for carrying out deep etch to nickel Al-Cr-Mo eutectic lamellar, which is characterized in that the step
The mass fraction of concentrated hydrochloric acid is 36%~38% in rapid 1.
4. the method according to claim 1 for carrying out deep etch to nickel Al-Cr-Mo eutectic lamellar, which is characterized in that described
Step 1 specifically: weigh chromium oxide according to the ratio that the chromium oxide quality being added in every 10mL concentrated hydrochloric acid is 2.5~3.5g；It presses
It is that 4~5:1 measures concentrated hydrochloric acid and deionized water according to deionized water and the volume ratio of concentrated hydrochloric acid, concentrated hydrochloric acid is poured into deionized water
In, it is uniformly mixed, adds chromium oxide, and stir and be completely dissolved to chromium oxide, the deep etch liquid can be obtained.
5. the method according to claim 1 for carrying out deep etch to nickel Al-Cr-Mo eutectic lamellar, which is characterized in that described
Step 2 is specifically implemented according to the following steps:
Step 2.1, the alloy after high-temperature process is subjected to Wire EDM, when cutting along with tissue growth direction in 0 °~
90 ° of direction carries out, if obtaining section dry sample different from tissue growth orientation angle；The alloy is directional freeze method
Preparation, the high-temperature process temperature are 1100~1250 DEG C, and the high-temperature process time is 50~400h；
Step 2.2, the sample cut in step 2.1 is polished with sand paper；The detailed process of polishing is that sample is successively
Waterproof abrasive paper through 80 mesh, 240 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh is polished；
Step 2.3, the sample polished is polished on polishing machine using diamond polishing cream；Using 3.5 granularities or 5.0
The diamond polishing cream of granularity.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63105991A (en) * | 1986-10-22 | 1988-05-11 | Nippon Steel Corp | Production of high quality surface treated steel sheet for vessel having superior corrosion resistance, weldability and paintability |
| JPH04116192A (en) * | 1990-09-05 | 1992-04-16 | Nkk Corp | Surface-treated steel sheet for uncoated can having superior corrosion resistance and weldability and production thereof |
| CN102321849A (en) * | 2011-09-05 | 2012-01-18 | 广西盛隆冶金有限公司 | Preparation method of nickel-chrome alloy steel |
| CN105606426A (en) * | 2015-12-18 | 2016-05-25 | 北京有色金属研究总院 | Metallurgical analysis etching method of layered metal composite material |
| CN106480351A (en) * | 2016-12-08 | 2017-03-08 | 西安理工大学 | A kind of method preparing the excellent nickel Al-Cr-Mo eutectic alloy of thermal structure stability |
-
2017
- 2017-06-21 CN CN201710475930.6A patent/CN107389419B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63105991A (en) * | 1986-10-22 | 1988-05-11 | Nippon Steel Corp | Production of high quality surface treated steel sheet for vessel having superior corrosion resistance, weldability and paintability |
| JPH04116192A (en) * | 1990-09-05 | 1992-04-16 | Nkk Corp | Surface-treated steel sheet for uncoated can having superior corrosion resistance and weldability and production thereof |
| CN102321849A (en) * | 2011-09-05 | 2012-01-18 | 广西盛隆冶金有限公司 | Preparation method of nickel-chrome alloy steel |
| CN105606426A (en) * | 2015-12-18 | 2016-05-25 | 北京有色金属研究总院 | Metallurgical analysis etching method of layered metal composite material |
| CN106480351A (en) * | 2016-12-08 | 2017-03-08 | 西安理工大学 | A kind of method preparing the excellent nickel Al-Cr-Mo eutectic alloy of thermal structure stability |
Non-Patent Citations (3)
| Title |
|---|
| Effect of Withdrawal Rate and Gd on the Microstructures of Directionally Solidified NiAl-Cr(Mo) Hypereutectic Alloy;LEI WANG et al;《JOM》;20160106;第68卷(第3期);第1038页左栏至右栏第1段 * |
| EFFECTS OF CHEMICAL COMPOSITION ON SOLIDIFICATION, MICROSTRUCTURE AND HARDNESS OF Co-Cr-W-Ni and Co-Cr-Mo-Ni ALLOY SYSTEMS;R. Liu et al;《IJRRAS》;20101130;第5卷(第2期);第110-122也 * |
| Micromechanical study on the deformation behavior of directionally solidified NiAl–Cr eutectic composites;Amritesh Kumar et al;《Journal of materials research》;20170214;第32卷(第11期);第2128-2129页第C小节 * |
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