CN109459284A - A kind of vanadium-base alloy microstructure examination preparation method of sample - Google Patents
A kind of vanadium-base alloy microstructure examination preparation method of sample Download PDFInfo
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- CN109459284A CN109459284A CN201811325223.XA CN201811325223A CN109459284A CN 109459284 A CN109459284 A CN 109459284A CN 201811325223 A CN201811325223 A CN 201811325223A CN 109459284 A CN109459284 A CN 109459284A
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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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Abstract
The invention discloses a kind of vanadium-base alloy microstructure examination preparation method of sample, comprising: step 1. samples on vanadium-base alloy material；Sample is embedded on resin matrix by step 2.；Step 3. carries out polishing processing to the sample on resin matrix by setting sequence by a variety of different sand paper；Step 4. is processed by shot blasting by a variety of different polishing agents by the good sample of setting sequence opposite grinding light processing using lubricant；The good sample of polishing treatment is first corroded 10~70s by step 5. in corrosive agent, again with saturation borax solution in and corrosive agent, then sample is taken out and successively sample is cleaned respectively with clear water and dehydrated alcohol, finally by clean sample drying to get the metallographic specimen of microstructure examination analysis.The present invention efficiently solves vanadium-base alloy and is easy the technical issues of scaling-off and sand grains is embedded in sample preparation, and then reliably improves sample mass easyly, and display effect of the sample when subsequent survey is analyzed is good.
Description
Technical field
The present invention relates to microstructure examination technology, prepared by the sample of specifically a kind of vanadium-base alloy microstructure examination
Method.
Background technique
Vanadium-base alloy has excellent anti-neutron irradiation stability, low activation characteristic, hydrogen embrittlement, low heat expansion, resistance to
The features such as liquid metal corrosion, high thermal conductivity, is acknowledged as comparatively ideal fusion reactor structural material, in core in the world
Industry, aerospace, high-temperature field etc. all have broad application prospects.
In order to the quantitative relationship being well understood between the microscopic structure of metal material and various performances, need to metal
The metallographic structure of material is tested analysis, and the check analysis of metallographic structure is realized on the basis of sample preparation, that is to say, that
Metallographic sample preparation quality directly affects the correctness of inspection result, and metallographic sample preparation generally includes following technical process: this
Body sampling-sample inlays-sample polishing-sample polishing-sample etches etc., the microstructure examination analysis of vanadium-base alloy be also as
This.
However, since vanadium-base alloy quality is relatively soft tough, if its metallographic sample preparation technological measure is according to common steel metallographic system
Sampling technology is implemented like that, then vanadium-base alloy sample will be embedded in sand grains at polishing processing initial stage and form large area smears paste layer,
This will affect subsequent polishing and polishing treatment effect, and then just will affect the sample quality of vanadium-base alloy, i.e. influence vanadium base closes
The check analysis display effect of golden sample.
It can be seen that the particularity based on vanadium-base alloy, the sample of vanadium-base alloy microstructure examination is prepared than general
The sample technology of preparing of logical steel material microstructure examination is much more difficult, in order to effectively promote, using vanadium-base alloy, it would be highly desirable to
A kind of reliable microstructure examination sample preparation side easy, sample quality is high, display effect is good is researched and developed for vanadium-base alloy
Method, to ensure the reliability and accuracy of subsequent vanadium-base alloy microstructure examination analyzing evaluation result.
Summary of the invention
Technical purpose of the invention is: particularity and existing vanadium-base alloy metallographic structure inspection for above-mentioned vanadium-base alloy
The sample making technology tested is insufficient, the independent research one for vanadium-base alloy (including but not limited to vanadium evanohm and vanadium chromium titanium alloy)
The reliable metallographic structure preparation method of sample easy, sample quality is high, display effect is good of kind.
The present invention realizes technical solution used by its technical purpose, a kind of vanadium-base alloy microstructure examination sample system
Preparation Method, the preparation method includes following process steps:
Step 1. samples on vanadium-base alloy material；
Sample is embedded on resin matrix by step 2.；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process to sample using 120# waterproof abrasive paper, grinding depth is 0.3~0.6 mm；
2. is ground sample using 400# abrasive paper for metallograph, grinding removal is with a thickness of 0.15~0.45 mm；
3. is ground sample using 600# abrasive paper for metallograph, grinding removal is with a thickness of 0.05~0.1 mm；
4. is ground sample using 1000# abrasive paper for metallograph, grinding removal is with a thickness of 0.003~0.007 mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting by using the agent of 6um diamond polishing on canvas fabric, the time of the polishing treatment is 3
~8min；
2. sample is processed by shot blasting using the agent of 2.5um diamond polishing by navy wool fabric fabric, the polishing treatment when
Between be 2~10min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
For 3~15min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be 1~10min；
The good sample of polishing treatment is first corroded 10~70s by step 5. in corrosive agent, then is neutralized with the borax solution of saturation
Then sample is taken out and is successively cleaned respectively to sample with clear water and dehydrated alcohol by corrosive agent, finally by clean sample
The metallographic specimen that product dry up to get microstructure examination analysis.
One of preferably, sampling is in a manner of Wire EDM in vanadium-base alloy material described in step 1
Upper cutting sampling.
One of preferably, sampling is cut on vanadium-base alloy material in a manner of emery wheel cuts described in step 1
Sample is extracted, cutting speed is 0.3~5 mm/min, and the grinding wheel uses aluminum oxide grinding wheel.
One of preferably, the hardness of resin matrix described in step 2 is 45~55 HRC.
One of preferably, each sand paper of processing is polished described in step 3 when sequence switches, the sample with
Transfer sequence and relative to polish direction make 45~135 ° rotation adjustment.
One of preferably, it is lubricated when in step 3 1. process is polished with water.
One of preferably, 1., 2. and 3. used lubricant is with the original of following parts by weight to process in step 4
Material composition:
10~30 parts of glycerol,
50~250 parts of ethyl alcohol,
0.5~5 part of neopelex,
200~500 parts of water.
One of preferably, 4. used lubricant is formed with the raw material of following parts by weight to process in step 4:
50~250 parts of ethyl alcohol,
50~400 parts of water.
One of preferably, corrosive agent described in step 5 is formed with the raw material of following parts by weight:
5~60 parts of hydrofluoric acid,
20~50 parts of nitric acid,
5~15 parts of hydrogen peroxide
50~200 parts of water.
The method have the benefit that: the present invention is directed to vanadium-base alloy (including but not limited to vanadium evanohm and vanadium chromium
Titanium alloy) particularity and by polishing technique and polishing process respectively with four different step process step designs, it is with strong points, have with this
Effect solves vanadium-base alloy and is easy the technical issues of scaling-off and sand grains is embedded in sample preparation, and then reliably effectively increases easyly
Sample mass, display effect of the sample when subsequent survey is analyzed is good, can reliably ensure subsequent vanadium-base alloy metallographic structure
The reliability and accuracy of check analysis evaluation result.
Detailed description of the invention
Fig. 1 is the microstructure examination photo that VCr2 alloy prepares gained sample with the embodiment of the present invention one.
Fig. 2 is the microstructure examination photo that VCrTi1 alloy prepares gained sample with the embodiment of the present invention two.
Fig. 3 is the microstructure examination photo that VCrTi4 alloy prepares gained sample with the embodiment of the present invention three.
Specific embodiment
The present invention relates to microstructure examination technology, prepared by the sample of specifically a kind of vanadium-base alloy microstructure examination
Method, below with multiple embodiments to technical solution of the present invention content make it is clear, explain in detail.
Embodiment 1
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCr2 alloy, and the present invention includes following process steps:
Step 1. cutting sampling on VCr2 alloy material, the sample size cut in a manner of Wire EDM are about
20mm×15mm；
By sample hot insert on resin matrix, the solidification hardness requirement of the resin matrix after hot insert is embedding remains about step 2.
48HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.5mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 90 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.3mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 90 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.1 mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 90 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.005mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 5min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 7min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 9min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 6min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 18
Part, 130 parts of ethyl alcohol, 3 parts of neopelex, 350 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 150 parts of ethyl alcohol, water 280
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 35 parts of hydrofluoric acid, 35 parts of nitric acid, hydrogen peroxide 8
Part, 120 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 30s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Gained sample is prepared with the present embodiment, is analyzed through microstructure examination, the photo of gained metallographic structure is shown in Fig. 1 institute
Show.
Embodiment 2
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi1 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi1 alloy material, the sample size cut in a manner of Wire EDM are about
20mm×15mm；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 50HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.4mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 80 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.25mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 80 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.08mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 60 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.006mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 6min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 6min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 8min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 7min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 20
Part, 160 parts of ethyl alcohol, 2 parts of neopelex, 300 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 100 parts of ethyl alcohol, water 200
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 20 parts of hydrofluoric acid, 20 parts of nitric acid, hydrogen peroxide 10
Part, 100 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 40s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Gained sample is prepared with the present embodiment, is analyzed through microstructure examination, the photo of gained metallographic structure is shown in Fig. 2 institute
Show.
Embodiment 3
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi4 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi4 alloy material, the sample size cut in a manner of Wire EDM are about
20mm×15mm；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 52HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.3mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 45 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.2mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 45 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.06mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 50 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.004mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 7min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 8min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 12min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 8min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 25
Part, 200 parts of ethyl alcohol, 4 parts of neopelex, 400 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 200 parts of ethyl alcohol, water 350
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 45 parts of hydrofluoric acid, 40 parts of nitric acid, hydrogen peroxide 12
Part, 170 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 10s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Gained sample is prepared with the present embodiment, is analyzed through microstructure examination, the photo of gained metallographic structure is shown in Fig. 3 institute
Show.
Embodiment 4
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCr2 alloy, and the present invention includes following process steps:
Step 1. cutting sampling on VCr2 alloy material, cutting speed in a manner of emery wheel cuts are about 3mm/min, the sand
There is anti abrasive aluminum oxide grinding wheel, the sample size cut is about 20mm × 15mm on wheel；
By sample hot insert on resin matrix, the solidification hardness requirement of the resin matrix after hot insert is embedding remains about step 2.
48HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.6mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 100 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.15mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 100 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.09mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 100 °, using 1000# abrasive paper for metallograph to sample
Product are ground by single direction, and grinding removal thickness is about 0.006mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 4min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 5min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 7min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 5min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 10
Part, 50 parts of ethyl alcohol, 1 part of neopelex, 200 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 50 parts of ethyl alcohol, 50 parts of water；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 10 parts of hydrofluoric acid, 25 parts of nitric acid, hydrogen peroxide 6
Part, 80 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 20s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 5
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi1 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi1 alloy material, cutting speed in a manner of emery wheel cuts are about 0.3mm/min,
There is aluminum oxide grinding wheel, the sample size cut is about 20mm × 15mm on grinding wheel；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 49HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.3mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 135 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.3mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 45 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.05mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 45 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.004mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 4min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 6min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 8min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 3min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight to process: 13 parts of glycerol,
55 parts of ethyl alcohol, 0.5 part of neopelex, 200 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight respectively to process: 85 parts of ethyl alcohol, water
110 parts；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 50 parts of hydrofluoric acid, 43 parts of nitric acid, hydrogen peroxide 5
Part, 110 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 25s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 6
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi4 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi4 alloy material in a manner of emery wheel cuts, cutting speed are about 5 mm/min, should
There is aluminum oxide grinding wheel, the sample size cut is about 20mm × 20mm on grinding wheel；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 55HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.3mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 70 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.15mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 70 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.06mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 70 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.003mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 8min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 10min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 15min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 10min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 17
Part, 90 parts of ethyl alcohol, 2 parts of neopelex, 280 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 175 parts of ethyl alcohol, water 230
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 5 parts of hydrofluoric acid, 30 parts of nitric acid, 7 parts of hydrogen peroxide,
50 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed；
The good sample of polishing treatment is first corroded into about 35s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 7
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCr2 alloy, and the present invention includes following process steps:
Step 1. cutting sampling on VCr2 alloy material, the sample size cut in a manner of Wire EDM are about
15mm×15mm；
By sample hot insert on resin matrix, the solidification hardness requirement of the resin matrix after hot insert is embedding remains about step 2.
46HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.6mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 100 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.45mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 100 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.1mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 55 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.007 mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 3min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 2min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 3min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 4min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 30
Part, 250 parts of ethyl alcohol, 0.5 part of neopelex, 450 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 220 parts of ethyl alcohol, water 360
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 40 parts of hydrofluoric acid, 50 parts of nitric acid, hydrogen peroxide 7
Part, 200 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 50s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 8
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi1 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi1 alloy material, the sample size cut in a manner of Wire EDM are about
25mm×15mm；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 45HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.5mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 120 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.4mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 120 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.07mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 120 °, using 1000# abrasive paper for metallograph to sample
Product are ground by single direction, and grinding removal thickness is about 0.005mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 5min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 4min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 15min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 1min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 27
Part, 210 parts of ethyl alcohol, 3 parts of neopelex, 500 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 165 parts of ethyl alcohol, water 195
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 60 parts of hydrofluoric acid, 28 parts of nitric acid, hydrogen peroxide 15
Part, 185 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 45s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 9
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi4 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi4 alloy material, the sample size cut in a manner of Wire EDM are about
25mm×25mm；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 50HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.4mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 90 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.35 mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 90 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.08mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 90 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.006mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 6min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 3min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 13min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 7min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 20
Part, 160 parts of ethyl alcohol, 2 parts of neopelex, 375 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 120 parts of ethyl alcohol, water 400
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 30 parts of hydrofluoric acid, 42 parts of nitric acid, hydrogen peroxide 10
Part, 90 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 70s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 10
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCr2 alloy, and the present invention includes following process steps:
Step 1. cutting sampling on VCr2 alloy material, the sample size cut in a manner of Wire EDM are about
20mm×15mm；
By sample hot insert on resin matrix, the solidification hardness requirement of the resin matrix after hot insert is embedding remains about step 2.
53HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.3mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 55 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.25mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 60 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.06mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 75 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.004mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 5min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 5min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 10min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 2min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 14
Part, 100 parts of ethyl alcohol, 1 part of neopelex, 250 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 250 parts of ethyl alcohol, water 380
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 25 parts of hydrofluoric acid, 36 parts of nitric acid, hydrogen peroxide 9
Part, 150 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 60s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 11
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi1 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi1 alloy material, the sample size cut in a manner of Wire EDM are about
20mm×15mm；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 49HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.4mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 60 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.3mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 60 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.07 mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 60 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.005mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 4min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 5min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 10min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 7min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 19
Part, 110 parts of ethyl alcohol, 2 parts of neopelex, 300 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 140 parts of ethyl alcohol, 90 parts of water；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 28 parts of hydrofluoric acid, 45 parts of nitric acid, hydrogen peroxide 11
Part, 190 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 60s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
Embodiment 12
The present invention carries out sample preparation based on the analysis of the microstructure examination of VCrTi4 alloy, and the present invention includes following process step
It is rapid:
Step 1. cutting sampling on VCrTi4 alloy material, the sample size cut in a manner of Wire EDM are about
20mm×15mm；
Step 2. is by sample hot insert on resin matrix, and hardness requirement remains after the solidification of the resin matrix after hot insert is embedding
About 51HRC；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process by single direction to sample using 120# waterproof abrasive paper, with water lubrication in bruting process, polishing is deep
Degree is about 0.5mm；
2. adjusts sample relative to the rotation that process polishing direction 1. makees about 110 °, using 400# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.35mm；
3. adjusts sample relative to the rotation that process polishing direction 2. makees about 100 °, using 600# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.06mm；
4. adjusts sample relative to the rotation that process polishing direction 3. makees about 45 °, using 1000# abrasive paper for metallograph to sample
It is ground by single direction, grinding removal thickness is about 0.006mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting that the time of the polishing treatment is about using the agent of 6um diamond polishing by canvas fabric
For 8min；
2. sample is processed by shot blasting by using the agent of 2.5um diamond polishing on navy wool fabric fabric (long wool), at the polishing
The time of reason is about 3min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
About 9min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be about 4min；
In this step, 1., 2. and 3. used lubricant is formed with the raw material of following parts by weight respectively to process: glycerol 23
Part, 180 parts of ethyl alcohol, 5 parts of neopelex, 390 parts of water；
In this step, 4. used lubricant is formed with the raw material of following parts by weight to process: 130 parts of ethyl alcohol, water 220
Part；
Step 5. prepares corrosive agent according to the raw material composition of following parts by weight: 15 parts of hydrofluoric acid, 30 parts of nitric acid, hydrogen peroxide 14
Part, 160 parts of water；Preparation process is: hydrofluoric acid, nitric acid and water being first uniformly mixed, then hydrogen peroxide is added and is uniformly mixed i.e.
It can；
The good sample of polishing treatment is first corroded into about 38s in corrosive agent, then in the borax solution being saturated and corrosive agent, so
Sample is taken out afterwards and successively sample is cleaned respectively with clear water and dehydrated alcohol, is finally dried up clean sample, i.e.,
Obtain the metallographic specimen of microstructure examination analysis.
The above various embodiments is only to illustrate the present invention, rather than its limitations.Although referring to the various embodiments described above to this hair
It is bright to be described in detail, those skilled in the art should understand that: the present invention still can be to the various embodiments described above
In specific technical solution modify perhaps equivalent replacement of some of the technical features and these modifications or replace
It changes, the spirit and scope of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of vanadium-base alloy microstructure examination preparation method of sample, which is characterized in that the preparation method includes following
Processing step:
Step 1. samples on vanadium-base alloy material；
Sample is embedded on resin matrix by step 2.；
Step 3. carries out polishing processing to the sample on resin matrix by following procedures:
1. carries out grinding process to sample using 120# waterproof abrasive paper, grinding depth is 0.3~0.6 mm；
2. is ground sample using 400# abrasive paper for metallograph, grinding removal is with a thickness of 0.15~0.45 mm；
3. is ground sample using 600# abrasive paper for metallograph, grinding removal is with a thickness of 0.05~0.1 mm；
4. is ground sample using 1000# abrasive paper for metallograph, grinding removal is with a thickness of 0.003~0.007 mm；
Step 4. is processed by shot blasting using lubricant by the good sample of following technical process opposite grinding light processing:
1. sample is processed by shot blasting by using the agent of 6um diamond polishing on canvas fabric, the time of the polishing treatment is 3
~8min；
2. sample is processed by shot blasting using the agent of 2.5um diamond polishing by navy wool fabric fabric, the polishing treatment when
Between be 2~10min；
3. sample is processed by shot blasting by using the agent of 0.5um diamond polishing on plain velvet fabric, the time of the polishing treatment
For 3~15min；
4. sample is carried out polishing treatment using 0.05um aluminum oxide polishing agent by spun gold pile fabric, the polishing treatment
Time be 1~10min；
The good sample of polishing treatment is first corroded 10~70s by step 5. in corrosive agent, then is neutralized with the borax solution of saturation
Then sample is taken out and is successively cleaned respectively to sample with clear water and dehydrated alcohol by corrosive agent, finally by clean sample
The metallographic specimen that product dry up to get microstructure examination analysis.
2. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 1
It is described sampling be in a manner of Wire EDM on vanadium-base alloy material cutting sampling.
3. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 1
The sampling is that cutting sampling, cutting speed are 0.3~5 mm/min, institute on vanadium-base alloy material in a manner of emery wheel cuts
It states grinding wheel and uses aluminum oxide grinding wheel.
4. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 2
The hardness of the resin matrix is 45~55 HRC.
5. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 3
For each sand paper of the polishing processing when sequence switches, with transfer sequence, opposite direction of polishing makees 45~135 ° to the sample
Rotation adjustment.
6. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 4
1., 2. and 3. used lubricant is formed with the raw material of following parts by weight to process:
10~30 parts of glycerol,
50~250 parts of ethyl alcohol,
0.5~5 part of neopelex,
200~500 parts of water.
7. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 4
4. used lubricant is formed with the raw material of following parts by weight to process:
50~250 parts of ethyl alcohol,
50~400 parts of water.
8. vanadium-base alloy microstructure examination preparation method of sample according to claim 1, which is characterized in that in step 5
The corrosive agent is formed with the raw material of following parts by weight:
5~60 parts of hydrofluoric acid,
20~50 parts of nitric acid,
5~15 parts of hydrogen peroxide
50~200 parts of water.
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