CN109459284B - Preparation method of test sample for vanadium-based alloy metallographic structure inspection - Google Patents
Preparation method of test sample for vanadium-based alloy metallographic structure inspection Download PDFInfo
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- CN109459284B CN109459284B CN201811325223.XA CN201811325223A CN109459284B CN 109459284 B CN109459284 B CN 109459284B CN 201811325223 A CN201811325223 A CN 201811325223A CN 109459284 B CN109459284 B CN 109459284B
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Abstract
The invention discloses a method for preparing a sample for vanadium-based alloy metallographic structure inspection, which comprises the following steps: step 1, sampling on a vanadium-based alloy material; 2, inlaying the sample on a resin matrix; step 3, polishing the samples on the resin matrix by a plurality of different abrasive papers according to a set sequence; step 4, polishing the polished sample by adopting a lubricant through a plurality of different polishing agents according to a set sequence; and 5, eroding the polished sample in a corrosive agent for 10-70 s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain the metallographic sample for metallographic structure inspection and analysis. The invention effectively solves the technical problems that the vanadium-based alloy is easy to drop slag and embed sand grains when preparing a sample, thereby reliably and easily improving the quality of the sample and having good display effect of the sample during subsequent inspection and analysis.
Description
Technical Field
The invention relates to a metallographic structure inspection technology, in particular to a sample preparation method for metallographic structure inspection of vanadium-based alloy.
Background
The vanadium-based alloy has the characteristics of excellent neutron irradiation resistance stability, low activation characteristic, hydrogen embrittlement resistance, low thermal expansion, liquid metal corrosion resistance, high heat transfer rate and the like, is internationally recognized as an ideal fusion reactor structural material, and has wide application prospects in the fields of nuclear industry, aerospace, high temperature and the like.
In order to clearly understand the quantitative relationship between the microstructure and various properties of the metal material, the metallographic structure of the metal material needs to be inspected and analyzed, and the inspection and analysis of the metallographic structure are realized on the basis of sample preparation, that is, the correctness of the metallographic sample preparation directly affects the correctness of the inspection result, and the metallographic sample preparation generally comprises the following main process flows: bulk sampling-sample inlaying-sample polishing-sample corrosion, etc., as well as metallographic structure examination analysis of vanadium-based alloys.
However, because the vanadium-based alloy is soft and tough in texture, if the metallographic sample preparation process is performed as the metallographic sample preparation process of ordinary steel, sand grains are embedded into the vanadium-based alloy sample at the initial stage of polishing treatment, and a large-area smear layer is formed, which affects the subsequent polishing and polishing treatment effects, and further affects the sample preparation quality of the vanadium-based alloy, namely, the inspection analysis display effect of the vanadium-based alloy sample.
Therefore, based on the particularity of the vanadium-based alloy, the preparation of the sample for the metallographic structure examination of the vanadium-based alloy is more difficult than the preparation technology of the sample for the metallographic structure examination of the common steel material, and in order to effectively popularize and apply the vanadium-based alloy, the research and development of the preparation method of the sample for the metallographic structure examination of the vanadium-based alloy, which is reliable and easy to implement, high in sample preparation quality and good in display effect, is urgently needed so as to ensure the reliability and the accuracy of the subsequent metallographic structure examination, analysis and evaluation result of the vanadium-based alloy.
Disclosure of Invention
The technical purpose of the invention is as follows: aiming at the particularity of the vanadium-based alloy and the defects of the sample preparation technology for the metallographic structure inspection of the existing vanadium-based alloy, a reliable and feasible sample preparation method for the metallographic structure, high sample preparation quality and good display effect is independently developed for vanadium-based alloys (including but not limited to vanadium-chromium alloys and vanadium-chromium-titanium alloys).
The invention discloses a method for preparing a sample for vanadium-based alloy metallographic structure inspection, which adopts the technical scheme for realizing the technical purpose, and comprises the following process steps:
step 1, sampling on a vanadium-based alloy material;
2, inlaying the sample on a resin matrix;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample by using No. 120 waterproof abrasive paper, wherein the polishing depth is 0.3-0.6 mm;
secondly, grinding the sample by using No. 400 metallographic abrasive paper, wherein the thickness of the ground sample is 0.15-0.45 mm;
grinding the sample by using No. 600 metallographic abrasive paper, wherein the thickness of the ground sample is 0.05-0.1 mm;
grinding the sample by using No. 1000 metallographic abrasive paper, wherein the thickness of the ground sample is 0.003-0.007 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6-micron diamond polishing agent for 3-8 min;
secondly, polishing the sample on the navy fabric by adopting a 2.5um diamond polishing agent for 2-10 min;
polishing the sample on the velveteen fabric by adopting a 0.5um diamond polishing agent for 3-15 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent for 1-10 min;
and 5, eroding the polished sample in a corrosive agent for 10-70 s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain the metallographic sample for metallographic structure inspection and analysis.
Preferably, in the step 1, the sampling is performed by cutting and sampling on the vanadium-based alloy material in a wire-cut electric discharge manner.
As one of the preferable schemes, in the step 1, the sampling is performed by cutting and sampling on the vanadium-based alloy material in a grinding wheel cutting mode, the cutting speed is 0.3-5 mm/min, and an aluminum oxide grinding wheel is used as the grinding wheel.
Preferably, the resin matrix in the step 2 has a hardness of 45 to 55 HRC.
Preferably, when the sandpaper subjected to the polishing treatment in step 3 is sequentially switched, the sample is rotationally adjusted by 45 to 135 degrees with respect to the polishing direction along with the switching sequence.
As one preferable scheme, water is used for lubrication during grinding in the process (I) in the step 3.
As one of the preferable schemes, the lubricant adopted in the processes I, II and III in the step 4 is composed of the following raw materials in parts by weight:
10-30 parts of glycerol,
50-250 parts of ethanol,
0.5 to 5 parts of sodium dodecyl benzene sulfonate,
200-500 parts of water.
Preferably, the lubricant used in the step (4) is prepared from the following raw materials in parts by weight:
50-250 parts of ethanol,
50-400 parts of water.
As one preferable scheme, the corrosive agent in the step 5 is composed of the following raw materials in 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 beneficial technical effects of the invention are as follows: the invention designs the polishing process and the polishing process by four different procedures aiming at the particularity of vanadium-based alloy (including but not limited to vanadium-chromium alloy and vanadium-chromium-titanium alloy), has strong pertinence, effectively solves the technical problems of easy slag falling and sand embedding of the vanadium-based alloy during sample preparation, further reliably and easily improves the quality of a sample, has good display effect of the sample during subsequent inspection and analysis, and can reliably ensure the reliability and the accuracy of the subsequent metallographic structure inspection and analysis evaluation result of the vanadium-based alloy.
Drawings
FIG. 1 is a photograph of a metallographic examination of a sample of an alloy VCr2 prepared in accordance with one embodiment of the present invention.
FIG. 2 is a photograph of a metallographic examination of a sample of VCrTi1 alloy prepared according to example two of the present invention.
FIG. 3 is a photograph of a metallographic examination of a sample of VCrTi4 alloy prepared according to example three of the present invention.
Detailed Description
The invention relates to a metallographic structure inspection technology, in particular to a sample preparation method for a metallographic structure inspection of vanadium-based alloy, and the technical scheme content of the invention is clearly and specifically explained in detail by using a plurality of embodiments.
Example 1
The invention takes the metallographic structure inspection and analysis of the VCr2 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCr2 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the curing hardness requirement of the thermally inlaid resin matrix is kept to be about 48 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.5 mm;
rotating the sample by about 90 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.3 mm;
rotating the sample by about 90 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.1 mm;
rotating the sample by about 90 degrees relative to the polishing direction of the working procedure, and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.005 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 5 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 7 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 9 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 6 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 18 parts of glycerol, 130 parts of ethanol, 3 parts of sodium dodecyl benzene sulfonate and 350 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 150 parts of ethanol and 280 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 35 parts of hydrofluoric acid, 35 parts of nitric acid, 8 parts of hydrogen peroxide and 120 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 30s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
The sample obtained in this example was prepared and analyzed by metallographic examination, and the photograph of the metallographic structure obtained is shown in FIG. 1.
Example 2
The invention takes the metallographic structure inspection and analysis of VCrTi1 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi1 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 50 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.4 mm;
rotating the sample by about 80 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.25 mm;
rotating the sample by about 80 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.08 mm;
rotating the sample by about 60 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.006 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 6 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 6 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 8 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 7 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 20 parts of glycerol, 160 parts of ethanol, 2 parts of sodium dodecyl benzene sulfonate and 300 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 100 parts of ethanol and 200 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 20 parts of hydrofluoric acid, 20 parts of nitric acid, 10 parts of hydrogen peroxide and 100 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 40s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
The sample obtained in this example was prepared and analyzed by metallographic examination, and the photograph of the metallographic structure obtained is shown in FIG. 2.
Example 3
The invention takes the metallographic structure inspection and analysis of VCrTi4 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi4 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 52 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.3 mm;
rotating the sample by about 45 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.2 mm;
rotating the sample by about 45 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper according to a single direction to remove the thickness of about 0.06 mm;
rotating the sample by about 50 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.004 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 7 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 8 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 12 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 8 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 25 parts of glycerol, 200 parts of ethanol, 4 parts of sodium dodecyl benzene sulfonate and 400 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 200 parts of ethanol and 350 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 45 parts of hydrofluoric acid, 40 parts of nitric acid, 12 parts of hydrogen peroxide and 170 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 10s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
The sample obtained in this example was prepared and analyzed by metallographic examination, and the photograph of the metallographic structure obtained is shown in FIG. 3.
Example 4
The invention takes the metallographic structure inspection and analysis of the VCr2 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCr2 alloy material in a grinding wheel cutting mode, wherein the cutting speed is about 3mm/min, a wear-resistant aluminum oxide grinding wheel is arranged on the grinding wheel, and the size of a cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the curing hardness requirement of the thermally inlaid resin matrix is kept to be about 48 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.6 mm;
rotating the sample by about 100 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.15 mm;
rotating the sample by about 100 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.09 mm;
rotating the sample by about 100 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.006 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 4 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 5 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 7 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 5 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 10 parts of glycerol, 50 parts of ethanol, 1 part of sodium dodecyl benzene sulfonate and 200 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 50 parts of ethanol and 50 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 10 parts of hydrofluoric acid, 25 parts of nitric acid, 6 parts of hydrogen peroxide and 80 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 20s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 5
The invention takes the metallographic structure inspection and analysis of VCrTi1 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi1 alloy material in a grinding wheel cutting mode, wherein the cutting speed is about 0.3mm/min, an aluminum oxide grinding wheel is arranged on the grinding wheel, and the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 49 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.3 mm;
rotating the sample by about 135 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.3 mm;
rotating the sample by about 45 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.05 mm;
rotating the sample by about 45 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.004 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 4 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 6 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 8 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 3 min;
in the step, the lubricant adopted in the working procedures I, II and III is composed of the following raw materials in parts by weight: 13 parts of glycerol, 55 parts of ethanol, 0.5 part of sodium dodecyl benzene sulfonate and 200 parts of water;
in the step, the lubricant adopted in the procedure IV is respectively composed of the following raw materials in parts by weight: 85 parts of ethanol and 110 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 50 parts of hydrofluoric acid, 43 parts of nitric acid, 5 parts of hydrogen peroxide and 110 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 25s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 6
The invention takes the metallographic structure inspection and analysis of VCrTi4 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi4 alloy material in a grinding wheel cutting mode, wherein the cutting speed is about 5 mm/min, an aluminum oxide grinding wheel is arranged on the grinding wheel, and the size of a cut sample is about 20mm multiplied by 20 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 55 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.3 mm;
rotating the sample by about 70 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.15 mm;
rotating the sample by about 70 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.06 mm;
rotating the sample by about 70 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.003 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 8 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 10 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent, wherein the polishing time is about 15 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 10 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 17 parts of glycerol, 90 parts of ethanol, 2 parts of sodium dodecyl benzene sulfonate and 280 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 175 parts of ethanol and 230 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 5 parts of hydrofluoric acid, 30 parts of nitric acid, 7 parts of hydrogen peroxide and 50 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 35 seconds, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 7
The invention takes the metallographic structure inspection and analysis of the VCr2 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCr2 alloy material in a wire cut electrical discharge machining mode, wherein the size of a cut sample is about 15mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the curing hardness requirement of the thermally inlaid resin matrix is kept to be about 46 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.6 mm;
rotating the sample by about 100 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.45 mm;
rotating the sample by about 100 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.1 mm;
rotating the sample by about 55 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.007 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 3 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 2 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 3 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 4 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 30 parts of glycerol, 250 parts of ethanol, 0.5 part of sodium dodecyl benzene sulfonate and 450 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 220 parts of ethanol and 360 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 40 parts of hydrofluoric acid, 50 parts of nitric acid, 7 parts of hydrogen peroxide and 200 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 50s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 8
The invention takes the metallographic structure inspection and analysis of VCrTi1 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi1 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 25mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 45 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.5 mm;
rotating the sample by about 120 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.4 mm;
rotating the sample by about 120 degrees relative to the polishing direction of the working procedure II, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.07 mm;
rotating the sample by about 120 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.005 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 5 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 4 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent, wherein the polishing time is about 15 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 1 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 27 parts of glycerol, 210 parts of ethanol, 3 parts of sodium dodecyl benzene sulfonate and 500 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 165 parts of ethanol and 195 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 60 parts of hydrofluoric acid, 28 parts of nitric acid, 15 parts of hydrogen peroxide and 185 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 45s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 9
The invention takes the metallographic structure inspection and analysis of VCrTi4 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi4 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 25mm multiplied by 25 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 50 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.4 mm;
rotating the sample by about 90 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.35 mm;
rotating the sample by about 90 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.08 mm;
rotating the sample by about 90 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.006 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 6 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 3 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent, wherein the polishing time is about 13 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 7 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 20 parts of glycerol, 160 parts of ethanol, 2 parts of sodium dodecyl benzene sulfonate and 375 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 120 parts of ethanol and 400 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 30 parts of hydrofluoric acid, 42 parts of nitric acid, 10 parts of hydrogen peroxide and 90 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 70s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 10
The invention takes the metallographic structure inspection and analysis of the VCr2 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCr2 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the curing hardness requirement of the thermally inlaid resin matrix is kept to be about 53 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.3 mm;
rotating the sample by about 55 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.25 mm;
rotating the sample by about 60 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.06 mm;
rotating the sample by about 75 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.004 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 5 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 5 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 10 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 2 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 14 parts of glycerol, 100 parts of ethanol, 1 part of sodium dodecyl benzene sulfonate and 250 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 250 parts of ethanol and 380 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 25 parts of hydrofluoric acid, 36 parts of nitric acid, 9 parts of hydrogen peroxide and 150 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 60s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 11
The invention takes the metallographic structure inspection and analysis of VCrTi1 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi1 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the cured hardness requirement of the thermally inlaid resin matrix is kept to be about 49 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.4 mm;
rotating the sample by about 60 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.3 mm;
rotating the sample by about 60 degrees relative to the polishing direction of the working procedure II, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.07 mm;
rotating the sample by about 60 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.005 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 4 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 5 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 10 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 7 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 19 parts of glycerol, 110 parts of ethanol, 2 parts of sodium dodecyl benzene sulfonate and 300 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 140 parts of ethanol and 90 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 28 parts of hydrofluoric acid, 45 parts of nitric acid, 11 parts of hydrogen peroxide and 190 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
corroding the polished sample in a corrosive agent for about 60s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain a metallographic specimen for metallographic structure inspection and analysis.
Example 12
The invention takes the metallographic structure inspection and analysis of VCrTi4 alloy as the basis to prepare samples, and the invention comprises the following process steps:
step 1, cutting and sampling on a VCrTi4 alloy material in a wire cut electrical discharge machining mode, wherein the size of the cut sample is about 20mm multiplied by 15 mm;
step 2, thermally inlaying the sample on a resin matrix, wherein the hardness requirement of the thermally inlaid resin matrix after curing is kept to be about 51 HRC;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample in a single direction by using No. 120 waterproof abrasive paper, wherein the sample is lubricated by water in the polishing process, and the polishing depth is about 0.5 mm;
rotating the sample by about 110 degrees relative to the polishing direction of the first procedure, and grinding the sample by using No. 400 metallographic abrasive paper in a single direction to remove the thickness of about 0.35 mm;
rotating the sample by about 100 degrees relative to the polishing direction of the working procedure, and grinding the sample by 600# metallographic abrasive paper in a single direction to remove the thickness of about 0.06 mm;
rotating the sample by about 45 degrees relative to the polishing direction of the working procedure and grinding the sample by 1000# metallographic abrasive paper in a single direction to remove the thickness of about 0.006 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6um diamond polishing agent for about 8 min;
secondly, polishing the sample on the navy woolen fabric (plush) by adopting a 2.5um diamond polishing agent, wherein the polishing time is about 3 min;
polishing the sample on a velveteen fabric by adopting a 0.5um diamond polishing agent for about 9 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent, wherein the polishing time is about 4 min;
in the step, the lubricants adopted in the processes I, II and III respectively comprise the following raw materials in parts by weight: 23 parts of glycerol, 180 parts of ethanol, 5 parts of sodium dodecyl benzene sulfonate and 390 parts of water;
in the step, the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight: 130 parts of ethanol and 220 parts of water;
step 5, preparing the corrosive agent according to the following raw materials in parts by weight: 15 parts of hydrofluoric acid, 30 parts of nitric acid, 14 parts of hydrogen peroxide and 160 parts of water; the preparation process comprises the following steps: uniformly mixing hydrofluoric acid, nitric acid and water, and then adding hydrogen peroxide and uniformly mixing;
and (3) corroding the polished sample in a corrosive agent for about 38s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain the metallographic sample for metallographic structure inspection and analysis.
The above examples are intended to illustrate the invention, but not to limit it. Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: the present invention may be modified from the embodiments described above or substituted for some of the technical features, and such modifications or substitutions do not depart from the spirit and scope of the present invention.
Claims (5)
1. The preparation method of the sample for the metallographic structure inspection of the vanadium-based alloy is characterized by comprising the following process steps of:
step 1, sampling on a vanadium-based alloy material;
2, inlaying the sample on a resin matrix;
and 3, polishing the sample on the resin matrix according to the following procedures:
firstly, polishing a sample by using No. 120 waterproof abrasive paper, wherein the polishing depth is 0.3-0.6 mm;
rotating the sample by 45-135 degrees relative to the polishing direction of the first step, and grinding the sample by using No. 400 metallographic abrasive paper to remove the thickness of 0.15-0.45 mm;
rotating the sample by 45-135 degrees relative to the polishing direction of the second procedure, and grinding the sample by using No. 600 metallographic abrasive paper to remove the thickness of 0.05-0.1 mm;
rotating the sample at an angle of 45-135 degrees relative to the polishing direction of the step (c), and grinding the sample by using 1000# metallographic abrasive paper to remove the thickness of 0.003-0.007 mm;
and 4, polishing the polished sample by adopting a lubricant according to the following process:
firstly, polishing a sample on canvas fabric by adopting a 6-micron diamond polishing agent for 3-8 min;
secondly, polishing the sample on the navy fabric by adopting a 2.5um diamond polishing agent for 2-10 min;
polishing the sample on the velveteen fabric by adopting a 0.5um diamond polishing agent for 3-15 min;
polishing the sample on the gold velvet fabric by adopting 0.05um of aluminum oxide polishing agent for 1-10 min;
wherein, the lubricant adopted in the first, second and third procedures is composed of the following raw materials by weight:
10-30 parts of glycerol,
50-250 parts of ethanol,
0.5 to 5 parts of sodium dodecyl benzene sulfonate,
200-500 parts of water;
the lubricant adopted in the procedure IV is composed of the following raw materials in parts by weight:
50-250 parts of ethanol,
50-400 parts of water;
and 5, eroding the polished sample in a corrosive agent for 10-70 s, neutralizing the corrosive agent by using a saturated borax water solution, taking out the sample, sequentially and respectively cleaning the sample by using clear water and absolute ethyl alcohol, and finally drying the cleaned sample by blowing to obtain the metallographic sample for metallographic structure inspection and analysis.
2. The method for preparing the test sample for the metallographic structure examination of the vanadium-based alloy according to the claim 1, wherein the sampling in the step 1 is performed by cutting the sample on the vanadium-based alloy material in a wire-cut electric discharge manner.
3. The method for preparing the test sample for the metallographic structure examination of the vanadium-based alloy according to claim 1, wherein in the step 1, the sampling is performed by cutting and sampling on the vanadium-based alloy material in a grinding wheel cutting mode, the cutting speed is 0.3-5 mm/min, and an aluminum oxide grinding wheel is used as the grinding wheel.
4. The method for preparing the sample for the vanadium-based alloy metallographic structure examination according to claim 1, wherein the hardness of the resin matrix in the step 2 is 45-55 HRC.
5. The method for preparing the sample for the metallographic structure examination of the vanadium-based alloy according to claim 1, wherein the corrosive agent in the step 5 is prepared from the following raw materials in 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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