CN117845217A - Corrosion liquid and corrosion method for displaying prior austenite grain boundary of oriented silicon steel - Google Patents
Corrosion liquid and corrosion method for displaying prior austenite grain boundary of oriented silicon steel Download PDFInfo
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- CN117845217A CN117845217A CN202410257471.4A CN202410257471A CN117845217A CN 117845217 A CN117845217 A CN 117845217A CN 202410257471 A CN202410257471 A CN 202410257471A CN 117845217 A CN117845217 A CN 117845217A
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- 239000007788 liquid Substances 0.000 title claims abstract description 106
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 89
- 229910001566 austenite Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000005260 corrosion Methods 0.000 title abstract description 53
- 230000007797 corrosion Effects 0.000 title abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 87
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 229920000742 Cotton Polymers 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000005530 etching Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 7
- 230000003749 cleanliness Effects 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000005238 degreasing Methods 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 abstract description 6
- 239000010959 steel Substances 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 53
- 230000000052 comparative effect Effects 0.000 description 13
- 238000010587 phase diagram Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000003599 detergent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of steel material detection, in particular to a corrosive liquid and a corrosion method for displaying a prior austenite grain boundary of oriented silicon steel, wherein the composition of the corrosive liquid is regulated to be picric acid, jierten solution, panting hair conditioner and water; the prior austenite grain boundary of the corroded oriented silicon steel is clear and complete in a mode of fractional corrosion during corrosion, the grain size of the oriented silicon steel can be clearly observed under a metallographic microscope, and the method is suitable for rating software of the grain size.
Description
Technical Field
The invention relates to the technical field of steel material detection, in particular to a corrosive liquid and a corrosion method for displaying a prior austenite grain boundary of oriented silicon steel.
Background
The austenite grain size is measured by grain size index, which refers to the size of grains obtained by heating steel to a certain temperature and maintaining the temperature for a certain time. In the heat treatment process, the size of the prior austenite grains has important influence on the structure and performance of the steel, and the smaller the austenite grains are, the higher the strength, the good plasticity and the high impact toughness of the steel after heat treatment are. Austenite grains are coarse, the strength is low, the plasticity is poor, and the brittleness is increased. Austenite grain size is also an important parameter in assessing the quality of the heat treatment. Coarse grain steels are prone to cracking during cooling, and accurate grain size measurement is therefore very important. The prior austenite grain boundary corrosion method is quite a lot, but the grain boundary after corrosion of the oriented silicon steel is unclear and incomplete, the surface of a sample is blackened, and the electrolytic corrosion, the vibration corrosion and the like cannot achieve good effects.
Disclosure of Invention
In order to solve the problems in the prior art, the main purpose of the invention is to provide a corrosive liquid and a corrosion method for displaying the prior austenite grain boundary of oriented silicon steel.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein the solid-to-liquid ratio of picric acid to the Jierten solution is 1g (3.5-4.5) mL, and the volume ratio of the Jierten solution to the paning hair conditioner to the water is 1 (0.45-0.55) (4.5-5.5).
As a preferable scheme of the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel, the invention comprises the following steps: picric acid is in the form of powder, and water is distilled water.
As a preferable scheme of the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel, the invention comprises the following steps: the concentration of the Jiertangling solution is 0.1-0.5vol%.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
the preparation method of the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel comprises the following steps: taking raw materials according to the composition of the corrosive liquid; firstly adding picric acid, distilled water, a Jiertangling solution and a paning hair conditioner into a container; and stirring the raw materials added into the container by using a glass rod to obtain the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel.
The preparation method of the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel is preferably as follows: in the stirring process, the stability of the container is maintained, the container is stirred against the container wall, and the forward and reverse stirring is intermittently performed.
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
the corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 90-95 ℃ and then keeping the temperature constant;
s2, soaking absorbent cotton into the corrosive liquid in the beaker;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after 95-105S, and drying the sample after cleaning with clean water;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after 55-65S of the sample are kept;
s5, washing the sample and drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
As a preferable scheme of the corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel, the invention comprises the following steps: grinding, polishing and cleaning are carried out before the sample is corroded, so that the cleanliness of the surface to be corroded of the sample is ensured.
As a preferable scheme of the corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel, the invention comprises the following steps: in the step S2, all the absorbent cotton is immersed in the corrosive liquid for 35-45S.
As a preferable scheme of the corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel, the invention comprises the following steps: in the step S4, after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 55-65S above the beaker, and the corrosive surface of the sample is repeatedly wiped by using the absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
As a preferable scheme of the corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel, the invention comprises the following steps: in the step S5, the sample is rinsed with water, then rinsed with absolute ethanol, and finally dried.
The beneficial effects of the invention are as follows:
the invention provides a corrosive liquid and a corrosion method for displaying prior austenite grain boundaries of oriented silicon steel, wherein the corrosive liquid is adjusted to be picric acid, jierte solution, panting conditioner and water; the prior austenite grain boundary of the corroded oriented silicon steel is clear and complete in a mode of fractional corrosion during corrosion, the grain size of the oriented silicon steel can be clearly observed under a metallographic microscope, and the method is suitable for rating software of the grain size.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a golden phase diagram of a sample after corrosion in example 1 of the present invention.
FIG. 2 is a golden phase diagram of the sample after corrosion in comparative example 1 of the present invention.
FIG. 3 is a golden phase diagram of the sample after corrosion in comparative example 2 of the present invention.
FIG. 4 is a golden phase diagram of the sample after corrosion in comparative example 3 of the present invention.
FIG. 5 is a golden phase diagram of the sample after corrosion in comparative example 4 of the present invention.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
According to one aspect of the invention, the invention provides the following technical scheme:
the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein the solid-to-liquid ratio of picric acid to the Jierten solution is 1g (3.5-4.5) mL, and the volume ratio of the Jierten solution to the paning hair conditioner to the water is 1 (0.45-0.55) (4.5-5.5). Specifically, the solid to liquid ratio of picric acid to the clean solution may be, for example, in the range of any one or any two of 1g:3.5mL, 1g:3.6mL, 1g:3.7mL, 1g:3.8mL, 1g:3.9mL, 1g:4.0mL, 1g:4.1mL, 1g:4.2mL, 1g:4.3mL, 1g:4.4mL, 1g:4.5 mL; the volume ratio of the Jierten solution, the panting conditioner to the water may be, for example, in the range of 1:0.45:5, 1:0.5:5, 1:0.55:5, 1:0.5:4.5, 1:0.5:5.5, or any two of them.
Preferably, the picric acid is in the form of powder, and the water is distilled water; and (3) obtaining the Jielfenamic solution after water distribution of the Jielfenamic solution, wherein the concentration of the Jielfenamic solution is 0.1-0.5vol%. The panting conditioner is Pan Tingsi smooth series conditioners. Specifically, the concentration of the Jierten solution may be, for example, in a range between any one or any two of 0.1vol%, 0.2vol%, 0.3vol%, 0.4vol%, and 0.5vol%.
According to another aspect of the invention, the invention provides the following technical scheme:
the preparation method of the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel comprises the following steps: taking raw materials according to the composition of the corrosive liquid; firstly adding picric acid, distilled water, a Jiertangling solution and a paning hair conditioner into a container; and stirring the raw materials added into the container by using a glass rod, and stopping stirring after 110-130 s to obtain the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel.
Preferably, during the stirring process, the stability of the container is maintained, the container is stirred against the wall of the container, and the forward and reverse stirring is intermittently performed.
According to another aspect of the invention, the invention provides the following technical scheme:
the corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 90-95 ℃ and then keeping the temperature constant; specifically, the constant temperature may be, for example, any one or a range between any two of 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃;
s2, soaking absorbent cotton into the corrosive liquid in the beaker;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after 95-105S, and drying the sample after cleaning with clean water; placing the sample on absorbent cotton prevents the sample from contacting the overheated beaker, causing blackening of the surface. Specifically, the holding time may be, for example, in a range between any one or any two of 95s, 96s, 97s, 98s, 99s, 100s, 101s, 102s, 103s, 104s, 105 s;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after 55-65S of the sample are kept; specifically, the holding time may be, for example, any one or a range between any two of 55s, 56s, 57s, 58s, 59s, 60s, 61s, 62s, 63s, 64s, 65 s;
s5, washing the sample and drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
Preferably, grinding, polishing and cleaning are carried out before the sample is corroded, so that the cleanliness of the surface to be corroded of the sample is ensured.
Preferably, in the step S2, all the absorbent cotton is immersed in the etching solution for 35 to 45S. Specifically, the time for immersing the whole absorbent cotton in the etching liquid may be, for example, in a range between any one or any two of 35s, 36s, 37s, 38s, 39s, 40s, 41s, 42s, 43s, 44s, 45s.
Preferably, in the step S4, after the sample is taken out from the etching solution, the surface to be etched of the sample is kept downward for 55-65S above the beaker, and the etched surface of the sample is repeatedly wiped with alcohol by dipping absorbent cotton, so that black marks on the etched surface are wiped off. Specifically, the residence time may be, for example, in a range between any one or any two of 55s, 56s, 57s, 58s, 59s, 60s, 61s, 62s, 63s, 64s, 65 s.
Preferably, in the step S5, the sample is rinsed with water, then rinsed with absolute ethanol, and finally dried.
The technical scheme of the invention is further described below by combining specific embodiments.
The oriented silicon steel used in the following examples comprises the following components in percentage by mass: 0.04% of C, 2.6% of Si, 0.15% of Mn, 0.02% of P, 0.01% of S, 0.03% of Als, 0.06% of Cr, 0.07% of Sn, and the balance of Fe and unavoidable impurities.
Grinding, polishing and cleaning are carried out before the corrosion of the oriented silicon steel sample, so that the cleanliness of the surface to be corroded of the sample is ensured.
The preparation method of the corrosive liquid comprises the following steps: taking raw materials according to the composition of the corrosive liquid; firstly adding picric acid, distilled water, a Jiertangling solution and a paning hair conditioner into a container; and stirring the raw materials added into the container by using a glass rod, keeping the stability of the container in the stirring process, stirring the raw materials against the container wall, intermittently stirring the raw materials positively and negatively, and stopping stirring the raw materials for 120 seconds to obtain the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel.
Example 1
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to the Jierten solution is 1g to 4mL, and the volume ratio of the Jierten solution, the paning conditioner and the water is 1 to 0.5 to 5; picric acid is in powder form, and water is distilled water; the concentration of the Jierten solution is 0.3vol%; the panting conditioner is Pan Tingsi smooth series conditioners. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 94 ℃ and then keeping the temperature constant;
s2, soaking absorbent cotton into the corrosive liquid in the beaker; immersing all absorbent cotton into the corrosive liquid for 40s;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after 100 seconds, and drying the sample after cleaning the sample with clean water;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after maintaining for 60 seconds; after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 60s above the beaker, and the corrosive surface of the sample is repeatedly wiped by using absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
And S5, washing the sample with water, washing the sample with absolute ethyl alcohol, and finally drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
The golden phase diagram of the sample after corrosion in this example is shown in fig. 1, the grain boundary of the sample is clear, the display effect is clear, and the grain size grade is 8.0 as a result of adopting the grading software of grain size.
Example 2
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to the Jierten solution is 1g to 4.5mL, and the volume ratio of the Jierten solution, the paning conditioner and the water is 1 to 0.45 to 5.5; picric acid is in powder form, and water is distilled water; the concentration of the Jierten solution is 0.1vol%; the panting conditioner is Pan Tingsi smooth series conditioners. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 90 ℃ and then keeping the temperature constant;
s2, soaking absorbent cotton into the corrosive liquid in the beaker; immersing all absorbent cotton into the corrosive liquid for 45s;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after 105 seconds, washing the sample with clean water, and drying the sample;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after maintaining for 65 seconds; after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 65s above the beaker, and the corrosive surface of the sample is repeatedly wiped by using absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
And S5, washing the sample with water, washing the sample with absolute ethyl alcohol, and finally drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
The grain boundaries of the samples after corrosion in this example were clear, the display effect was clear, and the grain size grade was 8.0 as a result of the rating software using grain size.
Example 3
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to the Jierten solution is 1g to 3.5mL, and the volume ratio of the Jierten solution, the paning conditioner and the water is 1 to 0.55 to 4.5; picric acid is in powder form, and water is distilled water; the concentration of the Jierten solution is 0.5vol%; the panting conditioner is Pan Tingsi smooth series conditioners. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 95 ℃ and then keeping the temperature constant;
s2, soaking absorbent cotton into the corrosive liquid in the beaker; immersing all absorbent cotton into the corrosive liquid for 35s;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after the sample is kept for 95 seconds, and drying the sample after the sample is washed with clean water;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after maintaining for 55 seconds; after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 55s above the beaker, and the corrosive surface of the sample is repeatedly wiped by using absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
And S5, washing the sample with water, washing the sample with absolute ethyl alcohol, and finally drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
The grain boundaries of the samples after corrosion in this example were clear, the display effect was clear, and the grain size grade was 8.5 as a result of the rating software using grain size.
Comparative example 1
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to the Jierten solution is 1g to 4mL, and the volume ratio of the Jierten solution, the paning conditioner and the water is 1 to 0.5 to 5; picric acid is in powder form, and water is distilled water; the concentration of the Jierten solution is 0.3vol%; the panting conditioner is Pan Tingsi smooth series conditioners. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 94 ℃ and then keeping the temperature constant;
s2, placing the oriented silicon steel sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, taking out the sample after maintaining for 100 seconds, and drying the sample after cleaning with clean water.
S3, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after maintaining for 60 seconds; after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 60s above the beaker, and the corrosive surface of the sample is repeatedly wiped by using absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
And S4, washing the sample with water, washing the sample with absolute ethyl alcohol, and finally drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
The golden phase diagram of the sample after corrosion in this comparative example is shown in fig. 2, the sample is blackened as a whole, the display effect is poor, and the grain size grade is 8.5 as a result of the adoption of the rating software of grain size.
Comparative example 2
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, jieer' ing solution, detergent and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to Jierten solution is 1g to 4mL, and the volume ratio of Jierten solution, detergent and water is 1 to 0.5 to 5; picric acid is in powder form, and water is distilled water; the concentration of the Jielmie solution was 0.3vol%. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 94 ℃ and then keeping the temperature constant;
s2, soaking absorbent cotton into the corrosive liquid in the beaker; immersing all absorbent cotton into the corrosive liquid for 40s;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after 100 seconds, and drying the sample after cleaning the sample with clean water;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after maintaining for 60 seconds; after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 60s above the beaker, and the corrosive surface of the sample is repeatedly wiped by using absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
And S5, washing the sample with water, washing the sample with absolute ethyl alcohol, and finally drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
The golden phase diagram of the sample after corrosion in this comparative example is shown in FIG. 3, the grain boundary of the sample surface is discontinuous, and the grain size grade is 8.5 as a result of the rating software of grain size.
Comparative example 3
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to the Jierten solution is 1g to 4mL, and the volume ratio of the Jierten solution, the paning conditioner and the water is 1 to 0.5 to 5; picric acid is in powder form, and water is distilled water; the concentration of the Jierten solution is 0.3vol%; the panting conditioner is Pan Tingsi smooth series conditioners. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 94 ℃ and then keeping the temperature constant;
s2, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after 160S of holding; after the sample is taken out of the corrosive liquid, the surface to be corroded of the sample is kept downwards for 60s above the beaker, and the corrosive surface of the sample is repeatedly wiped by using absorbent cotton to dip alcohol, so that black marks on the corrosive surface are wiped off.
And S3, washing the sample with water, washing the sample with absolute ethyl alcohol, and finally drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
The golden phase diagram of the sample after corrosion in this comparative example is shown in FIG. 4, and the surface of the sample is blackened, and the grain size grade is 8.5 as a result of the use of the rating software of grain size.
Comparative example 4
The corrosion method for displaying the prior austenite grain boundary of the oriented silicon steel adopts the corrosion liquid for displaying the prior austenite grain boundary of the oriented silicon steel, and comprises the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein, 5g of picric acid, the solid-to-liquid ratio of picric acid to the Jierten solution is 1g to 4mL, and the volume ratio of the Jierten solution, the paning conditioner and the water is 1 to 0.5 to 5; picric acid is in powder form, and water is distilled water; the concentration of the Jierten solution is 0.3vol%; the panting conditioner is Pan Tingsi smooth series conditioners. The method comprises the following steps:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 94 ℃ and then keeping the temperature constant;
s2, placing the to-be-etched surface of the oriented silicon steel sample into etching liquid in a beaker, keeping for 160 seconds, taking out the sample, washing with clean water, and drying to display the prior austenite grain boundary of the oriented silicon steel.
The golden phase diagram of the sample after corrosion in this comparative example is shown in fig. 5, and the surface of the sample is blackened, and the grain size grade is 8.5 as a result of the use of the rating software of grain size.
As can be seen from the above examples and comparative examples, the composition of the corrosive liquid is adjusted to be picric acid, jielmie solution, manting hair conditioner and water; the prior austenite grain boundary of the corroded oriented silicon steel is clear and complete in a mode of fractional corrosion during corrosion, the grain size of the oriented silicon steel can be clearly observed under a metallographic microscope, and the method is suitable for rating software of the grain size.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel is characterized by comprising the following components: picric acid, a Jierte solution, a panting hair conditioner and water; wherein the solid-to-liquid ratio of picric acid to the Jierten solution is 1g (3.5-4.5) mL, and the volume ratio of the Jierten solution to the paning hair conditioner to the water is 1 (0.45-0.55) (4.5-5.5).
2. The etching solution for showing the prior austenite grain boundaries of oriented silicon steel according to claim 1, wherein picric acid is in the form of powder and water is distilled water.
3. The corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel according to claim 1, wherein the concentration of the clean-up solution is 0.1 to 0.5vol%.
4. A method for preparing the etchant for displaying the prior austenite grain boundaries of oriented silicon steel as set forth in any one of claims 1 to 3, comprising: taking raw materials according to the composition of the corrosive liquid; firstly adding picric acid, distilled water, a Jiertangling solution and a paning hair conditioner into a container; and stirring the raw materials added into the container by using a glass rod to obtain the corrosive liquid for displaying the prior austenite grain boundary of the oriented silicon steel.
5. The method for preparing a corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel according to claim 4, wherein the method for preparing a corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel is preferably performed by: in the stirring process, the stability of the container is maintained, the container is stirred against the container wall, and the forward and reverse stirring is intermittently performed.
6. A method for etching a prior austenite grain boundary of oriented silicon steel, characterized in that the etching solution for etching a prior austenite grain boundary of oriented silicon steel according to any one of claims 1 to 3 is used, comprising the steps of:
s1, adding corrosive liquid for displaying prior austenite grain boundaries of oriented silicon steel into a beaker, placing the beaker into a water bath, heating the water bath to 90-95 ℃ and then keeping the temperature constant;
s2, soaking absorbent cotton into the corrosive liquid in the beaker;
s3, slowly placing the oriented silicon steel sample on absorbent cotton soaked with corrosive liquid, enabling the surface to be corroded of the sample to be attached to the absorbent cotton, taking out the sample after 95-105S, and drying the sample after cleaning with clean water;
s4, placing the sample into the corrosive liquid in the beaker with the surface to be corroded facing downwards, and taking out the sample from the corrosive liquid after 55-65S of the sample are kept;
s5, washing the sample and drying the sample to display the prior austenite grain boundary of the oriented silicon steel.
7. The method for etching a prior austenite grain boundary showing oriented silicon steel according to claim 6, wherein grinding, polishing and cleaning are performed before the sample is etched, so that the cleanliness of the surface to be etched of the sample is ensured.
8. The method for etching a prior austenite grain boundary for displaying oriented silicon steel according to claim 6, wherein in the step S2, all the absorbent cotton is immersed in the etching solution for 35 to 45 seconds.
9. The method for etching a prior austenite grain boundary for displaying oriented silicon steel according to claim 6, wherein in the step S4, after the sample is taken out of the etching solution, the surface to be etched of the sample is left to face down for 55-65 seconds above the beaker, and the etched surface of the sample is repeatedly wiped with a degreasing cotton dipped with alcohol, so that black marks on the etched surface are wiped off.
10. The method for etching grain boundaries of prior austenite for displaying oriented silicon steel according to claim 6, wherein in the step S5, the sample is rinsed with water, then rinsed with absolute ethyl alcohol, and finally dried.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105865882A (en) * | 2016-03-25 | 2016-08-17 | 天津钢管集团股份有限公司 | Etching method of corrosion agent for displaying crystal boundary of quenched and tempered low-alloy chrome molybdenum steel austenite crystal grains |
| CN114858566A (en) * | 2022-04-29 | 2022-08-05 | 包头钢铁（集团）有限责任公司 | Method for displaying original austenite grain boundary of low-carbon medium-alloy 5Cr seamless pipe |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105865882A (en) * | 2016-03-25 | 2016-08-17 | 天津钢管集团股份有限公司 | Etching method of corrosion agent for displaying crystal boundary of quenched and tempered low-alloy chrome molybdenum steel austenite crystal grains |
| CN114858566A (en) * | 2022-04-29 | 2022-08-05 | 包头钢铁（集团）有限责任公司 | Method for displaying original austenite grain boundary of low-carbon medium-alloy 5Cr seamless pipe |
Non-Patent Citations (2)
| Title |
|---|
| 孙婷婷: ""终冷温度对X100管线钢组织和性能的影响"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 8, 15 August 2015 (2015-08-15), pages 39 - 40 * |
| 黄斌 等: ""碳素结构钢奥氏体晶界腐蚀剂选用及腐蚀参数的确定"", 《热加工工艺》, vol. 41, no. 16, 31 August 2015 (2015-08-31), pages 63 - 65 * |
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