CN103628062A - Metallographic corrosive for showing grain boundaries of steels - Google Patents
Metallographic corrosive for showing grain boundaries of steels Download PDFInfo
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- CN103628062A CN103628062A CN201310541067.1A CN201310541067A CN103628062A CN 103628062 A CN103628062 A CN 103628062A CN 201310541067 A CN201310541067 A CN 201310541067A CN 103628062 A CN103628062 A CN 103628062A
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Abstract
The invention relates to a corrosive, and particularly relates to a metallographic corrosive for showing grain boundaries of steels and a preparation method of the metallographic corrosive. The corrosive is composed of the following components in mass percentage: 8-15 percent of picric acid, 8-12 percent of sodium dodecyl sulfate, 0-1.5 percent of copper and the balance of water. The corrosive has the beneficial effects that by using the metallographic corrosive prepared by the preparation method and according to the proportions, grain boundaries of various steel iron materials can be clearly shown, and especially the metallographic corrosive has a very good effect on 10Ni5CrMoV steel in a quenching state, 10Ni5CrMoV steel in a tempering state, 10Ni5CrMoV steel in a quenching state and 38CrMoAl steel in a quenching state.
Description
Technical field
The present invention relates to a kind of etching reagent, more specifically metallographic etching agent of a kind of crystal boundary that shows steel and preparation method thereof.
Background technology
In the research process of metallic substance, after heat-treating by modes such as normalizing, annealing, quenching or tempering, can obtain the steel of different tissues state and performance, the performance of material depends on structural state, and the quality key of structural state is the size of grain fineness number.In order to obtain required performance and material property to be changed to mechanism, analyze, need to carry out metallurgical analysis to material.When organizing demonstration, want the grain fineness number of special concern material.
The generally demonstration of ferrous materials grain fineness number adopts saturated picric acid solution, 4% nitric acid alcohol, the reagent such as mixing solutions of saturated picric acid, concentrated nitric acid, concentrated hydrochloric acid and ethanol.Yet while adopting aforesaid method corrosion crystal boundary, in a lot of situations, Display of Grain Boundary is not clearly, and can cause the appearance of tissue topography, makes the measurement of grain fineness number be difficult to carry out.And above reagent is all only comparatively obvious to specific different materials and as-heat-treated condition effect comparatively speaking.
Summary of the invention
The object of the invention is the shortcoming existing for existing grain boundary corrosion agent, a kind of new etching reagent is provided, this etching reagent can make the crystal boundary in metallographic structure clear continuously, but can not make again metallographic structure obviously show simultaneously.Be very beneficial for carrying out the corrosion of crystal boundary to carrying out the ferrous materials of grain fineness number measurement.
For realizing the above object, technical scheme of the present invention is:
A metallographic etching agent that shows the crystal boundary of steel, is comprised of following component by mass percentage:
Picric acid: 8 ~ 15%
Sodium laurylsulfonate: 8 ~ 12%
Copper: 0 ~ 1.5%
All the other are water.
Optimize, above-mentioned metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 8.5-11.5%
Sodium laurylsulfonate: 8.5-11.5%
Copper: 0 ~ 1.2%
All the other are water.
Above-mentioned metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 10%
Sodium laurylsulfonate: 8.9%
Copper: 1.1%
All the other are water.
Above-mentioned metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 11.1%
Sodium laurylsulfonate: 11.1%
All the other are water.
Above-mentioned metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 8.6%
Sodium laurylsulfonate: 10%
Copper: 1.1%
All the other are water.
It is that after 8 ~ 15% picric acid, to splash into mass percent be 8 ~ 12% sodium laurylsulfonates that the preparation method of the metallographic etching agent of above-mentioned a kind of crystal boundary that shows steel comprises the steps: to take mass percent, adding mass percent is after 0 ~ 1.5% copper sheet, to add water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat that lather collapse can start corrosion.Corrosion sample under the condition of 80 ~ 100 ℃ immerses sample 3 ~ 10s absorbent cotton wiping in corrosive fluid at every turn, repeats 1 ~ 5 time, and after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
Optimize, it is that after 10% picric acid, to splash into mass percent be 8.9% sodium laurylsulfonate that the preparation method of the metallographic etching agent of above-mentioned a kind of crystal boundary that shows steel comprises the steps: to take mass percent, then after adding mass percent and be 1.1% copper, add water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, respectively at 8s, when 5s and 3s, sample is immersed to corrosive fluid and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
It is that after 11.1% picric acid, to splash into mass percent be 11.1% sodium laurylsulfonate that the preparation method of the metallographic etching agent of above-mentioned a kind of crystal boundary that shows steel comprises the steps: to take mass percent, then after adding water, stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, respectively at 10s, when 5s and 3s, sample is immersed to corrosive fluid and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
It is that after 11.1% picric acid, to splash into mass percent be 11.1% sodium laurylsulfonate that the preparation method of the metallographic etching agent of above-mentioned a kind of crystal boundary that shows steel comprises the steps: to take mass percent, then after adding water, stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, when 6s and 4s, sample is immersed to corrosive fluid respectively and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation
It is that after 8.6% picric acid, to splash into mass percent be 10% sodium laurylsulfonate that the preparation method of the metallographic etching agent of above-mentioned a kind of crystal boundary that shows steel comprises the steps: to take mass percent, then after the copper that mass percent is 1.1%, add water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, when 10s and 6s, sample is immersed to corrosive fluid respectively and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.The appearance that the effect of copper sheet is to promote the corrosion of crystal boundary and suppresses tissue topography.
The invention has the beneficial effects as follows: the crystal boundary of the various ferrous materials of metallographic etching agent of preparing by proportioning of the present invention and preparation method is shown especially the 10Ni5CrMoV steel of quenching state 10Ni5CrMoV steel, tempering state, quenching state 10Ni5CrMoV steel, quenching state 38CrMoAl steel are had to good effect clearly.
Accompanying drawing explanation
Fig. 1 is quenching state 10Ni5CrMoV steel, adopts picric acid corrosion, the unintelligible schematic diagram of Display of Grain Boundary;
Fig. 2 is tempering state 10Ni5CrMoV steel, adopts the corrosion of nitric acid alcohol, the unintelligible schematic diagram of Display of Grain Boundary;
Fig. 3 is quenching state 38CrMoAl steel, adopts concentrated hydrochloric acid and ethanol corrosion, the unintelligible schematic diagram of Display of Grain Boundary;
Fig. 4 is the metallographic schematic diagram of example 1;
Fig. 5 is the metallographic schematic diagram of example 2;
Fig. 6 is the metallographic schematic diagram of example 3.
Embodiment
The present invention will be further described with specific embodiment with reference to the accompanying drawings below, so that those skilled in the art can better understand the present invention, but therefore do not limit the present invention.
Take mass percent and be that to splash into mass percent after 8 ~ 15% picric acid be in 8 ~ 12% sodium laurylsulfonates, then the copper that is 0 ~ 1.5% by mass percent adds water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, produce a large amount of foams, till lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, sample is immersed to 3 ~ 10s in corrosive fluid at every turn, use absorbent cotton wiping, repeat 1 ~ 5 time, after the obfuscation of specimen surface burnt hair, water and dehydrated alcohol clean, air-dry rear observation.
Following embodiment all adopts aforesaid method.
Embodiment 1
First weigh in the balance and get picric acid 4.5g, after splash into therein 4g sodium laurylsulfonate, add copper sheet 0.5g, finally add water to 45ml.Post-heating to the solute that stirs dissolves, and solution seethes with excitement once.
By the quenching state 10Ni5CrMoV steel after polishing, be placed under the condition of 80 ~ 100 ℃ 8s in corrosion sample etching reagent, 5s, 3s all wipes corrosion product with absorbent cotton therebetween.Last water and dehydrated alcohol clean and dry up, and use metallography microscope sem observation.
Embodiment 2
With the 10Ni5CrMoV steel of above formula corrosion tempering state, sample is put into etching reagent 10s, 5s, 3s wipes corrosion product with absorbent cotton therebetween.Last water and dehydrated alcohol clean and dry up, and use metallography microscope sem observation.
Embodiment 3
First weigh in the balance and get 5g picric acid, after splash into therein 5g sodium laurylsulfonate, add water to 45ml.Post-heating to the solute that stirs dissolves, and solution seethes with excitement once.
Quenching state 10Ni5CrMoV steel is put into etching reagent 6s, and 4s wipes corrosion product with absorbent cotton therebetween.Last water and dehydrated alcohol clean and dry up, and use metallography microscope sem observation.
Embodiment 4
First weigh in the balance and get 3g picric acid, after splash into therein sodium laurylsulfonate 3.5g, copper sheet 0.4g, adds water to 35ml.Post-heating to the solute that stirs dissolves, and solution seethes with excitement once.
Quenching state 38CrMoAl steel is put into etching reagent 10s, and 6s wipes corrosion product with absorbent cotton therebetween.Last water and dehydrated alcohol clean and dry up, and use metallography microscope sem observation.
By accompanying drawing 1-7, adopt as seen formula of the present invention to corrode, can make the crystal boundary in metallographic structure clear continuously, and effectively avoided the appearance of material structure pattern.The ferrous materials that is very beneficial for carrying out grain fineness number test carries out the corrosion of crystal boundary.
Claims (10)
1. a metallographic etching agent that shows the crystal boundary of steel, is comprised of following component by mass percentage:
Picric acid: 8 ~ 15%
Sodium laurylsulfonate: 8 ~ 12%
Copper: 0 ~ 1.5%
All the other are water.
2. a kind of metallographic etching agent that shows the crystal boundary of steel according to claim 1, is characterized in that: described metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 8.5-11.5%
Sodium laurylsulfonate: 8.5-11.5%
Copper: 0 ~ 1.2%
All the other are water.
3. a kind of metallographic etching agent that shows the crystal boundary of steel according to claim 1 and 2, is characterized in that: described metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 10%
Sodium laurylsulfonate: 8.9%
Copper: 1.1%
All the other are water.
4. a kind of metallographic etching agent that shows the crystal boundary of steel according to claim 1 and 2, is characterized in that: described metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 11.1%
Sodium laurylsulfonate: 11.1%
All the other are water.
5. a kind of metallographic etching agent that shows the crystal boundary of steel according to claim 1 and 2, is characterized in that: described metallographic etching agent, is comprised of following component by mass percentage:
Picric acid: 8.6%
Sodium laurylsulfonate: 10%
Copper: 1.1%
All the other are water.
6. the preparation method of the metallographic etching agent of a kind of crystal boundary that shows steel according to claim 1, it is that after 8 ~ 15% picric acid, to splash into mass percent be in 8 ~ 12% sodium laurylsulfonates that the method comprises the steps: to take mass percent, then the copper that is 0 ~ 1.5% by mass percent adds water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, produce a large amount of foams, till lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, sample is immersed to 3 ~ 10s in corrosive fluid at every turn, use absorbent cotton wiping, repeat 1 ~ 5 time, after the obfuscation of specimen surface burnt hair, water and dehydrated alcohol clean, air-dry rear observation.
7. to comprise the steps: to take mass percent be that after 10% picric acid, to splash into mass percent be 8.9% sodium laurylsulfonate to the preparation method of the metallographic etching agent of a kind of crystal boundary that shows steel according to claim 1, then the copper that is 1.1% by mass percent adds water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, produce a large amount of foams, till lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, respectively at 8s, when 5s and 3s, sample is immersed to corrosive fluid and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
8. to comprise the steps: to take mass percent be that after 11.1% picric acid, to splash into mass percent be 11.1% sodium laurylsulfonate to the preparation method of the metallographic etching agent of a kind of crystal boundary that shows steel according to claim 1, then after adding water, stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, respectively at 10s, when 5s and 3s, sample is immersed to corrosive fluid and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
9. to comprise the steps: to take mass percent be that after 11.1% picric acid, to splash into mass percent be 11.1% sodium laurylsulfonate to the preparation method of the metallographic etching agent of a kind of crystal boundary that shows steel according to claim 1, then after adding water, stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, when 6s and 4s, sample is immersed to corrosive fluid respectively and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
10. to comprise the steps: to take mass percent be that after 8.6% picric acid, to splash into mass percent be 10% sodium laurylsulfonate to the preparation method of the metallographic etching agent of a kind of crystal boundary that shows steel according to claim 1, then after the copper that mass percent is 1.1%, add water to stir, heating, solute in solution is dissolved completely, during solution ebuillition of heated, can produce a large amount of foams, treat lather collapse, corrosion sample under the condition of 80 ~ 100 ℃, when 10s and 6s, sample is immersed to corrosive fluid respectively and then use absorbent cotton wiping, after the obfuscation of specimen surface burnt hair, be that used water and dehydrated alcohol clean, air-dry rear observation.
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| CN105334087A (en) * | 2015-10-13 | 2016-02-17 | 镇江耐丝新型材料有限公司 | Displaying method of austenite grain boundaries after quenching of sawing wire high carbon steel |
| CN106290356A (en) * | 2015-05-26 | 2017-01-04 | 中国科学院金属研究所 | A kind of display packing of 38CrNi3MoV crystal boundary |
| CN106947973A (en) * | 2017-03-20 | 2017-07-14 | 天津大学 | Corrosive agent and its application in low activation ferritic heat-resistant steel is handled |
| CN107523833A (en) * | 2017-08-22 | 2017-12-29 | 河南科技大学 | A kind of metallographic etching agent and its application in terms of carbide, crystal boundary in showing steel |
| CN112082912A (en) * | 2020-09-10 | 2020-12-15 | 中车戚墅堰机车车辆工艺研究所有限公司 | Steel grain size etching agent and application thereof |
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Cited By (6)
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| CN106290356A (en) * | 2015-05-26 | 2017-01-04 | 中国科学院金属研究所 | A kind of display packing of 38CrNi3MoV crystal boundary |
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| CN112082912A (en) * | 2020-09-10 | 2020-12-15 | 中车戚墅堰机车车辆工艺研究所有限公司 | Steel grain size etching agent and application thereof |
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