CN101706385B - Cold acid corrosion method used for displaying low-multiple branch crystals in billet - Google Patents
Cold acid corrosion method used for displaying low-multiple branch crystals in billet Download PDFInfo
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- CN101706385B CN101706385B CN2009101772978A CN200910177297A CN101706385B CN 101706385 B CN101706385 B CN 101706385B CN 2009101772978 A CN2009101772978 A CN 2009101772978A CN 200910177297 A CN200910177297 A CN 200910177297A CN 101706385 B CN101706385 B CN 101706385B
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Abstract
The invention relates to a cold acid corrosion method used for displaying low-multiple branch crystals in billet, which comprises the steps of leading the surface roughness of a billet sample to be less than or equal to 1.25 mu m by processing, conducting low-multiple branch crystal corrosion on the basis of low-multiple segregation corrosion by using the cold acid corrosion method, and then observing the displayed branch crystals and defects on the surface of the billet sample. The experimental method has the advantages of safeness, reliability, simple operation, low cost and the like.
Description
Technical field
The present invention relates to field of steel-making, be specifically related to show in a kind of STEELMAKING PRODUCTION the method for inside steel billet low power dendrite.
Background technology
In the steel of prior art are produced, when check inside steel billet crystallization situation, usually just with steel billet process low power segregation corrosion, to observe the degree of center segregation and center porosity.This method can only be observed the center segregation and the center porosity of steel billet, but for crackle of steel billet, the observation difficulty very then that defective such as is mingled with, the more important thing is the low power crystalline structure topographic profile that can't see steel billet clearly.In the sample detection of steel mill, also need observe steel billet low power crystalline structure distribution topographic profile and crackle, defective such as be mingled with, present off-line testing shows that the method for low power dendrite is also fewer.
Cold acid corrosion method of the prior art generally adopts etching tank and hanging apparatus specialized equipment, sample is put into etching tank corrode, and so both the equipment investment of labor and acid solution cost were prone to cause the acid solution contaminated environment simultaneously.
Summary of the invention
The objective of the invention is to propose a kind of method that is used for demonstrating the dendrite and its secondary tissue of steel billet, this realizes it being the comparison difficulty in the prior art.
For achieving the above object, the present invention adopts following technical proposals:
A kind ofly show the cold acid corrosion method used of inside steel billet low power arborescent structure and defective; After it is characterized in that the steel billet specimen surface is machined to surfaceness and is not more than 1.25 μ m; On the basis of low power segregation corrosion, carry out the corrosion of low power dendrite with cold acid corrosion method, observe dendrite and defective that the steel billet specimen surface is manifested then.
In a kind of embodiment of the present invention, said steel are structural carbon steel, alloy steel.
Of the present inventionly be used to show that the cold acid corrosion method of low-multiple branch crystals in billet may further comprise the steps:
A) the steel billet specimen surface is machined to surfaceness and is not more than 1.25 μ m;
B) with low power segregation corrosive liquid etch steel billet sample;
C) with the said steel billet sample of low power dendrite corrosive liquid etch.
In a kind of embodiment; Low power segregation corrosive liquid comprises first corrosive liquid and second corrosive liquid; Said first corrosive liquid is that mass percent concentration is 10～30% ammonium persulfate solution; Second corrosive liquid is the inorganic acid solution that is selected from sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, and its mass percent concentration is between 8～30%.
Wherein, the first corrosive liquid preferred mass percent concentration is 10～20% ammonium persulfate solution, and second corrosive liquid is the inorganic acid solution that is selected from sulfuric acid, hydrochloric acid, nitric acid, and its mass percent concentration is preferably between 15～30%.
In a kind of embodiment, low power dendrite corrosive liquid is the acid solution of chlorination cuprammonium, and its mass percent concentration can be between 5～25%, and preferably between 8～15%, the pH value of solution is between 1～6.
As preferably, said low power segregation corrosive liquid is applied to the surface of steel billet sample through wipe method.
As preferably, after the steel billet sample receives inspection face by low power segregation corrosion, further examined the cold corrosive liquid of face, removed cold corrosive liquid with flushing with clean water then with ammoniacal liquor-ethanolic solution neutralization.
In a kind of embodiment; The operation steps of low power dendrite corrosion is: 1. get the sample of doing low power segregation corrosion; Cupric chloride ammonia corrosion liquid is watered receiving on the inspection face at steel billet equably; Perhaps with corrosion resistant sprinkling equipment cupric chloride ammonia corrosion liquid is sprayed on steel billet equably and receives on the inspection face, 2. etching time is about 20 minutes, on the inspection face of receiving, observes dendrite and distributes and casting blank defect.
After the steel billet sample carries out low power dendrite corrosion, receive inspection face with 1000 orders or the 2000 order sand paper sample of slightly polishing, examined the face corrosion product up to sample and removed.
The present invention has following outstanding feature and remarkable advantage compared with prior art: the present invention adopts cold corrosive liquid that sample is examined the face wiping, watered erosion, uses the acid solution much less than existing etch method, has both saved the acid solution cost, also avoids the acid solution contaminated environment; Need not etching tank and hanging apparatus specialized equipment, then greatly save equipment investment; Simple, convenient; After polishing a little with sand paper after the corrosion, can directly be observed by bore hole, also available shooting style is taken record.Because experimental technique provided by the invention is simple, convenient, quick, safe and reliable again, does not have the discharging of waste liquid contaminated environment basically, thus be not only applicable to laboratory experiment, and be applicable to STEELMAKING PRODUCTION field experiment.
Description of drawings
Fig. 1 is the photo through the steel billet sample after embodiment 1 operational processes;
Fig. 2 is the photo through the steel billet sample after embodiment 2 operational processes.
Embodiment
The objective of the invention is to adopt the experimental technique of low power dendrite corrosion to demonstrate dendrite and its secondary tissue; Accurately measure Interventions Requested in the solidified structure; It is the area of tiny equiax crystal (chill), column crystal, intersection dendrite and center equiax crystal; Quantitative measurement dendrite secondary limb spacing, thereby the problem in the research solidification of molten steel.The method of operating of demonstration strand low power dendrite provided by the invention experiment can not cause environmental issue simply, easily and fast, and is safe and reliable, cost is low.
For achieving the above object, the present invention adopts following technical proposals:
After the steel billet specimen surface is machined to surfaceness and is not more than 1.25 μ m, on the basis of low power segregation corrosion, carry out the corrosion of low power dendrite, observe dendrite and defective that the steel billet specimen surface is manifested then with cold acid corrosion method.
Be used for the corrosive liquid that the corrosive liquid of low power segregation corrosion can use prior art to use, for example persulfate solutions such as sodium peroxydisulfate, potassium persulfate and ammonium persulfate.
In a kind of optimal way of the present invention; The corrosive liquid that is used for low power segregation corrosion comprises first corrosive liquid and second corrosive liquid; Wherein, first corrosive liquid is for being selected from persulfate solutions such as sodium peroxydisulfate, potassium persulfate and ammonium persulfate, wherein initiator system of ammonium persulfate solution; The mass percent concentration of first corrosive liquid can be between 10～30%, between preferred 10～20%.Second corrosive liquid is the inorganic acid solution that is selected from sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, wherein preferably sulfuric acid, hydrochloric acid and salpeter solution, and the mass percent concentration of second corrosive liquid can be between 8～30%, between preferred 15～30%.After with first corrosive liquid corrosion sample surfaces, corrode with second corrosive liquid again.
As preferably, after the steel billet sample receives inspection face by low power segregation corrosion, examined the cold corrosive liquid of face, removed cold corrosive liquid with flushing with clean water then with ammoniacal liquor-ethanolic solution neutralization.The volume ratio of ammoniacal liquor can be between 5～15% in ammoniacal liquor-ethanolic solution.
The corrosive liquid that in the present invention, can be used for low power dendrite corrosion is the acid solution of chlorination cuprammonium.The mass percent concentration of cupric chloride ammonia solution can be between 5～25%, preferably between 8～15%.The pH value of solution can be between 1～6.
The concentration of each corrosive liquid is not limited to above-mentioned scope, and it can be higher or lower, still, for different concentration, can respective change time of corrosion.For the corrosive liquid of high concentration, the time of corrosion should lack relatively, and for the corrosive liquid of low concentration, etching time should be grown relatively.
Can carry out above-mentioned segregation corrosion and dendrite corrosion with several different methods.For example, can be about to the steel billet sample and be immersed in appropriate time in the corrosive liquid, also can corrosive liquid be sprayed at specimen surface through the etch method.In a kind of optimal way of the present invention, adopt wipe method, promptly dip in and get corrosive liquid wiping specimen surface with sponge, absorbent cotton or other sorbing materials.This wiping can be carried out repeatedly, after the corrosive liquid of observing wiping is consumed by major part, carries out next wiping again, up to reaching required corrosive effect.
The steel billet sample can be removed the corrosion product that sample is examined face after carrying out low power dendrite corrosion, for example can use brush, fabric or other flexible material wiping specimen surfaces, can also receive inspection face with the sand paper sample of slightly polishing.
The present invention can accurately measure Interventions Requested in the solidified structure, the area of promptly tiny equiax crystal (chill), column crystal, intersection dendrite and center equiax crystal, quantitative measurement dendrite secondary limb spacing owing to added a dendrite corrosion step.
Of the present invention preferred aspect, also produce other advantage: owing to adopt cold corrosive liquid that sample is examined the face wiping, watered erosion, use the acid solution much less, both saved the acid solution cost, also avoid the acid solution contaminated environment than existing etch method; Need not etching tank and hanging apparatus specialized equipment, save equipment investment; Simple, convenient; After polishing a little with sand paper after the corrosion, can directly be observed by bore hole, also available shooting style is taken record.Because experimental technique provided by the invention is simple, convenient, quick, safe and reliable again, does not have the discharging of waste liquid contaminated environment basically, thus be not only applicable to laboratory experiment, and be applicable to STEELMAKING PRODUCTION field experiment.
The drawing of accompanying drawing is explained as follows:
Embodiment 1:
The steel billet sample is conventional carbon steel, sulfur-bearing 0.022%, carbon containing 0.13%.
After the steel billet specimen surface is machined to surfaceness and is not more than 1.25 μ m, on the basis of low power segregation corrosion, carry out the corrosion of low power dendrite, observe dendrite and defective that the steel billet specimen surface is manifested then with cold acid corrosion method.
Low power segregation corrosive liquid comprises first corrosive liquid and second corrosive liquid, the ammonium persulfate solution of the said first corrosive liquid mass percent concentration between 10～20%, and second corrosive liquid is a salpeter solution, its mass percent concentration is between 15～30%.
Low power dendrite corrosive liquid is the acid solution of chlorination cuprammonium, and its mass percent concentration is between 8～15%, and the pH value of solution is between 1～6.
Said low power segregation corrosive liquid is applied to the surface of steel billet sample through wipe method.
After the steel billet sample receives inspection face by low power segregation corrosion, further examined the cold corrosive liquid of face, removed cold corrosive liquid with flushing with clean water then with ammoniacal liquor-ethanolic solution neutralization.
The operation steps of low power dendrite corrosion is: 1. get the sample of doing low power segregation corrosion; Cupric chloride ammonia corrosion liquid is watered receiving on the inspection face at steel billet equably; Perhaps with corrosion resistant sprinkling equipment cupric chloride ammonia corrosion liquid being sprayed on steel billet equably receives on the inspection face; 2. etching time is about 20 minutes, on the inspection face of receiving, observes dendrite and distributes and casting blank defect.
After the steel billet sample carries out low power dendrite corrosion, receive inspection face with 1000 orders or the 2000 order sand paper sample of slightly polishing, examined the face corrosion product up to sample and removed.
The photo of Fig. 1 for taking with 1,000 ten thousand pixel digital cameras through the steel billet sample after embodiment 1 operational processes can obviously be seen dendrite and defective that the steel billet sample exists, and this can't realize in the prior art.
Embodiment 2:
The steel billet sample is the low-sulfur continuous casting billet, sulfur-bearing 0.013%, carbon containing 0.14%.
Used cold acid corrosion liquid is all identical with last example with the experimental implementation step of employing.
The photo of Fig. 2 for taking with 1,000 ten thousand pixel digital cameras through the steel billet sample after embodiment 2 operational processes can obviously be seen equiax crystal, dendrite and defective that the steel billet sample exists, and this can't realize in the prior art.
Claims (7)
1. one kind shows the cold acid corrosion method used of low-multiple branch crystals in billet, it is characterized in that, may further comprise the steps:
A) the steel billet specimen surface is machined to surfaceness and is not more than 1.25 μ m;
B) with low power segregation corrosive liquid wiping or water erosion steel billet sample;
C) with the corrosive liquid wiping of low power dendrite or water the erosion said steel billet sample,
Wherein, said low power dendrite corrosive liquid is the acid solution of chlorination cuprammonium, and the mass percent concentration of cupric chloride ammonia solution is between 5～25%, and the pH value of solution is between 1～6.
2. method according to claim 1; Wherein, Said low power segregation corrosive liquid comprises first corrosive liquid and second corrosive liquid; The said first corrosive liquid mass percent concentration is 10～30% ammonium persulfate solution, and second corrosive liquid is the inorganic acid solution that is selected from sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, and its mass percent concentration is between 8～30%.
3. method according to claim 2, wherein, said first corrosive liquid is 10～20% ammonium persulfate solution, and second corrosive liquid is the inorganic acid solution that is selected from sulfuric acid, hydrochloric acid, nitric acid, and its mass percent concentration is between 15～30%.
4. according to claim 2 or 3 described methods, wherein, after the steel billet sample receives inspection face by low power segregation corrosion, further examined the cold corrosive liquid of face, removed cold corrosive liquid with flushing with clean water then with ammoniacal liquor-ethanolic solution neutralization.
5. method according to claim 1 wherein, is applied to said low power segregation corrosive liquid through wipe method the surface of steel billet sample.
6. according to the said method of claim 1; Wherein, The operation steps of said low power dendrite corrosion is: 1. get the sample of doing low power segregation corrosion, cupric chloride ammonia corrosion liquid is watered the receiving on the inspection face of steel billet equably, perhaps with corrosion resistant sprinkling equipment cupric chloride ammonia corrosion liquid is sprayed on steel billet equably and receives on the inspection face; 2. etching time is about 20 minutes, on the inspection face of receiving, observes dendrite and distributes and casting blank defect.
7. method according to claim 1 wherein, after said steel billet sample carries out low power dendrite corrosion, receives inspection face with 1000 orders or the 2000 order sand paper sample of slightly polishing, and is examined the face corrosion product up to sample and removes.
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| CN102830054A (en) * | 2011-06-17 | 2012-12-19 | 南京梅山冶金发展有限公司 | Automatic low-power erosion detector |
| CN103323317B (en) * | 2013-05-31 | 2015-09-16 | 中国一拖集团有限公司 | A kind of discriminating judges that axostylus axostyle class and dish overlap the method for class steel components blank forming |
| CN104677714B (en) * | 2013-11-30 | 2017-12-05 | 中国科学院金属研究所 | The macrostructure of steel and defect etching reagent and detection method |
| CN106442077A (en) * | 2015-08-13 | 2017-02-22 | 上海梅山钢铁股份有限公司 | Low-power test reagent for diphase automobile steel with tensile strength of 590 MPa grade |
| CN109297444B (en) * | 2018-11-01 | 2021-01-05 | 中国航发成都发动机有限公司 | Stainless steel die forging blade streamline inspection method and corrosive liquid manufacturing method |
| CN110554162A (en) * | 2019-09-03 | 2019-12-10 | 安阳豫德机械有限公司 | Simple and rapid on-site hot-rolled steel defect detection method |
| CN110749718A (en) * | 2019-10-25 | 2020-02-04 | 成都先进金属材料产业技术研究院有限公司 | Dendritic crystal corrosive agent and corrosion method for maraging stainless steel |
| CN112362438A (en) * | 2020-11-17 | 2021-02-12 | 陕西龙门钢铁有限责任公司 | Application method of cold corrosion display reagent for macrostructure and defects of continuous casting steel billet |
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| CN1295241A (en) * | 2000-11-27 | 2001-05-16 | 宝山钢铁股份有限公司 | Cold erodent liquid pouring erosion process to detect low-multiple fault inside steel billet |
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| CN1295241A (en) * | 2000-11-27 | 2001-05-16 | 宝山钢铁股份有限公司 | Cold erodent liquid pouring erosion process to detect low-multiple fault inside steel billet |
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Application publication date: 20100512 Assignee: Hengyang Ramon Science & Technology Co., Ltd. Assignor: Tian Lu Contract record no.: 2015430000031 Denomination of invention: Cold acid corrosion method used for displaying low-multiple branch crystals in billet Granted publication date: 20121121 License type: Exclusive License Record date: 20150427 |
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