CN110470525A - Show the aggressive agent and corrosion method of IF steel crystal boundary - Google Patents

Show the aggressive agent and corrosion method of IF steel crystal boundary Download PDF

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Publication number
CN110470525A
CN110470525A CN201910710742.6A CN201910710742A CN110470525A CN 110470525 A CN110470525 A CN 110470525A CN 201910710742 A CN201910710742 A CN 201910710742A CN 110470525 A CN110470525 A CN 110470525A
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CN
China
Prior art keywords
steel
crystal boundary
aggressive agent
display
corrosion method
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Pending
Application number
CN201910710742.6A
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Chinese (zh)
Inventor
彭红兵
唐尧
颉震
汪晓勇
周超洋
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Jiangsu University of Science and Technology
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Jiangsu University of Science and Technology
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Publication date
Application filed by Jiangsu University of Science and Technology filed Critical Jiangsu University of Science and Technology
Priority to CN201910710742.6A priority Critical patent/CN110470525A/en
Publication of CN110470525A publication Critical patent/CN110470525A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

Abstract

The invention discloses a kind of aggressive agent and corrosion method for showing IF steel crystal boundary, the ingredients and proportion of the aggressive agent are as follows: perchloric acid 5%-10%, dehydrated alcohol 90%~95%, and disclose the method eroded using the aggressive agent.Grain-boundary attack agent provided by the invention and corrosion method, step is simple, and the time is short, easy to operate, can quickly obtain clearly IF steel crystal boundary and grain properties.

Description

Show the aggressive agent and corrosion method of IF steel crystal boundary
Technical field
The present invention relates to aggressive agent and corrosion methods, and in particular to it is a kind of show IF steel crystal boundary aggressive agent and erosion side Method.
Background technique
IF steel, i.e. gapless atomic steel are widely used in manufacturing car panel because of its excellent deep drawability.In reality In the production of border, C, N atom often fixed in steel by adding a small amount of Ti, Nb, to obtain the pure iron element of gap-free atom Body steel, the size and form of ferrite crystal grain will directly affect the performance of steel.
It is at room temperature pure ferritic structure since IF steel grain boundaries there's almost no interstitial atom, therefore using often The nital of rule corrodes, and hardly results in clearly crystal boundary and grain properties, and then influence sample grain size number, crystalline substance The evaluation of the mean intercept of grain etc. causes very big puzzlement to vast production and the metal lographic examination of researcher, also hinders The further research and development of the steel grade.
Chinese patent CN97100731.4 discloses a kind of method for displaying metallographic structure of cold rolled annealed gapless atomic steel, this is specially The sample edge polishing side erosion removal of milled is interfered layer first by benefit, after then utilizing the pre-etching of nitric acid alcohol, then uses 1-10% Sodium Metabisulfite, 3-20% Sodium Thio Sulphate(Anhydrous), remaining carries out corrosion until test face is all in for the reagent of distilled water It after light blue, rinses, clean light blue surface layer, clearly metallographic structure can be obtained;Chinese patent CN97119946.9 discloses " cold Roll annealed gapless atomic steel method for displaying metallographic structure ", which is polished to naked eyes first by metallographic sample sand paper grind away After not observing apparent scratch, with hydrogen peroxide 30-45%, oxalic acid 1.5-10%, hydrofluoric acid 0.1-1%, remaining is water Reagent dabs the corrosion interference layer of removal in examination face 25-50 seconds, is then that 1-10% is laid particular stress on 1-5% nitric acid alcohol pre-etching and ingredient Sodium sulfite, 3-20% Sodium Thio Sulphate(Anhydrous), remaining corrodes for the reagent of distilled water, can obtain clearly metallographic structure;China Patent CN201210371639.1 discloses " a kind of gapless atomic steel flat cold-rolled sheet method for displaying metallographic structure containing Ti ", should Sample after grinding is configured to using using dehydrated alcohol and water according to the volume ratio of 2:3~7:3 by patent during the polishing process Ethanol water polishing sample is prepared as lubricant after, then corroded using two-step method, first step corrosion uses The first corrosive agent that sulfuric acid oxalic acid aqueous solution adds hydrogen peroxide repeated hydrogenation fluoric acid to prepare is corroded, and second step corrosion uses nitric acid wine Smart solution is corroded, and clearly ferrite grain boundaries can be obtained.
Existing method is required to two kinds of corrosive agent of configuration, and corrosion step is relatively complicated, in practical operation, any link It is unclear unsuccessfully to will lead to Display of Grain Boundary, causes workload to double, brings great inconvenience to metal lographic examination.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of aggressive agents and corrosion method for showing IF steel crystal boundary, solve existing There is method to need two kinds of corrosive agent, corrosion step is cumbersome, the problem of be easy to causeing the failure of an experiment.
Technical solution: it is of the present invention display IF steel crystal boundary aggressive agent, component include: with volume percentage, The perchloric acid of 5%-10% and 90%~95% dehydrated alcohol.
Wherein, the perchloric acid uses weight percent for the high fluoric acid of 70-72%.
The corrosion method of the aggressive agent of display IF steel crystal boundary of the present invention, comprising the following steps:
(1) IF steel curved beam is pre-processed;
(2) the IF steel curved beam pre-processed is connected with the anode of DC power supply, using copper sheet or stainless steel substrates as cathode, The IF steel curved beam and cathode that have pre-processed are placed in aggressive agent relatively, erodes, obtains the metallographic of display IF steel crystal boundary Sample.
The step (1) specifically: IF steel curved beam is ground on silicon carbide waterproof abrasive paper, 0.5-1 μm is used on polishing machine Diamond paste polishing, it is as bright as a sixpence until specimen surface is without obvious scratch, then use washes of absolute alcohol surface, blow Blower drying.
When eroding in the step (2), the voltage of power supply is 14-30V, electric current 0.7-2.1A, time 10- 120s, temperature are RT-35 DEG C.
The utility model has the advantages that the method for the present invention is simple, easy to operate, etching time is short, after this method corrodes, can obtain clear Clear crystal boundary and grain properties,
Detailed description of the invention
Fig. 1 is IF steel crystal boundary and grain morphology after the corrosion of 4% nitric acid alcohol;
Fig. 2 is that embodiment 1 obtains IF steel crystal boundary and grain morphology;
Fig. 3 is that embodiment 2 obtains IF steel crystal boundary and grain morphology;
Fig. 4 is that embodiment 3 obtains IF steel crystal boundary and grain morphology.
Specific embodiment
Invention is further explained with reference to the accompanying drawing.
The chemical component for the IF steel that the present invention uses is as shown in table 1.
The chemical component of table 1IF steel
C Al Si P S Ti Mn N O Fe
0.002 0.016 0.018 0.005 0.002 0.06 0.2 0.0016 0.0022 Bal.
IF steel curved beam is successively ground on 600#, 1000#, 1500#, 2000# silicon carbide waterproof abrasive paper, then in polishing machine The upper diamond paste with 0.5 μm polishes, as bright as a sixpence until specimen surface is without obvious scratch, then clear with dehydrated alcohol Wash surface, hair dryer drying, in case corrosion is used.Crystal boundary and grain morphology after being corroded with 4% nitric acid alcohol, as shown in Figure 1.
It is eroded below using the present invention, specific as follows:
Embodiment 1
IF steel curved beam is successively ground on 600#, 1000#, 1500#, 2000# silicon carbide waterproof abrasive paper, then in polishing machine The upper diamond paste with 0.5 μm polishes, as bright as a sixpence until specimen surface is without obvious scratch, then clear with dehydrated alcohol Wash surface, hair dryer drying, in case corrosion is used.Taking 5ml weight percent is the perchloric acid solution of 70-72%, pours into 95ml's In dehydrated alcohol, stir evenly.Sample is connected with the anode of DC power supply, it is positive and negative using copper sheet or stainless steel substrates as cathode Extremely staggered relatively to be placed in etchant, voltage 26V, electric current 1.8A, time 20s, temperature is 20 DEG C, then takes out examination Sample, cleaning, drying, light microscopic testing result is as shown in Fig. 2, can be observed clearly crystal boundary and grain properties.
Embodiment 2
IF steel curved beam is successively ground on 600#, 1000#, 1500#, 2000# silicon carbide waterproof abrasive paper, then in polishing machine The upper diamond paste with 0.5 μm polishes, as bright as a sixpence until specimen surface is without obvious scratch, then clear with dehydrated alcohol Wash surface, hair dryer drying, in case corrosion is used.Taking 7ml weight percent is the perchloric acid solution of 70-72%, pours into 93ml's In dehydrated alcohol, stir evenly.Sample is connected with the anode of DC power supply, it is positive and negative using copper sheet or stainless steel substrates as cathode Extremely staggered relatively to be placed in etchant, voltage 24V, electric current 1.6A, time 13s, temperature is 30 DEG C, then takes out examination Sample, cleaning, drying, light microscopic detect as shown in figure 3, clearly crystal boundary and grain properties can be observed.
Embodiment 3
IF steel curved beam is successively ground on 600#, 1000#, 1500#, 2000# silicon carbide waterproof abrasive paper, then in polishing machine The upper diamond paste with 0.5 μm polishes, as bright as a sixpence until specimen surface is without obvious scratch, then clear with dehydrated alcohol Wash surface, hair dryer drying, in case corrosion is used.Taking 5ml weight percent is the perchloric acid solution of 70-72%, pours into 95ml's In dehydrated alcohol, stir evenly.Sample is connected with the anode of DC power supply, it is positive and negative using copper sheet or stainless steel substrates as cathode Extremely staggered relatively to be placed in etchant, voltage 26V, electric current 1.9A, time 10s, temperature is 20 DEG C, then takes out examination Sample, cleaning, drying, light microscopic detect as shown in figure 4, clearly crystal boundary and grain properties can be observed.

Claims (5)

1. a kind of aggressive agent for showing IF steel crystal boundary, which is characterized in that its component includes: with volume percentage, 5%-10% Perchloric acid and 90%~95% dehydrated alcohol.
2. the aggressive agent of display IF steel crystal boundary according to claim 1, which is characterized in that the perchloric acid uses weight hundred Divide than the high fluoric acid for 70-72%.
3. using the corrosion method of the aggressive agent such as the described in any item display IF steel crystal boundaries of claim 1-2, which is characterized in that The following steps are included:
(1) IF steel curved beam is pre-processed;
(2) the IF steel curved beam pre-processed is connected with the anode of DC power supply, it, will be pre- using copper sheet or stainless steel substrates as cathode The IF steel curved beam and cathode handled well are opposite to be placed in aggressive agent, is eroded, is obtained the metallographic specimen of display IF steel crystal boundary.
4. the corrosion method of the aggressive agent of display IF steel crystal boundary according to claim 3, which is characterized in that the step (1) specifically: IF steel curved beam is ground on silicon carbide waterproof abrasive paper, is thrown on polishing machine with 0.5-1 μm of diamond paste Light, until specimen surface is without obvious scratch, as bright as a sixpence, subsequent to use washes of absolute alcohol surface, hair dryer is dried up.
5. the corrosion method of the aggressive agent of display IF steel crystal boundary according to claim 3, which is characterized in that the step (2) when eroding in, the voltage of power supply is 14-30V, electric current 0.7-2.1A, time 10-120s, temperature RT-35 ℃。
CN201910710742.6A 2019-08-02 2019-08-02 Show the aggressive agent and corrosion method of IF steel crystal boundary Pending CN110470525A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110724999A (en) * 2019-10-23 2020-01-24 沈阳航空航天大学 Electrolyte for CoCrNi multi-principal-element alloy with high Cr content and corrosion process
CN112442692A (en) * 2020-12-07 2021-03-05 中国航发哈尔滨轴承有限公司 32Cr3MoVE material grain size corrosion method

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CN107462456A (en) * 2016-06-03 2017-12-12 宁波江丰电子材料股份有限公司 Method for displaying metallographic structure
CN111982641A (en) * 2019-05-22 2020-11-24 天津大学 FeCoNiCrMnAl high-entropy alloy electrolytic corrosion electrolyte and display method of metallographic structure thereof

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CN107462456A (en) * 2016-06-03 2017-12-12 宁波江丰电子材料股份有限公司 Method for displaying metallographic structure
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110724999A (en) * 2019-10-23 2020-01-24 沈阳航空航天大学 Electrolyte for CoCrNi multi-principal-element alloy with high Cr content and corrosion process
CN110724999B (en) * 2019-10-23 2021-09-28 沈阳航空航天大学 Electrolyte for CoCrNi multi-principal-element alloy with high Cr content and corrosion process
CN112442692A (en) * 2020-12-07 2021-03-05 中国航发哈尔滨轴承有限公司 32Cr3MoVE material grain size corrosion method
CN112442692B (en) * 2020-12-07 2022-09-23 中国航发哈尔滨轴承有限公司 32Cr3MoVE material grain size corrosion method

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Application publication date: 20191119