CN107843592A - A kind of austenitic stainless steel weld joint tissue corrosive agent and its application method - Google Patents
A kind of austenitic stainless steel weld joint tissue corrosive agent and its application method Download PDFInfo
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- CN107843592A CN107843592A CN201710942490.0A CN201710942490A CN107843592A CN 107843592 A CN107843592 A CN 107843592A CN 201710942490 A CN201710942490 A CN 201710942490A CN 107843592 A CN107843592 A CN 107843592A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
The invention discloses a kind of austenitic stainless steel weld joint tissue corrosive agent and its application method, and the corrosive agent is by concentrated hydrochloric acid, copper chloride, absolute ethyl alcohol composition.Application method includes following steps：（1）The preparation of metallographic specimen：Stainless steel weld joint coupon is ground and mechanically polished through different grain size silicon carbide paper successively；（2）The corrosion of metallographic specimen：Metallographic specimen is immersed in corrosive liquid and corroded；（3）The metallographic specimen observation of corrosion：Sample a large amount of water and the alcohol rinse corroded is taken out, arborescent structure is observed under the microscope after air-drying.A kind of austenitic stainless steel weld joint tissue corrosive liquid provided by the present invention, prepare simply, easily stored, easy to operation, corrosive effect is obvious；Melt run and weld seam dendrite after corrosion is obvious, and tissue is clear, without the uneven phenomenon of any excessive erosion or corrosion；The present invention has very great help to improving welding manner, and according to the bonding of austenitic stainless steel weld joint to each performance improvement of stainless steel welded part.
Description
Technical field
The invention belongs to metal lographic examination analysis technical field, and in particular to a kind of austenitic stainless steel weld joint tissue corrosive agent
And its application method.
Background technology
Austenitic stainless steel has stable austenite structure at normal temperatures, and entirety is nonmagnetic and has high tenacity and modeling
Property.Compared with other kinds of stainless steel, austenitic stainless steel is easier to welding, and phase occurs in no instance
Become, insensitive to hydrogen, welding point there are preferable plasticity and toughness under as-welded.But easily form fire check and intercrystalline corrosion etc. to lack
Fall into.The tissue quality of welding point directly affects the performance of whole weldment again.Therefore can be adjusted by observing seam organization
Whole suitable welding procedure and welding method, and then improve weldment performance.
Because contain Ni, Cr so that austenitic stainless steel has excellent corrosion resistance, so selecting suitable corrosive liquid to make weldering
Seam can clearly show that its crystal boundary and tissue are very important.Inspection information, related dendrite corrosive agent apply to carbon more
Steel and steel alloy or cast iron, stainless steel weld joint arborescent structure corrosive agent are seldom.The solution of the most frequently used corrosion stainless steel has king
Water, nitric acid, hydrochloric acid solution.During with chloroazotic acid and nitric acid corrosion weld seam, because its corrosivity is strong, excessive erosion easily is caused to sample, made
Corrosion inhomogeneities, and volatile, strong corrosion is integrally presented in specimen surface, certain potential safety hazard be present, experimenter is caused
Injury.
It is rotten described in publication number CN101144762A " a kind of corrosive agent and its compound method for showing silicon steel coagulation tissue "
Liquid is lost, is only applicable to silicon steel, and dosing need to be adjusted according to the species of specific alloying element in silicon steel chemical composition and content,
Solution is prepared more complicated.
Corrosive liquid described in application number 201410488828.6 " a kind of ferritic stainless steel face of weld caustic solution ", it is rotten
Corrosion is weak, is not suitable for corroding Ni and Cr contained austenitic stainless steel.
Application number 201410702250.X be " a kind of austenite stainless steel continuous casting slab oscillation mark area solidified structure and arborescent structure
Corrosive liquid and caustic solution " the corrosive liquid corrosive effect is also bad.
Research one kind can clearly identify melt run, clearly show the arborescent structure of weld seam, to improving welding manner
Being improved with the properties to stainless steel welded part to have very great help.
The content of the invention
The technical problems to be solved by the invention there is provided a kind of austenitic stainless steel weld joint tissue corrosive agent, while this
Invention additionally provides a kind of application method of austenitic stainless steel weld joint tissue corrosive agent.The present invention can clearly identify fusion
Line, the arborescent structure of weld seam is clearly shown, especially suitable for 316/316L/317/317L stainless steels and part high nitrogen stainless steel
Seam organization show.
In order to solve the above technical problems, the technical solution used in the present invention is：A kind of austenitic stainless steel weld joint tissue
Corrosive agent, the corrosive agent constituent include：Copper chloride, concentrated hydrochloric acid, absolute ethyl alcohol.
Copper chloride addition of the present invention is 2~3g, and concentrated hydrochloric acid addition is 30~50ml, and absolute ethyl alcohol addition is
50~80ml.
Mass fraction >=99% of copper chloride of the present invention；The concentrated hydrochloric acid mass fraction is 36%；The absolute ethyl alcohol
Concentration >=97%.
Corrosive agent configuration of the present invention comprises the following steps：Copper chloride is weighed first, pours into beaker；Then with graduated cylinder amount
Take concentrated hydrochloric acid to pour into beaker, and be stirred continuously with glass bar, make copper chloride grain dissolution, be eventually adding absolute ethyl alcohol, stirring is equal
It is even, 20min is stood, it is stand-by.
Present invention also offers a kind of application method of austenitic stainless steel weld joint tissue corrosive agent, methods described includes gold
The preparation of phase sample, the metallographic specimen observation of the burn into corrosion of metallographic specimen.
The preparation of metallographic specimen of the present invention comprises the following steps：
1）Sample is cut, and stainless steel welded sample is retained into weld metal zone and part mother metal, is cut into using cutting machine and is adapted to grinding
Metallographic specimen, and polish off on abrasive machine the wedge angle of sample；
2）Sample polishes, and on the mill of semi-automatic sample grinding machine, the silicon carbide paper through different meshes grinds sample successively；Per pass is ground
During sample, sample will keep a direction, so as to the cut neat and consistent ground；After often having ground one of sand paper, by sample
90 degree of parallel rotating carries out down grinding together again, ensures that lower one of polishing scratch can cover together upper；
3）Sample polishes, and the sample after grinding polishes on polishing machine, using diamond spray grinding and polishing；Alcohol rinse after polishing
Sample sightingpiston, is then dried up with hair-dryer.
Sample of the present invention polishing, the silicon carbide paper mesh number used successively are 240 mesh, 400 mesh, 800 mesh, 1200 mesh.
Sample polishing of the present invention, uses the silk polishing cloth without gum；Grinding and polishing is sprayed using the μ diamonds of granularity 1~5
Agent.
The corrosion of metallographic specimen of the present invention comprises the following steps：
1）With sample after tweezers gripping mill, putting it into the corrosive liquid prepared, corrosive liquid is totally submerged metallographic specimen surface,
When specimen surface is changed into silvery white completely from bright face, corrosion terminates；
2）The metallographic specimen that corrode is taken out, with the flushing of a large amount of water, then with alcohol rinse, is finally blown specimen surface with hair-dryer
It is dry.
The metallographic specimen observation of corrosion of the present invention, the metallographic specimen of corrosion just put light microscope in Imager M2m
Lower observation metallographic structure.
The preparation of metallographic specimen of the present invention comprises the following steps：Sample is cut, and stainless steel welded sample is retained into weld seam
Area and part mother metal, the metallographic specimen for being adapted to grinding is cut into using cutting machine, and the wedge angle of sample is polished off on abrasive machine；
Sample polishes, and on the mill of semi-automatic sample grinding machine, the silicon carbide paper through different meshes grinds sample successively.The mistake of per pass grind away
Cheng Zhong, sample will keep a direction, so as to the cut neat and consistent ground.After often having ground one of sand paper, by the parallel rotation of sample
It turn 90 degrees and carries out down grinding together again, ensures that every lower road polishing scratch can cover together upper；Sample is polished, and the sample after grinding is being thrown
Polished on ray machine, using diamond spray grinding and polishing.Humidity and dynamics are controlled during polishing, until specimen surface is without any stroke
Trace, throw trace and watermark.Finally air-dried after alcohol rinse sample sightingpiston with hair-dryer.
The austenitic stainless steel weld joint dendrite corrosive liquid of the present invention is formed by concentrated hydrochloric acid and copper chloride, alcohol, wherein
Concentrated hydrochloric acid is reproducibility acid, alcohol dissolving copper chloride, forms a kind of electrolyte solution.Stainless steel mutually in etchant solution with hydrochloric acid
Reduction chemical reaction occurs with copper chloride, forms extremely how small local cell.Part with negative potential turns into anode, molten
Enter in corrosive liquid and gradually dented；Part with positive potential turns into negative electrode, keeps original level.In light microscopic white light
Irradiation under, the interference effect of light makes each phase that different colors be presented, so as to recognize tissue.
It is using beneficial effect caused by above-mentioned technical proposal：1st, a kind of austenitic stainless steel provided by the present invention
Seam organization corrosive agent, prepare simply, easily stored, easy to operation, corrosive effect is obvious, within etching time 30min.2、
Melt run and weld seam dendrite of the present invention after corrosion are obvious, and tissue is clear, without the uneven phenomenon of any excessive erosion or corrosion.
3rd, the present invention changes to improving welding manner, and according to the bonding of austenitic stainless steel weld joint to each performance of stainless steel welded part
Enter to have very great help.
Brief description of the drawings
Fig. 1 is the 100 times of micro-organization charts of 316L stainless steel weld joints corroded with chloroazotic acid；
Fig. 2 is 100 times of micro-organization charts of 316L stainless steel weld joints in embodiment 1；
Fig. 3 is 100 times of micro-organization charts of high nitrogen stainless steel weld seam in embodiment 2；
Fig. 4 is 100 times of micro-organization charts of 316L stainless steel weld joints in embodiment 3.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further detailed explanation.
Embodiment 1
316L stainless steels are used in the present embodiment, the chemical composition of steel is shown in Table 1.
The chemical composition composition and weight/mass percentage composition of the 316L stainless steels of table 1（wt%）
316L stainless steel weld joint tissue corrosive agent and application method comprise the following steps：
1. the preparation of corrosive agent, is comprised the following steps that：
The copper chloride 3g of mass fraction 99% is weighed on electronic balance, is poured into beaker, 36% dense salt of mass fraction is measured with graduated cylinder
Sour 50ml, slowly pour into beaker along wall of cup, and be stirred continuously with glass bar, make copper chloride grain dissolution, be eventually adding 50ml
The absolute ethyl alcohol of concentration 97%, being gently mixed with glass bar makes to pour into volumetric flask after solution is well mixed, solution left standstill 20min, treats
With.
2. the preparation of metallographic specimen：
Retain weld seam and part mother metal area, 316L piece of stainless steel is cut into the metallographic specimen for being adapted to grinding using cutting machine,
Chamfering is carried out on abrasive machine；On the mill of semi-automatic sample grinding machine, successively through 240 mesh, 400 mesh, 800 mesh, the water mill of 1200 mesh
Sand paper grinds sample；Sample after grinding is mechanically polished using the silk polishing cloth without gum on polishing machine, using granularity 1~
5 μ diamond spray grinding and polishings, control humidity and dynamics during polishing, until specimen surface without any cut, throw trace and watermark；
Alcohol rinse sample sightingpiston is finally used, is then dried up with hair-dryer.
3. etching pit and observation
With the sample of tweezers gripping milled, put it into corrosive liquid, corrosive liquid is totally submerged metallographic specimen surface, corrosion
2min, when metallographic specimen surface is changed into silvery white from bright face, takes out rinsed under running water pipe with a large amount of water rapidly, then use wine
Fine is washed, and is finally dried up specimen surface with hair-dryer；The metallographic specimen of drying is just put under light microscope in ImagerM2m
Fig. 2 sees in tissues observed, micro-organization chart.
Embodiment 2
Originally apply in example and use 1Cr17Mn9Ni4N high nitrogen stainless steels, the chemical composition of steel is shown in Table 2.
The chemical composition composition and weight/mass percentage composition of the 1Cr17Mn9Ni4N high nitrogen stainless steels of table 2（wt%）
1Cr17Mn9Ni4N high nitrogen stainless steel seam organization corrosive agent and application method comprise the following steps：
1. the preparation of corrosive agent, is comprised the following steps that：
The copper chloride 2g of mass fraction 99% is weighed on electronic balance, is poured into beaker, 36% dense salt of mass fraction is measured with graduated cylinder
Sour 30ml, slowly pour into beaker along wall of cup, and be stirred continuously with glass bar, make copper chloride grain dissolution, be eventually adding 80ml
The absolute ethyl alcohol of concentration 97%, being gently mixed with glass bar makes to pour into volumetric flask after solution is well mixed, solution left standstill 20min, treats
With.
2. the preparation of metallographic specimen：
Retain weld seam and part mother metal area, 1Cr17Mn9Ni4N high nitrogen stainless steels block is cut into using cutting machine and is adapted to grinding
Metallographic specimen, chamfering is carried out on abrasive machine；On the mill of semi-automatic sample grinding machine, successively through 240 mesh, 400 mesh, 800 mesh,
The silicon carbide paper grinding sample of 1200 mesh；Sample after grinding using the silk polishing cloth without gum, throw by the machinery on polishing machine
Light, humidity and dynamics are controlled using the μ diamond spray grinding and polishings of granularity 1~5, during polishing, until specimen surface is without any stroke
Trace, throw trace and watermark；Alcohol rinse sample sightingpiston is finally used, is then dried up with hair-dryer.
3. etching pit and observation
With the sample of tweezers gripping milled, putting it into corrosive liquid, corrosive liquid is totally submerged metallographic specimen surface, corrodes 10s,
When metallographic specimen surface is changed into silvery white from bright face, takes out rinsed under running water pipe with a large amount of water rapidly, then rushed with alcohol
Wash, finally dried up specimen surface with hair-dryer；The metallographic specimen of drying is just being put into optical microphotograph Microscopic observation in ImagerM2m
Tissue, microscopic structure are shown in Fig. 3.
Embodiment 3
316L stainless steels are used in the present embodiment, the chemical composition of steel is shown in Table 3.
The chemical composition composition and weight/mass percentage composition of the 316L stainless steels of table 3（wt%）
316L stainless steel weld joint tissue corrosive agent and application method comprise the following steps：
1. the preparation of corrosive agent, is comprised the following steps that：
The copper chloride 2.5g of mass fraction 99% is weighed on electronic balance, is poured into beaker, it is dense to measure mass fraction 38% with graduated cylinder
Hydrochloric acid 40ml, slowly pour into beaker along wall of cup, and be stirred continuously with glass bar, make copper chloride grain dissolution, be eventually adding
The absolute ethyl alcohol of 65ml concentration 98%, being gently mixed with glass bar makes to pour into constant volume in volumetric flask, solution left standstill after solution is well mixed
20min, it is stand-by.
2. the preparation of metallographic specimen：
Retain weld seam and part mother metal area, 316L piece of stainless steel is cut into the metallographic specimen for being adapted to grinding using cutting machine,
Chamfering is carried out on abrasive machine.On the mill of semi-automatic sample grinding machine, successively through 240 mesh, 400 mesh, 800 mesh, the water mill of 1200 mesh
Sand paper grinds sample.Sample after grinding is mechanically polished using the silk polishing cloth without gum on polishing machine, using the μ of granularity 1
Diamond spray grinding and polishing, control humidity and dynamics during polishing, until specimen surface without any cut, throw trace and watermark.Most
After using alcohol rinse sample sightingpiston afterwards, air-dried with hair-dryer.
3. etching pit and observation
With the sample of tweezers gripping milled, put it into corrosive liquid, corrosive liquid is totally submerged metallographic specimen surface, corrosion
2.5min, when metallographic specimen surface is changed into silvery white from bright face, takes out rinsed under running water pipe with a large amount of water rapidly, then use
Alcohol rinse, finally specimen surface is dried up with hair-dryer.The metallographic specimen of drying is just put into optical microphotograph in Imager M2m
Microscopic observation tissue, tissue are shown in Fig. 4.
Above example is only to illustrative and not limiting technical scheme, although with reference to above-described embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that：Still the present invention can be modified or be waited
With replacing, any modification or partial replacement without departing from the spirit and scope of the present invention, it all should cover the power in the present invention
Among sharp claimed range.
Claims (10)
1. a kind of austenitic stainless steel weld joint tissue corrosive agent, it is characterised in that the corrosive agent constituent includes：Chlorination
Copper, concentrated hydrochloric acid, absolute ethyl alcohol.
A kind of 2. austenitic stainless steel weld joint tissue corrosive agent according to claim 1, it is characterised in that the copper chloride
Addition is 2~3g, and concentrated hydrochloric acid addition is 30~50ml, and absolute ethyl alcohol addition is 50~80ml.
A kind of 3. austenitic stainless steel weld joint tissue corrosive agent according to claim 1, it is characterised in that the copper chloride
Mass fraction >=99%；The concentrated hydrochloric acid mass fraction is 36%；Concentration >=97% of the absolute ethyl alcohol.
A kind of 4. austenitic stainless steel weld joint tissue corrosive agent according to claim 1, it is characterised in that the corrosive agent
Configuration comprises the following steps：Copper chloride is weighed first, pours into beaker；Then measure concentrated hydrochloric acid with graduated cylinder and pour into beaker, and use glass
Glass rod is stirred continuously, and is made copper chloride grain dissolution, is eventually adding absolute ethyl alcohol, stirs, and stands 20min, stand-by.
5. based on a kind of application method of austenitic stainless steel weld joint tissue corrosive agent described in claim 1-4 any one,
Characterized in that, methods described includes the preparation of metallographic specimen, the metallographic specimen observation of the burn into corrosion of metallographic specimen.
A kind of 6. application method of austenitic stainless steel weld joint tissue corrosive agent according to claim 5, it is characterised in that
The preparation of the metallographic specimen comprises the following steps：
1）Sample is cut, and stainless steel welded sample is retained into weld metal zone and part mother metal, is cut into using cutting machine and is adapted to grinding
Metallographic specimen, and polish off on abrasive machine the wedge angle of sample；
2）Sample polishes, and on the mill of semi-automatic sample grinding machine, the silicon carbide paper through different meshes grinds sample successively；Per pass is ground
During sample, sample will keep a direction, so as to the cut neat and consistent ground；After often having ground one of sand paper, by sample
90 degree of parallel rotating carries out down grinding together again, ensures that lower one of polishing scratch can cover together upper；
3）Sample polishes, and the sample after grinding polishes on polishing machine, using diamond spray grinding and polishing；Alcohol rinse after polishing
Sample sightingpiston, is then dried up with hair-dryer.
A kind of 7. application method of austenitic stainless steel weld joint tissue corrosive agent according to claim 5, it is characterised in that
Sample polishing, the silicon carbide paper mesh number used successively are 240 mesh, 400 mesh, 800 mesh, 1200 mesh.
8. a kind of application method of austenitic stainless steel weld joint tissue corrosive agent according to claim 5-7 any one,
Characterized in that, the sample polishing, uses the silk polishing cloth without gum；Grinding and polishing uses the μ diamond sprays of granularity 1~5.
9. a kind of application method of austenitic stainless steel weld joint tissue corrosive agent according to claim 5-7 any one,
Characterized in that, the corrosion of the metallographic specimen comprises the following steps：
1）With sample after tweezers gripping mill, putting it into the corrosive liquid prepared, corrosive liquid is totally submerged metallographic specimen surface,
When specimen surface is changed into silvery white completely from bright face, corrosion terminates；
2）The metallographic specimen that corrode is taken out, with the flushing of a large amount of water, then with alcohol rinse, is finally blown specimen surface with hair-dryer
It is dry.
A kind of 10. user of austenitic stainless steel weld joint tissue corrosive agent according to claim 5-7 any one
Method, it is characterised in that the metallographic specimen observation of the corrosion, the metallographic specimen of corrosion just put light microscope in Imager M2m
Lower observation metallographic structure.
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