CN110261207A - A kind of pair of two phase stainless steel-carbon steel composite board electro-beam welding joint position metallographic etching mode - Google Patents
A kind of pair of two phase stainless steel-carbon steel composite board electro-beam welding joint position metallographic etching mode Download PDFInfo
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- CN110261207A CN110261207A CN201810201526.4A CN201810201526A CN110261207A CN 110261207 A CN110261207 A CN 110261207A CN 201810201526 A CN201810201526 A CN 201810201526A CN 110261207 A CN110261207 A CN 110261207A
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- stainless steel
- beam welding
- metallographic
- carbon steel
- phase stainless
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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
Abstract
The invention discloses a kind of pair of two phase stainless steel-carbon steel composite board electro-beam welding joint position metallographic etching modes, the problem of can not adapting to electron beam welding higher heating rate of temperature fall present method solves traditional metallographic etching method, this method carries out etch using three kinds of etchant substeps, respectively 20% oxalic acid electro-etching, 20% sodium hydroxide solution electro-etching and hydrochloric acid-picric acid-compound etch solution of iron chloride-alcohol-acetone, in the case where not to base material part over etching, so that its fusion region metallographic is high-visible.
Description
Technical field
The invention belongs to welding technology field, especially a kind of pair of two phase stainless steel-carbon steel composite board electron beam weldings to connect
The metallographic etching mode of head position.
Background technique
The performance of metal and closely bound up with its microstructure, therefore metallographic observation is carried out to metal material be identification, sentence
The good method of disconnected metal material performance.When studying the mechanical property and corrosion behavior of metal, metal metallographic and metal are studied
Mechanical property and corrosion resistance between relationship become one of universal and effective research method.
Stainless Steel-Carbon Steel Clad Sheet is provided simultaneously with excellent corrosion resistance, mechanical property and more cheap cost.In corruption
It loses in environment, contact corrosion medium in stainless steel side undertakes to the corrosion proof requirement of workpiece.Mainly bear mechanics in carbon steel side
The requirement of performance.Wherein, two phase stainless steel becomes stainless due to its good corrosion resistance and preferable mechanics, processing performance
One of the good selection of stainless steel side in steel-carbon steel composite board.
It certainly, in actual use, is essential to the welding sequence between composite plate.Currently, compound to this kind
Plate is mainly to be carried out by way of multiple electric arc welding.However, the welding manner is not only complicated for operation, and to table
Layer stainless steel be when being welded, since the fusing of metal at high temperature and electric arc are to the stirring action in molten bath, lower layer's carbon steel
Part metals are easy the straight surface layer of turnup, become serious welding defect, substantially reduce its corrosion resistance.
Using the mode of electron beam welding, since its energy is higher, the depth of weld is larger, can complete in primary welding
Welding to stainless steel and carbon steel part whole.Simultaneously as electron beam welding heating and rate of temperature fall are very high,
Welding point has good mechanics and corrosion resistance.Simultaneously as melt pool is small, this kind welding small to the stirring action in molten bath
Mode is also less prone to welding defect.
However, carrying out metallographic etching to it using traditional metallographic etching method due to its higher heating rate of temperature fall
When, fusion area part completely can not etch go out metallographic.And when using the stronger etchant of aggressivity, base material part can then go out
Existing serious etching problem, can not show metallographic.Therefore, it in order to carry out metallographic research to this kind of welding point, needs to find
A kind of technique of novel metallographic etching, in the case where not to base material part over etching, so that its fusion region metallographic is clear
It is clear visible.Currently, this aspect research not yet someone carries out.
Summary of the invention
The present invention overcomes the disadvantages of the prior art, provides a kind of pair of two phase stainless steel-carbon steel composite board electron beam
The metallographic etching mode at welding point position.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of pair of two phase stainless steel-carbon steel composite board electro-beam welding joint position metallographic etching mode, according to following
Step carries out:
Step 1: being prepared to the weld joint samples of required observation:
Two phase stainless steel-carbon steel electro-beam welding joint is cut into pat, guarantees fusion area, the heat of welding point
The zone of influence, base material are in a sample, and using this face as working face, the back side of working face selected by the sample by well cutting makes
It is welded with copper conductor, and it is packaged using epoxy resin and PVC, after epoxy resin is fully cured, using to work
Face carries out sanding and polishing, alcohol degreasing, and is dried up with cold wind;
Step 2: the electrolysis of oxalic acid solution:
By working electrode, reference electrode and electrode being immersed in oxalic acid solution, immersion sequence is first to impregnate to electrode,
Working electrode is impregnated again, after working electrode is impregnated, is applied constant potential 10 seconds of 8V immediately, is closed constant potential polarization later,
After closing constant potential polarization, working electrode is taken out immediately, after making wash with distilled water, uses dehydration of alcohol, cold wind drying;
Step 3: the electrolysis of sodium hydroxide solution:
Using the three-electrode system in step 2, the sample of oxalic acid electrolysis will be carried out, applied in sodium hydroxide solution
It after 5V constant potential polarization 20 seconds, takes out, cleans, drying.
Step 4: the etch of compound etchant:
By the aqueous hydrochloric acid solution of 5-10 mass parts, the bitter taste aqueous acid of 1-2 mass parts, 5-10 mass parts chlorination molten iron
The aqueous acetone solution of solution, the alcohol of 100-200 mass parts and 100-200 mass parts is formulated as compound etchant, uses dropper
Compound etching solution is added dropwise in inclined specimen surface, uses distilled water flushing, dehydration of alcohol, cold wind drying after etching solution is added dropwise.
In the above-mentioned technical solutions, in step 1, the waterproof abrasive paper carries out working face to be polishing to 2000 mesh.
In the above-mentioned technical solutions, in step 1, the polishing process uses 0.5 micron of diamond polishing liquid.
In the above-mentioned technical solutions, in step 2, the concentration of the oxalic acid solution is that mass volume ratio is 15-
25%.
In the above-mentioned technical solutions, in step 3, the concentration of the sodium hydroxide solution is that mass volume ratio is 15-
25%
In the above-mentioned technical solutions, in step 4, the ingredient of the compound etchant is preferably 5-7 mass parts
Aqueous hydrochloric acid solution, the bitter taste aqueous acid of 1-2 mass parts, the ferric chloride in aqueous solution of 5-7 mass parts, 100-120 mass parts wine
The aqueous acetone solution of essence and 100-120 mass parts.
A kind of compound etch for two phase stainless steel-carbon steel composite board electro-beam welding joint position metallographic etching
Agent is formulated by following components: the aqueous hydrochloric acid solution of 5-10 mass parts, the bitter taste aqueous acid of 1-2 mass parts, 5-10 matter
Measure the ferric chloride in aqueous solution, the alcohol of 100-200 mass parts and the aqueous acetone solution of 100-200 mass parts of part.
Each etch step principle analysis and its effect of reagent:
1. oxalic acid is electrolysed.
Oxalic acid electrolysis is a kind of common standard of detection metal Susceptibility To Intergranular Corrosion, in metallographic etching use compared with
It is few.Electrolysis is carried out under the oxalic acid solution of high concentration with the etching action to crystal boundary and phase boundary.By the processing of the step
Afterwards, the fusion area of two phase stainless steel can be clearly envisioned.During oxalic acid is electrolysed, carbon steel does not corrode.
2. sodium hydroxide is electrolysed.
Sodium hydroxide electrolysis is one of common two phase stainless steel etching method.It is acted on mainly in two phase stainless steel
Ferrite coloured, while two-phase phase boundary is etched.The step is to show two phase stainless steel base material.Sodium hydroxide electricity
During solution, carbon steel does not corrode.
3. compound etching solution etch.
In the present invention, compound etching solution is used are as follows: the bitter taste sour water of the aqueous hydrochloric acid solutions of 5-10 mass parts, 1-2 mass parts
Solution, the ferric chloride in aqueous solution of 5-10 mass parts, the alcohol of 100-200 mass parts and 100-200 mass parts aqueous acetone solution.
Wherein, the ingredient for mainly playing erosion is hydrochloric acid and iron chloride, which can be provided with high concentration cl
Ion, the acidic environment of iron ion.Wherein, the addition of iron chloride increases the chlorine ion concentration of hydrochloric acid, improves to metal
Corrosivity, meanwhile, the effect of iron ion, but also intercrystalline corrosion effect is more significant.Therefore, the two make conventional method without
The carbon steel fusion area part metallographic of method etch is shown.
However, spot corrosion easily occurs due to the hydrogen ion chloride environment of high concentration, therefore, suitable picric acid is added,
Weaken the generation of spot corrosion significantly.
The effect of alcohol is mainly the solvent of above-mentioned three kinds of substances.However at this point, since plain steel and carbon steel heat
Area's corrosion resistance differs greatly.Under the action of galvanic corrosion, matrix easily over etching, and fusion area metallographic is still unobvious.Cause
Acetone is added in order to weaken the effect of galvanic corrosion in this, greatly increases the solution resistance of etching solution, weakens galvanic effect.
This etching solution is applicable to exist simultaneously the activation system metal etch that corrosion resistance differs greatly in the same plane.
It is not limited only to example illustrated by this patent.
Compared with prior art, the beneficial effects of the present invention are: present method solves traditional metallographic etching methods can not
The problem of adapting to electron beam welding higher heating rate of temperature fall, this method carry out etches, difference using three kinds of etchants substeps
It is molten for oxalic acid electro-etching, sodium hydroxide solution electro-etching and hydrochloric acid-picric acid-iron chloride-compound etch of alcohol-acetone
Liquid, this method is not in the case where to base material part over etching, so that its fusion region metallographic is high-visible.
Detailed description of the invention
Fig. 1-11:2205-Q235 two phase stainless steel-carbon steel composite board electro-beam welding joint metallograph, in which:
Fig. 1 is the metallograph under 2205 side low power lens.
Fig. 2 is 2205 and the metallograph under Q235 intersection low power lens.
Fig. 3 is the metallograph under the low power lens of the side Q235.
Fig. 4 is the metallograph under 2205 base materials-heat affected area-hot melt area high power lens.
Fig. 5 is the metallograph under 2205 hot melt area's high power lenses.
Fig. 6 is the metallograph under 2205-Q235 hot melt area's transition region high power lens.
Fig. 7 is the metallograph under the heat affected area 2205-Q235-hot melt area transition region high power lens.
Fig. 8 is the metallograph under 2205-Q235 base material-heat affected area transition region high power lens.
Fig. 9 is the metallograph under the heat affected area Q235-hot melt area high power lens (there are 2205 tissues in hot melt area).
Figure 10 is the metallograph under Q235 hot melt area's high power lens.
Figure 11 is the metallograph under the heat affected area Q235-hot melt area high power lens (hot melt area is without 2205 tissues).
Specific embodiment
Present invention is further described in detail with specific embodiment with reference to the accompanying drawing:
Embodiment 1
1. firstly, being prepared to 2205-q235 weld joint samples.
2205-q235 electro-beam welding joint is processed, 20*20mm pat is cut into, and guarantees to connect
Fusion area, heat affected area, the base material of head are in a sample.Using this face as working face.
The back side of working face selected by sample by well cutting is welded using copper conductor, and uses epoxy resin and PVC pairs
It is packaged.24 hours are stood, epoxy resin cure is waited.
It after epoxy resin is fully cured, is polished using waterproof abrasive paper working face, uses 0.5 after straight 2000 mesh of polishing
The diamond polishing liquid of micron is polished.Alcohol degreasing, cold wind drying are used after polishing.It is put into drying chamber stand-by.
Later, the etch of multistep metallographic is carried out.
2. carrying out the electrolysis of oxalic acid solution.
By working electrode, reference electrode and mass volume ratio is immersed in electrode (platinum plate electrode, graphite electrode) it is
In 20% oxalic acid solution.Immersion sequence is first to impregnate to electrode, then impregnate working electrode.
After working electrode is impregnated, the constant potential of 8V should be applied immediately 10 seconds.Constant potential polarization is closed later.
After closing constant potential polarization, working electrode is taken out immediately, after making the several seconds wash with distilled water, using dehydration of alcohol,
Cold wind drying.
3. carrying out the electrolysis of sodium hydroxide solution.
Using three-electrode system ibid, the sample of oxalic acid electrolysis will be carried out, and was 20% hydroxide in mass volume ratio
It after applying 5V constant potential polarization 20 seconds in sodium solution, takes out, cleans, drying.
4. carrying out the etch of the compound etchant of 5ml hydrochloric acid+1g picric acid+5g iron chloride+100ml alcohol+100ml acetone.
It carried out the sample that two one-step electrolysis soak and tries out compound etchant carrying out etch by above-mentioned.
Sample is placed in 45 degree angles, is added dropwise etching solution using dropper, and rate of addition control is in 1 drop per second left and right, and (1 drips and is
0.05mL).It is added dropwise 15 seconds, uses distilled water flushing, dehydration of alcohol, cold wind drying.
So far, etch is partially completed, and next can carry out metallographic observation.
Embodiment 2
1. firstly, being prepared to 2205-q235 weld joint samples.
2205-q235 electro-beam welding joint is processed, 20*20mm pat is cut into, and guarantees to connect
Fusion area, heat affected area, the base material of head are in a sample.Using this face as working face.
The back side of working face selected by sample by well cutting is welded using copper conductor, and uses epoxy resin and PVC pairs
It is packaged.24 hours are stood, epoxy resin cure is waited.
It after epoxy resin is fully cured, is polished using waterproof abrasive paper working face, uses 0.5 after straight 2000 mesh of polishing
The diamond polishing liquid of micron is polished.Alcohol degreasing, cold wind drying are used after polishing.It is put into drying chamber stand-by.
Later, the etch of multistep metallographic is carried out.
2. carrying out the electrolysis of oxalic acid solution.
By working electrode, reference electrode and mass volume ratio is immersed in electrode (platinum plate electrode, graphite electrode) it is
In 15% oxalic acid solution.Immersion sequence is first to impregnate to electrode, then impregnate working electrode.
After working electrode is impregnated, the constant potential of 8V should be applied immediately 10 seconds.Constant potential polarization is closed later.
After closing constant potential polarization, working electrode is taken out immediately, after making the several seconds wash with distilled water, using dehydration of alcohol,
Cold wind drying.
3. carrying out the electrolysis of sodium hydroxide solution.
Using three-electrode system ibid, the sample of oxalic acid electrolysis will be carried out, and was 15% hydroxide in mass volume ratio
It after applying 5V constant potential polarization 20 seconds in sodium solution, takes out, cleans, drying.
4. carrying out the etch of the compound etchant of 5ml hydrochloric acid+1g picric acid+5g iron chloride+100ml alcohol+100ml acetone.
It carried out the sample that two one-step electrolysis soak and tries out compound etchant carrying out etch by above-mentioned.
Sample is placed in 45 degree angles, is added dropwise etching solution using dropper, and rate of addition control is in 1 drop per second left and right, and (1 drips and is
0.05mL).It is added dropwise 15 seconds, uses distilled water flushing, dehydration of alcohol, cold wind drying.
So far, etch is partially completed, and next can carry out metallographic observation.
Metallographic observation results obtained in above embodiments are more approximate, and metallographic observation effect is as shown in figs. 1-11, it is seen that
The welding point each region has received good etch, organizes high-visible.
It describes the invention in detail, but content is only the preferred embodiment of the present invention, cannot be recognized above
For for limiting practical range of the invention.Any changes and modifications in accordance with the scope of the present application should all still return
Belong within patent covering scope of the invention.
Claims (4)
1. a kind of pair of two phase stainless steel-carbon steel composite board electro-beam welding joint position metallographic etching mode, it is characterised in that:
It is carried out according to the following steps:
Step 1: being prepared to the weld joint samples of required observation:
Two phase stainless steel-carbon steel electro-beam welding joint is cut into pat, guarantees fusion area, the heat affecting of welding point
Area, base material are in a sample, and using this face as working face, the back side of working face selected by the sample by well cutting uses copper
Conducting wire welding, and it is packaged using epoxy resin and PVC, after epoxy resin is fully cured, using waterproof abrasive paper to work
It polishes, and is polished as face, alcohol degreasing is used after polishing, cold wind drying is put into drying chamber stand-by;
Step 2: the electrolysis of 20% oxalic acid solution:
It being immersed in 20% oxalic acid solution by working electrode, reference electrode and to electrode, immersion sequence is first to impregnate to electrode,
Working electrode is impregnated again, after working electrode is impregnated, should apply the constant potential of 8V immediately 10 seconds, closes constant potential pole later
Change, after closing constant potential polarization, takes out working electrode immediately, after making the several seconds wash with distilled water, using dehydration of alcohol, cold wind is blown
It is dry;
Step 3: the electrolysis of 20% sodium hydroxide solution:
Using the three-electrode system in step 2, the sample of oxalic acid electrolysis will be carried out, applied in 20% sodium hydroxide solution
It after 5V constant potential polarization 20 seconds, takes out, cleans, drying;
Step 4: the etch of compound etchant:
The wine that the hydrochloric acid of 5-10 volume point, the picric acid of 1-2 mass point, the iron chloride of 5-10 mass point, 100-200 volume are divided
The acetone of essence and 100-200 volume point is formulated as compound etchant, and sample is placed in 45 degree of angles, compound leaching is added dropwise using dropper
Liquid is lost, rate of addition control is added dropwise 15 seconds in 1 drop per second left and right, uses distilled water flushing, dehydration of alcohol, cold wind drying, etch
Metallographic observation can be carried out after the completion.
2. a kind of pair of two phase stainless steel according to claim 1-carbon steel composite board electro-beam welding joint position metallographic
Etch mode, it is characterised in that: in step 1, the waterproof abrasive paper carries out working face to be polishing to 2000 mesh.
3. a kind of pair of two phase stainless steel according to claim 1-carbon steel composite board electro-beam welding joint position metallographic
Etch mode, it is characterised in that: in step 1, the polishing process uses 0.5 micron of diamond polishing liquid.
4. a kind of pair of two phase stainless steel according to claim 1-carbon steel composite board electro-beam welding joint position metallographic
Etch mode, it is characterised in that: in step 4, the ingredient of the compound etchant is preferably the hydrochloric acid of 5-7 volume point, 1-
The acetone that the alcohol and 100-120 volume that the picric acid of 2 mass point, the iron chloride of 5-7 mass point, 100-120 volume are divided divide.
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