CN108004549A - The metallographic etchant and caustic solution of ferrite/austenite Dissimilar Steel Welded Joint - Google Patents
The metallographic etchant and caustic solution of ferrite/austenite Dissimilar Steel Welded Joint Download PDFInfo
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- CN108004549A CN108004549A CN201810011074.3A CN201810011074A CN108004549A CN 108004549 A CN108004549 A CN 108004549A CN 201810011074 A CN201810011074 A CN 201810011074A CN 108004549 A CN108004549 A CN 108004549A
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- austenite
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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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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Abstract
The present invention provides the metallographic etchant and caustic solution of a kind of ferrite/austenite Dissimilar Steel Welded Joint.The component of the metallographic etchant includes ferric trichloride, nitric acid, glycerine and water, and ferric trichloride, nitric acid, the amount ratio of glycerine and water are (10 15g)：(20‑25mL)：(15‑20mL)：(25‑30mL).Metallographic structure near melt run can be transparent to show that out using the metallographic etchant and caustic solution of ferrite of the present invention/austenite Dissimilar Steel Welded Joint, and erosion process is slowly steady, is easy to operate and control；Heating and impressed current are not required to, can be carried out under room temperature and normal condition.
Description
Technical field
The invention belongs to material Physico-chemical tests analysis technical field, is related to a kind of ferrite/austenite different steel weld and connects
The metallographic etchant and caustic solution of head.
Background technology
Thermal power generation is occupied an leading position in China's power industry.To reduce the environmental problem, at the same time that thermal power generation is brought
Generating efficiency is improved, many high parameter large sized units put into operation in succession, require boiler superheater, reheater steam temperature therewith
Degree is continuously improved, but material cost in order to control, therefore super (super-) critical unit boiler heating surface high temperature section exit site uses more
Ferritic steel is generally adopted in austenitic heat-resistance steel, entrance side.Therefore inevitably exist in the heating surface of these units
The Dissimilar Steel Welded Joint of substantial amounts of austenitic steel and ferritic steel.After high temperature and pressure runs a period of time, different steel weld
The safety issue of connector is increasingly burst, and leakage accident occurs for existing multiple power plant, and leakage position is the fusion of ferritic steel side
Near line.Therefore, how the microstructure evolution near effective evaluation connector melt run, the safe handling to ensureing dissimilar steel joint has
It is significant.
In general, the metallographic etching agent of ferritic steel is using nital；The metallographic etching agent of austenitic steel is adopted
It is chloroazotic acid.Chloroazotic acid is volatile, corrosivity is strong, can be to artificial into harmful effect, and reacts violent, not easy to operate, that is, uses
Writing brush point dips in chloroazotic acid, is operated under Stereo microscope, it is also difficult to holds scale, often causes melt run ferritic steel side
Excessive erosion, or austenitic steel side corrosion less than situation, this to observation melt run near microstructure evolution bring difficulty.
The content of the invention
To solve problems of the prior art, it is an object of the invention to provide a kind of ferrite/austenite xenogenesis
The metallographic etchant and caustic solution of steel welded joint, can make corrosion process steady, easily operated, the connector fusion after corrosion
Line tissue around display effect is good.
The purpose of the present invention is achieved by the following technical programs：
On the one hand, the present invention provides a kind of metallographic etchant of ferrite/austenite Dissimilar Steel Welded Joint, and the metallographic is rotten
The component of erosion liquid includes ferric trichloride, nitric acid, glycerine and water, and ferric trichloride, nitric acid, the amount ratio of glycerine and water are (10-
15g)：(20-25mL)：(15-20mL)：(25-30mL).
In the metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, it is preferable that the metallographic etchant
Component includes the ferric trichloride of 13g, the nitric acid of 22mL, the glycerine of 18mL and the water of 27mL.
In the metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, it is preferable that the ferric trichloride,
The nitric acid and the glycerine are that analysis is pure；The water is distilled water.
In the metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, it is preferable that the quality of the nitric acid
Fraction is 68%.
On the other hand, the present invention also provides above-mentioned ferrite/austenite Dissimilar Steel Welded Joint metallographic etchant system
Preparation Method, it comprises the following steps：
Water is added into ferric trichloride, stirring dissolves ferric trichloride, is subsequently added into glycerine and stirs, finally
Add nitric acid to stir, after standing, obtain metallographic etchant.
In above-mentioned preparation method, it is preferable that the time of standing is 20-25min.
Another further aspect, the present invention also provides a kind of method for corroding ferrite/austenite Dissimilar Steel Welded Joint, it is used
The metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, comprises the following steps：
Welded Joints sample is pre-processed；Pretreated weld joint samples are sufficiently submerged in metallographic etchant
In, etching pit surface side, which is stood up, puts, and connects the bubble welding that fully speeds away using vibrations sample or agitation metallographic etchant
The surface of head sample, will not influence corrosive effect because bubble is attached to specimen surface, until etching pit face is etched presentation
Untill silver gray；Weld joint samples taking-up after erosion is rinsed with water, then is dried up with alcohol rinse, completes etching pit mistake
Journey.
In the method for above-mentioned corrosion ferrite/austenite Dissimilar Steel Welded Joint, it is preferable that Welded Joints sample carries out
The method of pretreatment is：Conventionally Welded Joints sample cut, roughly ground, fine grinding, mechanical polishing, ultrasonic wave it is clear
Wash, alcohol rinse and drying.
In the method for above-mentioned corrosion ferrite/austenite Dissimilar Steel Welded Joint, it is preferable that the weld joint samples exist
Erosion time in metallographic etchant is 10-20min.
Chloroazotic acid is 1:The mixture of 3 concentrated nitric acids and concentrated hydrochloric acid, it is volatile and there is strong corrosivity.The present invention avoids
Concentrated hydrochloric acid, but ferric trichloride is used, while the chlorion with coordination ability is provided (presence of nitric acid+chlorion,
The corrosive effect of chloroazotic acid is realized indirectly, but because concentration is not low, acid strong, therefore corrosivity weakens significantly), additionally provide with oxygen
The ferric ion of change ability.In addition, glycerine as activating agent, improves the corrosive effect of specimen surface；Water is as solvent
Addition, dilute the intensity of acid, make corrosion process steadily slow, it is easily operated, the synergistic effect of several components of the above and match somebody with somebody
Closing specific ratio causes the corrosive agent to have extraordinary effect on corrosion ferrite and austenite dissimilar steel joint.
Can significantly it be shown using the metallographic etchant and caustic solution of ferrite of the present invention/austenite Dissimilar Steel Welded Joint
Metallographic structure near melt run is shown, and erosion process is slowly steady, is easy to operate and control；It is not required to heating and outer power-up
Stream, can carry out under room temperature and normal condition.
Brief description of the drawings
Fig. 1 is to use writing brush point to dip in the erosion effect that chloroazotic acid contacts ferrite side near melt run in the embodiment of the present invention 4
Fruit metallographic structure figure；
Fig. 2 is to dip in chloroazotic acid using writing brush point in the embodiment of the present invention 4 to imitate not in contact with the erosion on Ovshinsky side near melt run
Fruit metallographic structure figure；
Fig. 3 is that weld joint samples immerse in nital the erosion effect metallographic corroded in the embodiment of the present invention 4
Organization chart；
Fig. 4 is that weld joint samples immerse in chloroazotic acid the erosion effect metallographic structure figure corroded in the embodiment of the present invention 4；
Fig. 5 is the erosion effect gold that weld joint samples immerse the metallographic etchant in embodiment 1 in the embodiment of the present invention 4
Phase constitution figure.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
This implementation provides a kind of metallographic etchant of ferrite/austenite Dissimilar Steel Welded Joint, the metallographic etchant
Nitric acid, the glycerine of 18mL and the distilled water of 27mL that component includes the ferric trichloride of 13g, the mass fraction of 22mL is 68%,
Wherein, ferric trichloride, nitric acid, glycerine are that analysis is pure.
This implementation also provides the preparation method of the metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, its
Comprise the following steps：
Ferric trichloride 13g is taken, is poured into beaker, adds distilled water 27mL, after dissolving ferric trichloride with glass bar stirring,
The glycerine of 18mL is added, stirring, the mass fraction for finally pouring into 22mL is 68% nitric acid, and is sufficiently stirred, and stands 20 points
Metallographic etchant is obtained after clock.
This implementation also provides a kind of method for corroding ferrite/austenite Dissimilar Steel Welded Joint, it uses above-mentioned iron
The metallographic etchant of ferritic/austenite Dissimilar Steel Welded Joint, comprises the following steps：
Ferrite/austenite Dissimilar Steel Welded Joint sample is conventionally cut, is roughly ground, fine grinding, machinery
Polishing, ultrasonic cleaning, alcohol rinse, drying；Pretreated weld joint samples are sufficiently submerged in metallographic etchant, gold
The edge-on placement of phase erosional surface, and bubble is fully speeded away weld joint samples using vibrations sample or agitation metallographic etchant
Surface, corrosive effect will not be influenced because bubble is attached to specimen surface, corrode about 15min, until etching pit face is invaded
Untill silver gray is presented in erosion；Weld joint samples taking-up after erosion is rinsed with water, then is dried up with alcohol rinse, completes metallographic
Corrosion process, obtains metallographic specimen to be seen.
Embodiment 2
This implementation provides a kind of metallographic etchant of ferrite/austenite Dissimilar Steel Welded Joint, the metallographic etchant
Nitric acid, the glycerine of 15mL and the distilled water of 25mL that component includes the ferric trichloride of 10g, the mass fraction of 25mL is 68%,
Wherein, ferric trichloride, nitric acid, glycerine are that analysis is pure.
This implementation also provides the preparation method of the metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, its
Comprise the following steps：
Ferric trichloride 10g is taken, is poured into beaker, adds distilled water 25mL, after dissolving ferric trichloride with glass bar stirring,
The glycerine of 15mL is added, stirring, the mass fraction for finally pouring into 25mL is 68% nitric acid, and is sufficiently stirred, and stands 20 points
Metallographic etchant is obtained after clock.
This implementation also provides a kind of method for corroding ferrite/austenite Dissimilar Steel Welded Joint, it uses above-mentioned iron
The metallographic etchant of ferritic/austenite Dissimilar Steel Welded Joint, comprises the following steps：
Ferrite/austenite Dissimilar Steel Welded Joint sample is conventionally cut, is roughly ground, fine grinding, machinery
Polishing, ultrasonic cleaning, alcohol rinse, drying；Pretreated weld joint samples are sufficiently submerged in metallographic etchant, gold
The edge-on placement of phase erosional surface, and bubble is fully speeded away weld joint samples using vibrations sample or agitation metallographic etchant
Surface, corrosive effect will not be influenced because bubble is attached to specimen surface, corrode about 10min, until etching pit face is invaded
Untill silver gray is presented in erosion；Weld joint samples taking-up after erosion is rinsed with water, then is dried up with alcohol rinse, completes metallographic
Corrosion process.
Embodiment 3
This implementation provides a kind of metallographic etchant of ferrite/austenite Dissimilar Steel Welded Joint, the metallographic etchant
Nitric acid, the glycerine of 15mL and the distilled water of 25mL that component includes the ferric trichloride of 15g, the mass fraction of 20mL is 68%,
Wherein, ferric trichloride, nitric acid, glycerine are that analysis is pure.
This implementation also provides the preparation method of the metallographic etchant of above-mentioned ferrite/austenite Dissimilar Steel Welded Joint, its
Comprise the following steps：
Ferric trichloride 15g is taken, is poured into beaker, adds distilled water 25mL, after dissolving ferric trichloride with glass bar stirring,
The glycerine of 15mL is added, stirring, the mass fraction for finally pouring into 20mL is 68% nitric acid, and is sufficiently stirred, and stands 20 points
Metallographic etchant is obtained after clock.
This implementation also provides a kind of method for corroding ferrite/austenite Dissimilar Steel Welded Joint, it uses above-mentioned iron
The metallographic etchant of ferritic/austenite Dissimilar Steel Welded Joint, comprises the following steps：
Ferrite/austenite Dissimilar Steel Welded Joint sample is conventionally cut, is roughly ground, fine grinding, machinery
Polishing, ultrasonic cleaning, alcohol rinse, drying；Pretreated weld joint samples are sufficiently submerged in metallographic etchant, gold
The edge-on placement of phase erosional surface, and bubble is fully speeded away weld joint samples using vibrations sample or agitation metallographic etchant
Surface, corrosive effect will not be influenced because bubble is attached to specimen surface, corrode about 20min, until etching pit face is invaded
Untill silver gray is presented in erosion；Weld joint samples taking-up after erosion is rinsed with water, then is dried up with alcohol rinse, completes metallographic
Corrosion process.
4 contrast experiment of embodiment
Ferrite/austenite Dissimilar Steel Welded Joint sample is corroded to obtain metallographic specimen to be measured using chloroazotic acid, its
Erosion effect metallographic structure figure is as shown in Figure 1, Figure 2 and Figure 4；Use the nital that volume fraction is 10% plain to iron
Body/austenite Dissimilar Steel Welded Joint sample is corroded to obtain metallographic specimen to be measured, its erosion effect metallographic structure figure such as Fig. 3
It is shown；The metallographic specimen to be measured corroded using 1 metallographic etchant of the embodiment of the present invention, its erosion effect metallographic structure
Figure is as shown in Figure 5.
In Fig. 1, chloroazotic acid is dipped in using writing brush point, is operated under Stereo microscope, chloroazotic acid contacts melt run ferrite nearby
Side, causes melt run ferrite side metallographic structure excessive erosion nearby；In Fig. 2, chloroazotic acid is dipped in using writing brush point, under Stereo microscope
Operation, chloroazotic acid cause the neighbouring Ovshinsky side of melt run not corroded and metallographic structure not in contact with Ovshinsky side near melt run；By scheming
1 and Fig. 2 can be seen that to be corroded using chloroazotic acid, and scale is difficult to be held, it is difficult to operation.
Weld joint samples are immersed in chloroazotic acid in Fig. 4 and are corroded, can be seen with reference to Fig. 4 erosion effects metallographic structure figure
Go out, Ovshinsky side, which is corroded, metallographic structure but the excessive erosion of ferrite side.
Weld joint samples are immersed in the nital that volume fraction is 10% in Fig. 3 and are corroded, is corroded and imitated by Fig. 3
Fruit metallographic structure figure, which can be seen that ferrite side, has corroded and metallographic structure but Ovshinsky side does not corrode and metallographic structure.
Fig. 5 is the erosion effect metallographic structure for the metallographic specimen that 1 metallographic etchant of the embodiment of the present invention is corroded
Figure, nearby ferrite side and Ovshinsky side can show perfect metallographic structure to melt run as seen from Figure 5.
Claims (9)
- A kind of 1. metallographic etchant of ferrite/austenite Dissimilar Steel Welded Joint, it is characterised in that：The group of the metallographic etchant Dividing includes ferric trichloride, nitric acid, glycerine and water；Ferric trichloride, nitric acid, the amount ratio of glycerine and water are (10-15g)： (20-25mL)：(15-20mL)：(25-30mL).
- 2. the metallographic etchant of ferrite according to claim 1/austenite Dissimilar Steel Welded Joint, it is characterised in that： The component of the metallographic etchant includes the ferric trichloride of 13g, the nitric acid of 22mL, the glycerine of 18mL and the water of 27mL.
- 3. the metallographic etchant of ferrite according to claim 1 or 2/austenite Dissimilar Steel Welded Joint, its feature exist In：The ferric trichloride, the nitric acid and the glycerine are that analysis is pure；The water is distilled water.
- 4. according to the metallographic etchant of claim 1-3 any one of them ferrite/austenite Dissimilar Steel Welded Joint, it is special Sign is：The mass fraction of the nitric acid is 68%.
- 5. the preparation method of the metallographic etchant of any one of the claim 1-4 ferrites/austenite Dissimilar Steel Welded Joint, It comprises the following steps：Water is added into ferric trichloride, stirring dissolves ferric trichloride, is subsequently added into glycerine and stirs, be eventually adding Nitric acid stirs, and after standing, obtains metallographic etchant.
- 6. preparation method according to claim 5, it is characterised in that：The time of standing is 20-25min.
- 7. a kind of method for corroding ferrite/austenite Dissimilar Steel Welded Joint, it uses claim 1-4 any one of them The metallographic etchant of ferrite/austenite Dissimilar Steel Welded Joint, comprises the following steps：Welded Joints sample is pre-processed；Pretreated weld joint samples are sufficiently submerged in metallographic etchant, gold The edge-on placement of phase erosional surface, and bubble is fully speeded away weld joint samples using vibrations sample or agitation metallographic etchant Surface, until etching pit face be etched present silver gray untill；Weld joint samples taking-up after erosion is rinsed with water, Dried up again with alcohol rinse, complete etching pit process.
- 8. according to the method described in claim 7, it is characterized in that：The method that Welded Joints sample is pre-processed is：Press More solito Welded Joints sample is cut, is roughly ground, fine grinding, mechanical polishing, ultrasonic cleaning, alcohol rinse and is blown It is dry.
- 9. according to the method described in claim 7, it is characterized in that：Erosion of the weld joint samples in metallographic etchant Time is 10-20min.
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| CN108896476A (en) * | 2018-09-04 | 2018-11-27 | 鞍钢股份有限公司 | A kind of evaluation method of Dissimilar Steels welding point atmospheric corrosion resistance |
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