CN104087940B - A kind of corrosion resistant alloy macrostructure and defect manifest acid etching method - Google Patents
A kind of corrosion resistant alloy macrostructure and defect manifest acid etching method Download PDFInfo
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- CN104087940B CN104087940B CN201410315421.3A CN201410315421A CN104087940B CN 104087940 B CN104087940 B CN 104087940B CN 201410315421 A CN201410315421 A CN 201410315421A CN 104087940 B CN104087940 B CN 104087940B
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Abstract
The present invention relates to a kind of corrosion resistant alloy macrostructure and defect manifests acid etching method, it comprises the steps:<b>i</b>cut corrosion resistant alloy sample, specimen surface to be seen of polishing, the roughness R on surfaceaIt is not more than 1.6 μm；<b>iI</b>sample is put in electric heater unit；<b>iII</b>adding technical hydrochloric acid in electric heater unit, technical hydrochloric acid liquid level exceedes specimen surface 50mm to be seen；<b>iV</b>electric heater unit design temperature 85 DEG C 90 DEG C, electrified regulation；<b>v</b>technical hydrochloric acid reaches 85 DEG C 90 DEG C, and is incubated；<b>vI</b><b />take out sample, bleed off volume 0.5 ± 0.05 hydrochloric acid, put into sample；<b>vII</b><b />adding new technical hydrochloric acid, technical hydrochloric acid liquid level exceedes specimen surface 50mm to be seen；<b>vIII</b><b />the heating-up temperature of electric heater unit 85 DEG C 90 DEG C；<b>Ⅸ</b><b />it is incubated 90 ± 5 minutes；<b>Ⅹ</b><b />acid solution in discharge electric heater unit, takes out sample.This corrosion resistant alloy macrostructure and defect manifest acid etching method, make manifesting of corrosion resistant alloy macrostructure and defect clear.
Description
Technical field
The present invention relates to a kind of corrosion resistant alloy macrostructure and defect manifests acid etching method, particularly corrosion resistant alloy N08028 macrostructure and defect manifest acid etching method.
Background technology
Corrosion resistant alloy (N08028) is largely used to oil exploitation aspect, and production difficulty is relatively big, and the detection project of this series products is also more, relates to the inspection of mechanics, high power (metallographic), the chemical and grand tissue of burn into and defect.
Inspection for the grand tissue of product and defect, generally take on steel material, to intercept cross section sample, secondly through the cross section materialsed being carried out the processing of milling machine and grinding machine, then using relevant acid solution acid etching, and observing and judge tissue and the defect situation of cross section.The quality of acid etching effect directly affects the observation to steel sample tissue and defect and judgement.
Five kinds of acid etching methods of GB/T14999.2 and ASTME340 standard recommendation.
The sample processed with milling machine and grinding machine result of the test by the following method is as follows:
1,1:1(water: technical hydrochloric acid) HCl solution method, to the sample being positioned in 1:1 hydrochloric acid solution groove, process steam was heated to 65-80 DEG C and is incubated, through the acid etching of about 12 days, it is impossible to see macrostructure and the defect situation of sample.
2, industry HCl solution method, to the sample being positioned in hydrochloric acid solution groove, through being electrically heated to 65-80 DEG C and being incubated, continuously across more than 5 hours acid etchings, acid etching DeGrain, and makes specimen surface turn black.
3, the FeCl of variable concentrations3+HNO3+ HCl solution method, to the FeCl being positioned over variable concentrations3+HNO3Sample in+HCl solution groove, through being electrically heated to boiling, after 3-15min, extent of corrosion ratio is more serious, and bad control easily produces excessive erosion.
4、40mlH2O2+100mlHCl+100H2O solwution method, to being positioned over 40mlH2O2+100mlHCl+100H2Sample in O solution tank, through being electrically heated to boiling, and by H2O2Add in mixed solution point several times, add till fashionable need wait until the lather collapse produced last time every time.Owing to adding H2O2Time the foam that produces too many, spillage solution groove, large losses solution, operating difficulties, the method is inapplicable.
5, room temperature CuSO4Solution soaking is tested
Adopt CuSO4Solution (75gCuSO4+17.5mlH2SO4+ 250mlHCl) soak different time (5,15,20,30 minutes) after, specimen surface is along with the prolongation of soak time, and the extent of corrosion of sample is deepened, and the sample soaking 15min can see tissue and the defect of specimen surface clearly.
From the result of above five kinds of methods, only fifth method can go out good effect by acid etching, but the method can produce a large amount of irritative gas in the process of acid etching, does not have again good protective approach, and staff's health is produced obvious hidden danger.
Summary of the invention
In order to overcome existing corrosion resistant alloy macrostructure and defect to manifest the above-mentioned deficiency of acid etching method, it is provided that a kind of manifest corrosion resistant alloy macrostructure and defect clearly making corrosion resistant alloy macrostructure and defect manifests acid etching method.
This invention address that the technical scheme of above-mentioned technical problem is:
First have to from solving to manifest consideration effect, it is possible to it can be clearly seen that the form of tissue and defect, possess the condition of artificial judgment.The operating time is shortened in its secondary consideration as far as possible.Moreover be exactly reduce the injury to human body as far as possible.
This corrosion resistant alloy macrostructure and defect manifest acid etching method and include following step successively:
I to cut bar-shaped corrosion resistant alloy (N08028) cross section sample thickness be within 25mm, or cut at N08028 steel plate and to fail to grow up in 450mm, the wide sample being not more than 50mm along rolling direction, after specimen surface vertical knee-type milling machine to be seen is processed, with sand papering specimen surface to be seen, and clean with absorbent cotton and wipes of alcohol, the roughness R of specimen surface to be seenaIt is not more than 1.6 μm and without greasy dirt.
II in ventilated chamber, places the electric heater unit (voltage 220 V, power 3000W) of acidproof water-stop, opens the sealing lid of electric heater unit, and sample is put in electric heater unit.
III adds technical hydrochloric acid (GB320-2006 definite quality concentration >=31.0%) in the electric heater unit of water-stop, and technical hydrochloric acid liquid level exceedes specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop.
The electric heater unit of IV water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and after safety inspection, energising begins to warm up.
In the electric heater unit of V water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and starts insulation, is incubated 90 ± 5 minutes.
VI after insulation, opens sealing lid and takes out sample, cleans down the chloride of specimen surface to be seen with brush, will bleed off the 0.5 ± 0.05 of volume with rear hydrochloric acid simultaneously, put into the sample after cleaning in the electric heater unit of water-stop in clear water.
VII adds new technical hydrochloric acid (GB320-2006 definite quality concentration >=31.0%) again in the electric heater unit of water-stop, keeps technical hydrochloric acid liquid level to exceed specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop.
The electric heater unit of VIII water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and after safety inspection, energising begins to warm up.
In the electric heater unit of Ⅸ water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and second time starts insulation, is incubated 90 ± 5 minutes.
Ⅹ cuts off the electricity supply, and opens sealing and covers, and the acid solution in the electric heater unit of discharge water-stop, to neutralization pond, is discharged after to be neutralized, takes out sample and cleans up in the hot water, and with compressing air blow drying.
Above-mentioned corrosion resistant alloy macrostructure and defect manifest acid etching method, and its steps characteristic is:
13 pieces of samples (namely totally 24 pieces of samples) are cut again in step I；After specimen surface vertical knee-type milling machine to be seen is processed, with sand papering specimen surface to be seen, and by absorbent cotton and wipes of alcohol totally, the roughness R of specimen surface to be seenaIt is not more than 1.6 μm and without greasy dirt；
When step II is put in the electric heater unit of water-stop at sample, it is not less than the Glass rod of 4mm with diameter between every sample two pieces adjacent and separates.
The specimen surface 50mm to be seen of the superiors' sample is exceeded in step III technical hydrochloric acid liquid level；
The specimen surface 50mm to be seen of the superiors' sample is exceeded in step VII technical hydrochloric acid liquid level.
Above-mentioned corrosion resistant alloy macrostructure and defect manifest in acid etching method, described electric heater unit is for overlooking the rectangular heating tank in direction, electrical bar is installed in heating tank, heating tank is covered with sealing lid, notch surrounding at heating tank has the water sealed tank of water, seal lid when covering on heating tank, water sealed tank is dropped on the lower edge sealing lid, water-stop heating tank.
Obtain the specimen surface of macrostructure and defect clear (finger of macrostructure here with the naked eye or observes tissue-grainiess and the size cases of erosional surface by means of the magnifier of less than 10 times) and defect clearly (defect clearly refers to the naked eye or magnifier by means of less than 10 times can be clearly apparent whether there is the content such as field trash and crackle).
Beneficial effects of the present invention
Recent years is carried out the problem be hard to tell and do not see that manifests of domestic-developed corrosion resistant alloy (N08028) macrostructure and defect and is addressed by the present invention, compared with manifesting acid etching method with existing corrosion resistant alloy macrostructure and defect, solution corrosion weak, operating time is short, human influence is less, can obtain clear macrostructure and defect manifests effect.Disclosure satisfy that the acid etching requirement of corrosion resistant alloy N08028 macro-graph.
Detailed description of the invention
Following embodiment is clear in detail illustrates the specific embodiment of the present invention, but the specific embodiment of the present invention is not limited to following embodiment.
Embodiment one
I to cut φ 400mm garden rod corrosion resistant alloy (N08028) cross section sample thickness be 25mm mono-piece, after sample face to be seen vertical knee-type milling machine is processed, with 60 order sand paper manual polishing specimen surface 3 minutes, and clean with absorbent cotton and wipes of alcohol, specimen surface roughness RaIt is not more than 1.6 μm and without greasy dirt.
II in ventilated chamber, places the electric heater unit (voltage 220 V, power 3000W) of an acidproof water-stop, and sample is put into the bottom of the electric heater unit of water-stop.
III adds technical hydrochloric acid (GB320-2006 definite quality concentration >=31.0%) in the electric heater unit of water-stop, and technical hydrochloric acid liquid level exceedes specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop.
The electric heater unit of IV water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and after safety inspection, energising begins to warm up.
In the electric heater unit of V water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and starts insulation, is incubated 90 minutes.
VI after insulation, opens sealing lid and takes out sample, cleans down the chloride of specimen surface to be seen with brush, will bleed off the 0.5 of volume with rear hydrochloric acid simultaneously, put into the sample after cleaning in the electric heater unit of water-stop in clear water.
VII adds new technical hydrochloric acid (GB320-2006 definite quality concentration >=31.0%) again in the electric heater unit of water-stop, and technical hydrochloric acid liquid level exceedes specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop.
The electric heater unit of VIII water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and after safety inspection, energising begins to warm up.
In the electric heater unit of Ⅸ water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and second time starts insulation, is incubated 90 minutes.
Ⅹ cuts off the electricity supply, and opens sealing and covers, and the acid solution in the electric heater unit of discharge water-stop, to neutralization pond, is discharged after to be neutralized, takes out sample and cleans up in the hot water, and with compressing air blow drying.
Obtain macrostructure and defect specimen surface clearly.
Embodiment two
I to cut φ 400mm garden rod corrosion resistant alloy (N08028) cross section sample thickness be 25mm mono-piece be the first sample, cutting another batch of φ 400mm garden rod corrosion resistant alloy (N08028) cross section sample thickness again be 25mm mono-piece is the second sample, after sample face to be seen vertical knee-type milling machine is processed, with 60 order sand paper manual polishing specimen surface 3 minutes, and clean with absorbent cotton and wipes of alcohol, specimen surface roughness RaIt is not more than 1.6 μm and without greasy dirt.
II in ventilated chamber, place the electric heater unit (voltage 220 V of an acidproof water-stop, power 3000W), first sample is put into the bottom of the electric heater unit of water-stop, specimen surface to be seen at the first sample places the Glass rod of two diameter 6mm, distance between two Glass rods is 200mm, then places the second sample on two Glass rods.
III adds technical hydrochloric acid (GB320-2006 definite quality concentration >=31.0%) in the electric heater unit of water-stop, and technical hydrochloric acid liquid level, more than the second sample specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop.
The electric heater unit of IV water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and after safety inspection, energising begins to warm up.
In the electric heater unit of V water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and starts insulation, is incubated 90 minutes.
VI after insulation, opens sealing lid and takes out sample, cleans down the chloride of specimen surface to be seen with brush, will bleed off the 0.5 of volume with rear hydrochloric acid simultaneously, put into the sample after cleaning in the electric heater unit of water-stop in clear water.
VII adds new technical hydrochloric acid (GB320-2006 definite quality concentration >=31.0%) again in the electric heater unit of water-stop, and technical hydrochloric acid liquid level, more than the specimen surface 50mm to be seen of the second sample, covers the sealing lid of the electric heater unit of water-stop.
The electric heater unit of VIII water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and after safety inspection, energising begins to warm up.
In the electric heater unit of Ⅸ water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and second time starts insulation, is incubated 90 minutes.
Ⅹ cuts off the electricity supply, and opens and seals lid, and the acid solution in the electric heater unit of discharge water-stop is to neutralization pond, and after to be neutralized, discharge, takes out the first sample and the second sample cleans up in the hot water, and with compressing air blow drying.
Obtain macrostructure and the specimen surface to be seen of defect the first sample clearly and the second sample.
Claims (3)
1. corrosion resistant alloy macrostructure and defect manifest an acid etching method, and it includes following step successively:
I to cut bar-shaped corrosion resistant alloy N08028 cross section sample thickness be within 25mm, or cut at N08028 steel plate and to fail to grow up in 450mm, the wide sample being not more than 50mm along rolling direction, after specimen surface vertical knee-type milling machine to be seen is processed, with sand papering specimen surface to be seen, and clean with absorbent cotton and wipes of alcohol, the roughness R of specimen surface to be seenaIt is not more than 1.6 μm and without greasy dirt；
II in ventilated chamber, places the electric heater unit of acidproof water-stop, opens the sealing lid of electric heater unit, and sample is put in the electric heater unit of water-stop；
III adds technical hydrochloric acid in the electric heater unit of water-stop, and technical hydrochloric acid liquid level exceedes specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop；
The electric heater unit of IV water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and energising begins to warm up；
In the electric heater unit of V water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and starts insulation, is incubated 90 ± 5 minutes；
VI after insulation, opens sealing lid and takes out sample, cleans down the chloride of specimen surface to be seen with brush, will bleed off the 0.5 ± 0.05 of volume with rear hydrochloric acid simultaneously, put into the sample after cleaning in the electric heater unit of water-stop in clear water；
VII adds new technical hydrochloric acid again in the electric heater unit of water-stop, keeps technical hydrochloric acid liquid level to exceed specimen surface 50mm to be seen, covers the sealing lid of the electric heater unit of water-stop；
The electric heater unit of VIII water-stop passes through temperature controller design temperature 85 DEG C 90 DEG C, and energising begins to warm up；
In the electric heater unit of Ⅸ water-stop, technical hydrochloric acid reaches 85 DEG C 90 DEG C, and second time starts insulation, is incubated 90 ± 5 minutes；
Ⅹ cuts off the electricity supply, and opens sealing and covers, and the acid solution in the electric heater unit of discharge water-stop, to neutralization pond, is discharged after to be neutralized, takes out sample and cleans up in the hot water, and with compressing air blow drying.
2. corrosion resistant alloy macrostructure according to claim 1 and defect manifest acid etching method, and its steps characteristic is:
13 pieces of samples are cut again in step I；After specimen surface vertical knee-type milling machine to be seen is processed, with sand papering specimen surface to be seen, and by absorbent cotton and wipes of alcohol totally, the roughness R of specimen surface to be seenaIt is not more than 1.6 μm and without greasy dirt；
It is put in the electric heater unit of water-stop in step II at sample, is not less than the Glass rod of 4mm with diameter between every sample two pieces adjacent and separates；
The specimen surface 50mm to be seen of the superiors' sample is exceeded in step III technical hydrochloric acid liquid level；
The specimen surface 50mm to be seen of the superiors' sample is exceeded in step VII technical hydrochloric acid liquid level.
3. corrosion resistant alloy macrostructure according to claim 1 and 2 and defect manifest acid etching method, it is characterized in that: described electric heater unit is vertical view direction is rectangular heating tank, electrical bar is installed in heating tank, heating tank is covered with sealing lid, notch surrounding at heating tank has the water sealed tank of water, when sealing lid covers on heating tank, water sealed tank is dropped on the lower edge sealing lid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201222020Y (en) * | 2008-06-10 | 2009-04-15 | 耐博检测技术(上海)有限公司 | Macroscopic structure heat etching apparatus |
| CN101975742A (en) * | 2010-10-31 | 2011-02-16 | 广东省韶铸集团有限公司 | Low-power cold corrosion detection method |
| CN102297785A (en) * | 2011-04-18 | 2011-12-28 | 首钢水城钢铁（集团）有限责任公司 | Method for exposing profile tiny tissue defects of high-carbon steel continuous casting billet |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201222020Y (en) * | 2008-06-10 | 2009-04-15 | 耐博检测技术(上海)有限公司 | Macroscopic structure heat etching apparatus |
| CN101975742A (en) * | 2010-10-31 | 2011-02-16 | 广东省韶铸集团有限公司 | Low-power cold corrosion detection method |
| CN102297785A (en) * | 2011-04-18 | 2011-12-28 | 首钢水城钢铁（集团）有限责任公司 | Method for exposing profile tiny tissue defects of high-carbon steel continuous casting billet |
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