CN107764620A - A kind of Pb-Ca-Sn-Al alloy metallographic preparation method - Google Patents
A kind of Pb-Ca-Sn-Al alloy metallographic preparation method Download PDFInfo
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- CN107764620A CN107764620A CN201711127186.7A CN201711127186A CN107764620A CN 107764620 A CN107764620 A CN 107764620A CN 201711127186 A CN201711127186 A CN 201711127186A CN 107764620 A CN107764620 A CN 107764620A
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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 present invention is a kind of Pb-Ca-Sn-Al alloy metallographic preparation method.This method includes sampling, corase grind, fine grinding, mechanical polishing, chemical polishing and erosion, and polishing fluid is the mixture of glacial acetic acid and hydrogenperoxide steam generator, and the formula of corrosive liquid is per adding 5 ~ 10g of 15 ~ 20g of citric acid and ammonium molybdate in 90g distilled water.This method adjusts the polishing etch time, the method polished using multiple chemical is eliminated cut and obtained clearly organizing by selecting the species of polishing agent.This method formula is simple, practical.
Description
Technical field
The invention belongs to microstructure of the alloy preparation field, and in particular to the lead calcium tin aluminium to a kind of lead acid accumulator plate grid closes
The metallographic technology of preparing of gold.
Background technology
The performance of Pb-Ca-Sn-Al alloy depends on its institutional framework.Frequently by research metallographic group in engineering and scientific research
Knit to judge the performance of alloy, the structure of metallographic structure shows often by a series of modes such as polishing etch to realize
's.
One group of good metallographic structure should be no marking, corrosion is uniform, organize clearly to organize.But current lead-calcium alloy
Mechanical polishing all suffers from difficulty with chemical polishing in metallographic technology of preparing, and its main cause has at following 2 points：One is lead calcium
Sn-Al alloy hardness is extremely low, and cut is difficult to avoid that during grinding-polishing；The second is the alloy corrosion resistance is poor, extent of corrosion is difficult
To hold.Metallographic is prepared crucial mainly in two links of polishing and corrosion, the selection one that at present there is chemical polishing agent in research
Determine the hydrochloric acid hydrogen peroxide of volume ratio, etching time 1~3 minute；Some carries out chemistry from acetic acid hydrogen peroxide methyl alcohol mixed liquor and invaded
Erosion, and hydrochloric acid belongs to strong acid, the alloy improper use for this acid labile of lead calcium tin aluminium easily causes alloy corrosion
Weight, structure observation effect is less desirable, along with methanol is toxic, is also easy to damage laboratory technician's health.
The content of the invention
The invention aims to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of Pb-Ca-Sn-Al alloy metallographic system
Preparation Method.This method is adjusted the polishing etch time, eliminated using the method for multiple chemical polishing by selecting the species of polishing agent
Cut, has obtained clearly organizing.This method formula is simple, can effectively eliminate cut so that tissue corrosion is uniform.
The technical scheme is that：
A kind of Pb-Ca-Sn-Al alloy metallographic preparation method, comprises the following steps：
The first step samples：Initial metallographic specimen is obtained using wire cutting machine interception Pb-Ca-Sn-Al alloy parent material；
Second step is roughly ground：Ground successively using 1000#, 1500# waterproof abrasive paper, the milling time of every kind of waterproof abrasive paper is 1~2 point
Clock；
3rd step is refined：Ground successively using 2500#, 3000# waterproof abrasive paper, the milling time of every kind of waterproof abrasive paper is 2~3 points
Clock；
4th step mechanically polishes：Using polishing machine, sample is polished 1~3 minute；Wherein, the rotating speed of polishing machine is 600r/
Min~800r/min；
5th step chemical polishing：The sample that upper step is obtained carries out 3~6 chemical polishings；The step of each chemical polishing
For：Polishing fluid is dripped into specimen surface with dropper, polishing fluid keeps 20~40s after being saturated with specimen surface, and subsequent running water rinses
Fall surface polishing fluid, then sample immersion is kept into 4~5s in glacial acetic acid；
Wherein, polishing fluid is the mixture of hydrogenperoxide steam generator and glacial acetic acid, hydrogenperoxide steam generator (mass fraction 35%)
It is 1: 4~6 with glacial acetic acid volume ratio；
6th step corrodes：Chemical erosion is carried out to specimen surface：The completely upper step of corrosion drop is obtained into metallographic specimen surface, protected
Hold 10~20s；Wherein, the formula of corrosive liquid is per 5~10g of addition 15~20g of citric acid and ammonium molybdate in 90g distilled water；
Suds are dripped on waterproof abrasive paper in the 3rd described step lapping process.
The 4th described step polishing process polishing cloth is soft silk polishing cloth, should to avoid specimen surface from aoxidizing in polishing
Constantly add water.
The composition of described Pb-Ca-Sn-Al alloy is：0.06~0.08wt%Ca, 0.60~1.40wt%Sn, 0.02~
0.03wt%Al, remaining is Pb.
The present invention substantive distinguishing features be：It is a comprehensive process that alloy structure, which shows, and it is metallographic that it, which is polished with erosion,
The link of preparation method core, this method adjust the proportioning of polishing agent, take multiple chemical to throw by selecting the species of polishing agent
Light method gradually falls undercut corrosion；And chemical erosion is combined, erosion time is adjusted, tissue is shown.
Beneficial effects of the present invention are：
This method preparation process is simply efficient, rejects harmful liquid, reduces the harm to experimenter's health；Can effectively it disappear
Except cut, the problem of corrosion is improper is avoided, clearly shows the tissue of alloy.In chemical polishing, once change relative to tradition
Its polishing etch degree of the method for optical polishing is difficult to hold, and this method is polished by multiple chemical, and extent of corrosion is easily held.
Brief description of the drawings
Fig. 1 is the photo using Pb-Ca-Sn-Al alloy metallographic structure made from current techniques；
The photo for the Pb-Ca-Sn-Al alloy metallographic structure that Fig. 2 obtains for embodiment 2, multiplication factor 200；
The photo for the Pb-Ca-Sn-Al alloy metallographic structure that Fig. 3 obtains for embodiment 3, multiplication factor 200；
The photo for the Pb-Ca-Sn-Al alloy metallographic structure that Fig. 4 obtains for embodiment 4, multiplication factor 200.
Embodiment
Pb-Ca-Sn-Al alloy metallographic preparation method is further illustrated below in conjunction with example：
Embodiment 1
Hand sample is carried out to the metal of casting, then carries out edge sample with epoxy resin, after sample fixation, is used respectively
240#, 400# waterproof abrasive paper enter water-filling wet-milling, untill surface is without obvious thick trace, then by sample (alloying component 0.080wt%
Ca, 1.2wt%Sn, 0.030wt%Al, remaining is Pb) carry out polishing (1min) throwing in short-term with 1000# waterproof abrasive papers on polishing machine
Light liquid 4%Cr2O3Amidin.Sample is in grey black after polishing, and sample is immersed into acetic acid dioxygen in chemical polishing solution in time
Water (hydrogen peroxide of 75% acetic acid+25%), teetertotter sample about several seconds, and chemical polishing carries out mechanical throwing again after stopping
Light, then cleaned with distilled water, dehydration of alcohol, cold wind drying, that is, be available for observing under the microscope.
(the present embodiment is quoted from (the research of maintenance-free lead accumulator anode grid materials perhaps of heap of stone of current techniques Literature
[D] Kunming University of Science and Technology, 2008) experimentation and experimental result of statement.)
As a result accompanying drawing 1 is seen, it can be seen that metallographic structure shows extremely unintelligible in the metallographic preparation scheme, first without jettisoning
Cut, it can be seen that the thick cut of black is a lot, influences structure observation；Secondly the metallographic structure chemical polishing degree not enough (is changed
Optical polishing also has the effect of erosion concurrently), do not see clearly crystal boundary, do not fall undercut corrosion yet, visual field blur, office
The patch that there is black in portion is that corrosion is overweight.
Embodiment 2
A using wire cutting machine interception Pb-Ca-Sn-Al alloy parent material obtain initial metallographic specimen, its size be Φ 10mm ×
10mm, wherein, the Pb-Ca-Sn-Al alloy composition being related in the present embodiment is 0.065wt%Ca, 1.4wt%Sn, 0.025wt%
Al, remaining is Pb.
B is lightly ground sample by hand using 1000#, 2000# waterproof abrasive paper successively, and sample adjusts 90 ° of directions, water after grinding 30s
A little suds are dripped on sand paper to continue to grind, and are ground 1 minute on every kind of sand paper.
C is lightly ground sample, mill 90 ° of directions of sample adjustment, water after 30 seconds by hand using 2500#, 3000# waterproof abrasive paper successively
A little suds are dripped on sand paper to continue to grind, and are ground 1 minute on every kind of sand paper.
Silk cloth is arranged on polishing machine by d, and adjustment polishing machine rotating speed is 700r/min, silk cloth is moistened with water, to examination
Sample polishes, and polishes 3 minutes.
E polishing fluids：Glacial acetic acid (purity >=99.5wt%, following examples are same) and hydrogenperoxide steam generator (mass fraction
35%, following examples are same) match somebody with somebody liquid by volume for 3: 1, use rubber head dropper to draw polishing fluid, drip full specimen surface holding
50 seconds, subsequent running water rinsed specimen surface, and sample finally is immersed in into glacial acetic acid (purity >=99.5wt%, following examples
5 seconds in together).Then it is repeated 8 times above-mentioned chemical polishing process.
Rubber head dropper is rinsed well and draws corrosive liquid (90g distilled water+12g citric acid+12g ammonium molybdates) by f, drips full sample
Surface is kept for 10 seconds, and running water rinses specimen surface well and then uses dehydration of alcohol, cold wind drying.
Tissues observed structure under g metallographic microscopes.
As a result accompanying drawing 2 is seen, it can be seen that although chemical polishing process jettisoning cut, organize effective effect to pay no attention to
Think, overall relatively fuzzy, black is presented in subregion, and corrosion is uneven.
Embodiment 3
A using wire cutting machine interception Pb-Ca-Sn-Al alloy parent material obtain initial metallographic specimen, its size be Φ 10mm ×
10mm, wherein, the Pb-Ca-Sn-Al alloy composition being related in the present embodiment is 0.065wt%Ca, 1.3wt%Sn, 0.023wt%
Al, remaining is Pb.
B is lightly ground sample by hand using 1000#, 2000# waterproof abrasive paper successively, and sample adjusts 90 ° of directions, water after grinding 30s
A little suds are dripped on sand paper to continue to grind, and are ground 1 minute on every kind of sand paper.
C is lightly ground sample, mill 90 ° of directions of sample adjustment, water after 30 seconds by hand using 2500#, 3000# waterproof abrasive paper successively
A little suds are dripped on sand paper to continue to grind, and are ground 1 minute on every kind of sand paper.
Silk cloth is arranged on polishing machine by d, and adjustment polishing machine rotating speed is 700r/min, silk cloth is moistened with water, to examination
Sample polishes, and polishes 3 minutes.
E polishing fluids：Glacial acetic acid and hydrogenperoxide steam generator match somebody with somebody liquid for 7: 1 by volume, use the rubber head dropper to draw polishing
Liquid, drip full specimen surface and kept for 15 seconds, subsequent running water rinses specimen surface, finally by sample immersion 5 seconds in glacial acetic acid.So
After be repeated 2 times above-mentioned chemical polishing process.
Rubber head dropper is rinsed well and draws corrosive liquid (90g distilled water+10g citric acid+4g ammonium molybdates) by f, drips full sample
Surface is kept for 10 seconds, and running water rinses specimen surface well and then uses dehydration of alcohol, cold wind drying.
Tissues observed structure under g metallographic microscopes.
As a result to see accompanying drawing 3, it is more fuzzy can to see that institutional framework shows, crystal boundary shows imperfect, or even can't see crystal boundary,
Local cut does not have jettisoning.
Embodiment 4
A using wire cutting machine interception Pb-Ca-Sn-Al alloy parent material obtain initial metallographic specimen, its size be Φ 10mm ×
10mm, wherein, the Pb-Ca-Sn-Al alloy composition being related in the present embodiment is 0.070wt%Ca, 1.3wt%Sn, 0.022wt%
Al, remaining is Pb.
B is lightly ground sample by hand using 1000#, 2000# waterproof abrasive paper successively, and sample adjusts 90 ° of directions, water after grinding 30s
A little suds are dripped on sand paper to continue to grind, and are ground 2 minutes on every kind of sand paper.
C is lightly ground sample, mill 90 ° of directions of sample adjustment, water after 30 seconds by hand using 2500#, 3000# waterproof abrasive paper successively
A little suds are dripped on sand paper to continue to grind, and are ground 2 minutes on every kind of sand paper.
Silk cloth is arranged on polishing machine by d, and adjustment polishing machine rotating speed is 600r/min, silk cloth is moistened with water, to examination
Sample polishes, and polishes 1 minute.
E polishing fluids：Glacial acetic acid and hydrogenperoxide steam generator match somebody with somebody liquid for 4: 1 by volume, use the rubber head dropper to draw polishing
Liquid, drip full specimen surface and kept for 20 seconds, subsequent running water rinses specimen surface, finally by sample immersion 5 seconds in glacial acetic acid.So
After be repeated 6 times above-mentioned chemical polishing process.
Rubber head dropper is rinsed well and draws corrosive liquid (90g distilled water+16g citric acid+6g ammonium molybdates) by f, drips full sample
Surface is kept for 10 seconds, and running water rinses specimen surface well and then uses dehydration of alcohol, cold wind drying.
Tissues observed structure under g metallographic microscopes.
As a result accompanying drawing 2 is seen：From metallographic structure it can be seen that no cut, crystal boundary understand, corrosive effect is good, and institutional framework shows
It is now clear.
Embodiment 5
A using wire cutting machine interception Pb-Ca-Sn-Al alloy parent material obtain initial metallographic specimen, its size be Φ 10mm ×
10m, wherein, the Pb-Ca-Sn-Al alloy composition being related in the present embodiment is 0.068wt%Ca, 1.2wt%Sn, 0.024wt%Al,
Remaining is Pb.
B is lightly ground sample by hand using 1000#, 2000# waterproof abrasive paper successively, and sample adjusts 90 ° of directions, water after grinding 30s
A little suds are dripped on sand paper to continue to grind, and are ground 2 minutes on every kind of sand paper.
C is lightly ground sample, mill 90 ° of directions of sample adjustment, water after 30 seconds by hand using 2500#, 3000# waterproof abrasive paper successively
A little suds are dripped on sand paper to continue to grind, and are ground 2 minutes on every kind of sand paper.
Silk cloth is arranged on polishing machine by d, and adjustment polishing machine rotating speed is 700r/min, silk cloth is moistened with water, to examination
Sample polishes, and polishes 2 minutes.
E polishing fluids：Glacial acetic acid and hydrogenperoxide steam generator match somebody with somebody liquid for 5: 1 by volume, use the rubber head dropper to draw polishing
Liquid, drip full specimen surface and kept for 25 seconds, subsequent running water rinses specimen surface, finally by sample immersion 5 seconds in glacial acetic acid.So
After be repeated 3 times above-mentioned chemical polishing process.
Rubber head dropper is rinsed well and draws corrosive liquid (90g distilled water+15g citric acid+8g ammonium molybdates) by f, drips full sample
Surface is kept for 15 seconds, and running water rinses specimen surface well and then uses dehydration of alcohol, cold wind drying.
Tissues observed structure under g metallographic microscopes.Its institutional framework is the same as embodiment 4.
Embodiment 6
A use wire cutting machine interception Pb-Ca-Sn-Al alloy parent material obtain its size of initial metallographic specimen for Φ 10mm ×
10mm, wherein, the Pb-Ca-Sn-Al alloy composition being related in the present embodiment is 0.068wt%Ca, 1.4wt%Sn, 0.025wt%
Al, remaining is Pb.
B is lightly ground sample by hand using 1000#, 2000# waterproof abrasive paper successively, and sample adjusts 90 ° of directions, water after grinding 30s
A little suds are dripped on sand paper to continue to grind, and are ground 2 minutes on every kind of sand paper.
C is lightly ground sample, mill 90 ° of directions of sample adjustment, water after 30 seconds by hand using 2500#, 3000# waterproof abrasive paper successively
A little suds are dripped on sand paper to continue to grind, and are ground 2 minutes on every kind of sand paper.
Silk cloth is arranged on polishing machine by d, and adjustment polishing machine rotating speed is 800r/min, silk cloth is moistened with water, to examination
Sample polishes, and polishes 3 minutes.
E polishing fluids：Glacial acetic acid and hydrogenperoxide steam generator match somebody with somebody liquid for 6: 1 by volume, use the rubber head dropper to draw polishing
Liquid, drip full specimen surface and kept for 40 seconds, subsequent running water rinses specimen surface, finally by sample immersion 5 seconds in glacial acetic acid.So
After be repeated 5 times above-mentioned chemical polishing process.
Rubber head dropper is rinsed well and draws corrosive liquid (90g distilled water+20g citric acid+10g ammonium molybdates) by f, drips full sample
Surface is kept for 20 seconds, and running water rinses specimen surface well and then uses dehydration of alcohol, cold wind drying.
Tissues observed structure under g metallographic microscopes.Its institutional framework is the same as embodiment 4.
Embodiment 4-6, the results showed that：Use Pb-Ca-Sn-Al alloy metallographic preparation method tissue no marking of the present invention, corrosion
Uniformly, tissue is clear.
Unaccomplished matter of the present invention is known technology.
Claims (4)
- A kind of 1. Pb-Ca-Sn-Al alloy metallographic preparation method, it is characterized in that this method comprises the following steps：The first step samples：Initial metallographic specimen is obtained using wire cutting machine interception Pb-Ca-Sn-Al alloy parent material；Second step is roughly ground：Ground successively using 1000#, 1500# waterproof abrasive paper, the milling time of every kind of waterproof abrasive paper is 1 ~ 2 minute；3rd step is refined：Ground successively using 2500#, 3000# waterproof abrasive paper, the milling time of every kind of waterproof abrasive paper is 2 ~ 3 minutes；4th step mechanically polishes：Using polishing machine, sample is polished 1 ~ 3 minute；Wherein, the rotating speed of polishing machine be 600r/min ~ 800r/min；5th step chemical polishing：The sample that upper step is obtained carries out 3 ~ 6 chemical polishings；The step of each chemical polishing is：With Polishing fluid is dripped to specimen surface by dropper, and polishing fluid keeps 20 ~ 40s after being saturated with specimen surface, and subsequent running water rinses out surface Polishing fluid, then sample immersion is kept into 4 ~ 5s in glacial acetic acid；Wherein, polishing fluid is the mixture of hydrogenperoxide steam generator and glacial acetic acid, hydrogenperoxide steam generator（Mass fraction 35%）With ice vinegar Sour volume ratio is 1: 4 ~ 6；6th step corrodes：Chemical erosion is carried out to specimen surface：The completely upper step of corrosion drop is obtained into metallographic specimen surface, keeps 10 ~20s；Wherein, the formula of corrosive liquid is per 5 ~ 10g of addition 15 ~ 20g of citric acid and ammonium molybdate in 90g distilled water.
- 2. Pb-Ca-Sn-Al alloy metallographic preparation method as claimed in claim 1, it is characterized in that the 3rd described step lapping process In to drip suds on waterproof abrasive paper.
- 3. Pb-Ca-Sn-Al alloy metallographic preparation method as claimed in claim 1, it is characterized in that the 4th described step polishing process Polishing cloth is soft silk polishing cloth, to avoid specimen surface from aoxidizing in polishing, should constantly add water.
- 4. Pb-Ca-Sn-Al alloy metallographic preparation method as claimed in claim 1, it is characterized in that described Pb-Ca-Sn-Al alloy Form and be：0.06 ~ 0.08wt%Ca, 0.60 ~ 1.40wt%Sn, 0.02 ~ 0.03wt% Al, remaining is Pb.
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Cited By (3)
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| CN109855932A (en) * | 2019-01-02 | 2019-06-07 | 中铝材料应用研究院有限公司 | A method of preparing rolling aluminium alloy sheet EBSD sample |
| CN110987576A (en) * | 2019-11-26 | 2020-04-10 | 昆明理工大学 | Corrosive agent for displaying fine austenite grain boundary of low-carbon microalloyed steel and use method |
| CN113092203A (en) * | 2021-03-29 | 2021-07-09 | 北京科技大学 | Metallographic phase preparation method of lead bismuth alloy |
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Application publication date: 20180306 |