CN103900887A - Method for displaying macro morphology of as-cast lead or lead alloy - Google Patents
Method for displaying macro morphology of as-cast lead or lead alloy Download PDFInfo
- Publication number
- CN103900887A CN103900887A CN201210584488.8A CN201210584488A CN103900887A CN 103900887 A CN103900887 A CN 103900887A CN 201210584488 A CN201210584488 A CN 201210584488A CN 103900887 A CN103900887 A CN 103900887A
- Authority
- CN
- China
- Prior art keywords
- sample
- etchant
- seen
- cast condition
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- ing And Chemical Polishing (AREA)
Abstract
The invention discloses a method for displaying macro morphology of as-cast lead or lead alloy. The method comprises three steps of manually sanding, chemically polishing, and corroding. A polishing solution is composed of H2O2 and CH3COOH, and an erosion solution is composed of a concentrated nitric acid, ammonium molybdate and deionized water. The method has the advantages that few grinding procedures are carried out, the sample preparation method is simple and convenient, and the prepared sample is real in tissue, visual in grain shape, and high in accuracy rate of estimation on the average grain size.
Description
Technical field
The invention belongs to technical field of metallographic sample preparation, be specifically related to the method for a kind of energy clear demonstration as cast condition lead or lead alloy macro morphology.
Background technology
Because plumbous hardness is little, lead and alloy thereof are very soft, under low-pressure, will deform, in the time adopting classic method to prepare lead and lead alloy metallographic sample, larger surface can occur in grinding and polishing process flows and is out of shape, will cover true tissue if thoroughly do not removed this deformation layer, create a false impression, bring difficulty to preparing metallographic sample.In bruting process, should avoid abrasive particle to embed sample surfaces, to organized really as far as possible.The lead of deformation and Deformation recrystallization, the crystallite dimension of lead alloy sample are less, utilize optical microscopy/scanning electron microscopy/EBSD technology can clearly show the shape of each crystal grain and can estimate exactly the average grain size of sample; And the crystallite dimension of as cast condition lead, lead alloy is larger, under minimum enlargement factor, still can not show a full die, the average grain size that causes intactly showing the shape of each crystal grain and accurately estimate as cast condition lead, lead alloy sample.Therefore, reduce the grinding step of as cast condition lead, lead alloy and select can clear demonstration as cast condition lead, the etchant of lead alloy sample macro morphology, not only can simplify sample-preparation processes, real tissue is provided, also can greatly improves the estimation accuracy of as cast condition lead, lead alloy sample average crystallite dimension.
Summary of the invention
For the problems referred to above of prior art, the invention provides the method for the clear demonstration as cast condition of a kind of energy lead, lead alloy metallographic macrostructure.
For achieving the above object, do invention and comprise following technical scheme:
A method that shows as cast condition lead or lead alloy macro morphology, the method comprises the steps:
A. manual grinding: with 200#～1000# liquid honing as cast condition lead or lead alloy sample surface to be seen, make to be seen of as cast condition lead or lead alloy sample smooth;
B. chemical polishing: drip polishing fluid on the pure plumbous sample of as cast condition or lead alloy sample surface to be seen, this polishing fluid is by H
2o
2and CH
3cOOH is 0.5～0.8: 1.2～1.5 compositions by volume, and dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, nitric acid, ammonium heptamolybdate and the deionized water that this etchant is 60～70wt% by concentration by weight 20～50: 5～10: 50～150 form, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 5～15s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 5～10 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
Method as above, preferably, in described lead alloy, lead content is greater than 80%.
Method as above, preferably, described method comprises the steps:
A. manual grinding: with the 800# pure plumbous sample of liquid honing as cast condition surface to be seen, make plumbous to be seen of the sample of as cast condition smooth;
B. chemical polishing: drip polishing fluid on the pure plumbous sample of as cast condition surface to be seen, this polishing fluid is by H
2o
2and CH
30.5: 1.5 by volume composition of COOH, dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, this etchant is made up of by weight nitric acid (concentration is 68wt%), ammonium heptamolybdate and deionized water at 50: 5: 150, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 15s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 10 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
Method as above, preferably, described method comprises the steps:
A. manual grinding: with 800# liquid honing as cast condition lead alloy surface to be seen, make to be seen of as cast condition lead alloy sample smooth;
B. chemical polishing: drip polishing fluid on the pure lead alloy sample of as cast condition surface to be seen, this polishing fluid is by H
2o
2and CH
30.8: 1.2 by volume composition of COOH, dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, this etchant is made up of by weight nitric acid (concentration is 68wt%), ammonium heptamolybdate and deionized water at 20: 10: 50, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 5s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 5 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
Method as above, preferably, described method comprises the steps:
A. manual grinding: with 800# liquid honing as cast condition lead alloy surface to be seen, make to be seen of as cast condition lead alloy sample smooth;
B. chemical polishing: drip polishing fluid on the pure lead alloy sample of as cast condition surface to be seen, this polishing fluid is by H
2o
2and CH
30.7: 1.3 by volume composition of COOH, dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, this etchant is made up of by weight nitric acid (concentration is 68wt%), ammonium heptamolybdate and deionized water at 40: 8: 120, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 10s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 10 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
Beneficial effect of the present invention is: the present invention takes the method for making sample of one manual grinding operation, with hydrogen peroxide and glacial acetic acid composition polishing fluid, nitric acid and ammonium molybdate composition etchant, successfully having prepared can clear demonstration as cast condition lead, the sample of lead alloy macrostructure pattern.The method grinding step passage is few, and sample preparation methods is easy, and the sample tissue of preparation is true, grain shape is visual, and average grain size estimation accuracy rate is high.
Accompanying drawing explanation
Fig. 1 is the macro morphology photo that the inventive method is prepared the pure plumbous sample of as cast condition air cooling.
Fig. 2 is the macro morphology photo that the inventive method is prepared as cast condition Pb-0.6%Ag water-cooled sample.
Fig. 3 is that the inventive method is prepared the macro morphology photo of as cast condition Pb-0.6%Ag with the cold sample of stove.
Embodiment
The invention is further illustrated by the following examples.These embodiment are not limitations of the present invention, any be equal to replace or known change all belong to protection domain of the present invention.
From the pure lead pig of as cast condition air cooling, cut 1 sample, sample is processed through following:
1. manual grinding: with the 800# pure plumbous sample of liquid honing as cast condition surface to be seen, make to be seen of the pure plumbous sample of as cast condition smooth.
2. chemical polishing: drip H with glue head dropper on the pure plumbous sample of as cast condition surface to be seen
2o
2and CH
3cOOH volume ratio is the chemical brightening solution of 0.5: 1.5 composition, and dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product.
3. corrode: with glue head dropper through step 2 sample surfaces after treatment dropping nitric acid (massfraction is 68%), ammonium heptamolybdate ((NH
4)
6mo
7o
244H
2o) and the weight part ratio of deionized water be 50: 5: 150 composition etchant, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 15s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed on and in alcohol, soaks 10s, taking-up dries up with cold wind, obtains the pure plumbous sample of as cast condition of the clear demonstration of macro morphology.As shown in Figure 1, the grain structure pattern of the pure lead of as cast condition air cooling is clear for result, and crystal grain is equiax crystal, and crystallite dimension is about 1.5mm left and right.
Embodiment 2
From as cast condition Pb-0.6%Ag water-cooled alloy pig (this as cast condition pb-ag alloy sample, the content of Ag is 0.6 % by weight, and surplus is Pb), cut 1 sample, sample is processed through following:
1. manual grinding: with 800# liquid honing as cast condition Pb-0.6%Ag water-cooled alloy sample surface to be seen, make to be seen of as cast condition Pb-0.6%Ag water-cooled alloy sample smooth;
2. chemical polishing: drip H with glue head dropper on as cast condition Pb-0.6%Ag water-cooled alloy sample surface to be seen
2o
2and CH
3cOOH volume ratio is the chemical brightening solution of 0.8: 1.2 composition, and dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
3. corrode: with glue head dropper be the etchant forming at 20: 10: 50 at the weight part ratio that drips nitric acid (massfraction is 68%), ammonium molybdate and deionized water through step 2 sample surfaces after treatment, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 5s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed on and in alcohol, soaks 5s, taking-up dries up with cold wind, obtains the as cast condition Pb-0.6%Ag water-cooled alloy sample of the clear demonstration of macro morphology.As shown in Figure 2, the grain structure pattern of as cast condition Pb-0.6%Ag water-cooled alloy is clear for result, and crystal grain is typical dendritic crystalline, and crystallite dimension is about 1.5mm left and right.
Embodiment 3
From as cast condition Pb-0.6%Ag, with cutting 1 sample in the cold alloy of stove (this as cast condition pb-ag alloy sample, the content of Ag is 0.6 % by weight, and surplus is Pb) ingot, sample is processed through following:
1. manual grinding: with the cold alloy sample of stove surface to be seen, make as cast condition Pb-0.6%Ag smooth with to be seen of the cold alloy sample of stove with 800# liquid honing as cast condition Pb-0.6%Ag;
2. chemical polishing: drip H at as cast condition Pb-0.6%Ag on the cold alloy sample of stove surface to be seen with glue head dropper
2o
2and CH
3cOOH volume ratio is the chemical brightening solution of 0.7: 1.3 composition, and dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
3. corrode: with glue head dropper be the etchant forming at 40: 8: 120 at the weight part ratio that drips nitric acid (massfraction is 68%), ammonium molybdate and deionized water through step 2 sample surfaces after treatment, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 10s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed on and in alcohol, soaks 10s, taking-up dries up with cold wind, obtains the Pb-0.6%Ag of the clear demonstration of macro morphology with the cold alloy sample of stove.As shown in Figure 3, as cast condition Pb-0.6%Ag is clear with the grain structure pattern of the cold alloy of stove for result, and crystal grain is equiax crystal, and crystallite dimension is about 1.2mm left and right.
Claims (5)
1. a method that shows as cast condition lead or lead alloy macro morphology, is characterized in that, the method comprises the steps:
A. manual grinding: with 200#～1000# liquid honing as cast condition lead or lead alloy sample surface to be seen, make to be seen of as cast condition lead or lead alloy sample smooth;
B. chemical polishing: drip polishing fluid on the pure plumbous sample of as cast condition or lead alloy sample surface to be seen, this polishing fluid is by H
2o
2and CH
3cOOH is 0.5～0.8: 1.2～1.5 compositions by volume, and dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, nitric acid, ammonium heptamolybdate and the deionized water that this etchant is 60～70wt% by concentration by weight 20～50: 5～10: 50～150 form, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 5～15s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 5～10 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
2. the method for claim 1, is characterized in that, in described lead alloy, lead content is greater than 80%.
3. method as claimed in claim 2, is characterized in that, described method comprises the steps:
A. manual grinding: with the 800# pure plumbous sample of liquid honing as cast condition surface to be seen, make plumbous to be seen of the sample of as cast condition smooth;
B. chemical polishing: drip polishing fluid on the pure plumbous sample of as cast condition surface to be seen, this polishing fluid is by H
2o
2and CH
30.5: 1.5 by volume composition of COOH, dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, this etchant is made up of by weight nitric acid (concentration is 68wt%), ammonium heptamolybdate and deionized water at 50: 5: 150, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 15s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 10 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
4. method as claimed in claim 2, is characterized in that, described method comprises the steps:
A. manual grinding: with 800# liquid honing as cast condition lead alloy surface to be seen, make to be seen of as cast condition lead alloy sample smooth;
B. chemical polishing: drip polishing fluid on the pure lead alloy sample of as cast condition surface to be seen, this polishing fluid is by H
2o
2and CH
30.8: 1.2 by volume composition of COOH, dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, this etchant is made up of by weight nitric acid (concentration is 68wt%), ammonium heptamolybdate and deionized water at 20: 10: 50, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 5s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 5 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
5. method as claimed in claim 2, is characterized in that, described method comprises the steps:
A. manual grinding: with 800# liquid honing as cast condition lead alloy surface to be seen, make to be seen of as cast condition lead alloy sample smooth;
B. chemical polishing: drip polishing fluid on the pure lead alloy sample of as cast condition surface to be seen, this polishing fluid is by H
2o
2and CH
30.7: 1.3 by volume composition of COOH, dropping limit, limit deionized water rinsing, until sample surface to be seen generates without black/gray product;
C. corrode: dripping etchant through step B sample surfaces after treatment, this etchant is made up of by weight nitric acid (concentration is 68wt%), ammonium heptamolybdate and deionized water at 40: 8: 120, in the time that etchant covers sample surfaces completely, stop dripping etchant, after 10s, use deionized water lavage specimens product surface, subsequently the sample after rinsing is placed in ethanol and was soaked for 10 seconds, taking-up dries up with cold wind, obtains the sample of the clear demonstration of macro morphology.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210584488.8A CN103900887A (en) | 2012-12-28 | 2012-12-28 | Method for displaying macro morphology of as-cast lead or lead alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210584488.8A CN103900887A (en) | 2012-12-28 | 2012-12-28 | Method for displaying macro morphology of as-cast lead or lead alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103900887A true CN103900887A (en) | 2014-07-02 |
Family
ID=50992350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210584488.8A Pending CN103900887A (en) | 2012-12-28 | 2012-12-28 | Method for displaying macro morphology of as-cast lead or lead alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103900887A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS549572A (en) * | 1977-06-24 | 1979-01-24 | Fujitsu Ltd | Sample production method for transmission electronic microscope |
| SU1486851A1 (en) * | 1986-10-29 | 1989-06-15 | Mo I Stali I Splavov | Reagent for detecting microstructure of lead and its alloys |
| CN1800813A (en) * | 2006-01-19 | 2006-07-12 | 北京科技大学 | Process for preparing metallographic lead sample and displaying structure |
| CN101319974A (en) * | 2008-07-18 | 2008-12-10 | 昆明理工大学 | Method for preparing aluminum/lead system laminar composite material metallic phase example and display organization |
| CN101788413A (en) * | 2010-02-08 | 2010-07-28 | 宁波华舜铝材有限公司 | Method for preparing lead and lead alloy metallic phase samples and exposing texture |
| CN102486443A (en) * | 2010-12-03 | 2012-06-06 | 北京有色金属研究总院 | Method for preparing Pb/Pb alloy metallographic and/or EBSD (electron back scattering diffraction) sample |
-
2012
- 2012-12-28 CN CN201210584488.8A patent/CN103900887A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS549572A (en) * | 1977-06-24 | 1979-01-24 | Fujitsu Ltd | Sample production method for transmission electronic microscope |
| SU1486851A1 (en) * | 1986-10-29 | 1989-06-15 | Mo I Stali I Splavov | Reagent for detecting microstructure of lead and its alloys |
| CN1800813A (en) * | 2006-01-19 | 2006-07-12 | 北京科技大学 | Process for preparing metallographic lead sample and displaying structure |
| CN101319974A (en) * | 2008-07-18 | 2008-12-10 | 昆明理工大学 | Method for preparing aluminum/lead system laminar composite material metallic phase example and display organization |
| CN101788413A (en) * | 2010-02-08 | 2010-07-28 | 宁波华舜铝材有限公司 | Method for preparing lead and lead alloy metallic phase samples and exposing texture |
| CN102486443A (en) * | 2010-12-03 | 2012-06-06 | 北京有色金属研究总院 | Method for preparing Pb/Pb alloy metallographic and/or EBSD (electron back scattering diffraction) sample |
Non-Patent Citations (2)
| Title |
|---|
| 岗特•裴卓: "《金相浸蚀手册》", 31 August 1982, 科学普及出版社 * |
| 李德高: "《金属显微组织分析》", 30 November 2000, 东北大学出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101701886B (en) | Metallographical corrosive, method for eroding copper and method for displaying metallographical organization of copper | |
| CN105734588B (en) | A kind of abyssal environment high-performance aluminium alloy sacrificial anode and preparation method thereof | |
| CN105386057A (en) | Erosion agent capable of displaying solidified dendritic structure of Fe-36 Ni invar alloy and erosion method of erosion agent | |
| CN110565159B (en) | Method for preparing titanium and titanium alloy EBSD sample | |
| CN103741202B (en) | The electrolytic polishing liquid of a kind of aluminum-silicon alloy intermetallic compound and finishing method | |
| CN104048867A (en) | Method for preparing 5083 aluminum plate and 6061 aluminum plate welded joint metallographic sample | |
| CN105780005A (en) | Cold corrosion agent for displaying dendritic structure of 800 H nickel base corrosion resistant alloy and corrosion method | |
| CN102888606B (en) | Chemical corrosive liquid for magnesium alloy microsection and application of chemical corrosive liquid | |
| CN109055875A (en) | A kind of heat treatment process improving aluminium alloy extrusions intensity | |
| CN105063538B (en) | A kind of high aluminium thermal spraying solid core wire material and preparation method and application | |
| CN102486443A (en) | Method for preparing Pb/Pb alloy metallographic and/or EBSD (electron back scattering diffraction) sample | |
| CN102230211A (en) | Electrolytic polishing solution for improving surface quality of Ni5at.%W alloy base band and application method thereof | |
| CN106435273B (en) | A kind of high-plasticity corrosion-resistance Zn-Cu-Ti alloys and preparation method thereof | |
| CN112680774A (en) | Electrochemical corrosive for high-temperature alloy heat treatment metallographic structure and application method thereof | |
| Hassani et al. | Effect of friction stir processing on corrosion behavior of cast AZ91C magnesium alloy | |
| CN101383228A (en) | Formation method of electrode foil for low voltage low leakage aluminum electrolysis capacitor | |
| CN107541768A (en) | A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples | |
| CN103913362B (en) | A kind of method preparing as cast condition lead or metal EBSD sample | |
| CN103900887A (en) | Method for displaying macro morphology of as-cast lead or lead alloy | |
| CN105603432B (en) | Taking off plating solution and its take off electroplating method for aluminium alloy | |
| Barrera et al. | Natural sesquiterpene lactones are active against Leishmania mexicana | |
| CN104439191A (en) | Production method of 6-sereis alloy ingots | |
| CN106637377A (en) | Nickel-based alloy electrolytic polishing liquid and polishing method thereof | |
| CN110528059A (en) | 8 line aluminium alloy electrolytic polishing liquids of one kind and its preparation and polishing method | |
| CN106769354B (en) | Polishing method for aluminium alloy metallographic specimen |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140702 |