CN101806684B - Specimen preparation and organization exposure method of metallic phase of zinc and alloy thereof - Google Patents
Specimen preparation and organization exposure method of metallic phase of zinc and alloy thereof Download PDFInfo
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Abstract
The invention discloses a specimen preparation and organization exposure method of metallic phase of zinc and alloy thereof. The method comprises the following steps: performing wet grinding with a flat file with fine teeth, performing mechanical polishing, performing chemical polishing and exposing organization, wherein the chemical polishing step adopts the chemical polishing liquid composed of sulfuric acid, lactic acid, hydrogen peroxide and water; and the organization exposure step adopts the etching agent composed of potassium metabisulfite, sodium sulfate, chromium oxide and water, thus samples for metallographic observation can be successfully prepared. The operation is simple and convenient, the time for sample preparation is short, the consumption of material is low; and the organization exposure definition of the prepared samples is high, thus the method is particularly suitable for the specimen preparation and organization exposure of metallic phase of zinc and alloy thereof.
Description
Technical field
The present invention relates to preparation of zinc and alloy metallographic specimen thereof and organization exposure experimental technique field, preparation of a kind of zinc and alloy metallographic specimen thereof and organization exposure method particularly are provided, be applicable to preparation zinc and alloy metallographic specimen thereof.
Background technology
As everyone knows, zinc mineral deposits, output and consumption in non-ferrous metal are only second to aluminium and copper, occupy the third place in the world.The physical property of zinc: its atomic number 30, relative atomic mass 65.38, close-packed hexagonal crystal structure.The chemical property of zinc: zinc has corrosion resisting property preferably in dry air and rural stmosphere, its corrosion speed is 0.001～0.0001mm/a, and in the atmosphere of manufacturing district, because water vapor often is acid, the corrosion speed of zinc is increased, and is about 0.005mm/a.Zinc is quite stable in fresh water, big in fresh water of the etch ratio in soft water.The pH value of solution has material impact to the corrosion of zinc.The standard electrode potential of zinc is-0.76V.The recrystallization temperature of zinc is very low, and pure zinc is crystallization more at room temperature.Pressure processing is little to the influence of zinc corrosion resisting property, but presents the work softening phenomenon.Zinc and alloy thereof have a lot of incomparable characteristics of other metal materials, and combination property is also outstanding.The friction factor of zinc is little, and is big to oily affinity, and the mechanical property excellence can be made high-abrasive material (as bearing shell) and bronze equivalent material.Zinc fusing point low (419.5 ℃), casting and good processability can be used for various mechanical industries.Because zinc and alloy plurality of advantages and unusual phenomenon (work softening), the existing similar method for preparing metallographic specimen brings difficulty, its basic step for preparation zinc and alloy metallographic sample thereof: corase grind: sample is earlier through 400
#Silit waterproof abrasive paper → 600
#Silit waterproof abrasive paper → 800
#Silit waterproof abrasive paper polishing under clean flowing water flushing → clean; Fine grinding: 800
#Silit abrasive paper for metallograph → 1000
#Silit abrasive paper for metallograph → 1200
#The silit abrasive paper for metallograph polishes → rinses well, and one sand paper of every replacing all will rotate 90 degree along the polishing scratch direction with sample, the thick throwing: spray brilliant polish → clean on rough polishing is weaved cotton cloth; The smart throwing: changes thin polishing cloth and on polishing is weaved cotton cloth, spray brilliant polish → polishing velocity clean at 300～500r/min → ultrasonic vibration washer; Special-purpose etchant corrode → clean → dries up → microscopic examination.Check in data: (the modern metallographic technology of preparing of Li Jiong brightness China Metal is processed online 2008.11.7) this whole process complexity of method for preparing zinc and alloy metallographic specimen thereof, the required standard time of per pass operation is about 1～2min, what a prepares can need the long period for the zinc of observing itself and alloy metallographic specimen; Moreover, because zinc and alloy thereof have unique work softening phenomenon, under low pressure deformation will take place; Existing prepare the particle that metallographic specimen carborundum paper when the polishing comes off with class methods and very easily embed specimen surface, may be judged by accident as non-metallic inclusion; Zinc and the long easy heating of alloy sample polishing time thereof simultaneously, the very easily oxidation owing to generate heat, generate grey " oxidation film layer " deposition that does not secretly work at specimen surface, check in data (the complete works of metallographic specimen technology of preparing of up-to-date non-ferrous metal fractograph .2006.03 metallurgical industry publishing house).Remove " oxidation film layer " deposition, usually need repeatedly polishing and etch, check in data (poplar tills the land, Wang Dahai, the microstructure of deposition of lead-tin alloys thing [J]. SanXia University's journal (natural science edition), 2002,24 (5): 456-457).Prepare a good zinc itself and alloy metallographic specimen and will cross many difficult problems.Check in data (preparation of iron and steel, alloying metal metallographic specimen shows and quantitative metallography inspection technology manual of standards. the mechanical-chemical polishing of employing such as metallurgical industry publishing house-2006,10 prepares the kirsite sample, and its preparation process is still complicated, is difficult for grasp.Very easily cause the polishing friction to be generated heat if secondly pressure is excessive in polishing process, polishing time is long, owing to pressure is excessive sizable metal flow can take place also when this moment, grey " oxidation film layer " that do not work deposited presenting dark cause surface texture deformation, these surface deformation tissues can be covered true tissue, create a false impression, cause certain difficulty to metallographic structure analysis.Relevant documents and materials and related data are spoken of the few of zinc metal metallographic preparation method of sample both at home and abroad at present, and all are to be centered around under traditional metallographic specimen preparation method to carry out.Though increase, working time and sample making course that the consumptive material expense that the preparation sample produces, preparation sample produce all not too make us very satisfied.In recent years, along with developing rapidly of modern metallographic experimental technique, to the higher scientific experiment technology of metallographic specimen preparation needs of zinc and alloy thereof.
Summary of the invention
Technical matters to be solved by this invention is to provide preparation of a kind of zinc and alloy metallographic specimen thereof and organization exposure method, to reach simple to operation and can effectively appear the purpose of zinc and alloy metallographic structure thereof.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: zinc of the present invention and preparation of alloy metallographic specimen and organization exposure method is characterized in that may further comprise the steps:
A. wet-milling: sample through the flat file polishing of serration, is made cooling medium and lubricant with circulating water earlier, carries out mechanical buffing then;
B. mechanical buffing: the sample after the wet-milling is cleaned up, on polishing flannelet, carry out mechanical buffing then, mechanical buffing is that the brilliant polish of 0.3～1.0 μ m is called in the suspending liquid that stirs in the water as polishing fluid with granularity, simultaneously this polishing fluid also be cooling medium be again lubricant, polishing velocity is 200～500r/min, examine under a microscope the specimen surface state, confirm to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the sample that mechanical buffing is good immerses in the chemical brightening solution and carries out chemical polishing, to remove the grey oxidation film layer that generates through the mechanical buffing specimen surface, the complete obiteration of range estimation specimen surface grey oxidation film layer vestige, specimen surface present as bright as a sixpence polished surface and get final product; Chemical brightening solution is by H
2O
2, H
2SO
4, CH
3CHOHCOOH and H
2O is 40～60: 18～30 according to volume ratio: 1.0～3.0: 80～130 mixed solutions of forming;
D. organization exposure: dip in cotton through the good sample of chemical polishing and to mix etchant and wipe the examination etch back and forth gently, wash clean sample, clean sample with absolute ethyl alcohol then, dry up, promptly obtain organizing the clear sample that appears with flowing water at sample surfaces; Etchant is by K
2S
2O
5, Na
2SO
4, H
2O and CrO
3According to weight ratio is 0.3～0.9: 1.2～2.0: 70～100: 15～25 mixed solutions of forming.
Described chemical brightening solution is preferably by H
2O
2, H
2SO
4, CH
3CHOHCOOH and H
2O is 50: 24: 2.0 according to volume ratio: 105 mixed solutions of forming.
Described etchant is preferably by K
2S
2O
5, Na
2SO
4, H
2O and CrO
3According to weight ratio is 0.6: 1.6: 85: 20 mixed solutions of forming.
H among the present invention
2SO
4Refer to the concentrated sulphuric acid.
Described brilliant polish can be selected aluminium oxide, chromium oxide etc. for use, but preferred aluminium oxide.As for the granularity of brilliant polish, too little words polishing efficiency is low, then is difficult to the polishing effect that reaches satisfied too greatly, so be advisable with 0.3～1.0.Comprehensive, brilliant polish preferably granularity is the aluminium oxide of 0.50 μ m.
The energy-conservation method for making sample of special wet-milling that the present invention takes, profit uses water as cooling medium and lubricant.But the frictional heat that wet-milling cooling samples, reduction can cause true tissue to change, thereby wet-milling can also wash away the abrasive dust on the flour milling tendency that reduces the embedding specimen surface; The energy-and time-economizing, the flat file of the serration that optimizes replaces traditional grind away consumptive material-silit waterproof abrasive paper and silit abrasive paper for metallograph, the polishing sample time only need be about 2～3min, the flat file of serration generally is that carbon tool steel (T12A, T13A) is made, reach HRC62～67 through heat treatment hardness, serration is firm file surface can not come off, to the sample polished surface can be the time because of grind away the grinding thing come off and embed specimen surface and cover true tissue, create a false impression.Material and hardness owing to file determines simultaneously, preparation zinc and alloy metallographic specimen one thereof can not use file for a long time and need change, and prepare silit waterproof abrasive paper and silit abrasive paper for metallograph polishing sample that a qualified metallographic specimen must be changed different size in traditional metallographic specimen method for making sample; Secondly: adopt wet-milling, avoided the metal flow that the heating of sample polished surface causes and cause unfavorable factor such as surface texture deformation; The whole flow process of preparation sample is short, only needs a few minutes,, the polish pressure excessive metal flow that cause long because of polishing time can not occur and cause surface texture deformation etc.; Optimize the chemical brightening solution that sulfuric acid, lactic acid, hydrogen peroxide and water are formed, and optimized the etchant that potassium metabisulfite, sodium sulphate, chromium oxide and water are formed, successfully having prepared can be for the sample of metallographic observation.It is simple, convenient, and the preparation sample tissue appears the sharpness height, is the preparation of zinc and alloy metallographic specimen thereof and the marked improvement of organization exposure experimental technique.
Description of drawings
Fig. 1 is the metallograph with the prepared industrial-purity zinc sample of the inventive method.
Fig. 2 is the metallograph with the prepared superfine pure zinc sample of the inventive method.
Fig. 3 is the metallograph with the prepared ZA4-3 allumen sample of the inventive method.
Fig. 4 is the metallograph with the prepared ZA4-1 allumen sample of the inventive method.
Fig. 5 is the metallograph with the prepared Zn--Cu--Ti alloy alloy sample of the inventive method.
Fig. 6, Fig. 7 are the metallograph with the prepared ZA8-1 alloy sample of the inventive method.
Fig. 8, Fig. 9 are the metallograph with the prepared ZA27--2 alloy sample of the inventive method.
Figure 10 is the metallograph with the prepared ZA22 alloy sample of the inventive method.
Figure 11 is the metallograph with the prepared ZA10 alloy sample of the inventive method.
Embodiment
Below in conjunction with embodiment and Comparative Examples the present invention is described in further detail.
The sample preparation flow process of following all embodiment is: sampling → sample preparation → wet-milling → mechanical buffing → chemical polishing → organization exposure → clean drying up → microscopic examination.
Example one
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on the technical pure zinc ingot metal.Concrete implementation step is as follows:
A. wet-milling: sample through the flat file polishing of serration, is made cooling medium and lubricant with circulating water earlier, carries out mechanical buffing then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 300r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 50ml H
2O
2+ 24ml H
2SO
4+ 2ml CH
3CHOHCOOH+105mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.6g K with cotton
2S
2O
5+ 1.6g Na
2SO
4+ 20gCrO
3+ 85gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 1 is the metallograph of the industrial-purity zinc ingot casting sample of present embodiment preparation, enlargement factor 100 *, on microscope, observe the clear industrial-purity zinc casting gold phase constitution figure that appears, its crystal grain is thicker, because zinc belongs to the close-packed hexagonal crystal structure, slip system is few, therefore is easy to generate twinning deformation under external force, sample produces the pattern of some twins easily at intracrystalline when carrying out mechanical buffing.The zinc that distinct methods is smelted, its dopant species difference, but common impurity is lead, iron, tin, cadmium etc. in the industrial-purity zinc.
Example two
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on the pure zinc sample of superfine.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 300r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 40ml H
2O
2+ 30ml H
2SO
4+ 1ml CH
3CHOHCOOH+130mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.3g K with cotton
2S
2O
5+ 2.0g Na
2SO
4+ 25gCrO
3+ 100gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 2 is the metallograph of superfine pure Zinc material (as cast condition) sample of present embodiment preparation, its enlargement factor is 100 *, as seen from the figure, it is low to observe in the clear superfine pure zinc that appears impurity content on microscope, cast sturcture presents the homogeneous structure pattern, and crystal grain is thick.
Example three
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on ZA4-3 allumen sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 200r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 60ml H
2O
2+ 18ml H
2SO
4+ 3ml CH
3CHOHCOOH+80mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.9g K with cotton
2S
2O
5+ 1.2g Na
2SO
4+ 15gCrO
3+ 70gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 3 is the metallograph of ZA4-3 alloy material (as cast condition) sample of present embodiment preparation, enlargement factor is 100 *.The tissue explanation:
The alloy nominal composition is Zn-3.5～4.5Al-2.5～3.5Cu-0.05～0.1Mg, belongs to cast zinc alloy.Press the analysis of Zn-Al-Cu ternary phase diagram, in its cast sturcture, white dendrite is a Zn based solid solution primary crystal.L → Zn+Al Zn+CuZn takes place in the alloy graining process
3Eutectic reaction, wherein Al Zn → Al (Zn)+Zn (Al)+CuZn takes place in eutectoid temperature in Al Zn compound
3Eutectoid reaction, black part is divided into eutectic mixture, and final phase composition thing is: Zn (Al) solid solution+Al (Zn) solid solution+CuZn
3Compound.
Example four
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on ZA4-1 allumen sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 500r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 55ml H
2O
2+ 20ml H
2SO
4+ 2ml CH
3CHOHCOOH+100mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.6g K with cotton
2S
2O
5+ 1.2g Na
2SO
4+ 17gCrO
3+ 90g H
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 4 is the metallograph of the ZA4-1 aluminium alloy material sample of present embodiment preparation, enlargement factor 250 *, the clear metallographic structure that appears of microscopic examination is: organize the explanation of constituent thing and phase composition fabric texture: this alloy nominal composition is that Zn-3.5-4.5Al-0.75～1.25Cu-0.03～0.08Mg is a cast zinc alloy, and copper content is lower in the alloy.White is zinc solid solution in the tissue, and around the primary crystal is that eutectic mixture is Zn+ZnAl, and ZnAl compound wherein eutectoid again is decomposed into Al (Zn)+Zn (Al)+CuZn
3Eutectoid is the alternate synusia shape of black and white.The last phase composition thing of alloy is Zn (Al)+Al (Zn)+CuZn
3, this alloy flowability is good, good casting property, and mechanical property is good, is widely used in diecast parts, the foundry goods of complicated shape.
Example five
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on the Zn--Cu--Ti alloy sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 300r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 50ml H
2O
2+ 25ml H
2SO
4+ 2ml CH
3CHOHCOOH+100mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.8g K with cotton
2S
2O
5+ 1.5g Na
2SO
4+ 22gCrO
3+ 80gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 5 is the metallograph of Zn--Cu--Ti alloy material (the cold-chamber die casting machine die casting attitude) sample of present embodiment preparation, enlargement factor 250 *, sample is examined under a microscope clear being organized as of appearing: the nominal composition of alloy is Zn-0.55Cu-0.12Ti, belong to typical deformation zinc alloy, white base is the solid solution of Zn under the as cast condition, and there is CuZn in the interdendritic
3Compound, Cu improves intensity and plasticity in the alloy, and Ti is with tiny TiZn
15Distribute mutually, the energy crystal grain thinning, the recrystallization temperature of raising creep-resistant property and alloy, crystal grain is thick when avoiding high temperature to use, and Ti increases the Zn-Cu alloy rigidity.The Zn-Cu-Ti alloy is mainly used in produces plate, also can be used for die casting.
Example six
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on ZA8-1 allumen sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 400r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 50ml H
2O
2+ 25ml H
2SO
4+ 2ml CH
3CHOHCOOH+100mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.5g K with cotton
2S
2O
5+ 1.8g Na
2SO
4+ 18gCrO
3+ 85gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 6 is the metallograph of ZA8--1 aluminium alloy material (swage as cast condition) sample of present embodiment preparation, enlargement factor 100 *, sample is examined under a microscope clear being organized as of appearing: the nominal composition of alloy is: Zn-8.0～8.8Al-0.8～1.3Cu-0.015～0.03Mg, white dendrite are Al based solid solution (solubleness of Zn reaches 82.8%).Black is eutectic mixture Zn (Al)+ZnAl, and wherein the eutectoid decomposition takes place again the ZnAl compound, becomes Al (Zn)+Zn (Al) eutectoid potpourri.Form at last and be mutually: Zn (Al)+Al (Zn).Fig. 7 is the metallograph of ZA8--1 aluminium alloy material (sand mo(u)ld as cast condition) sample of present embodiment preparation, enlargement factor 100 * and, the phase composition thing is identical with Fig. 6.White is Al (Zn) solid solution, and black is the eutectoid potpourri.
Example seven
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on ZA27-2 allumen sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 300r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 48ml H
2O
2+ 25ml H
2SO
4+ 2ml CH
3CHOHCOOH+110mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.6g K with cotton
2S
2O
5+ 1.6g Na
2SO
4+ 20gCrO
3+ 85gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Fig. 8 is the metallograph of Zn27-2 aluminium alloy material (as cast condition) sample of present embodiment preparation, enlargement factor 100 *.The nominal composition of alloy is: Zn-25～28Al-2.0～2.5Cu-0.01～0.02Mg.The white dendrite is Al (Zn) solid solution primary crystal α
1, reduce with temperature, by α
1Decomposite α
2(α
2Still be Al (Zn) solid solution, but wherein the solubleness of Zn increase).α takes place to 275 ℃
2→ α
1+ Zn (Al)+CuZn3 eutectoid reaction.Last phase composition thing is: Zn (Al)+Al (Zn)+CuZn3 three-phase.Fig. 9 is the metallograph of Zn27-2 aluminium alloy material (as cast condition) sample of present embodiment preparation, and the tissue explanation: the phase composition thing is identical with Figure 11.White is Al (Zn) solid solution, and black is the eutectoid potpourri.
Example eight
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on ZA-22 allumen sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 300r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 55ml H
2O
2+ 27ml H
2SO
4+ 2ml CH
3CHOHCOOH+120mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.6g K with cotton
2S
2O
5+ 1.6g Na
2SO
4+ 20gCrO
3+ 85gH
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Figure 10 is the metallograph of ZA-22 aluminium alloy material (as cast condition) sample of present embodiment preparation, enlargement factor 2500 *.The nominal composition of ZA22 alloy is: the Zn-22Al-Cu alloy, and the tiny even eutectoid structure that after organizing granular to handle, obtains, this alloy is tiny even owing to organizing, and has superplasticity.
Example nine
Hacksaw intercepting specification is one of 20mm * 20mm sample by hand on ZA10 allumen sample.Concrete implementation step is as follows:
A. wet-milling: make cooling medium and lubricant with circulating water, sample through the flat file polishing of serration, carries out mechanical buffing earlier then;
B. mechanical buffing: the sample that wet-milling is good places the water that contains washing agent to clean through the ultrasonic vibration washer, carries out mechanical buffing 2～5min: polishing velocity 300r/min then; This moment polishing fluid be cooling medium be again lubricant; To drip granularity be that 0.5 μ m aluminium oxide is called in the suspending liquid that stirs in the water as polishing fluid in spray on the microporous fabrics polishing flannelet, with the sample polishing, examines under a microscope the specimen surface state, confirms to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the effect of chemical polishing is that grey " oxidation film layer " vestige that will generate through the mechanical buffing specimen surface is removed, and the sample that mechanical buffing is good immerses 45ml H
2O
2+ 25ml H
2SO
4+ 2ml CH
3CHOHCOOH+90mlH
2Carry out chemical polishing 1～3 second in the O mixed solution, range estimation treats that through good sample surfaces grey " oxidation film layer " the vestige complete obiteration of mechanical buffing specimen surface presents as bright as a sixpence polished surface and gets final product;
D. organization exposure: the sample good through chemical polishing dips in 0.6g K with cotton
2S
2O
5+ 1.6g Na
2SO
4+ 20gCrO
3+ 85g H
2O mixing etchant is wiped examination etch 5-10 second back and forth gently at sample surfaces, washes clean sample with flowing water, cleans sample with absolute ethyl alcohol then, dries up, and can obtain organizing the clear sample that appears this moment.Figure 11 is the metallograph of the ZA-10 allumen sample specimens of present embodiment preparation, enlargement factor 500 *.As seen in Zn (Al) primary crystal,, solubleness is decomposed into eutectoid at last because of reducing the ZnAl compound of separating out.
Claims (4)
1. preparation of zinc and alloy metallographic specimen thereof and organization exposure method is characterized in that may further comprise the steps:
A. wet-milling: sample through the flat file polishing of serration, is made cooling medium and lubricant with circulating water earlier, carries out mechanical buffing then;
B. mechanical buffing: the sample after the wet-milling is cleaned up, on polishing flannelet, carry out mechanical buffing then, mechanical buffing is that the brilliant polish of 0.3～1.0 μ m is called in the suspending liquid that stirs in the water as polishing fluid with granularity, simultaneously this polishing fluid also be cooling medium be again lubricant, polishing velocity is 200～500r/min, examine under a microscope the specimen surface state, confirm to carry out chemical polishing after the complete obiteration of specimen surface file cut;
C. chemical polishing: the sample that mechanical buffing is good immerses in the chemical brightening solution and carries out chemical polishing, to remove the grey oxidation film layer that generates through the mechanical buffing specimen surface, the complete obiteration of range estimation specimen surface grey oxidation film layer vestige, specimen surface present as bright as a sixpence polished surface and get final product; Chemical brightening solution is by H
2O
2, the concentrated sulphuric acid, CH
3CHOHCOOH and H
2O is 40～60: 18～30 according to volume ratio: 1.0～3.0: 80～130 mixed solutions of forming;
D. organization exposure: dip in cotton through the good sample of chemical polishing and to mix etchant and wipe the examination etch back and forth gently, wash clean sample, clean sample with absolute ethyl alcohol then, dry up, promptly obtain organizing the clear sample that appears with flowing water at sample surfaces; Etchant is by K
2S
2O
5, Na
2SO
4, H
2O and CrO
3According to weight ratio is 0.3～0.9: 1.2～2.0: 70～100: 15～25 mixed solutions of forming.
2. method according to claim 1 is characterized in that described chemical brightening solution is by H
2O
2, the concentrated sulphuric acid, CH
3CHOHCOOH and H
2O is 50: 24: 2.0 according to volume ratio: 105 mixed solutions of forming.
3. method according to claim 1 and 2 is characterized in that described etchant is by K
2S
2O
5, Na
2SO
4, H
2O and CrO
3According to weight ratio is 0.6: 1.6: 85: 20 mixed solutions of forming.
4. method according to claim 1 and 2 is characterized in that described brilliant polish is that granularity is the aluminium oxide of 0.50 μ m.
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| CN102252888B (en) * | 2011-06-30 | 2012-10-10 | 首钢总公司 | Preparation and tissue display method of ultralow carbon ultrathin cold heading steel wire metallographical sample |
| CN102621148B (en) * | 2012-03-14 | 2014-08-27 | 东莞市科力钢铁线材有限公司 | Method for measuring nonmetallic inclusion in steel |
| CN102735520B (en) * | 2012-07-07 | 2014-07-02 | 西部金属材料股份有限公司 | Method for observing metallographic structure on Monel alloy/steel surfacing interface |
| CN102866047A (en) * | 2012-09-28 | 2013-01-09 | 昆明理工大学 | Method for preparing metallographic display sample made of Ti-Al laminated composite material |
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| CN105628479A (en) * | 2015-12-18 | 2016-06-01 | 中国民航大学 | Polishing method aiming at metallographic specimen of of pore-closed type porous material |
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