CN1912570A - Method for analysing metallographic structure in aluminium alloy - Google Patents

Method for analysing metallographic structure in aluminium alloy Download PDF

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CN1912570A
CN1912570A CN 200610127317 CN200610127317A CN1912570A CN 1912570 A CN1912570 A CN 1912570A CN 200610127317 CN200610127317 CN 200610127317 CN 200610127317 A CN200610127317 A CN 200610127317A CN 1912570 A CN1912570 A CN 1912570A
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aluminium alloy
alloy
phase
electrolytic solution
aluminium
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赵群
任智森
张英
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Aluminum Corp of China Ltd
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Aluminum Corp of China Ltd
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Abstract

A method for analyzing metallographic structure in aluminium alloy includes using aluminium alloy test piece as positive electrode and stainless steel plate as negative electrode as well as citric acid as electrolyte, carrying out electrolysis reaction on aluminum alloy test piece, entering pure aluminium in aluminium alloy into electrolyte after reaction, falling the second phase in alloy into electrolyte by particle state, filtering electrolyte, analyzing solid separated matter after washing and drying to obtain 3D information of the second phase in aluminium alloy.

Description

A kind of method of analyzing metallographic structure in the aluminium alloy
Technical field
A kind of method of analyzing metallographic structure in the aluminium alloy relates to and is used for analyzing aluminium alloy second phase method.
Background technology
Aluminium is the metal that is most widely used except that iron and steel, has that it is in light weight, specific strength is high, characteristics such as corrosion-resistant and easy recovery, and is also more and more deep for the research of aluminium alloy.By traditional method aluminum alloy materials is carried out fabric analysis, to carry out sample preparation earlier, employing is thick, fine sandpaper grinds off all corase grind traces of specimen surface, again on buffing machine respectively with chrome green slightly throw, fine grained is carefully thrown and superfine aluminium oxide powder is smart throws, some aluminum alloy specimen also needs to carry out electropolishing.The sample that makes is observed at microscopically, can observe second phase in the alloy, as metallic compound, eutectic phase, hypereutectic phase and be mingled with etc.
Because what sample preparation was had to is a plane of alloy, observed image is a plane of material internal also, and what obtain is two-dimensional signal.And material inside organization special second is three-dimensional mutually, so its three-dimensional information can't obtain by classic method, if as second being sheet mutually, classic method is observed just may to be strip, sheet or bulk, can't determine.In addition, in sample making course, because aluminum substrate is softer, some second phase hardness is big, little with the adhesion of aluminum substrate, easily comes off from material in polishing process, therefore is difficult for being observed.Particularly in the polishing process, embed polishing particles at specimen surface in the aluminium alloy sample preparation easily, as alundum (Al, the result produces interference to metallographic examination.
AlTiB is present most popular aluminum grain refiner, and application technology is very ripe, but has dispute for its mechanism of action always, in it and TiB 2The existing way of two-phase and interaction are very unclear always, and Al 3The shape and size of Ti have very big influence to the action effect of grain refiner.By traditional metallographic examination method, can observe distribution and the size of the second phase particle in aluminum substrate, determine but its shape is bad.As shown in Figure 1, it is particle or sheet that the polygon second among the figure be difficult to be judged mutually, and the strong or sheet that might be pin mutually of the rod-short second among the figure owing to can only observe a plane of second phase, is therefore brought difficulty to judgement.
The AlTiC grain refiner is the New Refiners of developing recent years, because it has remedied poisoning and aggregation phenomenon that the AlTiB grain refiner in use exists in theory, therefore promises to be the substitute of AlTiB grain refiner.It is so desirable that the grain refining effect of AlTiC is not estimated, little with the grain refining effect difference of AlTiB, do not embody its due advantage but in actual use.Therefore, need carry out deep research to the mechanism of action of AlTiC grain refiner.Fig. 3 is the metallograph of AlTiC bar, and second in the pattern that can observe second phase that exists in the matrix and Figure 1A lTiB bar do not have marked difference mutually, and its mechanism of action relatively caused difficulty.
The Al-Si alloy is a kind of very important Birmasil, and hypereutectic Al-Si is applied to fields such as piston of automobile owing to its good intensity and anti-wear performance, and range of application enlarges gradually.Thing basic composition is α-Al phase, Eutectic Silicon in Al-Si Cast Alloys and primary silicon mutually mutually in the hypereutectic Al-Si alloy, in Fig. 5, be the Eutectic Silicon in Al-Si Cast Alloys that is of needle-like, and be the granular primary silicon that is, and the form of α-Al phase is not really clear, and relatively difficulty is observed also in the corrosion back.
Summary of the invention
The objective of the invention is to analyze the problem that exists in the second phase process in the aluminium alloy at traditional metallographic method, propose the method for metallographic structure in a kind of analysis aluminium alloy of the three-dimensional information of the second phase particle in the aluminum alloy specimen effectively being observed, accurately obtained second phase in the aluminium alloy at above-mentioned prior art.
To achieve these goals, the present invention realizes by the following technical solutions.
A kind of method of analyzing metallographic structure in the aluminium alloy, it is characterized in that its analytic process is is electrolytic solution with aluminum alloy specimen for positive pole, stainless steel substrates negative pole, citric acid solution, aluminum alloy specimen is carried out electrolytic reaction, enter electrolytic solution after the fine aluminium reaction in the aluminium alloy, in the alloy second falls into electrolytic solution with graininess, filter electrolytic solution, fully the dry back of washing is analyzed the solid separator, obtains the three-dimensional information of second phase in the aluminium alloy.
Method of the present invention is characterized in that the electrolyte weight composition that adopts is 15%~45% citric acid, 1%~4% hydrochloric acid, and surplus is a water.
Method of the present invention is characterized in that the operating voltage of the electrolysis adopted is 5~20V.
Method of the present invention is characterized in that it is to adopt SEM or XRD method that the solid separator is analyzed.
Method of the present invention, with aluminum alloy specimen is anodal, the stainless steel substrates negative pole, citric acid solution is an electrolytic solution, aluminum alloy specimen is carried out electrolytic reaction, enter electrolytic solution after the fine aluminium reaction in the aluminium alloy, in the alloy second falls into electrolytic solution with graininess, suitably add hydrochloric acid or sulfuric acid, connect direct current, the anode aluminum alloy specimen is dissolved fast, filter electrolytic solution and obtain undissolved solid phase in the aluminium alloy, fully the dry back of washing is analyzed solid extract, and method is identical with analysed for powder, comprise SEM, means such as XRD obtain the three-dimensional information of second phase in the aluminium alloy.
Method of the present invention is applicable to second phase of research in the aluminium alloy, is particularly suitable for that size is less in the aluminium alloy, hardness is higher, distributes than the research of compound between dissipated metal.
Owing to adopted technique scheme, method of the present invention can realize the feature of second phase in the aluminium alloy is carried out three-dimensional description.Adopt method of the present invention can access size, shape, existence and the three-dimensional information of second phase in the aluminium alloy, make the understanding of second phase in the aluminium alloy more comprehensive.
Method of the present invention is applicable to second phase of analyzing in the aluminium alloy, comprises binary or mutually polynary and intermetallic compound that elements such as Al and Mg, Si, Cu, Mn, Fe, Ti, Zr, Zn, RE are formed, or the compound of forming with elements such as B, C mutually.Be particularly suitable in aluminium alloy in traditional sample making course because softer and caducous small crisply study firmly mutually of aluminum substrate, as TiB 2, the TiC phase.Utilize fine aluminium phase good electric conductivity and other difference mutually in the aluminium alloy, make the optimum solvation of fine aluminium phase.Electrolytic solution uses the more weak organic acid of aluminium alloy dissolubility is main body, as citric acid, regulates the dissolubility of electrolytic solution to aluminium alloy by adding mineral acid example hydrochloric acid or sulfuric acid.The granular substance that extracts in the aluminium alloy is adopted the research method identical with powder body material mutually, as methods such as metaloscope, SEM, XRD, obtain the information of each thing phase in the aluminium alloy that classic method can't obtain, comprise the information of three dimensional shapes, size and part existence.
Description of drawings
The metallograph of Fig. 1 AlTiB bar;
The pattern of second phase in the AlTiB bar that Fig. 2 embodiment 1 obtains;
Fig. 3 AlTiC bar metallograph
Second phase in the AlTiC bar that Fig. 4 embodiment 2 obtains;
Fig. 5 transcocrystallized Al-Si alloy metallograph;
Second phase of Al-18Si in the hypereutectic Al-Si that Fig. 6-1 embodiment 3 obtains;
Second phase of A390 in the hypereutectic Al-Si that Fig. 6-2 embodiment 3 obtains.
Embodiment
A kind of method of analyzing metallographic structure in the aluminium alloy, it is characterized in that its analytic process is is electrolytic solution with aluminum alloy specimen for positive pole, stainless steel substrates negative pole, citric acid solution, the electrolyte weight composition is 15%~45% citric acid, 1%~4% hydrochloric acid, and surplus is a water; Aluminum alloy specimen is carried out electrolytic reaction, and the operating voltage of electrolysis is 5~20V; Enter electrolytic solution after the reaction of fine aluminium in the aluminium alloy, second in the alloy falls into electrolytic solution with graininess, filters electrolytic solution, fully wash drying after, employing SEM or XRD method are analyzed the solid separator, obtain the three-dimensional information of second phase in the aluminium alloy.
Below by specific embodiment method of the present invention is described further.
Embodiment 1
Analyze the metallographic structure of AlTiB aluminum alloy specimen; The AlTiB bar of the long 3cm of one joint is steady with the wire clamp folder, connect positive pole; Negative pole connects a L type stainless steel substrates, uses stabilized voltage supply, operating voltage 20V; Electrolyte weight is than the hydrochloric acid+H that consists of 45% citric acid+1% 2O (surplus), ambient operation.During the beginning electrolysis voltage is increased gradually, keep stable pole span, the dissolution velocity of aluminium is relevant with electrolytic solution liquid composition with voltage.With electrolyte filtering, with the residue on hot water injection's filter paper, repeatedly washing back band filter paper took out after electrolysis finished, and the back sample analysis is done in 50~70 ℃ of roars of laughter in baking oven.The granular that obtains is carried out XRD analysis, prove that exist in the particulate samples is TiB 2And Al 3The Ti phase.By the pattern of SEM observation particle, can find to exist fibrous AlTi phase, be petal-shaped on a small quantity, most AlTi exists mutually in the form of sheets, is shaped as fairly regular square (see figure 2).
Embodiment 2
Analyze the metallographic structure of AlTiC aluminum alloy specimen; The AlTiC bar of one joint 2cm is steady with the wire clamp folder, connect positive pole; Negative pole connects a L type stainless steel substrates, uses stabilized voltage supply, and Control of Voltage is at 5V; The electrolyte weight ratio consists of: the hydrochloric acid+H of 15% citric acid+3% 2O (surplus), experiment is at room temperature carried out.When electrolysis begins voltage is slowly increased, and keeps stable pole span, fine aluminium under electrochemical action with the electrolytic solution preferential reaction, its dissolution velocity is relevant with voltage and bath composition.With electrolyte filtering, be not higher than the residue on hot water injection's filter paper of 80 ℃ with temperature after electrolysis finishes, repeatedly washing back band filter paper takes out, and the back sample analysis are done in 50~70 ℃ of roars of laughter in baking oven.The granular that obtains is carried out XRD analysis, prove that exist in the particulate samples is Al 3The Ti phase.By the pattern of SEM observation particle, can find to exist cubic granular AlTi phase, and not have fibrous and petal-like AlTi; Observe by metaloscope, most AlTi exists mutually in the form of sheets, is shaped as the comparatively square of rule, and what be the black cubic shape should be TiC particle (see figure 4).
Embodiment 3
Analyze the hypereutectic Al-Si aluminum alloy specimen, be cut into the square that length is 3cm, surely connect positive pole with the wire clamp folder with consisting of the Al-18Si alloy; Negative pole connects a L type stainless steel substrates, uses stabilized voltage supply, and Control of Voltage is at 15V; The electrolyte weight ratio consists of: the hydrochloric acid+H of 20% citric acid+4% 2O (surplus), ambient operation.When electrolysis begins voltage is slowly increased, just observe a large amount of particles and separate out and sink to electrolytic cell bottom very soon from anode.With electrolyte filtering, with the residue on hot water injection's filter paper, repeatedly washing back band filter paper took out after electrolysis finished, and the back sample analysis is done in 50~70 ℃ of roars of laughter in baking oven.Fig. 6-1 can find almost not have the particle of needle-like to exist for by the observed granule-morphology of metaloscope, therefore concludes that the shape of the Eutectic Silicon in Al-Si Cast Alloys in the alloy should be sheet.The particle of observing regular shape should be primary silicon, and primary silicon forms by a plurality of grain growths together, and on-monocrystalline.
Embodiment 4
Analyze the hypereutectic Al-Si aluminum alloy specimen, trade mark alloy A 390 is cut into the square that length is 2cm, surely connect positive pole with the wire clamp folder; Negative pole connects a L type stainless steel substrates, uses stabilized voltage supply, and Control of Voltage is at 10V; Electrolytic solution consists of: the hydrochloric acid+H of 30% citric acid+2% 2O (surplus), ambient operation.When electrolysis begins voltage is slowly increased, just observe a large amount of particles and separate out and sink to electrolytic cell bottom very soon from anode.With electrolyte filtering, with the residue on hot water injection's filter paper, repeatedly washing back band filter paper took out after electrolysis finished, and the back sample analysis is done in 50~70 ℃ of roars of laughter in baking oven.Fig. 6-2 can find almost not have the particle of needle-like to exist for by the observed granule-morphology of metaloscope, therefore concludes that the shape of the Eutectic Silicon in Al-Si Cast Alloys in the alloy should be sheet.The particle of observing regular shape should be primary silicon, and primary silicon forms by a plurality of grain growths together, and on-monocrystalline.
Embodiment 5
Granule-morphology in contrast Al-18Si alloy and the trade mark alloy A 390 can be found, remove with the Al-18Si alloy in outside the identical Eutectic Silicon in Al-Si Cast Alloys and primary silicon, the second phase kind is more among the A390, the color differential responses go out the difference of its chemical constitution, and are mostly to have a large amount of granules reunions agglomerate of formation together.Can also obtain more information by means such as SEM and XRD.

Claims (4)

1. method of analyzing metallographic structure in the aluminium alloy, it is characterized in that its analytic process is is electrolytic solution with aluminum alloy specimen for positive pole, stainless steel substrates negative pole, citric acid solution, aluminum alloy specimen is carried out electrolytic reaction, enter electrolytic solution after the fine aluminium reaction in the aluminium alloy, in the alloy second falls into electrolytic solution with graininess, filter electrolytic solution, fully the dry back of washing is analyzed the solid separator, obtains the three-dimensional information of second phase in the aluminium alloy.
2. method according to claim 1 is characterized in that the electrolyte weight composition that adopts is 15%~45% citric acid, 1%~4% hydrochloric acid, and surplus is a water.
3. method according to claim 1 is characterized in that the operating voltage of the electrolysis adopted is 10~20V.
4. method according to claim 1 is characterized in that it is to adopt SEM or XRD method that the solid separator is analyzed.
CN 200610127317 2006-09-14 2006-09-14 Method for analysing metallographic structure in aluminium alloy Pending CN1912570A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
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CN101545887A (en) * 2008-03-28 2009-09-30 中国科学院金属研究所 Quantitative analysis method for boride
CN102798591A (en) * 2012-07-31 2012-11-28 沈阳黎明航空发动机(集团)有限责任公司 Metallographic detection method for flame sprayed NiCrAl/NiC coating
CN103048325A (en) * 2011-10-13 2013-04-17 沈阳黎明航空发动机(集团)有限责任公司 Metallographic evaluation method for quality of plasma spraying NiCrAl coating
CN103048324A (en) * 2011-10-13 2013-04-17 沈阳黎明航空发动机(集团)有限责任公司 Metallographic evaluation method for quality of plasma spraying CoCrW coating
CN103093231A (en) * 2012-12-20 2013-05-08 刘冰滨 Automatic identification and quantitative analysis method of second phase in alloy
CN104458372A (en) * 2014-11-28 2015-03-25 内蒙古包钢钢联股份有限公司 Sample preparation method of mixed material containing soft metal
CN104928519A (en) * 2015-07-07 2015-09-23 内蒙古科技大学 Method for extracting second phase in Al-Mg-Si system aluminum alloy
CN106248704A (en) * 2016-07-21 2016-12-21 国网河北省电力公司电力科学研究院 A kind of micro-grain size of fine aluminium and morphologic observation method
CN110579501A (en) * 2019-09-27 2019-12-17 苏州大学 Method for extracting three-dimensional shape of aluminum alloy phase
CN115772601A (en) * 2022-11-30 2023-03-10 立中四通轻合金集团股份有限公司 Aluminum-based intermediate alloy second-phase particle extracting agent and method for obtaining second-phase particles

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101545887A (en) * 2008-03-28 2009-09-30 中国科学院金属研究所 Quantitative analysis method for boride
CN101545887B (en) * 2008-03-28 2013-07-10 中国科学院金属研究所 Quantitative analysis method for boride
CN103048325A (en) * 2011-10-13 2013-04-17 沈阳黎明航空发动机(集团)有限责任公司 Metallographic evaluation method for quality of plasma spraying NiCrAl coating
CN103048324A (en) * 2011-10-13 2013-04-17 沈阳黎明航空发动机(集团)有限责任公司 Metallographic evaluation method for quality of plasma spraying CoCrW coating
CN102798591A (en) * 2012-07-31 2012-11-28 沈阳黎明航空发动机(集团)有限责任公司 Metallographic detection method for flame sprayed NiCrAl/NiC coating
CN103093231A (en) * 2012-12-20 2013-05-08 刘冰滨 Automatic identification and quantitative analysis method of second phase in alloy
CN103093231B (en) * 2012-12-20 2015-08-05 刘冰滨 The automatic identification of second-phase and quantitative analysis method in a kind of alloy
CN104458372A (en) * 2014-11-28 2015-03-25 内蒙古包钢钢联股份有限公司 Sample preparation method of mixed material containing soft metal
CN104928519A (en) * 2015-07-07 2015-09-23 内蒙古科技大学 Method for extracting second phase in Al-Mg-Si system aluminum alloy
CN106248704A (en) * 2016-07-21 2016-12-21 国网河北省电力公司电力科学研究院 A kind of micro-grain size of fine aluminium and morphologic observation method
CN110579501A (en) * 2019-09-27 2019-12-17 苏州大学 Method for extracting three-dimensional shape of aluminum alloy phase
CN115772601A (en) * 2022-11-30 2023-03-10 立中四通轻合金集团股份有限公司 Aluminum-based intermediate alloy second-phase particle extracting agent and method for obtaining second-phase particles

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