CN103308355A - Metallographic test sample preparation method of aluminum-based ceramic mould core and silicon-based ceramic mould core - Google Patents
Metallographic test sample preparation method of aluminum-based ceramic mould core and silicon-based ceramic mould core Download PDFInfo
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- CN103308355A CN103308355A CN2012104517111A CN201210451711A CN103308355A CN 103308355 A CN103308355 A CN 103308355A CN 2012104517111 A CN2012104517111 A CN 2012104517111A CN 201210451711 A CN201210451711 A CN 201210451711A CN 103308355 A CN103308355 A CN 103308355A
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Abstract
The invention provides a metallographic test sample preparation method of an aluminum-based ceramic mould core and a silicon-based ceramic mould core. An automatic sampling machine is used for manufacturing metallographic test samples of the aluminum-based ceramic mould core and the silicon-based ceramic mould core through grinding and polishing so as to avoid the defects that the stress on the section of the test samples cannot be controlled in manual operation. Different types of metallographic abrasive paper is selected in rough grinding and fine grinding processes during sample preparation, pressure on the surface of the test samples and test sample preparation time are reasonably controlled, liquid suspended silicon in a test sample preparation process is applied, and a rotary speed value of grinding and an abrasive disc are reasonable controlled to obtain ideal sections of the metallographic test samples of the aluminum-based ceramic mould core and the silicon-based ceramic mould core. The interfaces of the metallographic test samples of the aluminum-based and silicon-based ceramic mould cores are clean and outlines of all combination phases are clear; material base bodies have no obvious stripping phenomena and have no preparation scratches; the metallographic test sample preparation method has the characteristic of simple and feasible preparation method.
Description
Technical field
Present technique is the preparation for ceramic metallographic specimen, specifically for the aluminium base test parameters that provides with the preparation of silicon-base ceramic core metallographic specimen.
Background technology
In the epoch of current scientific and technological high speed development, stupalith has been not only a so-called handicraft among the people, but a science.Because it is subjected to acid and alkali corrosion hardly, non-conductive, hardness is high, and chemical stability is high especially, and is high temperature resistant, ageing-resistant, the characteristics such as radioresistance, and at electronics, aviation, space flight, medical science etc. field more and more comes into one's own, and is widely used.Yet, generally mainly concentrate on its performance, composition, preparation technology's discussion for the research of stupalith, and rare its metallographic structure is inquired into, its basic reason is that stupalith fragility is large, can easily prepare desirable metallographic specimen not as metal material possesses certain toughness like that.But stupalith is in the process of research and development, if can in conjunction with the analysis of metallographic micromechanism, will bring for the research and development of stupalith immeasurable prospect.So how prepare a desirable stupalith metallographic specimen, become we break through this problem primary factor.
Aluminium base and silicon-base ceramic core is China's aeromotor foundry goods core commonly used, in order further to improve the shop characteristic of ceramic core, the author has carried out analysis of experiments to its mechanical property and micromechanism, has obtained a kind of desirable aluminium base and silicon-base ceramic core metallography preparation technology in this process.
In aluminium base, the silica-based ceramic mold core material metallographic specimen preparation process, all be to adopt the machine manual operations to obtain metallographic specimen in the past.Because human factor accounts for leading role, in the preparation process, the stability of sample, the dynamics that sample is controlled in operator's hand, in abrasive paper for metallograph or polishing disk mill, time of throwing, to selection of polishing fluid or antiscuffing paste etc., these factors all affected sample and prepare final mass when sample prepared.
Summary of the invention
Thereby affect the deficiency of sample mass for the effect that overcomes the human factor that exists in the prior art, the present invention proposes the metallographic specimen preparation method of a kind of Al-base ceramic core and silicon-base ceramic core.
Detailed process of the present invention is:
The first step: make sample.Intercept a plurality of samples at the position that the Al-base ceramic material will be observed, and the difference mark, one group of sample obtained.
Second step: the detection faces of determining sample.
The 3rd step: inlay sample.Each sample is put into respectively each metallographic specimen embedding die.
The 4th step: clamping sample.
The 5th step: grinding sample.There are the anchor clamps of each epoxy resin to be installed on the Automatic Grinding Prototype clamping.Start Automatic Grinding Prototype, with varigrained SIC abrasive paper for metallograph sample is carried out grinding.During grinding, the sand paper granularity is from coarse to fine carries out successively.Pressure in the grinding is 3～5Psi/mt.The grinding time of every sand paper is 30～60 seconds.The rotating speed of Automatic Grinding Prototype mill is 250～300RPM.The different grain size of described sand paper is respectively 320#, 500# or 600#, 800#, 1000# or 1200#.
The 6th step: polishing sample.The process of polishing sample is identical with the polishing process of metal metallographic specimen.During rough polishing, adopt the mixed liquor of 6 μ diamond polishing liquids and DP-Lu bricant Blue to polish 1～2 minute.The ratio of described 6 μ diamond polishing liquids and DP-Lu bricant Blue is 1:30.During finishing polish, adopt the mixed liquor of liquid suspension silicon and water as polishing fluid.In the described polishing fluid, the volume ratio of liquid suspension silicon and water is 1:10.Polishing time is 1 minute.When sample was polished, the rotating speed of Automatic Grinding Prototype mill was 300RPM, and polish pressure is 4Psi/mt.
The purpose of the invention provides a kind of reasonable and effective aluminium base, silicon-base ceramic core material microstructure preparation method of sample, obtain desirable microstructure sample interface, provide effective technical guarantee to analysis aluminium base, silica-based ceramic mold core material metallographic micromechanism.
Because stupalith is more crisp, when using hand grinding, easily cause grinding face uneven, produce illusion.But can remedy the impact of application of force inequality by mechanical sample preparation, so that sample is stressed evenly, reduce to greatest extent the breakage rate of specimen surface.Fig. 3 is exactly the good microstructure interface of adopting step of the present invention to obtain.
The present invention is by automatic sample mechanism sample, and the sample of having avoided sample preparation hand-manipulated to produce prepares the stressed uncontrollability in cross section.Select the abrasive paper for metallograph of different model in corase grind and the correct grinding process, and the choosing of polishing fabric in the sample polishing process, so that specimen surface reaches desirable polishing effect.In the preparation process, the utilization of liquid suspension silicon in the pressure of rationally definite specimen surface, sample preparation time, the sample preparation, and the tachometer value of rationally controlling grinding and dumping, be and obtain desirable aluminium base and silicon-base ceramic core metallographic specimen cross section and lay a good foundation.Aluminium base and the silicon-base ceramic core metallographic specimen that the present invention is prepared passes through the metaloscope microexamination, and sample interface is clean, and each forms the sharp outline of phase, and material matrix is without obvious peeling phenomenon, without the preparation cut.The present invention provides reliable guarantee for aluminium base and silica-based ceramic mold core material metallographic structure Micro-Structure Analysis, and has simple, workable characteristics.
Description of drawings
Fig. 1 is that Automatic Grinding Prototype prepares the metallographic structure of Al-base ceramic core under pressure 3Psi/mt; Wherein Fig. 1 a be Al-base ceramic 50 *; Fig. 1 b be Al-base ceramic 200 *;
Fig. 2 is that Automatic Grinding Prototype prepares the silicon-base ceramic core metallographic structure under pressure 4Psi/mt; Wherein Fig. 2 a be silicon based ceramic 50 *, Fig. 2 ab be silicon based ceramic 200 *;
Fig. 3 is the good aluminium base and silicon based ceramic metallographic structure that technology of preparing of the present invention obtains, and wherein: Fig. 3 a is Al-base ceramic core microstructure; Fig. 3 b is the silicon-base ceramic core microstructure;
Fig. 4 is process flow diagram of the present invention.
Embodiment
Embodiment one
The present embodiment is the method that a kind of stupalith is prepared into the microstructure sample.Described stupalith is the Al-base ceramic core that aero engine turbine blades DZ125 uses.The detailed process of the present embodiment is:
The first step: make sample.Intercept a plurality of samples at the position that the Al-base ceramic core material will be observed, and the difference mark, one group of sample obtained.In the present embodiment, the quantity of sample is 5.
Second step: the detection faces of determining sample.With the surface of opposed flattened in two surfaces of each sample of the intercepted detection faces as this sample.
The 3rd step: inlay sample.Each sample is put into respectively each metallographic specimen embedding die.According to a conventional method, use epoxy resin: dibutyl phthalate: agent is inlayed in the ethylenediamine preparation; Described epoxy resin: dibutyl phthalate: the mass ratio of ethylenediamine is 100:18:10.The agent of inlaying that obtains is poured in the metallographic specimen embedding die that each sample is housed, and with mould leave standstill solidify fully to epoxy resin till, by inlaying agent that each sample in the mould is fastening, sample is contacted closely with inlaying material, be convenient to mechanical grinding.
The 4th step: clamping sample.After epoxy resin in each metallographic specimen embedding die solidifies fully, each epoxy resin is taken out from metallographic specimen embedding die separately, and clamping, be fixed tightly on the anchor clamps of Automatic Grinding Prototype.Make the abrasive surface of each epoxy resin be in same level in the clamping.
The 5th step: grinding sample.There are the anchor clamps of each epoxy resin to be installed on the Automatic Grinding Prototype clamping.The head model that described Automatic Grinding Prototype adopts Denmark stuers company to produce is TegraForc-5, and the base model is the Automatic Grinding Prototype of TegraPol-35.Start Automatic Grinding Prototype, with varigrained sand paper sample is carried out grinding.During grinding, the sand paper granularity is from coarse to fine carries out successively.The different grain size of described sand paper is respectively 320#, 500# or 600#, 800#, 1000# or 1200#.Described sand paper is the SIC abrasive paper for metallograph.Pressure in the grinding is 3～5Psi/mt; The grinding time of every sand paper is 30～60 seconds; The rotating speed of Automatic Grinding Prototype mill is 250～300RPM.The different grain size of sand paper described in the present embodiment is respectively 320#, 500#, 800#, 1200#; Pressure in the grinding is 3Psi/mt; The grinding time of every sand paper is 30 seconds; The rotating speed of Automatic Grinding Prototype mill is 300RPM.
The 6th step: polishing sample.During the polishing sample, according to the process that the metal metallographic specimen is polished,, as polishing cloth the sample through grinding is polished with the woollen cloth of undercoat, to remove the residual polishing scratch of specimen surface abrasive paper for metallograph, make it reach desirable polishing effect.The process of polishing sample comprises rough polishing and finishing polish.
During rough polishing, adopt the mixed liquor of 6 μ diamond polishing liquids and DP-Lu bricant Blue to polish 2 minutes; The ratio of described 6 μ diamond polishing liquids and DP-Lu bricant Blue is 1:30.Described DP-Lu bricant Blue is the polishing additive that Denmark stuers company produces.
Change polishing cloth, carry out finishing polish; When carrying out finishing polish, adopt the mixed liquor of liquid suspension silicon and water as polishing fluid; In the described polishing fluid, the volume ratio of liquid suspension silicon and water is 1:10.Polishing time is 1 minute.The liquid suspension silicon of described polishing usefulness all adopts the product of stuers company.
When sample was polished, the rotating speed of Automatic Grinding Prototype mill was 300RPM, and polish pressure is 3Psi/mt.
The 7th step: sample cleans.Adopt alcohol to clean polishing complete sample, and dry with hair dryer.Obtain the metallographic specimen of Al-base ceramic core.
Metallographic specimen to the Al-base ceramic core that obtains under metaloscope is observed, and it is organized as shown in Figure 1a.
Embodiment two
The present embodiment is the method that a kind of stupalith is prepared into the microstructure sample.Described stupalith is the silicon-base ceramic core that aero engine turbine blades DD6 uses.The detailed process of the present embodiment is:
The first step: make sample.Intercept a plurality of samples at the position that the silica-based ceramic mold core material will be observed, and the difference mark, one group of sample obtained.In the present embodiment, the quantity of sample is 5
Second step: the detection faces of determining sample.With the surface of opposed flattened in two surfaces of each sample of the intercepted detection faces as this sample.
The 3rd step: inlay sample.Each sample is put into respectively each metallographic specimen embedding die.According to a conventional method, use epoxy resin: dibutyl phthalate: agent is inlayed in the ethylenediamine preparation; Described epoxy resin: dibutyl phthalate: the mass ratio of ethylenediamine is 100:18:10.The agent of inlaying that obtains is poured in the metallographic specimen embedding die that each sample is housed, and with mould leave standstill solidify fully to epoxy resin till, by inlaying agent that each sample in the mould is fastening, sample is contacted closely with inlaying material, be convenient to mechanical grinding.
The 4th step: clamping sample.After epoxy resin in each metallographic specimen embedding die solidifies fully, each epoxy resin is taken out from metallographic specimen embedding die separately, and clamping, be fixed tightly on the anchor clamps of Automatic Grinding Prototype.Make the abrasive surface of each epoxy resin be in same level in the clamping.
The 5th step: grinding sample.There are the anchor clamps of each epoxy resin to be installed on the Automatic Grinding Prototype clamping.The head model that described Automatic Grinding Prototype adopts stuers company to produce is TegraForc-5, and the base model is the Automatic Grinding Prototype of TegraPol-35.Start Automatic Grinding Prototype, with varigrained sand paper sample is carried out grinding.During grinding, the sand paper granularity is from coarse to fine carries out successively.The different grain size of described sand paper is respectively 320#, 500# or 600#, 800#, 1000# or 1200#.Described sand paper is the SIC abrasive paper for metallograph.Pressure in the grinding is 3～5Psi/mt; The grinding time of every sand paper is 30～60 seconds; The rotating speed of Automatic Grinding Prototype mill is 250～300RPM.The different grain size of sand paper described in the present embodiment is respectively 320#, 600#, 800#, 1200#; Pressure in the grinding is 4Psi/mt; The grinding time of every sand paper is 30 seconds; The rotating speed of Automatic Grinding Prototype mill is 300RPM.
The 6th step: polishing sample.During the polishing sample, according to the process that the metal metallographic specimen is polished,, as polishing cloth the sample through grinding is polished with the woollen cloth of undercoat, to remove the residual polishing scratch of specimen surface abrasive paper for metallograph, make it reach desirable polishing effect.The process of polishing sample comprises rough polishing and finishing polish.
During rough polishing, adopt the mixed liquor of 6 μ diamond polishing liquids and DP-Lu bricant Blue to polish 1～2 minute; The ratio of described 6 μ diamond polishing liquids and DP-Lu bricant Blue is 1:30.In the present embodiment, polishing is to be 2 minutes.Described DP-Lu bricant Blue is the polishing additive that Denmark stuers company produces.
Change polishing cloth, carry out finishing polish; When carrying out finishing polish, adopt the mixed liquor of liquid suspension silicon and water as polishing fluid; In the described polishing fluid, the volume ratio of liquid suspension silicon and water is 1:10.Polishing time is 1 minute.The liquid suspension silicon of described polishing usefulness all adopts the product of stuers company.
When sample was polished, the rotating speed of Automatic Grinding Prototype mill was 300RPM, and polish pressure is 4Psi/mt.
The 7th step: sample cleans.Adopt alcohol to clean polishing complete sample, and dry with hair dryer.Obtain the metallographic specimen of silicon-base ceramic core.
Metallographic specimen to the silicon-base ceramic core that obtains under metaloscope is observed, and its tissue is shown in Fig. 1 b.
Claims (2)
1. the metallographic specimen preparation method of an Al-base ceramic core and silicon-base ceramic core is characterized in that, detailed process is:
The first step: make sample; Intercept a plurality of samples at the position that the Al-base ceramic material will be observed, and the difference mark, one group of sample obtained;
Second step: the detection faces of determining sample;
The 3rd step: inlay sample; Each sample is put into respectively each metallographic specimen embedding die;
The 4th step: clamping sample;
The 5th step: grinding sample; There are the anchor clamps of each epoxy resin to be installed on the Automatic Grinding Prototype clamping; Start Automatic Grinding Prototype, with varigrained SIC abrasive paper for metallograph sample is carried out grinding; During grinding, the sand paper granularity is from coarse to fine carries out successively; Pressure in the grinding is 3～5Psi/mt; The grinding time of every sand paper is 30～60 seconds; The rotating speed of Automatic Grinding Prototype mill is 250～300RPM;
The 6th step: polishing sample; The process of polishing sample is identical with the polishing process of metal metallographic specimen; During rough polishing, adopt the mixed liquor of 6 μ diamond polishing liquids and DP-Lu bricant Blue to polish 1～2 minute; The ratio of described 6 μ diamond polishing liquids and DP-Lu bricant Blue is 1:30; During finishing polish, adopt the mixed liquor of liquid suspension silicon and water as polishing fluid; In the described polishing fluid, the volume ratio of liquid suspension silicon and water is 1:10; Polishing time is 1 minute; When sample was polished, the rotating speed of Automatic Grinding Prototype mill was 300RPM, and polish pressure is 4Psi/mt.
2. the metallographic specimen preparation method of Al-base ceramic core and silicon-base ceramic core as claimed in claim 1 is characterized in that, the different grain size of described sand paper is respectively 320#, 500# or 600#, 800#, 1000# or 1200#.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103624657A (en) * | 2013-11-28 | 2014-03-12 | 潘刚 | Wet-type mirror face grinding and polishing method |
| CN104251792A (en) * | 2014-08-19 | 2014-12-31 | 格力电器（合肥）有限公司 | Method for detecting dark cracks in surface mount capacitor |
| CN104669071A (en) * | 2015-01-22 | 2015-06-03 | 湖南大学 | Composite material grinding and polishing technology |
| CN105277399A (en) * | 2014-07-02 | 2016-01-27 | 西安航空动力股份有限公司 | Preparation method of TiAl penetrating layer metallographic specimen |
| CN104251792B (en) * | 2014-08-19 | 2017-01-04 | 珠海格力电器股份有限公司 | The detection method secretly split inside patch capacitor |
| CN107860637A (en) * | 2017-11-09 | 2018-03-30 | 中国航发贵州黎阳航空动力有限公司 | A kind of preparation method of spring-like part metallographic specimen |
| CN108458914A (en) * | 2018-03-20 | 2018-08-28 | 苏州欧睿检测技术有限公司 | A kind of metallographic specimen method for embedding |
| CN109946130A (en) * | 2019-03-14 | 2019-06-28 | 珠海凯利得新材料有限公司 | A kind of preparation method of micrometer level porous ceramic metallographic specimen |
| CN111397987A (en) * | 2020-04-21 | 2020-07-10 | 广州领拓仪器科技有限公司 | Method for manufacturing concrete metallographic specimen |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103624657A (en) * | 2013-11-28 | 2014-03-12 | 潘刚 | Wet-type mirror face grinding and polishing method |
| CN103624657B (en) * | 2013-11-28 | 2016-04-13 | 深圳市泽米诺科技有限公司 | The method of a kind of wet type mirror ultrafinish polishing |
| CN105277399A (en) * | 2014-07-02 | 2016-01-27 | 西安航空动力股份有限公司 | Preparation method of TiAl penetrating layer metallographic specimen |
| CN104251792A (en) * | 2014-08-19 | 2014-12-31 | 格力电器（合肥）有限公司 | Method for detecting dark cracks in surface mount capacitor |
| CN104251792B (en) * | 2014-08-19 | 2017-01-04 | 珠海格力电器股份有限公司 | The detection method secretly split inside patch capacitor |
| CN104669071A (en) * | 2015-01-22 | 2015-06-03 | 湖南大学 | Composite material grinding and polishing technology |
| CN107860637A (en) * | 2017-11-09 | 2018-03-30 | 中国航发贵州黎阳航空动力有限公司 | A kind of preparation method of spring-like part metallographic specimen |
| CN108458914A (en) * | 2018-03-20 | 2018-08-28 | 苏州欧睿检测技术有限公司 | A kind of metallographic specimen method for embedding |
| CN109946130A (en) * | 2019-03-14 | 2019-06-28 | 珠海凯利得新材料有限公司 | A kind of preparation method of micrometer level porous ceramic metallographic specimen |
| CN111397987A (en) * | 2020-04-21 | 2020-07-10 | 广州领拓仪器科技有限公司 | Method for manufacturing concrete metallographic specimen |
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Application publication date: 20130918 |