CN103900878B - A kind of electrical steel conduction preparation method of metallographic sample - Google Patents
A kind of electrical steel conduction preparation method of metallographic sample Download PDFInfo
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- CN103900878B CN103900878B CN201410108554.3A CN201410108554A CN103900878B CN 103900878 B CN103900878 B CN 103900878B CN 201410108554 A CN201410108554 A CN 201410108554A CN 103900878 B CN103900878 B CN 103900878B
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Abstract
A kind of electrical steel conduction preparation method of metallographic sample, its preparation process is as follows:Stamping-out polishing sample; 2. prepare conductive electrode; 3. paste conductive tape; 4. inlay. A kind of electrical steel conduction preparation method of metallographic sample provided by the invention, its advantage is: prepare easy, quick, cost is low, consistent reliable, do not need to use Special Equipment, in common lab, can complete, the sample after inlaying can carry out electrochemical polish and metallographic, SEM and EBSD analytical test.
Description
Technical field
The present invention relates to electrical steel technical field of metallographic sample preparation, specifically a kind of electrical steel conduction preparation method of metallographic sample.
Background technology
Electrical steel is widely used on the various equipments such as transformer, generator, motor, choke coil, electromagnetic mechanism, relay, measuring instrument, is the soft magnetic materials of consumption maximum in engineering. Electrical steel is divided into hot rolling and cold rolling two classes, and hot rolling electrical steel is because electromagnetic performance is poor, loss is large, substantially superseded. Electrical steel is divided into oriented electric silicon steel by grain orientation difference and without oriented electric silicon steel, grain orientation distributes and microscopic structure is the important technology index of electrical steel, and the preparation of analytic sample affects to a great extent electrical steel grain orientation and distributes and microscopic examination result.
The thickness of electrical steel is generally all between 0.2 ㎜～0.5 ㎜, the thickest 0.7 ㎜ that is no more than, therefore, while preparing the analysis and observation such as metallographic and ESEM and EBSD sample, first all to inlay, to sample is carried out to the pre-treatments such as follow-up pre-grinding, polishing, corrosion, for ensuing analysis provides satisfactory sample. Electrochemical polish requires sample conduction, using sample as anode, makes it and form closed electrolysis loop in electrolyte and between the negative electrode of insoluble petal composition. When connect sample (anode) and negative electrode between power supply time, between anode and cathode, there is electric current to pass through, thereby the microscopic protrusions part generation selective dissolution that anode is polished sample surfaces forms smooth surface, make sample surfaces become gradually smooth, final acquisition is suitable for the sample surfaces that metallographic and ESEM and EBSD etc. analyze. Therefore, conduction is the precondition of electrical steel metallographic and ESEM and EBSD analytic sample.
At present, the preparation method of electrical steel conducting sample has: 1. conductive mosaic material method. This method is, sample is put on pointing machine, pours appropriate conductive mosaic material into, applies the pressure of regulation and is heated to uniform temperature (being generally 150 DEG C～250 DEG C), keeps, after a period of time, after cool to room temperature, taking out. The shortcoming of this method is: when 1. sample heats, the tissue of material change in various degree can occur, impact analysis result. 2. the sample preparation time longer, sample needs about one hour, is unfavorable for preparation in batches. 3. conductive mosaic material itself also can react with electrolyte, affects the electrochemical polish effect of sample. 4. inlay price is higher. 2. boring method. Sample adopts the various non-conducting materials such as epoxy resin to inlay, when electrochemical polish, in the boring energising of the back of inlaying samples. The shortcoming of this method is, 1. because electrical steel sample is thinner, generally all between 0.2 ㎜～0.5 ㎜, and there is again one deck coatings on surface, operates more difficult, and success rate is not high. 2. the residual electrolyte and the follow-up corrosive liquid that immerse between inlay and sample gap are difficult for cleaning out, and easily cause sample corrosion and contamination analysis instrument.
Summary of the invention
The object of this invention is to provide a kind of easy, quick, with low cost, reliable and stable electrical steel conduction preparation method of metallographic sample.
A kind of electrical steel conduction preparation method of metallographic sample provided by the invention, its step is as follows:
(1) stamping-out polishing sample: it is the disk of φ 23 ㎜ that sample stamping-out is become to diameter, with polish a gently surface of sample of 180Cw carborundum paper or file, removing insulating coating, expose substrate metal gloss and be limited, the area of polishing is 12 ㎜ × 12 ㎜;
(2) prepare conductive electrode: the fine copper plate thick with 0.5 ㎜, 5 ㎜ are wide is pressed into spill conductive electrode as shown in Figure 1 and Figure 2, the oxide layer on copper coin surface can slightly be polished with 180Cw carborundum paper;
(3) paste conductive tape: one end of conductive electrode is vertically put on the sample surfaces of polish, the conductive tape that use is cut into 8 ㎜ × 12 ㎜ sizes is in advance by conductive electrode one end and the sample surperficial close adhesion of polishing; With plastics pole roll extrusion conductive tape surface firmly a little, until completely bonding with sample and conductive electrode, and with the electric conductivity between universal meter sample for reference and conductive electrode;
(4) inlay: the sample pasting is put into φ 30 ㎜ silica gel and inlays in mould, liquid inlay is poured into and inlayed in mould, under normal temperature 8～10 minutes, after inlay setting and hardening, sample can be taken out, prepared by conducting sample.
Described conductive tape is 3M board 1181 type copper foil tapes or collects firelight or sunlight board JY-02 type conductive tape.
Described conductive tape taking Copper Foil as tape base, thickness 0.066mm, scribble the quick acrylic acid adhesive of two laminations, the viscosity to steel plate: 3.8N/10mm, contact resistance: 0.005ohm.
Described inlay is the mill prestige cold inlay of board acrylic resin or the three cold inlays of clever CMR type metallographic or resistance to rich cold inlay.
The advantage of a kind of electrical steel conduction preparation method of metallographic sample provided by the invention is: prepare easy, quick, cost is low, consistent reliable, do not need to use special equipment, in common lab, can complete, the sample after inlaying can carry out electrochemical polish and ESEM, EBSD analytical test.
Brief description of the drawings
Fig. 1 is conductive electrode structure front view in electrical steel conduction preparation method of metallographic sample of the present invention.
Fig. 2 is conductive electrode structure side view in electrical steel conduction preparation method of metallographic sample of the present invention.
Fig. 3 inlays rear sample schematic diagram in electrical steel conduction preparation method of metallographic sample of the present invention.
Wherein, 1--sample, 2--conductive electrode, 3--conductive tape, 4--inlay.
Detailed description of the invention
The invention provides a kind of electrical steel conduction preparation method of metallographic sample, its preparation process is as follows:
1. stamping-out polishing sample: it is the disk of φ 23 ㎜ that sample 1 stamping-out is become to diameter, with polish a gently surface of sample 1 of 180Cw carborundum paper or file, removing insulating coating, expose substrate metal gloss and be limited, the area of polishing is 12 ㎜ × 12 ㎜;
2. prepare conductive electrode: the fine copper plate thick with 0.5 ㎜, 6 ㎜ are wide is pressed into the conductive electrode 2 of spill as shown in Figure 1 and Figure 2, and the oxide layer on copper coin surface can slightly be polished with 180Cw carborundum paper;
3. paste conductive tape: one end of conductive electrode 2 is vertically put into sample 1 surface of having polished upper, by the size surperficial close adhesion that to be 8 ㎜ × 12 ㎜ conductive tapes 3 polish conductive electrode 2 and sample 1; In the present embodiment, for ensureing that electric conductivity is good, can be with plastics pole roll extrusion conductive tape 3 firmly a little, until completely bonding with sample 1 and conductive electrode 2, use the conduction situation between universal meter sample for reference 1 and conductive electrode 2;
In the present embodiment, conductive tape 3 is selected 3M board 1181 type copper foil tapes or is collected firelight or sunlight board JY-02 type conductive tape, conductive tape 3 taking Copper Foil as tape base, thickness 0.066mm, scribble the quick acrylic acid adhesive of two laminations, the viscosity to steel plate: 3.8N/10mm contact resistance: 0.005ohm.
4. inlay: the sample 1 pasting is put into φ 30 ㎜ silica gel and inlays in mould, liquid inlay 4 is poured into and inlayed in mould, under normal temperature 8～10 minutes, after inlay 4 sclerosis, sample can be taken out, prepared by conducting sample.
In this enforcement, inlay 4 is the mill prestige cold inlay of board acrylic resin or the three cold inlays of clever CMR type metallographic or resistance to rich cold inlay. This inlay 4 is easy to operate, without heating, pressurization, can harden rapidly at normal temperatures, and filling capacity is good, and after sclerosis, corrosion resisting property is good, is convenient to sample and preserves for a long time.
Claims (4)
1. an electrical steel conduction preparation method of metallographic sample, is characterized in that: its preparationStep is as follows:
1. stamping-out polishing sample: it is the disk of 23 ㎜ that sample stamping-out is become to diameter, uses 180CwA polish gently surface of sample of carborundum paper or file, to remove insulating coating, to exposeSubstrate metal gloss is limited, and polishing area is 12 ㎜ × 12 ㎜;
2. prepare conductive electrode: the fine copper plate thick with 0.5 ㎜, 6 ㎜ are wide is pressed dished conductionElectrode, the oxide layer on copper coin surface is slightly polished with 180Cw carborundum paper;
3. paste conductive tape: one end of conductive electrode is vertically put into the sample surfaces of having polishedAbove, with the conductive tape of big or small 10 ㎜ × 12 ㎜, conductive electrode and sample are polished to surface closelyBonding, with plastics poles roll extrusion conductive tape firmly a little, until conductive tape is completely and sampleBonding with conductive electrode, and with the electric conductivity between universal meter sample for reference and conductive electrode;
4. inlay: the sample pasting is put into φ 30 ㎜ silica gel and inlays in mould, liquid is inlayedPanel is poured into and is inlayed in mould, under normal temperature 8～10 minutes, after inlay sclerosis, sample can be gotGo out, prepared by conducting sample.
2. a kind of electrical steel conduction preparation method of metallographic sample as claimed in claim 1,It is characterized in that, described conductive tape can be selected 3M board 1181 type copper foil tapes or collect firelight or sunlight boardJY-02 type conductive tape.
3. a kind of electrical steel conduction preparation method of metallographic sample as claimed in claim 1,It is characterized in that, described conductive tape taking Copper Foil as tape base, thickness is 0.066mm, scribbles twoThe quick acrylic acid adhesive of lamination, the viscosity to steel plate: 3.8N/10mm, contact resistance: 0.005ohm。
4. a kind of electrical steel conduction preparation method of metallographic sample as claimed in claim 1,It is characterized in that, described inlay can be selected the mill prestige cold inlay of board acrylic resin or three spiritsThe cold inlay of CMR type metallographic or resistance to rich cold inlay.
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| CN201410108554.3A CN103900878B (en) | 2014-03-21 | 2014-03-21 | A kind of electrical steel conduction preparation method of metallographic sample |
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| CN201410108554.3A CN103900878B (en) | 2014-03-21 | 2014-03-21 | A kind of electrical steel conduction preparation method of metallographic sample |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396368A (en) * | 2018-03-02 | 2018-08-14 | 上海大学 | A kind of electrolytic polishing method of metalwork |
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| CN104655465A (en) * | 2014-11-21 | 2015-05-27 | 沈阳工业大学 | Preparation method of metallographic specimen of silicon steel oxidized scale |
| CN105300777A (en) * | 2015-11-13 | 2016-02-03 | 广西玉柴机器股份有限公司 | Metallographic specimen and hardness specimen embedding method |
| CN108106913A (en) * | 2017-11-20 | 2018-06-01 | 东北大学 | A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests |
| CN109142415B (en) * | 2018-11-02 | 2021-07-20 | 首钢智新迁安电磁材料有限公司 | Analysis method of inhibitor in oriented silicon steel |
| CN110542604B (en) * | 2019-10-22 | 2021-03-19 | 昆明理工大学 | Pretreatment method for high-purity indium sample for glow discharge mass spectrum detection |
| CN111257092A (en) * | 2020-04-10 | 2020-06-09 | 昆明理工大学 | Fixing method for polished metal and mineral sheet samples |
| CN111879593A (en) * | 2020-07-02 | 2020-11-03 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Embedded metallographic sample suitable for electropolishing instrument and preparation method thereof |
| CN112985935B (en) * | 2021-01-28 | 2022-06-21 | 西安交通大学 | A mould for preparing resin soaks paper electricity branch sample |
| CN113281140A (en) * | 2021-05-10 | 2021-08-20 | 天津大学 | Conductive multifunctional metallographic hot-embedding auxiliary device and using method thereof |
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| CN102095623A (en) * | 2011-01-16 | 2011-06-15 | 首钢总公司 | Preparation method for silicon steel metallographic sample |
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| JP2010197272A (en) * | 2009-02-26 | 2010-09-09 | Jeol Ltd | Sample coating method of electron microscope |
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Patent Citations (3)
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| CN101581637A (en) * | 2009-06-19 | 2009-11-18 | 武汉钢铁(集团)公司 | Method for preparing electron microscope film sample with silicon steel sheet coating |
| CN102095623A (en) * | 2011-01-16 | 2011-06-15 | 首钢总公司 | Preparation method for silicon steel metallographic sample |
| CN102661883A (en) * | 2012-04-23 | 2012-09-12 | 天津立中合金集团有限公司 | Method for quickly preparing metallographic samples for AS7G03/AS8U3 aluminum alloy |
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| CN108396368A (en) * | 2018-03-02 | 2018-08-14 | 上海大学 | A kind of electrolytic polishing method of metalwork |
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