CN103063496B - Brass dezincification-resistance sample preparation method - Google Patents
Brass dezincification-resistance sample preparation method Download PDFInfo
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- CN103063496B CN103063496B CN201310006361.2A CN201310006361A CN103063496B CN 103063496 B CN103063496 B CN 103063496B CN 201310006361 A CN201310006361 A CN 201310006361A CN 103063496 B CN103063496 B CN 103063496B
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Abstract
The invention discloses a brass dezincification-resistance sample preparation method. The method comprises the following steps: inlaying a brass sample to be tested, grinding, polishing, and corroding in a 75DEG C CuCl2.2H2O solution for 24h; slicing the corroded brass sample to be tested, and corroding and cleaning the surface of the obtained slice with anhydrous ethanol; coating the cleaned slice surface with a glue to form a protection layer, wherein the protection layer fully contacts with the brass sample surface; carrying out resin inlaying of the slice surface; grinding the inlaid slice surface with metallographic sandpaper; polishing the ground slice surface on a polishing machine; and corroding the polished slice surface in a solution composed of 1-3g of ferric trichloride, 10-20ml of hydrochloric acid and 80-150ml of alcohol. The preparation method solves the dezincification layer chamfering and spalling problems, effectively prevent the water stain from appearing, and makes the dezincification layer depth be clear; and the concentrations and the proportions of the above corrosion solutions are adjusted to improve the corrosion effect in order to make the dezincification layer depth be clearly displayed in the corrosion state.
Description
Technical field
The present invention relates to brass anti-dezincify sample technology of preparing, more particularly, relate to the anti-dezincify preparation method of sample of a kind of brass.
Background technology
The purposes of brass part in life is very extensive, as water tank belt, supply and discharge water pipe, corrugated tube, coiled pipe, condenser pipe, shell case and various complex-shaped punching product, ironware etc.Environment residing for part is easy to contact corrosion medium, therefore there are certain requirements the corrosion resistance of brass part, and therefore, before product uses, carry out Dezincification corrosion resistant service check to it is necessary.Dezincify often appears at containing in higher alpha brass, particularly the alpha+beta brass of zinc.Zinc electrode current potential is far below copper, and first the zinc that electrode potential is low dissolved in neutral saline solutions, and copper then remains in surface in porous membrane, and forms micro cell with subsurface brass, makes brass become anode and be accelerated corrosion.
The bioassay standard of current brass Dezincification corrosion resistant performance mainly contains GB/T10119-2008, AS2345-2006, ISO6509-1981.Sample is inlayed, after polishing, polishing, at the CuCl of 75 DEG C by standard regulation
22H
224 hours of corrosion experiments are carried out in O solution.After corrosion experiment completes, carry out cut into slices (perpendicular to sample exposed surface), subsequently metallographic specimen preparation is carried out to section, and measure dezincify layer depth.
In above-mentioned experimentation, section is carried out in process prepared by metallographic specimen because brass sample is positioned at inlay the most edge of resin, therefore in the process of grinding and polishing, the chamfering easily forming dezincify layer with peel off, larger error is easily caused to experimental result.
Summary of the invention
For the defect existed in prior art, the object of this invention is to provide the anti-dezincify preparation method of sample of a kind of brass.
For achieving the above object, the present invention adopts following technical scheme:
The anti-dezincify preparation method of sample of a kind of brass, the concrete steps of the anti-dezincify preparation method of sample of this brass are:
A. brass sample to be measured is inlayed, after polishing, polishing, at the CuCl of 75 DEG C
22H
224 hours of corrosion are carried out in O solution;
B. the cutting perpendicular to corrosion surface is carried out to brass sample to be measured after corrosion, obtain two pieces of sections, adopt absolute ethyl alcohol to clear up any section of one piece of section and the surface of corrosion;
C. using the corrosion surface coating after cleaning, above glue is as protective seam, and protective seam fully need contact with brass specimen surface;
D. sliced surfaces is carried out resin to inlay;
E. the sliced surfaces abrasive paper for metallograph after inlaying is polished;
F. the sliced surfaces of polishing is placed in polishing on buffing machine;
G. the sliced surfaces after polishing is placed in the solution be made up of the alcohol of the ferric trichloride of 1g ~ 3g, the hydrochloric acid of 10ml ~ 20ml and 80ml ~ 150ml to corrode after 20 ~ 50 seconds, carries out observing under being placed in metaloscope and measure dezincify layer thickness.
Glue in described step C adopts 502 glue.
In described step C, the thickness range of protective seam is 1 ~ 3mm.
The concrete steps of described step D are:
Adopt cold method for embedding, will powder be inlayed and inlay liquid and to be mixed into the ratio of 5:2 volume ratio and to inlay resin, sliced surfaces is placed in mould bottom surface, pour mixed resin of inlaying into mould, and apply the pressure of 1.0 ~ 5.0Bar, wait for after 20 ~ 30 minutes, the demoulding also takes out sample.
The concrete steps of described step e are:
Sliced surfaces after inlaying is adopted 600 orders, 800 orders, 1000 orders, 1500 object abrasive paper for metallograph polishings successively, and 600 order sand paper are to occur that can test dezincify layer surface is as the criterion, and other every procedures are as the criterion to eliminate front one polishing scratch.
The concrete steps of described step F are:
Grinded sliced surfaces is placed in polishing on buffing machine, and adopt 5 μm, 2.5 μm, 0.25 μm diamond polishing liquid to carry out polishing successively, the time of every procedure is 20 ~ 50 seconds, and every procedure is as the criterion to eliminate front one polishing scratch.
Compared with prior art, a kind of brass of the present invention anti-dezincify preparation method of sample is adopted to have following technique effect:
1, the sample preparation flow after adopting preparation method of the present invention solves chamfering and the spallation problems of dezincify layer;
What in grinding and polishing, corrosion process, 2, remain in brass part and inlay between resin, the hole of brass part dezincify layer and gap is water stain more, at metallography microscope Microscopic observation, measure in the process of dezincify layer, water stainly to separate out at specimen surface, easily error is caused to the measurement result of dezincify layer thickness, protective seam is added in sample preparation flow after improvement, effectively prevent water stain precipitation, make the degree of depth of dezincify layer high-visible;
3, in corrosion process, the most advanced and sophisticated position of dezincify layer easily forms illusion because corrosion is too serious, in the preparation flow therefore after improvement, improves corrosive effect by the concentration and ratio adjusting each etchant solution, clear display dezincify layer depth under making etch state.
Accompanying drawing explanation
Fig. 1 is 100 times of dezincify layer pattern schematic diagram of embodiments of the invention 3;
Fig. 2 is 500 times of dezincify layer pattern schematic diagram of embodiments of the invention 3;
Fig. 3 is 1000 times of dezincify layer pattern schematic diagram of embodiments of the invention 3;
Fig. 4 is the instrumentation plan of the dezincify layer depth of embodiments of the invention 3.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with drawings and Examples.
The anti-dezincify preparation method of sample of a kind of brass, the concrete steps of the anti-dezincify preparation method of sample of this brass are:
Brass sample to be measured is inlayed by 11., after polishing, polishing, at the CuCl of 75 DEG C
22H
224 hours of corrosion are carried out in O solution;
After 12. pairs of corrosion, brass sample to be measured carries out the cutting perpendicular to corrosion surface, obtains two pieces of sections, adopts absolute ethyl alcohol to clear up any section of one piece of section and the surface of corrosion;
Corrosion surface after cleaning is applied upper glue as protective seam by 13., and protective seam fully need contact with brass specimen surface;
Sliced surfaces is carried out resin by 14. inlays;
Sliced surfaces abrasive paper for metallograph after inlaying polishes by 15.;
The sliced surfaces of polishing is placed in polishing on buffing machine by 16.;
Sliced surfaces after polishing is placed in the solution be made up of the alcohol of the ferric trichloride of 1g ~ 3g, the hydrochloric acid of 10ml ~ 20ml and 80ml ~ 150ml by 17. corroded after 20 ~ 50 seconds, carries out observing and measure dezincify layer thickness under being placed in metaloscope.
Preferably, the glue in step 13 adopts 502 glue, and the thickness range of protective seam is 1 ~ 3mm.
The concrete steps of described step 14 are:
Adopt cold method for embedding, to powder be inlayed and inlay liquid and to be mixed into the ratio of 5:2 volume ratio and to inlay resin, sliced surfaces is placed in mould bottom surface, pour mixed resin of inlaying into mould, and apply the pressure of 1.0 ~ 5.0Bar, wait for after 20 ~ 30 minutes, the demoulding also takes out sample, it should be noted that: 1Bar=1.0 × 10
5pa;
The concrete steps of described step 15 are:
Sliced surfaces after inlaying is adopted 600 orders, 800 orders, 1000 orders, 1500 object abrasive paper for metallograph polishings successively, and 600 order sand paper are to occur that can test dezincify layer surface is as the criterion, and other every procedures are as the criterion to eliminate front one polishing scratch, and the time is not easily long.
The concrete steps of described step 16 are:
Grinded sliced surfaces is placed in polishing on buffing machine, and adopt 5 μm, 2.5 μm, 0.25 μm diamond polishing liquid to carry out polishing successively, the time of every procedure is 20 ~ 50 seconds, and every procedure is as the criterion to eliminate front one polishing scratch, and the time is not easily long.
Further illustrate technical scheme of the present invention by the following examples:
Embodiment 1:
According to AS2345-2006 standard, after standard Damascene pressed by brass sample to be measured, after polishing, polishing, at the CuCl of 75 DEG C
22H
224 hours of corrosion experiments are carried out in O solution.After corrosion experiment completes, carry out cut into slices (perpendicular to sample exposed surface), subsequently following procedures carried out to section:
(1) polished by 600 orders, 800 orders, 1000 orders, 1500 object abrasive paper for metallograph successively by the sample after section, every procedure is as the criterion to eliminate front one polishing scratch, and every procedure is about 20s, firmly evenly, and Impact direction and plane-parallel; (2) will the polished specimen and be placed in polishing on buffing machine, adopt 5 μm, 2.5 μm, 0.25 μm diamond polishing liquid to carry out polishing successively, every procedure is about 25s; (3) sample after polishing is placed in the corrosion of ferric trichloride (2g) hydrochloric acid (10ml) alcohol (100ml) solution and is about 30s, carry out observing under being placed in metaloscope and measure dezincify layer thickness.
In above-mentioned experimentation, owing to lacking step 12 of the present invention, 13 and 14, therefore the sample after section is in grinding and polishing process, easy formation chamfering, the not easily polishing of specimen surface cut, therefore occurs not observing dezincify layer depth, dezincify layer depth than untrue phenomenons such as actual value reductions when measurement dezincify layer thickness.
Embodiment 2:
According to AS2345-2006 standard, after standard Damascene pressed by sample, after polishing, polishing, at the CuCl of 75 DEG C
22H
224 hours of corrosion experiments are carried out in O solution.After corrosion experiment completes, carry out serial operation:
(1) by the sample section after corrosion experiment, and absolute ethyl alcohol is utilized sample corrosion surface and slice surface to be cleaned out; (2) adopt cold method for embedding, will powder be inlayed and inlay liquid and to be mixed into the ratio of 5:2 volume ratio and to inlay resin, sliced surfaces is placed in mould bottom surface, pour mixed resin of inlaying into mould, and apply the pressure of 2.0Bar, wait for after 20 ~ 30 minutes, the demoulding also takes out sample; (3) by the sample after inlaying by 600 orders, 800 orders, 1000 orders, 1500 object abrasive paper for metallograph polishings, every procedure is as the criterion to eliminate front one polishing scratch, and every procedure is about 20s, firmly evenly, and Impact direction and plane-parallel; (4) will the polished specimen and be placed in polishing on buffing machine, adopt 5 μm, 2.5 μm, 0.25 μm diamond polishing liquid to carry out polishing successively, every procedure is about 25s; (5) sample after polishing is placed in the corrosion of ferric trichloride (2g) hydrochloric acid (10ml) alcohol (100ml) solution and is about 30s, carry out observing under being placed in metaloscope and measure dezincify layer thickness.
In above-mentioned experimentation, owing to lacking step 13 of the present invention, therefore the sample after section is after again inlaying, in grinding and polishing process, be easy to reach not chamfering and the bright and clean requirement of specimen surface, ensure clearly under the microscope to observe dezincify layer, but when observing dezincify layer depth after polishing or corrosion, sample with inlay resin and see and be easy to form small gap or hole, moisture is caused to enter, constantly overflow in observation process, cause accurately measuring dezincify layer depth (when particularly dezincify layer depth is larger), the precision that impact is measured and observed.
Embodiment 3:
According to AS2345-2006 standard, after standard Damascene pressed by sample, after polishing, polishing, at the CuCl of 75 DEG C
22H
224 hours of corrosion experiments are carried out in O solution.After corrosion experiment completes, carry out serial operation:
(1) by the sample section after corrosion experiment, and absolute ethyl alcohol is utilized sample corrosion surface and slice surface to be cleaned out; (2) specimen surface be exposed in corrosion experiment process in solution painting is covered with 502 glue as protective seam, the thickness of protective seam ensures at 2mm, and fully need contact with brass specimen surface; (3) adopt cold method for embedding, will powder be inlayed and inlay liquid and to be mixed into the ratio of 5:2 volume ratio and to inlay resin, sliced surfaces is placed in mould bottom surface, pour mixed resin of inlaying into mould, and apply the pressure of 2.0Bar, wait for after 20 ~ 30 minutes, the demoulding also takes out sample; (4) by the sample after inlaying successively by 600 orders, 800 orders, 1000 orders, 1500 object abrasive paper for metallograph polishings, every procedure is as the criterion to eliminate front one polishing scratch, and every procedure is about 20s, firmly evenly, and Impact direction and plane-parallel; (5) will the polished specimen and be placed in polishing on buffing machine, adopt 5 μm, 2.5 μm, 0.25 μm diamond polishing liquid to carry out polishing successively, every procedure is about 25s; (6) sample after polishing is placed in the corrosion of ferric trichloride (2g) hydrochloric acid (10ml) alcohol (100ml) solution and is about 30s, carry out observing under being placed in metaloscope and measure dezincify layer thickness.
After above-mentioned experimentation, under the microscope the degree of depth of dezincify layer is measured, under 100 times (specifically seeing Fig. 1), 500 times (specifically seeing Fig. 2), 1000 times (specifically seeing Fig. 3), measure dezincify layer depth respectively, Fig. 4 is the instrumentation plan of dezincify layer depth.
Those of ordinary skill in the art will be appreciated that, above embodiment is only used to object of the present invention is described, and be not used as limitation of the invention, as long as in essential scope of the present invention, the change of the above embodiment, modification all will be dropped in the scope of claim of the present invention.
Claims (6)
1. the anti-dezincify preparation method of sample of brass, is characterized in that:
The concrete steps of the anti-dezincify preparation method of sample of this brass are:
A. brass sample to be measured is inlayed, after polishing, polishing, at the CuCl of 75 DEG C
22H
224 hours of corrosion are carried out in O solution;
B. the cutting perpendicular to corrosion surface is carried out to brass sample to be measured after corrosion, obtain two pieces of sections, adopt absolute ethyl alcohol to clear up any section of one piece of section and the surface of corrosion;
C. using the corrosion surface coating after cleaning, above glue is as protective seam, and protective seam fully need contact with brass specimen surface;
D. sliced surfaces is carried out resin to inlay;
E. the sliced surfaces abrasive paper for metallograph after inlaying is polished;
F. the sliced surfaces of polishing is placed in polishing on buffing machine;
G. the sliced surfaces after polishing is placed in the solution be made up of the alcohol of the ferric trichloride of 1g ~ 3g, the hydrochloric acid of 10ml ~ 20ml and 80ml ~ 150ml to corrode after 20 ~ 50 seconds, carries out observing under being placed in metaloscope and measure dezincify layer thickness.
2. the anti-dezincify preparation method of sample of brass according to claim 1, is characterized in that:
Glue in described step C adopts 502 glue.
3. the anti-dezincify preparation method of sample of brass according to claim 1, is characterized in that:
In described step C, the thickness range of protective seam is 1 ~ 3mm.
4. the anti-dezincify preparation method of sample of brass according to claim 1, is characterized in that:
The concrete steps of described step D are:
To inlay powder and inlay liquid and to be mixed into the ratio of 5:2 volume ratio and to inlay resin, sliced surfaces is placed in mould bottom surface, pours mixed resin of inlaying into mould, and apply the pressure of 1.0 ~ 5.0Bar, wait for after 20 ~ 30 minutes, the demoulding also takes out sample.
5. the anti-dezincify preparation method of sample of brass according to claim 1, is characterized in that:
The concrete steps of described step e are:
Sliced surfaces after inlaying is adopted 600 orders, 800 orders, 1000 orders, 1500 object abrasive paper for metallograph polishings successively, and 600 order sand paper are to occur that can test dezincify layer surface is as the criterion, and other every procedures are as the criterion to eliminate front one polishing scratch.
6. the anti-dezincify preparation method of sample of brass according to claim 1, is characterized in that:
The concrete steps of described step F are:
Grinded sliced surfaces is placed in polishing on buffing machine, and adopt 5 μm, 2.5 μm, 0.25 μm diamond polishing liquid to carry out polishing successively, the time of every procedure is 20 ~ 50 seconds, and every procedure is as the criterion to eliminate front one polishing scratch.
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| CN103471883B (en) * | 2013-08-20 | 2015-10-14 | 中国石油天然气股份有限公司 | Method for manufacturing rock slice in visual real core model |
| CN104422606B (en) * | 2013-08-27 | 2017-03-29 | 中芯国际集成电路制造(上海)有限公司 | A kind of chip failure analyzes the preparation method of sample |
| CN109208001A (en) * | 2018-11-12 | 2019-01-15 | 中国工程物理研究院材料研究所 | A kind of method that metal surface regional area accurately corrodes |
| CN110514503A (en) * | 2019-10-14 | 2019-11-29 | 上海宝冶工程技术有限公司 | A kind of preparation method of pure copper samples |
| CN111351694A (en) * | 2020-04-30 | 2020-06-30 | 上海宝冶工程技术有限公司 | Preparation method of metallographic specimen without water seepage and stain edge microstructure |
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| CN101440443A (en) * | 2008-12-10 | 2009-05-27 | 宁波博威集团有限公司 | Dezincification corrosion resistant low-stibium aluminum yellow brass alloy and manufacturing method thereof |
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| CN101440443A (en) * | 2008-12-10 | 2009-05-27 | 宁波博威集团有限公司 | Dezincification corrosion resistant low-stibium aluminum yellow brass alloy and manufacturing method thereof |
| CN102692425A (en) * | 2012-06-28 | 2012-09-26 | 武汉大学 | T/P91 steel ageing rating method based on precipitated phase fractional area |
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