CN110514503A - A kind of preparation method of pure copper samples - Google Patents

A kind of preparation method of pure copper samples Download PDF

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Publication number
CN110514503A
CN110514503A CN201910972970.0A CN201910972970A CN110514503A CN 110514503 A CN110514503 A CN 110514503A CN 201910972970 A CN201910972970 A CN 201910972970A CN 110514503 A CN110514503 A CN 110514503A
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China
Prior art keywords
polishing
preparation
pure copper
sample
copper samples
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Pending
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CN201910972970.0A
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Chinese (zh)
Inventor
毛泽宁
钱锟
王嘉畅
韩波
沈明强
赵卫华
刘晓
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Shanghai Baoye Group Corp Ltd
Shanghai Baoye Engineering Technology Co Ltd
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Shanghai Baoye Group Corp Ltd
Shanghai Baoye Engineering Technology Co Ltd
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Priority to CN201910972970.0A priority Critical patent/CN110514503A/en
Publication of CN110514503A publication Critical patent/CN110514503A/en
Pending legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/2005Preparation of powder samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising

Abstract

The invention belongs to the preparation field of metalwork sample, in particular to a kind of preparation method of pure copper samples, preparation method includes the following steps that Mechanical polishing: pure copper samples polishing is handled, until polishing surface is visible by naked eyes scratch;Mechanical polishing: electrobrightening: by sample be anode, same material fine copper is cathode, connects D.C. regulated power supply with conducting wire, is then immersed in electrolytic polishing liquid the two poles of the earth simultaneously and carries out electrobrightening;Polish pole span 10-30mm, polishing time 5-10min;Cleaning;Secondary mechanical polishing;Re-electrolysis polishing.The present invention is while removing surface residual stress layer purpose, the defects of effectively removing surface relief, point, pit, obtains bright and clean even curface.The occurrence of pure copper samples prepared through the invention, fault location when reducing subsequent EBSD analysis test can not generate diffraction pattern, substantially increase the calibration rate of Kikuchi style, style calibration rate >=95%.

Description

A kind of preparation method of pure copper samples
Technical field
The invention belongs to the preparation field of metalwork sample, in particular to a kind of preparation method of pure copper samples.
Background technique
Metallic copper applies status in occupation of highly important in national economy every field.In metal fine copper structure observation When, polishing treatment can remove metallographic specimen surface scratch defect, bright and clean smooth metallographic surface be obtained, to obtain optimal Organize observed result.Most commonly used technological means is mechanical polishing in the prior art, but since fine copper quality is softer, polishing Rear fine copper metallographic surface can remaining have it is tiny it is mechanical throw trace, and due to cutting stress, the surface after polishing has that there are one Layer residual stress layer.On the one hand the presence of the stressor layers influences whether the accuracy of surface microhardness measurement;On the other hand exist When EBSD (electron backscatter diffraction) test analysis, it is difficult to the clear diffraction pattern that can effectively demarcate is obtained, it is serious to reduce flower Sample calibration rate, influences test result.
To solve this problem, electrobrightening can be generally carried out after mechanical polishing, throw trace to reach removal metallographic surface And the purpose of residual stress layer.But when Traditional DC electrobrightening, low voltage can make fine copper sample surfaces be easy to generation table The defects of face is embossed, point, pit, sample surfaces can generate the wavy contoured surface of polishing again when overtension, thus difficult To obtain smooth bright and clean wide area surface, nano impress, EBSD Measurement results are had an impact.Furthermore electrolytic polishing liquid Ingredient type is complex, there is the nocuousness such as methanol, sulfuric acid, Acid constituents, has certain wind to environment and experiment operator It is dangerous.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of pure copper samples, in the same of removal surface residual stress layer purpose When, the defects of effectively removing embossed specimen surface, point, pit, obtain bright and clean even curface, allow sample preferably Subsequent detection for nano-indenter test, EBSD test etc..
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of pure copper samples, preparation method include the following steps,
(1), Mechanical polishing: pure copper samples polishing is handled, until polishing surface is visible by naked eyes scratch;
Preferably, 400 can be used#、800#、1000#Silicon carbide abrasive paper for metallograph carries out the polishing processing of different passages.
(2), it mechanically polishes:
Abrasive pastes or antiscuffing paste are applied to polishing cloth surface, in survey dropwise addition clear water in sample to keep burnishing surface wet, Sample is inversely slowly moved along mill rotation simultaneously;
Preferably, speed of grinding plate 600-1000r/min.It is further preferred that speed of grinding plate is 1000r/min.If turning Speed is excessively high, will increase the speed of frictional heat generation, is unfavorable for the heat dissipation of burnishing surface, to cause surface oxidation dimmed, and revolving speed It is excessively high also burnishing surface scratch to be made to increase, it is difficult to remove.Revolving speed is too low to will increase polishing time, increases polishing and removes scoring processes Difficulty.
Preferably, the abrasive pastes are the diamond paste that granularity is 0.5 μm;The antiscuffing paste is partial size less than 1 μm Al2O3Antiscuffing paste.Polishing process is to be acted on by abrasive pastes particle the machine cut in sample face, keeps any surface finish smooth.It is pure Copper is softer, if choosing, abrasive pastes granularity is excessive, and coarseer obvious mechanical throwing trace can be remained on burnishing surface.On the contrary, if granularity mistake It is small, then polishing time can be made too long.
(3), electrobrightening:
By the sample in step (2) be anode, same material fine copper is cathode, connects D.C. regulated power supply with conducting wire, then The two poles of the earth are immersed in electrolytic polishing liquid simultaneously and carry out electrobrightening;Polish pole span 10-30mm, polishing time 5-10min;
Preferably, the voltage of direct-flow voltage regulation is 2.8V;Polish pole span 20mm, polishing time 10min.It is suitable by selecting Voltage, polishing pole span, polishing time, the severe degree of anode reaction can be reduced, effectively avoid high voltage polish caused by Wavy surface rises and falls and the surface defect of various complexity.It is anti-in polishing initial stage influence anode electrochemical that polishing pole span crosses conference The starting response answered, causes electrolyte to generate chemical attack to sample, so that sample surfaces oxidation is dimmed.Too small pole span can be made It is unstable at electric current, influence quality of finish.
Electrolytic polishing liquid is H3PO4With the mixed liquor of deionized water.It is further preferred that the electrolytic polishing liquid is H3PO4 The mixed liquor for being 7:1 according to volume ratio with deionized water, H3PO4Concentration be greater than 85%.The component proportion letter of the electrolytic polishing liquid It is single, it is safe and harmless, it is not volatile nonirritant, it long-term preservation and can be used for multiple times, greatly reduce cost.
In order to cooperate the distinctive electricity of the present invention to throw technique, electrolytic polishing liquid of the present invention is only with H3PO4With go from For sub- water mixed liquid as electrolytic polishing liquid, component proportion is simple, safe and harmless, not volatile nonirritant, can long-term preservation simultaneously It is used for multiple times.And electrolytic polishing liquid and deionized water of the invention according to volume ratio is that 7:1 is that technical effect is best, if Volume ratio height and 7:1, then being unfavorable for flowing, if volume ratio is lower than 7:1, it is poor that electricity throws effect.
(4), it cleans:
Electrolytic polishing sample is taken out rapidly, is first rinsed with clear water, is placed in ethyl alcohol and is cleaned, cold wind drying;
(5), secondary mechanical polishes:
Repeat the process of step (2);Preferably, it is 0.1 μm of diamond paste, speed of grinding plate that abrasive pastes, which select granularity, Degree is 600r/min.Sample surfaces have been the burnishing surface compared with low roughness at this time, and secondary mechanical polishing selects partial size more tiny Abrasive pastes will not extend polishing time to serious.Purpose is to reduce residual as far as possible during throwing eventually in order to which essence is thrown at this time Throw the depth of trace.
(6), re-electrolysis polishes:
Repeat the process of step (3), and washed samples.Preferably, the polishing time is 5min.Electrolysis is thrown at this time Light is also smart polishing working, it is therefore an objective to Surface stress layer is removed, polishing time should suitably reduce, in case crossing polishing causes surface quality It is deteriorated.
The beneficial effects of the present invention are:
1, the present invention is using secondary mechanical polishing and re-electrolysis polishing, while removing surface residual stress layer purpose, The defects of effectively removing surface relief, point, pit obtains bright and clean even curface.
The present invention by introducing secondary mechanical finishing polish, re-electrolysis finishing polish process, realization to specimen surface into One step is finely corrected, and by selecting suitable burnishing parameters, so that burnishing surface quality is further enhanced, while being not apparent from increasing Add the time of sample operation.
2, the pure copper samples prepared through the invention, fault location when reducing subsequent EBSD analysis test can not generate The occurrence of diffraction pattern, substantially increases the calibration rate of Kikuchi style, style calibration rate >=95%.
3, the present invention cooperates special electricity to throw electrolytic polishing liquid used by technique only with H3PO4It is mixed with deionized water For liquid as electrolytic polishing liquid, component proportion is simple, safe and harmless, not volatile nonirritant, long-term preservation and can be used for multiple times, Greatly reduce cost.
4, operation of the present invention is easy, and control is easy, and effect is good, and device therefor is simple and easy to get, and experimental period is shorter, and experiment is wanted Ask lower, experimental procedure is easier.
Specific embodiment
Below with reference to embodiment, the invention will be further described:
Embodiment 1:
1) Mechanical polishing: by 10 × 10 × 8mm of well cutting3Anaerobic fine copper TU1 sample successively uses 400#、800#、1000# Silicon carbide abrasive paper for metallograph carries out the polishing of different passages, until surface is visible by naked eyes scratch.
2) it mechanically polishes: choosing the diamond paste that granularity is 0.5 μm and be applied to polishing cloth surface, be applied to polishing cloth Speed of grinding plate 1000r/min is chosen on surface, inversely slowly moves sample along mill rotation while polishing, and clear water is added dropwise, directly To the mirror image burnishing surface for obtaining light;
3) electrobrightening: it is H that 40ml volume components ratio is added into beaker3PO4(analysis is pure): H2The electrolysis of O=7:1 is thrown Light liquid, using sample to be thrown as anode, same material fine copper is cathode, and room temperature polishes 10min under 2.8V DC voltage.It is needed when polishing The two poles of the earth are immersed in electrolytic polishing liquid simultaneously, polish pole span 20mm.
4) it cleans: after polishing, taking out sample rapidly and rinsed with clear water, then cleaned with ethyl alcohol.
5) secondary mechanical polishes: it is identical as the method in step 2) mechanical polishing, it is simply that abrasive pastes are changed to granularity and are 0.1 μm of diamond paste, polishing machine revolving speed 600r/min.
6) re-electrolysis polishes: identical as the method in the electrobrightening in step 3), only polishing time is changed to 5min.It takes out sample after electrobrightening to be cleaned with clear water, ethyl alcohol respectively, cold wind drying saves.
Comparative example 1
1) Mechanical polishing: by 10 × 10 × 8mm of well cutting3Anaerobic fine copper TU1 sample successively uses 400#、800#、1000# Silicon carbide abrasive paper for metallograph carries out the polishing of different passages, until surface is visible by naked eyes scratch.
2) it mechanically polishes: choosing the diamond paste that granularity is 0.5 μm and be applied to polishing cloth surface, be applied to polishing cloth Speed of grinding plate 1000r/min is chosen on surface, inversely slowly moves sample along mill rotation while polishing, and clear water is added dropwise, directly To the mirror image burnishing surface for obtaining light;
3) electrobrightening: it is H that 40ml volume components ratio is added into beaker3PO4(analysis is pure): H2The electrolysis of O=7:1 is thrown Light liquid, using sample to be thrown as anode, same material fine copper is cathode, and room temperature polishes 10min under 2.8V DC voltage.It is needed when polishing The two poles of the earth are immersed in electrolytic polishing liquid simultaneously, polish pole span 20mm.
4) it cleans: after polishing, taking out sample rapidly and rinsed with clear water, then cleaned with ethyl alcohol, cold wind drying saves.
By white light confocal microscopy sample burnishing surface quality and measure surface roughness, at the same using SEM into Row EBSD test detects Kikuchi style and records calibration rate, as a result see the table below 1.
Table 1:
Above data comparison can obtain as can be seen that the fine copper polishing method for making sample designed using the present invention and take into account table Face is bright and clean smooth and removes the fine copper metallographic specimen of surface residual stress layer characteristic, while any surface finish zero defect, greatly improves The calibration rate of EBSD Kikuchi style.
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to disclosed in the embodiment Content.So all do not depart from the lower equivalent or modification completed of spirit disclosed in this invention, the model that the present invention protects is both fallen within It encloses.

Claims (7)

1. a kind of preparation method of pure copper samples, preparation method include the following steps,
(1), Mechanical polishing: pure copper samples polishing is handled, until polishing surface is visible by naked eyes scratch;
(2), it mechanically polishes:
Abrasive pastes or antiscuffing paste are applied to polishing cloth surface, clear water is added dropwise on the inside of sample to keep burnishing surface wet, simultaneously Sample is inversely slowly moved along mill rotation;
(3), electrobrightening:
By the sample in step (2) be anode, same material fine copper is cathode, D.C. regulated power supply is connected with conducting wire, then by two Pole is immersed in electrolytic polishing liquid carries out electrobrightening simultaneously;Polish pole span 10-30mm, polishing time 5-10min;
(4), it cleans:
Electrolytic polishing sample is taken out rapidly, is first rinsed with clear water, is placed in ethyl alcohol and is cleaned, cold wind drying;
(5), secondary mechanical polishes:
Repeat the process of step (2);
(6), re-electrolysis polishes:
Repeat the process of step (3), and washed samples.
2. the preparation method of pure copper samples according to claim 1, it is characterised in that: the mill in the step (2) turns Speed is 600-1000r/min.
3. the preparation method of pure copper samples according to claim 2, it is characterised in that: the abrasive pastes are 0.5 μm of granularity Diamond paste;The antiscuffing paste is Al of the partial size less than 1 μm2O3Antiscuffing paste.
4. the preparation method of pure copper samples according to claim 1, it is characterised in that: the direct current in the step (3) Pressure is 2.8V;Electrolytic polishing liquid is H3PO4With the mixed liquor of deionized water.
5. the preparation method of pure copper samples according to claim 4, which is characterized in that the electrolytic polishing liquid is H3PO4With The mixed liquor that deionized water is 7:1 according to volume ratio, H3PO4Concentration be greater than 85%.
6. the preparation method of pure copper samples according to claim 1, which is characterized in that selecting granularity in step (5) is 0.1 μm diamond paste, speed of grinding plate degree be 600r/min.
7. the preparation method of pure copper samples according to claim 1, which is characterized in that when polishing in the step (6) Between be 5min.
CN201910972970.0A 2019-10-14 2019-10-14 A kind of preparation method of pure copper samples Pending CN110514503A (en)

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CN110967356A (en) * 2019-12-18 2020-04-07 浙江华电器材检测研究所有限公司 Method for improving surface quality of plastic metal electron back scattering diffraction sample
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
CN111521462A (en) * 2020-05-06 2020-08-11 中国航发成都发动机有限公司 Metallographic preparation method of coating
CN111826706A (en) * 2020-07-16 2020-10-27 宁波江丰电子材料股份有限公司 Electrolytic polishing process of ultra-pure Cu or ultra-pure Cu alloy target
CN112924255A (en) * 2021-01-29 2021-06-08 上海微谱化工技术服务有限公司 Positive sample micropore processing method and application thereof
CN114892258A (en) * 2022-05-23 2022-08-12 浙江工业大学 Electrolytic polishing device and method for thinning flat plate tensile sample

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CN110967356A (en) * 2019-12-18 2020-04-07 浙江华电器材检测研究所有限公司 Method for improving surface quality of plastic metal electron back scattering diffraction sample
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
CN111521462A (en) * 2020-05-06 2020-08-11 中国航发成都发动机有限公司 Metallographic preparation method of coating
CN111521462B (en) * 2020-05-06 2023-07-18 中国航发成都发动机有限公司 Metallographic preparation method of coating
CN111826706A (en) * 2020-07-16 2020-10-27 宁波江丰电子材料股份有限公司 Electrolytic polishing process of ultra-pure Cu or ultra-pure Cu alloy target
CN111826706B (en) * 2020-07-16 2023-01-17 宁波江丰电子材料股份有限公司 Electrolytic polishing process of ultra-pure Cu or ultra-pure Cu alloy target
CN112924255A (en) * 2021-01-29 2021-06-08 上海微谱化工技术服务有限公司 Positive sample micropore processing method and application thereof
CN112924255B (en) * 2021-01-29 2023-08-15 上海微谱化工技术服务有限公司 Positive sample micropore processing method and application thereof
CN114892258A (en) * 2022-05-23 2022-08-12 浙江工业大学 Electrolytic polishing device and method for thinning flat plate tensile sample

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