CN107402150A - A kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis - Google Patents
A kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis Download PDFInfo
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- CN107402150A CN107402150A CN201710604923.1A CN201710604923A CN107402150A CN 107402150 A CN107402150 A CN 107402150A CN 201710604923 A CN201710604923 A CN 201710604923A CN 107402150 A CN107402150 A CN 107402150A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to non-ferrous metal analysis technical field, and in particular to a kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis, specifically include following steps：(1) sample processing early stage：Size is less than 7mm × 6mm × 4mm, the quasi- metallographic processing of the advanced rower of test surfaces and mechanical polishing；(2) portable unit is built：Sample connects positive source, and stainless steel plate connection power cathode, electrolyte bottom is equipped with magnetic stirring apparatus；(3) electrolyte configures：According to volume ratio, perchloric acid 4%~12%, methanol 55%~65%, n-butanol surplus；Electrolyte total amount 700ml, is placed in 1L beakers；(4) electrolysis processing and cleaning-drying：Temperature control is at 30 DEG C~20 DEG C, and voltage is controlled in 25V~35V, and polishing time is 40s~55s.Present invention processing surface area of sample is big, is suitable for each composition of different processing methods preparation and the titanium aluminium base alloy sample preparation of each test purpose.Convenient and flexible operation, do not limited by site facility etc., polishing effect is good, high yield rate.Portable devices, mobility is strong, and cost is low, is easy to promote, has a extensive future.
Description
Technical field
The invention belongs to non-ferrous metal analysis technical field, and in particular to a kind of titanium aluminium base alloy EBSD sample for analysis
Electrobrightening preparation method.
Background technology
From the nineties in last century, electron backscattered style crystal microcell orientation and crystal based on scanning electron-microscopy
Structural analysis technique development is swift and violent, and realizes its extensive use in microstructure sign.The technology is referred to as
EBSD technology, hereinafter referred to as English name Electron Backscattered Diffraction, EBSD skills
Art.Origin on the technology can trace back to or so twenties in last century, and people watcher in SEM solves
Shi Shi, it is not intended in be found that re-diffraction style, referred to as Kikuchi style, the theoretical foundation of EBSD technologies has been established in the discovery.
In 40~50 years afterwards, the development of the technology seems to lie on the table always.Until the seventies in last century, the technology starts prominent fly
Precipitately develop, people are found that EBSD angle of elevation Kikuchi band, 80~nineties, Dingley and Hjelen first
Et al. by computer technology be applied to demarcation orientation EBSD equipment, promoted the commercial applications of the technology.To last century 90
Age, the technology and spectroscopic technique, the combination of in-situ techniques and computer technology are even closer so that EBSD turns into material
A kind of irreplaceable important analysis and testing technology in terms of institutional framework.
Almost the development with EBSD technologies has also entered into laboratory in same stage, titanium aluminium base alloy, and it is as a kind of gold
Compound between category, there is the excellent spies such as low-density, high intensity, Gao Biqiang, the high natural frequency of vibration, resistance to high temperature oxidation, operation at high temperature
Point, it is considered to be the high-temperature structural material for the most prospect that Ni based high-temperature alloys can be substituted and widely applied.Titanium aluminium base alloy
It is with considerable scale to develop into today, and realizes commercial Application.However, also just because of the intrinsic fragility of its intermetallic compound
Feature, it is faced with some difficulties in terms of preparing processing always in its research and development and application process.When the development of material runs into bottle
, it is necessary to be assaulted fortified position with powerful theoretical research during neck, the pattern of leapfroging of Practice theory practice-theory is material science
The eternal path of development.EBSD technologies are widely used in titanium aluminium base alloy fabric analysis and characterized and in last decade or so, the skill
Prepared by processing of the art for titanium aluminium base alloy, either casting, thermal deformation processing, or powder metallurgy etc., by phase, crystalline substance
The investigation of boundary, orientation, textural behavio(u)r etc., prepared by the processing to the alloy have great importance, has become the alloy and grinds
Indispensable analysis and characterization means during hair.
According to EBSD technical principles, to obtain the EBSD data and image of feasible high quality, EBSD sample preparation right and wrong
The step of Chang Guanjian.In EBSD test process, projectile energy and sample surfaces are in 70 ° of inclinations angle, in sample top layer about 50nm
A diffraction zone is formed in thickness range, it is desirable to which lattice does not strain, without pollution and oxide layer etc. in the region, otherwise will
Can not be detected or picture quality extreme difference and can not use.For the EBSD samples of metal or alloy, surface treatment method
Including mechanical polishing method, chemical corrosion method, ion milling method and electrobrightening method.Mechanical polishing method is dispelled to sample skin stress
Effect is relatively poor, for titanium aluminium base alloy, needs longer polishing time；Chemical corrosion method easily causes titanium aluminium base alloy each
Mutually corrode uneven situation so that top layer is uneven, and has a strong impact on EBSD test results；Ion milling method success rate is very high,
Demarcation rate can generally achieve more than 90%, but this method processing area is smaller, big brilliant particularly with casting titanium aluminium base alloy etc.
Grain requires not applying in the interior test case for finding typical organization in a big way；By contrast, electrobrightening method be can yet be regarded as
The preferable preparation method of titanium aluminium base alloy EBSD samples, this method equipment cost is low, simple portable, and operation is easy, can be according to survey
Examination demand prepares large-size sample, and by rationally controlling the technological parameter during electrobrightening, sample preparation yield rate is close to
100%.
At present, being shown according to patent, the domestic research to metal and alloy EBSD sample electrolysis polishing methods is relatively fewer,
Also most of in existing data is on Fe based alloys and Al based alloys, is also had on a small quantity on non-ferrous metal and special alloy
Report.The preparation method of shaping ring sample is rolled in the 42CrMo steel casting for being used for EBSD tests of Guilin Electronic Science and Technology Univ.'s research and development,
Patent publication No. is CN106896009A, and sample carries out standard gold phase processor first, and electrobrightening is carried out using home-built equipment, electricity
It is 0.6mA~0.8mA to press as 25V~30V, electric current, and the time is 50s~60s；A kind of low-carbon of He Gang limited companies research and development
The preparation method of steel EBSD sample for analysis, sample also carry out standard gold phase processor first, are then banged using high-energy argon ion beam
Sample tested surface 40min~120min is hit, this method equipment is expensive, and it is smaller to prepare area；Second Group (Deyang) weight equipment
The nickel-base alloy electrolyte and its polishing method of limited company's research and development, phosphoric acid 50%~75% (volume ratio), sulfuric acid
8%~15%, ammonium thiocyanate 1%~5%, 1,4 butynediols 5%~15%, dimethylglyoxime 1%~8%, polyethylene glycol 1%
~5%, guar gum 1%~3%, the electrolyte coordinate with suitable glossing cause polishing after can equipment corrosion resistance
Can be improved, but do not refer to processing after sample be used for EBSD detection and analysis；A kind of electrolysis of Chongqing University of Technology's research and development is thrown
The method that light prepares two-phase zircaloy EBSD samples, sample equally carries out standard gold phase processor first, next in 5%~12%
Perchloric acid, 65%~80% methanol, 10%~25% ethylene glycol monobutyl ether and -25 DEG C or so, 20V voltages and 20s~100s
Under the conditions of carry out electrobrightening, EBSD tests can obtain high demarcation rate.At present, it there is no and prepared on titanium aluminium base alloy electrobrightening
The detailed explanation of sample method, in view of significant application value of the EBSD analysis and testing technologies in titanium aluminium base alloy, it would be highly desirable to establish
The electrobrightening preparation method of the titanium aluminium base alloy EBSD test samples of complete set.
The content of the invention
It is contemplated that establishing the EBSD titanium aluminium base alloy sample electrobrightening preparation methods of complete set, this method is set
Standby system is simple, practical, easy to operate, and preparation effect is good, has good economic benefit and promotional value.
To achieve these goals, technical scheme：
A kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis, comprises the following steps：
(1) sample processing early stage
Sample, line cutting slow wire feeding are cut using wire cutting or water knife；Cut sample size 10mm × 10mm × 5mm with
Under, wherein 5mm is the limiting value of height of specimen, and the direction is the ND directions during sample test；Wipe out surface and oil contaminant, two
Individual bottom surface is polished using 40#~400# sand paper, and one of face is that test surfaces continue to use 800# according to standard metallographic preparation method
~7000# sand paper is polished, and is first mechanically polished；Next, surface oil is thoroughly cleaned using alcohol, acetone sonic oscillation
It is dirty；
(2) portable unit is built
The part of electrobrightening equipment includes power supply, magnetic stirring apparatus, wire and stainless steel plate, thermometer, corrosion
Liquid and liquid nitrogen；Building method is：Wire one end connection stainless steel plate is placed in beaker bottom, and wire other end connection power supply is born
Pole, electrolyte is put into beaker, and cooling and thermometer thermometric are carried out using liquid nitrogen, electrolyte stirred using magnetic stirring apparatus
Mix, positive source connects polished sample with tweezers by wire；
(3) electrolyte configures
According to volume ratio, perchloric acid 4%~12%, methanol 55%~65%, n-butanol surplus；
(4) electrolysis processing and cleaning-drying
Titanium aluminium base alloy sample uses as anode, stainless steel plate as negative electrode, power-on and magnetic stirring apparatus, sample
Tweezers clamp, and are placed in electrolyte, and polished face is relative with stainless steel plate；During electrobrightening, temperature control is at -30 DEG C
~-20 DEG C, voltage control is controlled in 40s~55s in 25V~35V, polishing time；It is put at once in absolute ethyl alcohol after polishing, and
Sonic oscillation is carried out immediately, then is placed in acetone and is carried out sonic oscillation；Finally picked up with tweezers and quickly dry up surface with blower fan.
Preferably, sample size (5~7) mm × (3~6) mm × (2~4) mm cut in step (1), wherein (2~4)
Mm is short transverse, i.e. the ND directions of EBSD tests, and sample length and width are inconsistent in favor of the RD directions of identification EBSD tests.
Preferably, in step (2), according to sample size and sample concrete condition, beaker volume is 1L, and electrolyte is matched somebody with somebody altogether
700ml is put, coordinates 10cm diameter stainless steel plates to be placed in electrolyte bottom and is used as negative electrode, stainless steel plate with wire interconnecting piece point
Unsintered tape and anticorrosion adhesive plaster wrap up for more than two layers.
Preferably, negative electrode stainless steel plate selects 304 stainless steels.
Preferably, in step (3), according to volume ratio, perchloric acid 5%~7%, methanol 60%, n-butanol surplus.
Preferably, in step (4), voltage control is 30V.
Preferably, in step (4), temperature control is in -30 DEG C~-25 DEG C, electrobrightening time when electrobrightening starts
45s~50s.
Preferably, in step (4), during electrobrightening, magnetic stirring apparatus is located at electrolyte bottom, adjusts magnetic agitation
Device, make rotor drive electrolyte to form the whirlpool run through up and down, the bubble of sample surfaces is attached in polishing process of taking, improve
Polishing effect.
Preferably, in step (4), during electrobrightening, sample is clamped using tweezers, the height apart from stainless steel plate should
So that sectional area 0.6cm2~1cm2Sample, its initial current is in 0.9A~1.2A scopes.
Advantages of the present invention and beneficial effect are：
(1) present invention processing sample area is big, is suitable for each composition of different processing methods preparation and each test purpose
Titanium aluminium base alloy.
(2) convenient and flexible operation of the present invention, do not limited by site facility etc., polishing effect is good, high yield rate.
(3) present device is portable, and mobility is strong, and cost is low, is easy to promote.
Brief description of the drawings
Fig. 1 is mechanical polishing and electrobrightening sample macro morphology：Wherein sample " 1. " is to be cut after hot simulation compression is tested
The sheet specimens taken surface topography after standard gold phase processor, mechanical polishing；Sample " 2. " is to be cut after hot simulation compression is tested
Sheet specimens after standard gold phase processor, mechanical polishing, electrobrightening surface topography；Sample " 3. " is after tensile tests at room
The sheet specimens of selection surface topography after standard gold phase processor, mechanical polishing, electrobrightening；Sample " 4. " is that drawing by high temperature is real
Test rear strip sheet specimens surface topography after standard gold phase processor, mechanical polishing, electrobrightening.
Fig. 2 is 2. number sample central area EBSD test results：(a) contrast figure；(b) unique crystal grain color diagram；(c) γ master
Phase pole figure.
Fig. 3 is 3. number sample central area EBSD test results：(a) Eulerian angles figure；(b) phasor.
Fig. 4 is 4. number sample central area EBSD test results：(a) dynamic recrystallization figure；(b) inverse pole figure.
Embodiment
In specific implementation process, the electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis of the present invention includes
Following steps：
(1) sample processing early stage：
Titanium aluminium base alloy is hard as a kind of intermetallic compound quality, and hardness is up to HRC50~HRC60, and at room temperature
It is more crisp, wire cutting or water knife can be used to cut sample (during wire cutting slow wire feeding, in order to subsequently polish), sample should not use milling
Bed, lathe and grinding machine processing.For the BESD sample sizes cut generally in 10mm × 10mm × below 5mm, 5mm therein is sample
The limiting value of height, the short transverse of sample are also the ND directions (normal direction) in test process.Preferably, the BESD samples cut
Size (5~7) mm × (3~6) mm × (2~4) mm, wherein (2~4) mm is short transverse, sample length and width dimensions difference is beneficial to
Identify " RD " direction.
Next, wiping out surface and oil contaminant, two bottom surfaces of sample are used by 40# using mill or belt sander or manual mode
~400# sand paper is polished, and one of face contacts conducting resinl in EBSD test process, and (polishing off wire cutting vestige can ensure
Electric conductivity is good in test process), another face continues to polish standby in electrobrightening using 800#~7000# sand paper.It is preferred that
, in step (1) sample test face finally using 7000# sand paper polish, and mechanically polished first to surface-brightening without draw
Trace, be so advantageous to further lift follow-up electrobrightening effect.It turns out that face processing is more bright, be more advantageous to later
Electrobrightening effect.Next, surface and oil contaminant is thoroughly cleaned under sonic oscillation using alcohol, acetone.
(2) portable unit is built：
Electrobrightening equipment is built simply, and portability is strong.Chief component includes portable power supplies, and (maximum output voltage surpasses
Cross 50V), portable magnetic agitator, wire and stainless steel plate, thermometer etc..Building method is：Stainless steel plate is placed in bottom of the beaker
Portion simultaneously connects the outside wire wrapped up in insulating bag, the other end connection power cathode of the wire, and electrolyte is put into simultaneously in beaker
It is cooled using liquid nitrogen, thermometer connects polished sample to its thermometric, positive source by wire and tweezers etc..
According to sample size and specific sample situation, the preferred beaker volume of experience is 1L, coordinates suitable electrolyte volume
(reaching preferable liquid level) 700ml, beneficial to electrobrightening effect.Negative electrode stainless steel plate selects 304 stainless steels,
A diameter of 10cm.Stainless steel plate is necessarily wrapped with wire interconnecting piece point, and unsintered tape and anticorrosion adhesive plaster multilayer can be used to wrap up,
Once electrolyte penetrates into, then wire will be changed into negative electrode, have a strong impact on electrobrightening effect.
(3) electrolyte configures：
According to volume ratio, perchloric acid 4%~12%, methanol 55%~65%, n-butanol surplus.Pay attention in configuration process,
Perchloric acid should be poured into other two kinds of liquid to avoid splashing.
(4) electrolysis processing and cleaning-drying：
Titanium aluminium base alloy sample is as anode, and stainless steel plate is as negative electrode, power-on and magnetic stirring apparatus, sample tweezer
Sub-folder is held, and is placed in electrolyte, and polished face is relative with the stainless steel plate of beaker bottom.Temperature control is -30 DEG C~-20
DEG C, voltage is controlled in 25V~35V, and time control is in 40s~55s.It is put into absolute ethyl alcohol after polishing, also uses polishing at once
Tweezers quickly rinse.Then sonic oscillation will be carried out in the present absolute ethyl alcohol of sample at once, then moves to progress ultrasound in acetone and shake
Swing.Finally picked up with tweezers and quickly dried up with blower fan, avoid surface from leaving spot.Sample is with clean filter paper parcel or in sample
Deposited in QC, in view of titanium aluminium base alloy characteristic, it is not necessary to take sample anti-oxidation measure.
During electrobrightening, sample is clamped using tweezers, the height apart from stainless steel plate should cause sectional area about
0.6cm2~1cm2Its initial current size of sample 0.9A~1.2A scopes (sample apart from the more near then electric current of stainless steel plate more
Greatly).
The present invention is described in detail in conjunction with specific embodiment, it is whereby that advantage of the present invention and feature description is clearer,
But these embodiments do not form any restrictions to the scope of the present invention.
Embodiment 1
In the present embodiment, for carrying out high temperature compressed titanium aluminium base alloy using Gleeble hot modeling test machines, using electricity
Solve polishing method and prepare EBSD sample for analysis, comprise the following steps：
(1) preparation of samples：
Along the laminar sample that thickness under compression direction wire cutting is 0.5mm first at caked sample center, due to sample
Product are small and thin, need wire slowly to reduce wire cutting vestige depth；Wire cutting sample surfaces greasy dirt is wiped out, to the thin slice cut
Shape sample two sides is polished using 40#~800# sand paper, wherein one side (test surfaces) then requires to continue to use standard metallographic method
1000#~5000# sand paper is polished；Thin sample gluing is mechanically polished to surface-brightening, Ran Houyong with 502 in iron block surface
Acetone soak removes chip sample, by it in alcohol and acetone sonic oscillation fully clean it is standby.Sample shape after mechanical polishing
1. number sample in looks such as Fig. 1.
(2) electrobrightening Preparatory work of experiment：
By perchloric acid 5%, methanol 60%, n-butanol 35% (being volume ratio) configuration electrolyte 700ml；According to hair
Bright content (2) step builds electrobrightening experiment porch, electrolyte as in 1L beakers, pour into liquid nitrogen make electrolyte be cooled to-
25 DEG C or so；Power-on is adjusted to 30V, opens magnetic stirring apparatus, clamps sample with tweezers, gets out manual time-keeping, prepare into
Row electrobrightening.Clamp, whole strip surface can effectively be polished along long extreme direction.
(3) electrolysis processing and cleaning-drying：
Start electrobrightening, timing time 45s；Tweezers clamp sample as in electrolyte so that initial current is
1.1A or so, sample is moved horizontally in polishing process, but avoid enter into whirlpool region, elapsed over time, it is found that electric current is gradual
It is decreased to below 1A；Take out sample immediately to the stipulated time to be put into alcohol, and carry out cleaned by ultrasonic vibration 5min as early as possible, connect
Get off and be placed in sonic oscillation 5min in acetone again；Surface is dried up with air duct rapidly after taking out sample with clean tweezers, avoids staying
The lower marking；Sample is stored using filter paper or sample cell, standby to be analyzed in EBSD.The 2. number sample of sample such as Fig. 1 after electrobrightening
Shown in product.From Fig. 1 1. and 2. number sample can be seen that electrobrightening after sample surfaces seem unlike mechanical polishing
Light, rule of thumb this belongs to normal phenomenon, though the special bright sample in surface can not be carried out subsequently after electrobrightening
EBSD is tested.
(4) EBSD tests electrobrightening effect：
Analysis test is carried out to electrobrightening sample using 1000 × multiplication factor and 0.35 μm of step-length.As a result image is shown
Demarcation rate reaches more than 95% (being caused by sample itself defect in the unidentified region in result), and Fig. 2 is to be done according to test result
The pole figure of the contrast figure, unique crystal grain color diagram and the principal phase γ phases that go out.
The electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis is can be seen that from this embodiment, is operated
Simplicity, significant effect.
Embodiment 2
In the present embodiment, for the sheet titanium aluminium base alloy I-shaped part by room temperature tensile, using electrolytic polishing method system
Standby EBSD sample for analysis, comprises the following steps：
(1) preparation of samples：
Lower fritter is broken at gauge length with pliers, (1.9mm is height of specimen to about 6mm × 5mm × 1.9mm, is tested as EBSD
In ND directions), two itself smoothers of 6mm × 5mm faces of sample (I-shaped part two sides using 800# sand paper polish), as above
Test surfaces are subjected to standard gold phase processor, polished using 1000#~7000# sand paper；Machinery is carried out using specimen holder clamping sample
Polishing；Then by sample in alcohol and acetone sonic oscillation fully clean it is standby.
(2) electrobrightening Preparatory work of experiment：
By perchloric acid 7%, methanol 59%, n-butanol 34% (being volume ratio) configuration electrolyte 700ml；According to hair
Bright content (2) step builds electrobrightening experiment porch, electrolyte as in 1L beakers, pour into liquid nitrogen make electrolyte be cooled to-
30℃；Power-on modulates 30V, opens magnetic stirring apparatus, tweezers clamping sample, gets out manual time-keeping, be ready for being electrolysed
Polishing.
(3) electrolysis processing and cleaning-drying：
Start electrobrightening, start timing, time 50s；Tweezers clamping sample is placed in electrolyte so that initial current
For 1.2A or so, transverse shifting sample in polishing process, elapse over time, it is found that electric current is also gradually decrease to below 1A；Arrive
Stipulated time takes out sample and is put into alcohol immediately, and cleaned by ultrasonic vibration 4min, is next placed in ultrasound in acetone again and shakes
Swing 5min；Surface is dried up after taking out sample with clean tweezers with air duct rapidly；Sample is stored using filter paper or sample cell, standby
Analyzed in EBSD.Sample after electrobrightening is as shown in Fig. 1 3. number sample.From Fig. 1 1. and 3. number sample it is also seen that
Sample surfaces after electrobrightening unlike mechanical polishing light, it is similar to the situation in example 1.
(4) EBSD tests electrobrightening effect：
Still analysis test is carried out to electrobrightening sample using 1000 × multiplication factor and 0.35 μm of step-length.As a result show
It is the Eulerian angles figure and phasor made according to test result that image calibration rate, which reaches more than 96%, Fig. 3,.
The electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis is can be seen that from this embodiment, is operated
Simply, work well.
Embodiment 3
In the present embodiment, for the sheet titanium aluminium base alloy I-shaped part by drawing by high temperature, using electrolytic polishing method system
Standby EBSD sample for analysis, comprises the following steps：
(1) preparation of samples：
For drawing by high temperature sample, because, there occurs superplastic deformation, the guage section of sample is in length under the experiment condition
Strip, lower fritter is broken with pliers, about 10mm × 3mm × 0.5mm (10mm length directions are RD directions, and draw direction)；Such as
On, the non-test face oxide layers of one of 10mm × 3mm are ground off, to test surfaces carry out standard gold phase processor, using 800#~
7000# sand paper is polished, and is sticked at metal derby surface and is mechanically polished；Polishing finishes, and it is ultrasonic in alcohol and acetone to remove sample
Vibration is cleaned standby.
(2) electrobrightening Preparatory work of experiment：
By perchloric acid 6%, methanol 60%, n-butanol 34% (being volume ratio) configuration electrolyte 700ml；According to hair
Bright content (2) step builds electrobrightening experiment porch, and electrolyte is placed in 1L beakers, pour into liquid nitrogen make electrolyte be cooled to-
27 DEG C or so；Power-on, voltage are adjusted to 30V, open magnetic stirring apparatus, tweezers clamping sample, get out manual time-keeping, prepare
Carry out electrobrightening.For this kind of strip sample, necessarily clamping the long end of sample with tweezers can have to whole strip surface
Effect polishing.
(3) electrolysis processing and cleaning-drying：
Start electrobrightening, timing time 45s；Tweezers clamping sample is placed in electrolyte so that initial current is
1.0A or so, transverse shifting sample in polishing process, is elapsed over time, it is found that electric current is also gradually decrease to about 0.5A or so；
Sample is taken out immediately to the stipulated time to be put into alcohol, and sonic oscillation cleaning 5min, ultrasound in acetone is next placed in again shakes
Swing 4min；Surface is dried up after taking out sample with clean tweezers with air duct rapidly；Sample is stored using filter paper or sample cell, standby
Analyzed in EBSD.Sample after electrobrightening is as shown in Fig. 1 4. number sample.From Fig. 1 1. and 4. number sample it is also seen that
Sample surfaces after electrobrightening seem the light unlike mechanical polishing, similar to the situation in example 1.
(4) EBSD tests electrobrightening effect：
EBSD test results are carried out using 1000 × multiplication factor and 0.4 μm of step-length to electrobrightening sample to show, image
It is the dynamic recrystallization figure and inverse pole figure made according to test result that demarcation rate, which reaches more than 98%, Fig. 4,.
The electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis is can be seen that from this embodiment, is operated
Simplicity, excellent effect, and do not influenceed by sample shape change.
Claims (9)
1. a kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis, it is characterised in that comprise the following steps：
(1) sample processing early stage
Sample, line cutting slow wire feeding are cut using wire cutting or water knife；Sample size is cut in 10mm × 10mm × below 5mm,
Wherein 5mm is the limiting value of height of specimen, and the direction is the ND directions during sample test；Wipe out surface and oil contaminant, two
Bottom surface is polished using 40#~400# sand paper, one of face be test surfaces according to standard metallographic prepare method continue using 800#~
7000# sand paper is polished, and is first mechanically polished；Next, surface and oil contaminant is thoroughly cleaned using alcohol, acetone sonic oscillation；
(2) portable unit is built
The part of electrobrightening equipment include power supply, magnetic stirring apparatus, wire and stainless steel plate, thermometer, corrosive liquid and
Liquid nitrogen；Building method is：Wire one end connection stainless steel plate is placed in beaker bottom, wire other end connection power cathode, burns
Electrolyte is put into cup, and cooling and thermometer thermometric are carried out using liquid nitrogen, electrolyte stirred using magnetic stirring apparatus, power supply
Positive pole connects polished sample with tweezers by wire；
(3) electrolyte configures
According to volume ratio, perchloric acid 4%~12%, methanol 55%~65%, n-butanol surplus；
(4) electrolysis processing and cleaning-drying
Titanium aluminium base alloy sample uses tweezers as anode, stainless steel plate as negative electrode, power-on and magnetic stirring apparatus, sample
Clamping, is placed in electrolyte, and polished face is relative with stainless steel plate；During electrobrightening, temperature control -30 DEG C~-
20 DEG C, voltage control is controlled in 40s~55s in 25V~35V, polishing time；It is put into absolute ethyl alcohol, exists side by side at once after polishing
Sonic oscillation is carried out, then is placed in acetone and carries out sonic oscillation；Finally picked up with tweezers and quickly dry up surface with blower fan.
2. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that sample size (5~7) mm × (3~6) mm × (2~4) mm cut in step (1), wherein (2~4) mm is
The ND directions of short transverse, i.e. EBSD test, sample length and width are inconsistent in favor of the RD directions of identification EBSD tests.
3. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that in step (2), according to sample size and sample concrete condition, beaker volume is 1L, and electrolyte configures altogether
700ml, 10cm diameter stainless steel plates are coordinated to be placed in electrolyte bottom as negative electrode, stainless steel plate is with wire interconnecting piece point using life
Adhesive tape and anticorrosion adhesive plaster wrap up for more than two layers.
4. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 3, its feature exists
In negative electrode stainless steel plate selects 304 stainless steels.
5. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that in step (3), according to volume ratio, perchloric acid 5%~7%, methanol 60%, n-butanol surplus.
6. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that in step (4), voltage control is 30V.
7. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that in step (4), when electrobrightening starts temperature control at -30 DEG C~-25 DEG C, the electrobrightening time be 45s~
50s。
8. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that in step (4), during electrobrightening, magnetic stirring apparatus is located at electrolyte bottom, adjusts magnetic stirring apparatus, makes
Rotor drives electrolyte to form the whirlpool run through up and down, and the bubble of sample surfaces is attached in polishing process of taking, and improves polishing
Effect.
9. according to the electrobrightening preparation method of the titanium aluminium base alloy EBSD sample for analysis described in claim 1, its feature exists
In, it is preferred that in step (4), during electrobrightening, sample is clamped using tweezers, the height apart from stainless steel plate should cause
Sectional area 0.6cm2~1cm2Sample, its initial current is in 0.9A~1.2A scopes.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1358240A (en) * | 1999-06-25 | 2002-07-10 | 欧洲核研究组织 | Bath composition for electropolishing of titanium and method for using same |
| CN102899711A (en) * | 2012-11-20 | 2013-01-30 | 重庆大学 | Electrolytic polishing solution for titanium and titanium alloys and electrolytic polishing process |
-
2017
- 2017-07-24 CN CN201710604923.1A patent/CN107402150A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1358240A (en) * | 1999-06-25 | 2002-07-10 | 欧洲核研究组织 | Bath composition for electropolishing of titanium and method for using same |
| CN102899711A (en) * | 2012-11-20 | 2013-01-30 | 重庆大学 | Electrolytic polishing solution for titanium and titanium alloys and electrolytic polishing process |
Non-Patent Citations (2)
| Title |
|---|
| 李华清 等: "钛合金材料OIM 试样的电解抛光及制备工艺", 《钛工业进展》 * |
| 林均品 等: "大尺寸铸造高铌TiAl合金的组织和拉伸性能", 《2004年材料科学与工程进展》 * |
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