CN106404501A - Electrolytic corrosive agent of industrial pure titanium TA2 and electrolytic polishing corrosion method - Google Patents
Electrolytic corrosive agent of industrial pure titanium TA2 and electrolytic polishing corrosion method Download PDFInfo
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- CN106404501A CN106404501A CN201610763735.9A CN201610763735A CN106404501A CN 106404501 A CN106404501 A CN 106404501A CN 201610763735 A CN201610763735 A CN 201610763735A CN 106404501 A CN106404501 A CN 106404501A
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- pure titanium
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses an electrolytic corrosive agent of industrial pure titanium TA2 and an electrolytic polishing corrosion method, and belongs to the field of metallographic structure detection in an industrial pure titanium physical and chemical detection technology. The method comprises the following steps: 1) grinding and cleaning pretreated industrial pure titanium TA2 to prepare a to-be-corroded test sample; and 2) performing electrolytic polishing corrosion method on the surface of the to-be-corroded test sample by the electrolytic corrosive agent. The electrolytic corrosive agent is simple in preparation, good in corrosion effect and pollution-free; and the industrial pure titanium TA2 is subjected to metallographic examination, so that the microscopic structure of the industrial pure titanium TA2 can be displayed well, and the microstructure of the TA2, the form of alpha phase, the grain boundary and the like can be reflected objectively. The electrolytic polishing corrosion method is good in effect, stable in corrosion process, good in display effect of the microstructure of the test sample after corrosion, and high in operability.
Description
Technical field
The invention belongs to metallographic structure detection field is and in particular to a kind of industrially pure titanium in industrially pure titanium physico-chemical examination technique
The electrolytic etching agent of TA2 and electrobrightening caustic solution.
Background technology
Titanium and its titanium alloy have more and more been applied to field of aerospace, and because its density ratio steel is light, machinery is strong
Degree is but similar to steel and heat-resist, therefore, obtains the concern of more and more people.Titanium and its alloy are according to its ambient-temp-stable
Mutually it is divided into：Alpha titanium alloy, alpha-beta diphasic titanium alloy and beta-titanium alloy, in addition, also two big class：Near αtitanium alloy and nearly β titanium close
Gold.Alpha titanium alloy is but existed to the difficulty of metallographic preparation, and industrially pure titanium is just more difficult to prepare due to its flexibility.Industry
Pure titanium needs lower removal rates and polishing speed in sample preparation.Excessive grinding and polishing process can be in the metallographic section of alpha titanium alloy
Upper generation deformation twin.Pure titanium can produce grinding and polishing vestige with grinding and polishing direction during grinding and polishing, similar to metal surface flowing
Phenomenon.Due to during Mechanical polishing, it is impossible to meet the evaluation of metallographic sample well, electrolytic etching polishing is as a kind of new
Technology of preparing obtain the favor of more and more testing crews.
Electrolytic etching polishing is the principle by electrochemistry, industrially pure titanium is carried out the electrolysis on surface, so far reaches sample
The effect of product polishing etch.It can be very good the specimen surface cut that will produce during traditional mechanical grinding and polishing, surface metal
Flowing phenomenon eliminate, and can be clear the metallographic structure of industrially pure titanium is presented.
Industrial pure titanium TA2, in terms of electrobrightening, yet there are no the electrobrightening agent of fine polishing effect, all the time
Few people are studied, and its conventional etchant solution is：Distilled water 85ml+ Fluohydric acid. 10ml+ nitric acid 5ml.Generally speaking right
In biphase titanium alloy, the effect of this caustic is fine, but the corrosive effect for industrial pure titanium TA2 is unsatisfactory, and
When sample just can see its tissue in the intact situation of grinding and polishing.Artificial craft carries out grinding and polishing needs operator to have good work
To prepare as experience, but the bad operation for new experiment operator.
Content of the invention
It is an object of the invention to provide a kind of electrolytic etching agent of industrial pure titanium TA2 and electrobrightening caustic solution, should
Electrolytic etching agent corrosive effect is good, pollution-free, stability strong, and compound method is quick, efficiently；This electrobrightening caustic solution effect
Good, steadily, after corrosion, sample tissue pattern display effect is good, workable for corrosion process.
The present invention is to be achieved through the following technical solutions：
A kind of electrolytic etching agent of industrial pure titanium TA2, in this electrolytic etching agent, HF：CH3CH2OH：The volume ratio of water is：
(8-10):(19-21):(35-37)；And it has been also added with (NH- in this electrolytic etching agent4)2S2O8, addition is：Every 8-10mL
HF adds 1-1.2g (NH4)2S2O8.
Water is distilled water.
The invention also discloses a kind of electrobrightening caustic solution of industrial pure titanium TA2, comprise the following steps：
1) pretreated industrial pure titanium TA2 is ground and cleaning treatment, makes and treat corrosion sample；
2) electrobrightening corrosion treatmentCorrosion Science is carried out treating corrosion sample surface using electrolytic etching agent；
Wherein, in described electrolytic etching agent, HF：CH3CH2OH：The volume ratio of water is (8-10):(19-21):(35-37)；
And it has been also added with (NH in this electrolytic etching agent4)2S2O8, addition is：Every 8-10mL HF adds 1-1.2g (NH4)2S2O8；
Described electrobrightening corrosion treatmentCorrosion Science condition is：
Polishing voltage：45-55V, flow of electrolyte 15-25, polishing time 45-55s；
Corrosion potentials：20-25V, flow of electrolyte 15-25, etching time 3-7s.
Step 1) described in grinding be to be ground with the water-proof abrasive paper of 120#, 320#, 600# or 1000# successively, and often
One grinding will be read sample after terminating and be carried out, the residual abrasive material of one procedure in elimination.
Pretreated industrial pure titanium TA2 is to be inlayed the industrial pure titanium TA2 of annealed state with dental base acrylic resin powder and then solidify
Gained.
Water is distilled water.
Compared with prior art, the present invention has following beneficial technique effect：
The electrolytic etching agent of industrial pure titanium TA2 disclosed by the invention, in electrolytic etching agent, HF is a kind of very strong oxygen of acidity
Agent, adds (NH4)2S2O8Be to play the effect strengthening HF oxidisability, and ethanol is then to merge both well
Together, as a kind of diluent.This electrolytic etching agent is prepared simply, and erosion effect is good, pollution-free, and industrial pure titanium TA2 is entered
Row metallographic examination, can preferably show the microscopic structure of industrial pure titanium TA2, can objectively reflect the tissue topography of TA2,
The form of α phase and grain boundary etc..
The electrobrightening caustic solution of industrial pure titanium TA2 disclosed by the invention, using electrochemical corrosion to milled processed after
TA2 surface corroded, polish voltage：45-55V, flow of electrolyte 15-25, polishing time 45-55s；Corrosion potentials：20-
25V, flow of electrolyte 15-25, etching time 3-7s.Then observe its microscopic structure under an optical microscope；The method can
Clearly detect depleted layer, provide intuitively Detection results for metallographic method detection depleted layer, and corrosive effect is preferably, be a kind of inspection
Survey the effective ways of industrial pure titanium TA2, do not interfere with the metallographic testing result of TA2.
Brief description
Fig. 1 is the corrosive effect figure after the embodiment of the present invention 1 electrobrightening corrosion treatmentCorrosion Science；
Fig. 2 is the corrosive effect figure after comparative example 1 of the present invention electrobrightening corrosion treatmentCorrosion Science；
Fig. 3 is the corrosive effect figure after comparative example 2 of the present invention electrobrightening corrosion treatmentCorrosion Science；
Fig. 4 is the corrosive effect figure after comparative example 3 of the present invention electrobrightening corrosion treatmentCorrosion Science；
Fig. 5 is the corrosive effect figure after comparative example 4 of the present invention electrobrightening corrosion treatmentCorrosion Science.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, described be explanation of the invention and
It is not to limit.
The invention provides a kind of electrobrightening caustic solution of industrial pure titanium TA2, described method is to use electrochemistry
Corrosion is corroded to the TA2 surface after milled processed, and the polishing etch time is 50s, then observes it under an optical microscope
Microscopic structure；Substantial amounts of test is carried out by the formula of change electrolytic etching solvent, standing time, etch time etc., finally
It is concluded that：Using the present invention (No. 1) electrolytic etching agent it can be deduced that tissue is clear, the clearly demarcated polishing etch in grain boundary
Effect.
No. 1 bath composition is：HF：90ml, (NH4)2S2O8：10g, CH3CH2OH：200ml, distilled water：360ml；
Meanwhile, in process of the present invention, give the electrolytic etching agent of two comparative examples, the effect of its electrobrightening corrosion is all
The metallographic structure of TA2 clearly cannot be displayed.
No. 2 electrolytic etching agent：Proportioning is HF:HNO3:H2O=1：2：3 (volume ratios)；
No. 3 electrolytic etching agent：Proportioning is HF:CH2CH3OH:H2O=1：2：4 (volume ratios).
No. 2 caustic are to be improved on the basis of conventional titanium alloy caustic, and No. 3 caustic are then to corrode at No. 2
On the basis of agent, carry out the contrast caustic that the replacing of solution ratio thing obtains.
Embodiment 1
By the industrial pure titanium TA2 of annealed state, inlayed using dental base acrylic resin powder, according to the preparation side of metallographic specimen after solidification
Method, adopts 120# successively, and the sand paper of 320#, 600# (1000#) is ground.Change grinding direction and upper track sand paper after sand paper
Polishing scratch is vertical, and the polishing scratch of last process is removed.After every kind of sand paper grinds end, all sample should be carried out, it is to avoid
The residual abrasive material of upper one procedure is remained in next process, to protect sample surfaces.
Grind the sample finishing, using No. 1 electrolytic etching agent (HF：90ml, (NH4)2S2O8：10g, CH3CH2OH：200ml,
Distilled water：360ml) carry out electrolytic etching, electrolytic etching parameter is：Polishing voltage：50V, flow of electrolyte：20, electrobrightening
Etching time 50s；Corrosion potentials：25V, flow of electrolyte 20, etching time 5s.Corrosive effect is shown in Fig. 1, it will be seen from figure 1 that
Metallographic structure is clear, and the effect of the clearly demarcated polishing etch in grain boundary can clean the tissue crystal grain finding out TA2, essentially isometry
α phase.
Comparative example 1
By the industrial pure titanium TA2 of annealed state, inlayed using dental base acrylic resin powder, according to the preparation side of metallographic specimen after solidification
Method, adopts 120# successively, and the sand paper of 320#, 600# (1000#) is ground.Change grinding direction and upper track sand paper after sand paper
Polishing scratch is vertical, and the polishing scratch of last process is removed.After every kind of sand paper grinds end, all sample should be carried out, it is to avoid
The residual abrasive material of upper one procedure is remained in next process, to protect sample surfaces.
Grind the sample finishing, using No. 2 electrolytic etching agent (HF:HNO3:H2O=1：2：3 (volume ratios)) carry out electrolysis corruption
Lose, electrolytic etching parameter is：Polishing voltage：40V, flow of electrolyte：20, polishing time 8s；Corrosion potentials：25V, is electrolysed liquor stream
Amount 20, etching time 5s.Corrosive effect is shown in Fig. 2；Some grain boundaries can indistinctly be found out from the corrosive effect of in figure, but not complete
Whole, tissue morphology also has some fuzzy it is impossible to the tissue overall picture of very satisfactory display TA2.
Comparative example 2
By the industrial pure titanium TA2 of annealed state, inlayed using dental base acrylic resin powder, according to the preparation side of metallographic specimen after solidification
Method, adopts 120# successively, and the sand paper of 320#, 600# (1000#) is ground.Change grinding direction and upper track sand paper after sand paper
Polishing scratch is vertical, and the polishing scratch of last process is removed.After every kind of sand paper grinds end, all sample should be carried out, it is to avoid
The residual abrasive material of upper one procedure is remained in next process, to protect sample surfaces.
Grind the sample finishing, using No. 2 electrolytic etching agent (HF:HNO3:H2O=1：2：3 (volume ratios)) carry out electrolysis corruption
Lose, electrolytic etching parameter is：Polishing voltage：40V, flow of electrolyte：15, polishing time 8s；Corrosion potentials：25V, is electrolysed liquor stream
Amount 20, etching time 5s.Corrosive effect is shown in Fig. 3；It can be seen that more a little better than Fig. 2 corrosive effect, crystal grain shows
Come, but there is the relief sensation after corrosion, still there is the illusion after some corrosion, fail all to present tissue morphology
Come.
Comparative example 3
By the industrial pure titanium TA2 of annealed state, inlayed using dental base acrylic resin powder, according to the preparation side of metallographic specimen after solidification
Method, adopts 120# successively, and the sand paper of 320#, 600# (1000#) is ground.Change grinding direction and upper track sand paper after sand paper
Polishing scratch is vertical, and the polishing scratch of last process is removed.After every kind of sand paper grinds end, all sample should be carried out, it is to avoid
The residual abrasive material of upper one procedure is remained in next process, to protect sample surfaces.
Grind the sample finishing, using No. 3 electrolytic etching agent (HF:CH2CH3OH:H2O=1：2：4 (volume ratios)) carry out electricity
Solution is corroded, and electrolytic etching parameter is：Polishing voltage：45V, flow of electrolyte：15, polishing time 16s；Corrosion potentials：25V, electricity
Solution flow quantity 20, etching time 5s.Corrosive effect is shown in Fig. 4；It can be seen that corrosive effect is substantially not so good as first three width figure imitating
Really good, and the cut in rough grinding pass also clearly exists, the electrobrightening effect on driving birds is not good of this caustic.Crystal grain indistinctly presents
Out it is impossible to good recognize.
Comparative example 4
By the industrial pure titanium TA2 of annealed state, inlayed using dental base acrylic resin powder, according to the preparation side of metallographic specimen after solidification
Method, adopts 120# successively, and the sand paper of 320#, 600# (1000#) is ground.Change grinding direction and upper track sand paper after sand paper
Polishing scratch is vertical, and the polishing scratch of last process is removed.After every kind of sand paper grinds end, all sample should be carried out, it is to avoid
The residual abrasive material of upper one procedure is remained in next process, to protect sample surfaces.
Grind the sample finishing, using No. 3 electrolytic etching agent (HF:CH2CH3OH:H2O=1：2：4 (volume ratios)) carry out electricity
Solution is corroded, and electrolytic etching parameter is：Polishing voltage：45V, flow of electrolyte：15, polishing time 30s；Corrosion potentials：25V, electricity
Solution flow quantity 20, etching time 5s.Corrosive effect is shown in Fig. 5；It can be seen that there is relief in the crystal grain after electrolytic etching
There is the mottling of black around sense, and clear crystal grain, and yet suffer from the grain structure that some are not electrolysed out.
In sum, the electrobrightening caustic solution of the industrial pure titanium TA2 that the present invention provides, has an advantage in that：By adopting
With the caustic solution of the present invention, can clearly depleted layer, provide intuitively Detection results for metallographic method detection depleted layer.
Claims (6)
1. a kind of electrolytic etching agent of industrial pure titanium TA2 is it is characterised in that in this electrolytic etching agent, HF：CH3CH2OH：The body of water
Long-pending ratio is：(8-10):(19-21):(35-37)；And it has been also added with (NH in this electrolytic etching agent4)2S2O8, addition is：Often
8-10mL HF adds 1-1.2g (NH4)2S2O8.
2. the electrolytic etching agent of industrial pure titanium TA2 according to claim 1 is it is characterised in that water is distilled water.
3. a kind of electrobrightening caustic solution of industrial pure titanium TA2 is it is characterised in that comprise the following steps：
1) pretreated industrial pure titanium TA2 is ground and cleaning treatment, makes and treat corrosion sample；
2) electrobrightening corrosion treatmentCorrosion Science is carried out treating corrosion sample surface using electrolytic etching agent；
Wherein, in described electrolytic etching agent, HF：CH3CH2OH：The volume ratio of water is (8-10):(19-21):(35-37)；And
It has been also added with (NH in this electrolytic etching agent4)2S2O8, addition is：Every 8-10mL HF adds 1-1.2g (NH4)2S2O8；
Described electrobrightening corrosion treatmentCorrosion Science condition is：
Polishing voltage：45-55V, flow of electrolyte 15-25, polishing time 45-55s；
Corrosion potentials：20-25V, flow of electrolyte 15-25, etching time 3-7s.
4. the electrobrightening caustic solution of industrial pure titanium TA2 according to claim 3 is it is characterised in that step 1) described
Grinding be to be ground with the water-proof abrasive paper of 120#, 320#, 600# or 1000# successively, and every grind together terminate after will
Read sample to be carried out, the residual abrasive material of one procedure in elimination.
5. the electrobrightening caustic solution of industrial pure titanium TA2 according to claim 3 is it is characterised in that pretreated
Industrial pure titanium TA2 is to be inlayed the industrial pure titanium TA2 of annealed state with dental base acrylic resin powder and then solidified gained.
6. the electrobrightening caustic solution of industrial pure titanium TA2 according to claim 3 is it is characterised in that water is distilled water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112342604A (en) * | 2020-09-25 | 2021-02-09 | 深圳市裕展精密科技有限公司 | Metal product and preparation method thereof, and metal composite and preparation method thereof |
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| CN102939407A (en) * | 2010-03-18 | 2013-02-20 | 三星显示有限公司 | Etchant for metal wiring and method for manufacturing metal wiring using the same |
| CN105102584A (en) * | 2013-03-04 | 2015-11-25 | 高级技术材料公司 | Compositions and methods for selectively etching titanium nitride |
| CN105836698A (en) * | 2016-04-15 | 2016-08-10 | 首都师范大学 | Preparation method of gold-titanium dioxide composite nano-tube array and gold nano-tube array electrode |
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2016
- 2016-08-29 CN CN201610763735.9A patent/CN106404501A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793426A (en) * | 2005-12-30 | 2006-06-28 | 东北大学 | Process for copper coating on surface of magnesium and magnesium alloy |
| CN101597488A (en) * | 2009-06-26 | 2009-12-09 | 中国石油天然气股份有限公司 | High solid phase drilling fluid filter cake removal treating fluid |
| CN102939407A (en) * | 2010-03-18 | 2013-02-20 | 三星显示有限公司 | Etchant for metal wiring and method for manufacturing metal wiring using the same |
| CN105102584A (en) * | 2013-03-04 | 2015-11-25 | 高级技术材料公司 | Compositions and methods for selectively etching titanium nitride |
| CN105836698A (en) * | 2016-04-15 | 2016-08-10 | 首都师范大学 | Preparation method of gold-titanium dioxide composite nano-tube array and gold nano-tube array electrode |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112342604A (en) * | 2020-09-25 | 2021-02-09 | 深圳市裕展精密科技有限公司 | Metal product and preparation method thereof, and metal composite and preparation method thereof |
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