CN105063400A - Preparation method for nanometer porous titanium - Google Patents
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- CN105063400A CN105063400A CN201510590199.2A CN201510590199A CN105063400A CN 105063400 A CN105063400 A CN 105063400A CN 201510590199 A CN201510590199 A CN 201510590199A CN 105063400 A CN105063400 A CN 105063400A
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Abstract
The invention relates to a preparation method for nanometer porous titanium, and aims to solve the problem that a conventional preparation method is more complex, high in cost and unfavorable for engineering application. The method comprises the following steps of 1, preparing a precursor: performing linear cutting and pre-grinding machine grinding treatment on a TixAly intermetallic compound precursor to obtain a 10 to 200-micron de-alloying test sample; 2, performing de-alloying: performing de-alloying treatment on the de-alloying test sample obtained in step 1 to obtain a de-alloyed test sample; 3, performing subsequent treatment: taking out the de-alloyed test sample, repeatedly flushing the de-alloyed test sample with de-ionized water, placing the de-alloyed test sample in absolute ethyl alcohol, ultrasonically washing the de-alloyed test sample for 8 to 10min to remove other remaining impurity attachments, placing the test sample in a wet state in a vacuum drying oven, and drying the test sample for 5 to 8h to obtain nanometer porous titanium. The method is used for preparing nanometer porous titanium.
Description
Technical field
The present invention relates to a kind of preparation method of nanoporous titanium.
Background technology
Nano-porous materials, since appearance, has had been a great concern because it has many excellent properties.Now prove that nano-porous materials has huge potential using value in fields such as photochemical catalysis, chemical catalysis, electrode materials, activation, sensing, selective filter, damping noise reduction, environment protection, surface enhanced Raman scatterings (SERS) by experiment, these all give the credit to the pore passage structure of the very big specific surface area of nano-porous materials and its uniqueness had.
What current research was more is utilize corresponding alloy as presoma, by the preparation of the method for removal alloying have Pt, the Au of nanoscale, Ag, etc. the porous material of noble metal.In recent years, for consideration economically, some material supplier authors start then utilize non-noble metal alloy to prepare corresponding nano-porous materials, such as np-Cu, np-Ni, np-Pb, np-Nb, np-Mn etc.The presoma that existing removal alloying legal system uses for nano-porous materials mostly is sosoloid, and it is less to the research of single-phase intermetallic compound, and existing achievement in research pays attention to the analysis of Formation rule to its three-dimensional porous structure and chemical property, the many angles from diffusion of formation mechenism for nano-porous structure make an explanation, and research not deep too much to the crystal structure transition of presoma alloy in removal alloying process.The overwhelming majority utilizes removal alloying legal system to be also only confined to laboratory study for nano-porous materials, does not realize engineer applied.
Summary of the invention
The present invention will solve that existing preparation method is more complicated and cost is high, is unfavorable for the problem of engineer applied, and provides a kind of preparation method of nanoporous titanium.
The preparation method of a kind of nanoporous titanium of the present invention specifically carries out according to the following steps:
One, presoma is prepared: by Ti
xal
yintermetallic compound presoma adopts Linear cut and pre-mill to grind and processes, obtain thickness be 10 μm ~ 200 μm remove alloy sample;
Two, removal alloying: be that the alloy sample that goes of 10 μm ~ 200 μm carries out removal alloying process by the thickness obtained in step one, obtain the sample after removal alloying;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120 ~ 150s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 8min ~ 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 5h ~ 8h, can obtain nanoporous titanium.
Principle of the present invention: the present invention utilizes Ti
3al, TiAl, TiAl
3intermetallic compound, as presoma, prepares nanoporous titanium by the method for removal alloying, mainly contains two innovative points.Innovative point one adopts single-phase intermetallic compound instead of sosoloid as presoma, particularly utilizes Ti
3al, TiAl, TiAl
3three kinds of intermetallic compounds prepare nanoporous titanium does not also have bibliographical information; Innovative point two is compared with precious metal, and Ti is " low-priced " metal, both economical, and compared with other base metal, the density of Ti is little, corrosion resisting property good.Nanoporous titanium has very excellent performance in catalysis, sensing, gas storage and absorption etc.
Biocompatibility is the distinctive character of titanium or titanium alloy, but the Young's modulus of the titanium of densification or titanium alloy does not mate with natural skeleton, and its tensile strength, ultimate compression strength and bending strength are all much higher than people bone, load can be caused can not well to import adjacent bone tissue into by implant, form stress shielding, cause around implant and occur bone stress absorbing phenomenon, finally cause loosening and fracture of implant.And by removal alloying, fine and close titanium is become the titanium with nano-porous structure, implant can be made more close to intensity and the Young's modulus of people's bone, unique nano-porous structure is conducive to osteoblastic adhesion, propagation and differentiation, new bone tissue is impelled to grow into hole, make to form biological fixation between implant and bone, and a final formation entirety.
Beneficial effect of the present invention: process of the present invention is simple, and experimental installation and starting material are easy to get, easily-controlled experimental conditions; Traditional precious metal is compared, titanium belongs to " low-priced " metal, and therefore compared with other precious metal porous material, nanoporous titanium can reduce costs effectively; Other " low-priced " metallographic phase ratio, the advantages such as it is high that titanium has specific tenacity, and corrosion resisting property is good, therefore nanoporous titanium can be applied in the rugged environments such as soda acid.Titanium or titanium alloy is fabulous biomaterial, and nanoporous titanium has more wide application prospect at medical field; Nanoporous titanium is made ultracapacitor, finds that its ratio capacitance is up to 38.5F/g.
Accompanying drawing explanation
Fig. 1 is the surface topography map of the nanoporous titanium that embodiment one obtains;
Fig. 2 is the surface topography map of the nanoporous titanium that embodiment two obtains;
Fig. 3 is the surface topography map of the nanoporous titanium that embodiment five obtains;
Fig. 4 is the surface topography map of the nanoporous titanium that embodiment six obtains.
Embodiment
Embodiment one: the preparation method of a kind of nanoporous titanium of present embodiment specifically carries out according to the following steps:
One, presoma is prepared: by Ti
xal
yintermetallic compound presoma adopts Linear cut and pre-mill to grind and processes, obtain thickness be 10 μm ~ 200 μm remove alloy sample;
Two, removal alloying: be that the alloy sample that goes of 10 μm ~ 200 μm carries out removal alloying process by the thickness obtained in step one, obtain the sample after removal alloying;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s ~ 150s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 8min ~ 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 5h ~ 8h, can obtain nanoporous titanium.
Ti described in present embodiment step one
xal
yintermetallic compound presoma by casting pure Al and pure Ti, forging, rolling and to get rid of band obtained.
Described in present embodiment step 2, removal alloying is also named selective corrosion, refer to that each element of component alloy or the potential difference respectively between phase differ larger, by chemistry or electrochemical action, relatively active alloying element is dissolved, and remaining inert element is by the diffusion of atom, from recombination, formed there is nanoscale three-dimensional, continuously, the vesicular structure of opening.For Ti-Al system alloy, can be determined by inquiry mark electropotential handbook, the hydrogen mark electromotive force of Al is-2.300V, and in basic solution, be-0.882V by calculating the hydrogen mark electromotive force that can draw Ti, between visible Ti and Al two kinds of elements, there is larger electropotential difference, meet the condition that removal alloying occurs, therefore can obtain nanoporous titanium by the method for chemical removal alloying process or the process of electrochemistry removal alloying.
Present embodiment process is simple, and experimental installation and starting material are easy to get, easily-controlled experimental conditions; Traditional precious metal is compared, titanium belongs to " low-priced " metal, and therefore compared with other precious metal porous material, nanoporous titanium can reduce costs effectively; Other " low-priced " metallographic phase ratio, the advantages such as it is high that titanium has specific tenacity, and corrosion resisting property is good, therefore nanoporous titanium can be applied in the rugged environments such as soda acid.Titanium or titanium alloy is fabulous biomaterial, and nanoporous titanium has more wide application prospect at medical field; Nanoporous titanium is made ultracapacitor, finds that its ratio capacitance is up to 38.5F/g.
Embodiment two: present embodiment and embodiment one are unlike Ti described in step one
xal
yintermetallic compound is Ti
3al, TiAl or TiAl
3.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the process of removal alloying described in step 2 be by the thickness obtained in step one be 10 μm ~ 200 μm go alloy sample to be placed in corrosive fluid to carry out chemical removal alloying process; Acidic solution or the concentration of described corrosive fluid to be concentration be 0.1mol/L ~ 10mol/L are the basic solution of 0.1mol/L ~ 10mol/L, and the temperature of removal alloying process is 15 DEG C ~ 95 DEG C, and the time of removal alloying process is 2h ~ 120h.Other is identical with embodiment one or two.
Embodiment four: present embodiment and embodiment three are unlike the acidic solution of: described corrosive fluid to be concentration be 1mol/L ~ 5mol/L; Described acidic solution is HCl solution, H
2sO
4solution or HNO
3solution.Other is identical with embodiment three.
Embodiment five: present embodiment and embodiment three to four are unlike the basic solution of: described corrosive fluid to be concentration be 1mol/L ~ 5mol/L; Described basic solution is NaOH solution or KOH solution.Other is identical with embodiment three to four.
Embodiment six: one of present embodiment and embodiment one to five are be that the voltage of-2.5V ~ 3V that goes alloy sample to put to pass in the electrolytic solution of 10 μm ~ 200 μm carries out the process of electrochemistry removal alloying by the thickness obtained in step one unlike: the process of removal alloying described in step 2; The acidic solution of described electrolytic solution to be concentration be 0.1mol/L ~ 10mol/L, concentration are the basic solution of 0.1mol/L ~ 10mol/L or concentration is the neutral solution of 0.1mol/L ~ 10mol/L, the temperature of removal alloying process is 15 DEG C ~ 95 DEG C, and the time of removal alloying process is 5min ~ 360min.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment and embodiment six are the basic solution of 1mol/L ~ 5mol/L or concentration unlike the acidic solution of: described electrolytic solution to be concentration be 1mol/L ~ 5mol/L, concentration is the neutral solution of 1mol/L ~ 5mol/L.Other is identical with embodiment six.
Embodiment eight: present embodiment and embodiment six or seven unlike: described acidic solution is HCl solution, H
2sO
4solution or HNO
3solution.Other is identical with embodiment six or seven.
Embodiment nine: one of present embodiment and embodiment six to eight unlike: described basic solution is NaOH solution or KOH solution.Other is identical with one of embodiment six to eight.
Embodiment ten: one of present embodiment and embodiment six to nine unlike: described neutral solution is NaCl solution.Other is identical with one of embodiment six to nine.
Beneficial effect of the present invention is verified by following examples:
Embodiment one: a kind of preparation method of nanoporous titanium specifically carries out according to the following steps:
One, presoma is prepared: by Ti
3al intermetallic compound presoma adopt Linear cut become diameter to be 10mm, thickness is the thin slice of 400 μm, then uses 800#, 2000# sand papering respectively, then with mechanical polishing by specimen surface throw to light, obtain thickness be 100 μm remove alloy sample;
Two, removal alloying: by the thickness obtained in step one be 100 μm go alloy sample to be placed in corrosive fluid to carry out chemical removal alloying process; The NaOH solution of described corrosive fluid to be concentration be 1mol/L, the temperature of removal alloying process is 25 DEG C, and the time of removal alloying process is 120h, obtains the sample after removal alloying;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 8min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 8h, can obtain nanoporous titanium.
Fig. 1 is the surface topography map of the nanoporous titanium that embodiment one obtains; As can be seen from the figure the surface topography of nanoporous titanium is similar to the fracture of dimple fracture, but all has nano level hole in each dimple, and aperture is not at 10 ~ 120nm etc.
Embodiment two: a kind of preparation method of nanoporous titanium specifically carries out according to the following steps:
One, presoma is prepared: by Ti
3al intermetallic compound presoma adopt Linear cut become diameter to be 10mm, thickness is the thin slice of 400 μm, then uses 800#, 2000# sand papering respectively, then with mechanical polishing by specimen surface throw to light, obtain thickness be 100 μm remove alloy sample;
Two, removal alloying: the thickness obtained in step one is that the alloy sample that goes of 100 μm utilizes scolding tin to connect a copper conductor on the surface, and solder joint and face of weld is sealed with epoxy resin glue, only reserves 0.785cm
2area, then put and carry out the process of electrochemistry removal alloying in the electrolytic solution; The NaOH solution of described electrolytic solution to be concentration be 1mol/L, the temperature of removal alloying process is 25 DEG C, and the time of removal alloying process is 2h;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 8min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 8h, can obtain nanoporous titanium.
The present embodiment adopts three-electrode system, with the NaOH solution of 1mol/L for electrolytic solution, Ag/AgCl electrode is as reference electrode, parameters is as follows: initial voltage is-2.5V, and final voltage is 0V, and scanning speed is 0.001V/s, stopping the current potential place hold-time is 0s, sampling time interval is 0.01s, and time of repose is 2s, and the science of current sensitivity is counted as default value: 1.e-006A/V.
Fig. 2 is the surface topography map of the nanoporous titanium that embodiment two obtains; As can be seen from the figure its aperture is more even.Improve removal alloying technique further, can regulate and control nano-porous structure.
Embodiment three: a kind of preparation method of nanoporous titanium specifically carries out according to the following steps:
One, presoma is prepared: adopt Linear cut to become diameter to be 10mm TiAl intermetallic compound presoma, thickness is the thin slice of 400 μm, then use 800#, 2000# sand papering respectively, then with mechanical polishing by specimen surface throw to light, obtain thickness be 100 μm remove alloy sample;
Two, removal alloying: by the thickness obtained in step one be 100 μm go alloy sample to be placed in corrosive fluid to carry out chemical removal alloying process; The HNO of described corrosive fluid to be concentration be 1mol/L
3solution, the temperature of removal alloying process is 25 DEG C, and the time of removal alloying process is 48h, obtains the sample after removal alloying;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 8h, can obtain nanoporous titanium.
Embodiment four: a kind of preparation method of nanoporous titanium specifically carries out according to the following steps:
One, presoma is prepared: adopt Linear cut to become diameter to be 10mm TiAl intermetallic compound presoma, thickness is the thin slice of 400 μm, then use 800#, 2000# sand papering respectively, then with mechanical polishing by specimen surface throw to light, obtain thickness be 100 μm remove alloy sample;
Two, removal alloying: the thickness obtained in step one is that the alloy sample that goes of 100 μm utilizes scolding tin to connect a copper conductor on the surface, and solder joint and face of weld is sealed with epoxy resin glue, only reserves 0.785cm
2area, then put and carry out the process of electrochemistry removal alloying in the electrolytic solution; The HNO of described electrolytic solution to be concentration be 1mol/L
3solution, the temperature of removal alloying process is 25 DEG C, and the time of removal alloying process is 400s;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 8h, can obtain nanoporous titanium.
The present embodiment adopts three-electrode system, with the HNO of 1mol/L
3solution is electrolytic solution, Ag/AgCl electrode is as reference electrode, parameters is as follows: initial voltage is 0V, final voltage is 2V, scanning speed is 0.01V/s, and stopping the current potential place hold-time is 0s, and sampling time interval is 0.01s, time of repose is 2s, the science count value of current sensitivity: 1.e-001A/V.
Embodiment five: a kind of preparation method of nanoporous titanium specifically carries out according to the following steps:
One, presoma is prepared: by Ti
3al intermetallic compound presoma adopt Linear cut become diameter to be 10mm, thickness is the thin slice of 400 μm, then uses 800#, 2000# sand papering respectively, then with mechanical polishing by specimen surface throw to light, obtain thickness be 100 μm remove alloy sample;
Two, removal alloying: by the thickness obtained in step one be 100 μm go alloy sample to be placed in corrosive fluid to carry out chemical removal alloying process; The NaOH solution of described corrosive fluid to be concentration be 5mol/L, the temperature of removal alloying process is 25 DEG C, and the time of removal alloying process is 120h, obtains the sample after removal alloying;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 8h, can obtain nanoporous titanium.
Fig. 3 is the surface topography map of the nanoporous titanium that embodiment five obtains; Can find that from figure surface defines nano-porous structure, but skewness, also have certain alloy area not to be corroded.
Embodiment six: a kind of preparation method of nanoporous titanium specifically carries out according to the following steps:
Two, presoma is prepared: by Ti
3al intermetallic compound presoma adopt Linear cut become diameter to be 10mm, thickness is the thin slice of 400 μm, then uses 800#, 2000# sand papering respectively, then with mechanical polishing by specimen surface throw to light, obtain thickness be 100 μm remove alloy sample;
Two, removal alloying: the thickness obtained in step one is that the alloy sample that goes of 100 μm utilizes scolding tin to connect a copper conductor on the surface, and solder joint and face of weld is sealed with epoxy resin glue, only reserves 0.785cm
2area, then put and carry out the process of electrochemistry removal alloying in the electrolytic solution; The NaOH solution of described electrolytic solution to be concentration be 5mol/L, the temperature of removal alloying process is 25 DEG C, and the time of removal alloying process is 2h;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 8h, can obtain nanoporous titanium.
The present embodiment adopts three-electrode system, with the NaOH solution of 1mol/L for electrolytic solution, Ag/AgCl electrode is as reference electrode, parameters is as follows: initial voltage is 0V, and final voltage is 2V, and scanning speed is 0.01V/s, stopping the current potential place hold-time is 0s, sampling time interval is 0.01s, and time of repose is 2s, the science count value of current sensitivity: 1.e-006A/V.
Fig. 4 is the surface topography map of the nanoporous titanium that embodiment six obtains; Can find out, after the process of electrochemistry removal alloying, its removal alloying successful is better than chemical treatment, and its nanoporous size is also more even.Improve removal alloying technique further, can regulate and control nano-porous structure.
After nanoporous titanium embodiment two obtained cleans up, thermal treatment 2 hours at 500 DEG C, and then with the H of 1M
2sO
4be electrolytic solution with the HF acid of 1.0%, carry out anodic oxidation 60s under 30V voltage after, obtain the Ti/TiO with nano-porous structure
2matrix material, and made ultracapacitor, find that its ratio capacitance is up to 38.5F/g.
Claims (10)
1. a preparation method for nanoporous titanium, is characterized in that the preparation method of nanoporous titanium specifically carries out according to the following steps:
One, presoma is prepared: by Ti
xal
yintermetallic compound presoma adopts Linear cut and pre-mill to grind and processes, obtain thickness be 10 μm ~ 200 μm remove alloy sample;
Two, removal alloying: be that the alloy sample that goes of 10 μm ~ 200 μm carries out removal alloying process by the thickness obtained in step one, obtain the sample after removal alloying;
Three, subsequent disposal: the sample after removal alloying is taken out, first repeatedly rinse with deionized water, rinse 120s ~ 150s altogether, and then put into dehydrated alcohol, utilize ultrasonic cleaning 8min ~ 10min, to remove other residual impurity dirt settling, the sample under moisture state is put into vacuum drying oven, dry 5h ~ 8h, can obtain nanoporous titanium.
2. the preparation method of a kind of nanoporous titanium according to claim 1, is characterized in that Ti described in step one
xal
yintermetallic compound is Ti
3al, TiAl or TiAl
3.
3. the preparation method of a kind of nanoporous titanium according to claim 1, it is characterized in that the process of removal alloying described in step 2 be by the thickness obtained in step one be 10 μm ~ 200 μm go alloy sample to be placed in corrosive fluid to carry out chemical removal alloying process; Acidic solution or the concentration of described corrosive fluid to be concentration be 0.1mol/L ~ 10mol/L are the basic solution of 0.1mol/L ~ 10mol/L, and the temperature of removal alloying process is 15 DEG C ~ 95 DEG C, and the time of removal alloying process is 2h ~ 120h.
4. the preparation method of a kind of nanoporous titanium according to claim 3, is characterized in that described corrosive fluid to be concentration is the acidic solution of 1mol/L ~ 5mol/L; Described acidic solution is HCl solution, H
2sO
4solution or HNO
3solution.
5. the preparation method of a kind of nanoporous titanium according to claim 3, is characterized in that described corrosive fluid to be concentration is the basic solution of 1mol/L ~ 5mol/L; Described basic solution is NaOH solution or KOH solution.
6. the preparation method of a kind of nanoporous titanium according to claim 1, it is characterized in that the process of removal alloying described in step 2 be by the thickness obtained in step one be 10 μm ~ 200 μm go alloy sample to put to pass to-2.5V ~ 3V in the electrolytic solution carry out the process of electrochemistry removal alloying; The acidic solution of described electrolytic solution to be concentration be 0.1mol/L ~ 10mol/L, concentration are the basic solution of 0.1mol/L ~ 10mol/L or concentration is the neutral solution of 0.1mol/L ~ 10mol/L, the temperature of removal alloying process is 15 DEG C ~ 95 DEG C, and the time of removal alloying process is 5min ~ 360min.
7. the preparation method of a kind of nanoporous titanium according to claim 6, is characterized in that described electrolytic solution to be concentration is the acidic solution of 1mol/L ~ 5mol/L, basic solution that concentration is 1mol/L ~ 5mol/L or concentration is the neutral solution of 1mol/L ~ 5mol/L.
8. the preparation method of a kind of nanoporous titanium according to claim 6, is characterized in that described acidic solution is HCl solution, H
2sO
4solution or HNO
3solution.
9. the preparation method of a kind of nanoporous titanium according to claim 6, is characterized in that described basic solution is NaOH solution or KOH solution.
10. the preparation method of a kind of nanoporous titanium according to claim 6, is characterized in that described neutral solution is NaCl solution.
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