CN105039982B - A kind of Ti-Ni alloy surface prepares the method that CNT strengthens composite ceramic layer - Google Patents
A kind of Ti-Ni alloy surface prepares the method that CNT strengthens composite ceramic layer Download PDFInfo
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Abstract
The invention belongs to technical field of metal material surface modification, and in particular to a kind of titanium alloy surface prepares the method that CNT strengthens composite ceramic layer.A kind of method that Ti-Ni alloy surface prepares CNT enhancing composite ceramic layer uses double glow discharge alloying process technology in Ti-Ni alloy case-carbonizing, obtain titanium carbide modified layer, using double glow discharge alloying process technology in titanium carbide modified layer surface titanizing, form titanium carbide/titanium gradient modified layer, with titanium carbide/titanium gradient modified layer as anode, using differential arc oxidization technique, and CNT is added in micro-arc oxidation electrolyte, obtain CNT enhancing composite ceramic layer.High with substrate combinating strength, the hardness of modified layer, wearability, corrosion resistance and bio-compatible performance are effectively improved.
Description
Technical field
The invention belongs to technical field of metal material surface modification, and in particular to a kind of Ti-Ni alloy surface prepares carbon nanometer
The method that pipe strengthens composite ceramic layer.
Background technology
Ti-Ni alloy has the excellent intelligent characteristic such as SME and super-elasticity, in biomedical, space flight and machine
The fields such as tool engineering have important application value.But, Ti-Ni alloy has two, and one is in terms of machinery and building
Using when, because its hardness is relatively low, wearability has much room for improvement；Two is containing more nickel element in Ti-Ni alloy, as biology
During material, the precipitation of nickel ion can be damaged to human body, reduce its biocompatibility.Therefore, how Ti-Ni alloy is carried out
Surface is modified, and improves its tribological property, prevents the precipitation of nickel ion, improves biocompatibility, as the pass for restricting its application
Key factor.
The method of Ti-Ni alloy surface treatment mainly has ion implanting, oxidation processes, low temperature removal alloying etc., wherein passing through
Differential arc oxidation obtains titanium dioxide layer on Ti-Ni alloy surface, it is possible to reduce the precipitation of nickel ion, and with good biology
Compatibility, increasingly causes the attention of people.But, application titanium dioxide layer has two problems demands to solve at present：1. dioxy
Change titanium layer larger with basal body structure and performance difference, there is larger internal stress, compatible deformation ability；2. titanium dioxide layer is hard
Degree is not enough, under complicated carrying condition and fatigue load effect, crackle and spalling failure easily occurs.
The content of the invention
The technical problems to be solved by the invention are：How to reduce Ti-Ni alloy is carried out surface it is modified when, coating and base
How the otherness of body, improve the hardness and biocompatibility of superficial layer.
The technical solution adopted in the present invention is：A kind of Ti-Ni alloy surface prepares CNT enhancing composite ceramic layer
Method, it is characterised in that comprise the following steps：
Step one, with graphite as source electrode, using double glow discharge alloying process technology in the Ni-based material case-carbonizing of titanium, obtain
To titanium carbide modified layer；The carburizing process uses existing use double glow discharge alloying process technology, in Ti-Ni alloy table
Face generates titanium carbide, has prevented the contact of nickel and the external world.
Step 2, with pure titanium as source electrode, the titanium carbide obtained in step one using double glow discharge alloying process technology
Modified layer surface titanizing, forms titanium carbide/titanium gradient modified layer；Titanium carbide/titanium gradient modified layer on the one hand isolated nickel with it is outer
The contact on boundary, prevents the precipitation of nickel ion, improves biocompatibility, on the other hand enhances the consistency and elasticity on surface.
Step 3, with titanium carbide/titanium gradient modified layer for obtaining in step 2 as anode, using differential arc oxidization technique,
CNT enhancing composite ceramic layer is prepared in the micro-arc oxidation electrolyte of carbon nanotubes, it is therefore prevented that titanium dioxide layer
Generation, improves the wearability and hardness on surface so that Ti-Ni alloy had both been provided with itself good memory effect and super-elasticity
Etc. excellent intelligent characteristic, and nickel ion will not be separated out, while the hardness and wearability on surface are very high.
As a kind of preferred embodiment：Step 3 is specially using differential arc oxidization technique：At room temperature by many wall carbon after purification
Nanotube immerses dispersant for ultrasonic dispersion 45min, the carbon nano tube suspension stablized, by disodium hydrogen phosphate, calcium acetate
It is added in the carbon nano tube suspension of stabilization, forms the micro-arc oxidation electrolyte of carbon nanotubes, electrolyte is put into electrolysis
In groove, wherein, content of carbon nanotubes is 2-8 g/l in electrolytic cell, and disodium hydrogen phosphate content is 6.2~12.5 g/l, acetic acid
Calcium content is 15.8~31.6 g/l, and with electrolytic cell as negative electrode, the titanium carbide obtained in step 2/titanium gradient modified layer is sun
Pole, is 300~600V in pulse voltage, and 200~800Hz of frequency, 0~40 DEG C of temperature, 5~10min for the treatment of obtains CNT
Enhancing composite ceramic layer.
As a kind of preferred embodiment：Dispersant is 1 by cetyl trimethylammonium bromide and volume ratio:1 ethylene glycol water
Solution composition, cetyl trimethylammonium bromide content is 1 g/l.
As a kind of preferred embodiment：Multi-walled carbon nano-tubes purification process is：CNT is placed in sulfuric acid and nitric acid volume
Than being 3:In 1 mixed acid, 2h is heated at 100 DEG C, deionized water rinsing is used after filtering, make PH to neutrality, dried.
The beneficial effects of the invention are as follows：Double glow discharge alloying process alloying and differential arc oxidization technique are combined,
Solve the problems, such as that Ti-Ni alloy surface is difficult to prepare bioactivity coatings by differential arc oxidization technique；Gradient modified layer is in
Between transition zone, realize the seamlessly transitting to matrix mechanical property by surface, reduce the difference of matrix and coating, and effectively
Prevent the precipitation of nickel ion.The unmatched problem of performance between titanium dioxide layer and matrix is solved, the resistance to of Ti-Ni alloy is improve
Mill property and biocompatibility；Strengthen composite modified layer as reinforcement from CNT, due to CNT hardness with
Diamond quite, although scattered CNT is few in film layer, can make composite modified layer hardness be significantly improved.It is being subject to
During impulsive force, pressure, disperses impact forces can be undertaken, so as to protect matrix.It is simple to operate with method, good process repeatability,
The features such as low cost, can be widely used for Ti-Ni alloy surface treatment.
Specific embodiment
Embodiment 1
Step one, with graphite as source electrode, using double glow discharge alloying process technology in the Ni-based material case-carbonizing of titanium, obtain
To titanium carbide modified layer.
Cleaning workpiece surface：By containing the Ti-Ni alloy that atomic percent nickel is 50.8%, it is polishing to step by step with waterproof abrasive paper
2000#, after be polished, then it is used deionized water successively, acetone and absolute ethyl alcohol ultrasonic wave clean 15~30min, room temperature
Close drying.
Shove charge：Treated Ti-Ni alloy is put into double glow discharge alloying process stove, using graphite as source electrode
Target, die opening is 18~19mm, and sputter gas are the argon gas of high-purity.
Vacuumize and pre-sputtering：Mechanical pump is opened, below 5Pa is evacuated to, argon gas is passed through, air pressure is 35Pa；Open cloudy
Pole power supply, cathode voltage is 500V, and pre-sputtering is carried out to Ti-Ni alloy surface, cleans alloy surface, Ti-Ni alloy surface temperature
When being increased to 900 DEG C, be incubated 30min, it is therefore an objective to Ti-Ni alloy surface produce vacancy defect, be beneficial to carbon atom absorption and
Diffusion.
Insulation：Source electrode power supply is opened, slow elevated source voltage, while adjusting source voltage and cathode voltage, makes source electrode
Voltage is higher than cathode voltage, and pressure difference is 250~300V, and Ti-Ni alloy temperature is kept for 900 DEG C, and air pressure 35Pa is incubated 3h；Close cloudy
Pole power supply and source electrode power supply；Argon gas is closed after furnace cooling 2h；After Ti-Ni alloy is cooled to room temperature, cooling water is closed；Open
Body of heater takes out, and titanium carbide modified layer is obtained.
Step 2, with pure titanium as source electrode, the titanium carbide obtained in step one using double glow discharge alloying process technology
Modified layer surface titanizing, forms titanium carbide/titanium gradient modified layer.
Shove charge：The Ti-Ni alloy processed by step one that will be obtained in pure titanium and step one as source electrode is placed in bilayer
In glow plasma metal leakage furnace, die opening is 18~19mm, and sputter gas are the argon gas of high-purity.
Vacuumize and pre-sputtering：Mechanical pump is opened, below 5Pa is evacuated to, argon gas is passed through, air pressure is 35Pa；Open cloudy
Pole power supply, cathode voltage is 500V, and air pressure is 35Pa, and pre-sputtering is carried out to Ti-Ni alloy surface, cleans alloy surface, and titanium nickel is closed
When gold surface temperature is increased to 900 DEG C, be incubated 30min, it is therefore an objective to surface produce vacancy defect, be beneficial to titanium atom absorption and
Diffusion.
Insulation：Source electrode power supply is opened, slow elevated source voltage, while adjusting source voltage and cathode voltage, makes source electrode
Voltage is higher than cathode voltage, and pressure difference is 250~300V, and Ti-Ni alloy temperature is kept for 900 DEG C, and air pressure 35Pa is incubated 3h；Close cloudy
Pole power supply and source electrode power supply；Argon gas is closed after furnace cooling 2h；After Ti-Ni alloy is cooled to room temperature, cooling water is closed；Open
Body of heater takes out, and titanium carbide/titanium gradient modified layer is obtained.
Step 3, with titanium carbide/titanium gradient modified layer for obtaining in step 2 as anode, using differential arc oxidization technique,
CNT enhancing composite ceramic layer is prepared in the micro-arc oxidation electrolyte of carbon nanotubes.
Multi-walled carbon nano-tubes purification process is：It is 3 that CNT is placed in into sulfuric acid and nitric acid volume ratio:In 1 mixed acid,
2h is heated at 100 DEG C, is rinsed with ionized water after filtering, make PH to neutrality, dried, purified by this method and be conducive in dispersion
Ultrasonic disperse in agent.
Multi-walled carbon nano-tubes dispersant preparation method：Dispersant is in volume ratio by cetyl trimethylammonium bromide solution
1:Constituted in 1 glycol water, cetyl trimethylammonium bromide content is 1 g/l.
Multi-walled carbon nano-tubes after purification is immersed into dispersant for ultrasonic dispersion 45min at room temperature, the carbon stablized is received
Mitron suspension, disodium hydrogen phosphate, calcium acetate are added in the carbon nano tube suspension of stabilization, form the micro- of carbon nanotubes
Arc oxidation electrolyte, electrolytic cell is put into by electrolyte（Stainless steel plated film groove）In, wherein, electrolytic cell（Stainless steel plated film groove）Middle carbon
Nanotube content is 2 g/l, and disodium hydrogen phosphate content is 6.2 g/l, and acetic acid calcium content is 15.8 g/l, cetyl three
Methyl bromide ammonium content is 1 g/l（The volume of carbon nano tube suspension volume and dispersant and the volume of electrolyte almost phase
Together）, with electrolytic cell as negative electrode, the titanium carbide obtained in step 2/titanium gradient modified layer be anode, pulse voltage be 300~
600V, 200~800Hz of frequency, 0~40 DEG C of temperature, treatment 5min obtain CNT enhancing composite ceramic layer.
Embodiment 2
The present embodiment step one and step 2 are identical with embodiment 1.
Step 3, with titanium carbide/titanium gradient modified layer for obtaining in step 2 as anode, using differential arc oxidization technique,
CNT enhancing composite ceramic layer is prepared in the micro-arc oxidation electrolyte of carbon nanotubes.
Multi-walled carbon nano-tubes purification process is：It is 3 that CNT is placed in into sulfuric acid and nitric acid volume ratio:In 1 mixed acid,
2h is heated at 100 DEG C, is rinsed with ionized water after filtering, make PH to neutrality, dried.
Multi-walled carbon nano-tubes dispersant preparation method：Dispersant is in volume ratio by cetyl trimethylammonium bromide solution
1:Constituted in 1 glycol water, cetyl trimethylammonium bromide content is 1 g/l.
Multi-walled carbon nano-tubes after purification is immersed into dispersant for ultrasonic dispersion 45min at room temperature, the carbon stablized is received
Mitron suspension, disodium hydrogen phosphate, calcium acetate are added in the carbon nano tube suspension of stabilization, form the micro- of carbon nanotubes
Arc oxidation electrolyte, electrolytic cell is put into by electrolyte（Stainless steel plated film groove）In, wherein, electrolytic cell（Stainless steel plated film groove）Middle carbon
Nanotube content is 8 g/l, and disodium hydrogen phosphate content is 12.5 g/l, and acetic acid calcium content is 31.6 g/l, cetyl three
Methyl bromide ammonium content is 1 g/l（CNT, disodium hydrogen phosphate, calcium acetate are all solid, and liquid volume is several after its dissolving
It is constant）, with electrolytic cell as negative electrode, the titanium carbide obtained in step 2/titanium gradient modified layer is anode, is in pulse voltage
300~600V, 200~800Hz of frequency, 0~40 DEG C of temperature, treatment 10min obtain CNT enhancing composite ceramic layer.
Embodiment 3
Step 3, with titanium carbide/titanium gradient modified layer for obtaining in step 2 as anode, using differential arc oxidization technique,
CNT enhancing composite ceramic layer is prepared in the micro-arc oxidation electrolyte of carbon nanotubes.
Multi-walled carbon nano-tubes purification process is：It is 3 that CNT is placed in into sulfuric acid and nitric acid volume ratio:In 1 mixed acid,
2h is heated at 100 DEG C, is rinsed with ionized water after filtering, make PH to neutrality, dried.
Multi-walled carbon nano-tubes dispersant preparation method：Dispersant is in volume ratio by cetyl trimethylammonium bromide solution
1:Constituted in 1 glycol water, cetyl trimethylammonium bromide content is 1 g/l.
Multi-walled carbon nano-tubes after purification is immersed into dispersant for ultrasonic dispersion 45min at room temperature, the carbon stablized is received
Mitron suspension, disodium hydrogen phosphate, calcium acetate are added in the carbon nano tube suspension of stabilization, form the micro- of carbon nanotubes
Arc oxidation electrolyte, electrolytic cell is put into by electrolyte（Stainless steel plated film groove）In, wherein, electrolytic cell（Stainless steel plated film groove）Middle carbon
Nanotube content is 6 g/l, and disodium hydrogen phosphate content is 10 g/l, and acetic acid calcium content is 20 g/l, cetyl trimethyl
Ammonium bromide content is 1 g/l, and with electrolytic cell as negative electrode, the titanium carbide obtained in step 2/titanium gradient modified layer is anode,
Pulse voltage is 300~600V, and 200~800Hz of frequency, 0~40 DEG C of temperature, treatment 8min obtains CNT enhancing composite ceramic
Enamel coating.
Embodiment 1,2,3 reduces the otherness of coating and matrix by forming the transition zone of gradient components distribution, and adds
Enter CNT reinforcement to improve the hardness of superficial layer, the hardness than titanium dioxide layer is high.Composite ceramics layer surface is uniform, with
Substrate combinating strength is high, and the hardness of modified layer, wearability, corrosion resistance and bio-compatible performance are effectively improved.
The transition zone being distributed with gradient components is prepared in titanium nickel surface by double glow discharge alloying process technology, is
Solve the unmatched a kind of effective ways of performance between coating and matrix.The technology forms modified by sputtering, deposition, diffusion process
Layer, advantage is that can neatly control technological parameter to prepare required modified layer, in the absence of the problem of interface reduction.
CNT have high elastic modelling quantity and tensile strength, low density and linear expansion coefficient, good toughness,
High temperature resistant and chemical stability, therefore, the performance of metal-base composites is improved frequently as reinforcement.In titanium alloy surface
Adding a small amount of CNT can increase substantially the mechanical properties such as its elastic modelling quantity and hardness, even and if carbon at high temperature
Nanotube does not also react with titanium, still keeps original nanostructured.
Claims (4)
1. a kind of Ti-Ni alloy surface prepares the method that CNT strengthens composite ceramic layer, it is characterised in that including following step
Suddenly：
Step one, with graphite as source electrode, using double glow discharge alloying process technology in the Ni-based material case-carbonizing of titanium, obtain carbon
Change titanium modified layer；
Step 2, with pure titanium as source electrode, the titanium carbide obtained in step one using double glow discharge alloying process technology is modified
Layer surface oozes titanium, forms titanium carbide/titanium gradient modified layer；
Step 3, with titanium carbide/titanium gradient modified layer for obtaining in step 2 as anode, using differential arc oxidization technique, carbon containing
CNT enhancing composite ceramic layer is prepared in the micro-arc oxidation electrolyte of nanotube.
2. a kind of Ti-Ni alloy surface according to claim 1 prepares the method that CNT strengthens composite ceramic layer, its
It is characterised by：Step 3 is specially using differential arc oxidization technique：Multi-walled carbon nano-tubes after purification is immersed into dispersant at room temperature
Middle ultrasonic disperse 45min, the carbon nano tube suspension stablized receives the carbon that disodium hydrogen phosphate, calcium acetate are added to stabilization
In mitron suspension, the micro-arc oxidation electrolyte of carbon nanotubes is formed, electrolyte is put into electrolytic cell, wherein, electrolytic cell
Middle content of carbon nanotubes be 2-8 g/l, disodium hydrogen phosphate content be 6.2~12.5 g/l, acetic acid calcium content be 15.8~
31.6 g/l, with electrolytic cell as negative electrode, the titanium carbide obtained in step 2/titanium gradient modified layer is anode, is in pulse voltage
300~600V, 200~800Hz of frequency, 0~40 DEG C of temperature, 5~10min for the treatment of obtain CNT enhancing composite ceramic layer.
3. a kind of Ti-Ni alloy surface according to claim 2 prepares the method that CNT strengthens composite ceramic layer, its
It is characterised by：Dispersant is 1 by cetyl trimethylammonium bromide and volume ratio:1 glycol water composition, cetyl
Trimethylammonium bromide content is 1 g/l.
4. a kind of Ti-Ni alloy surface according to claim 2 or claim 3 any one claim prepares carbon
The method that nanotube strengthens composite ceramic layer, it is characterised in that：Multi-walled carbon nano-tubes purification process is：CNT is placed in sulphur
Acid and nitric acid volume ratio are 3:In 1 mixed acid, 2h is heated at 100 DEG C, deionized water rinsing is used after filtering, make pH into
Property, drying.
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| CN110965108A (en) * | 2019-12-27 | 2020-04-07 | 沈兰兰 | Zn-TiO2Method for producing a coating |
| CN111477899B (en) * | 2020-02-27 | 2022-12-09 | 太原理工大学 | Conductive corrosion-resistant metal bipolar plate for fuel cell and preparation method thereof |
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| JP2746505B2 (en) * | 1991-11-27 | 1998-05-06 | 新日本製鐵株式会社 | Ceramic coated member and method of manufacturing the same |
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| CN104087935A (en) * | 2014-07-25 | 2014-10-08 | 太原理工大学 | Preparation method of novel titanium-nickel medical implantation material |
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