CN104264203B - A kind of pure titanium of differential arc oxidation Ultra-fine Grained and its preparation method and application - Google Patents
A kind of pure titanium of differential arc oxidation Ultra-fine Grained and its preparation method and application Download PDFInfo
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- CN104264203B CN104264203B CN201410498739.XA CN201410498739A CN104264203B CN 104264203 B CN104264203 B CN 104264203B CN 201410498739 A CN201410498739 A CN 201410498739A CN 104264203 B CN104264203 B CN 104264203B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
Abstract
The invention discloses a kind of pure titanium of differential arc oxidation Ultra-fine Grained and its preparation method and application, belong to tooth-planting field of material technology.The technical scheme used for：Titanium bar material is handled through Equal-channel Angular Pressing the pure titanium of Ultra-fine Grained is made, then by the pure titanium of Ultra-fine Grained through lathe process into clinical planting body pattern, Microarc Oxidation Surface Treatment is carried out to the obtained pure titanium of Ultra-fine Grained with clinical planting body pattern again, the pure titanium of differential arc oxidation Ultra-fine Grained is obtained.The inventive method is simple to operate, easily realizes, is greatly promoted through the pure titanium mechanical strength of differential arc oxidation Ultra-fine Grained produced by the present invention, while also retains pure titanium material good biological safety and biocompatibility.
Description
Technical field
The invention belongs to tooth-planting field of material technology, and in particular to a kind of pure titanium of differential arc oxidation Ultra-fine Grained and its preparation
Methods and applications.
Background technology
Mouth cavity planting body is also known as tooth implant, also known as artificial tooth root.It is to be implanted into by way of surgical operation
In the upper mandibular at human body agomphosis position, after after the healing of its wound, the device for repairing artificial tooth is installed at an upper portion thereof.Oral cavity kind
Implant is different by its material, is divided into 1. Metal and Alloy material classes：Including gold, 316L stainless steels (iron-chromium-nickel alloy), casting
Make vitallium, titanium and alloy etc..2. ceramic material class：Including bio-inert ceramic, bioactive ceramics, biological degradability
Ceramics etc..3. carbon materials class：Including vitreous carbon, Low Temperature Isotropic Carbon etc..4. high polymer material class：Including acrylate
Class, polytetrafluoroethyl-ne alkenes etc..5. compound, such as metal surface spraying of composite class, i.e. both the above or two or more materials
Ceramics etc..The conventional material of current mouth cavity planting body is mainly pure titanium or titanium alloy, bioactive ceramics and some composite woods
Material.
Pure titanium and titanium alloy have superior biocompatibility, modulus of elasticity and resistance to corrosion close to bone tissue, energy
Preferable primary stability and synosteosis are reached, is the planting body material being most widely used.And titanium alloy is to possess pure titanium each
While planting advantage, its intensity, apparently higher than pure titanium, is a kind of ideal planting body material, but have metal ion spilling
Cause the shortcoming of metal toxicity.So that pure titanium becomes is applied to most commonly used planting body material in clinic at present, but pure titanium
Planting body still suffers from many problems.Such as mechanical strength is low, bioactivity is poor, lacks bone inductive effect, combined by force with surrounding tissue
Spend low, healing time length etc..Current titanium implant surface is modified the effective way for having become and improving implant surface performance, but
Its mechanical strength is low, and it is still to put in the previous urgent problem to be solved in our faces to easily cause the problem of planting body fractures to be.Hair
Bright content
In order to overcome the defect that above-mentioned prior art is present, it is an object of the invention to provide a kind of differential arc oxidation Ultra-fine Grained
Pure titanium and its preparation method and application, this method can solve the problem that the problem of pure titanium mechanical strength is low, through ultra-fine made from this method
Brilliant pure titanium high mechanical strength, with good biological safety and biocompatibility.
The present invention is to be achieved through the following technical solutions：
A kind of preparation method of the pure titanium of differential arc oxidation Ultra-fine Grained, is to handle titanium bar material through Equal-channel Angular Pressing to be made
The pure titanium of Ultra-fine Grained, then has clinical plantation through lathe process by the pure titanium of Ultra-fine Grained into clinical planting body pattern, then to obtained
The pure titanium of Ultra-fine Grained of body pattern carries out Microarc Oxidation Surface Treatment, obtains the pure titanium of differential arc oxidation Ultra-fine Grained.
A kind of preparation method of the pure titanium of differential arc oxidation Ultra-fine Grained, comprises the following steps：
1) the pure titanium of Ultra-fine Grained is prepared
At room temperature, copper-titanium rod is put into the mould of built-in angle passage, with omnipotent squeeze test machine using Bc paths as
Mode of entrance carries out the processing of 4 passage Equal-channel Angular Pressings, and enters again after heat treatment elimination internal stress after extrusion process every time
Row extrusion process next time, until extruding is completed, then peels off titanium bar material, then polished, corrosion treatment, and Ultra-fine Grained is made
Pure titanium；
Wherein, the copper-titanium rod is made of the copper rod center that a diameter of 6mm pure titanium rod is placed in a diameter of 10mm；It is interior
The extruding interior angle for putting the mould of angle passage is 100~140 °, and extruding exterior angle is 20 °, the extruding of omnipotent squeeze test compressing head
Speed is 5~8mm/s；It is described heat treatment be by the copper after each extrusion process-titanium rod at 150~400 DEG C temper, so
Air cooling afterwards；
2) Microarc Oxidation Surface Treatment
The pure titanium of obtained Ultra-fine Grained is cut into discoid test specimen, then by polishing, cleaning, is subsequently placed in differential arc oxidation and sets
Anode position in standby, using stainless steel plate as negative electrode, in phosphate system electrolyte, 450V, pulse, 500HZ, circulation
Cycle is that under conditions of 10~20%, differential arc oxidation Ultra-fine Grained pure titanium is made in 4~10min of Microarc Oxidation Surface Treatment.
Step 1) Equal-channel Angular Pressing processing when be put into lubricant in a mold, and the lubricant is with quality percentage
Than meter, by 10~20% MoS2With 80~90% graphite composition.
Step 1) described in polishing be that the titanium bar material that will be separated is polished to 2000~2500 mesh with SiC sand paper.
Step 1) described in the corrosive agent that uses of corrosion treatment with the HNO of volume percentage, including 15~25%3, 5~
10% HF and 70~80% water.
Step 1) described in refer to by mode of entrance of Bc paths per twice extrude between titanium bar material is turned clockwise
90 °, the passage of co-extrusion pressure 3~5.
Step 2) the pure titanium of obtained Ultra-fine Grained is cut into a diameter of 5~8mm, thickness is 2~4mm discoid test specimen.
Step 2) described in polishing be that discoid test specimen with SiC sand paper is polished to 1500~2500 mesh；Described is clear
Wash is to clean the test specimen after polishing with acetone, absolute ethyl alcohol and deionized water sonic oscillation successively.
The invention also discloses a kind of pure titanium of differential arc oxidation Ultra-fine Grained, the average thickness of the pure titanium of differential arc oxidation Ultra-fine Grained
7.833 ± 0.771 μm, roughness is 1.391 ± 0.143 μm, and adhesion is 23.900 ± 1.267N, and tensile strength reaches
791MPa, Vickers hardness reaches 2450MPa.
The invention also discloses preparing mouth cavity planting body material through the pure titanium of differential arc oxidation Ultra-fine Grained made from the inventive method
Application in material.
Compared with prior art, the present invention has following beneficial technique effect：
Titanium bar material through Equal-channel Angular Pressing is prepared the pure titanium of Ultra-fine Grained by the present invention, and then lathe process is into clinic
Planting body pattern, and Microarc Oxidation Surface Treatment is carried out, obtain the pure titanium of differential arc oxidation Ultra-fine Grained.It ensure that Deng channel pressings pure
Its mechanical strength is improved while titanium premium properties, and Microarc Oxidation Surface Treatment can then significantly increase the life of pure titanium material
Thing compatibility and bone guided.
The inventive method is simple to operate, easily realizes, big through the pure titanium mechanical strength of differential arc oxidation Ultra-fine Grained produced by the present invention
Big lifting (tensile strength is promoted to 791MPa by 407MPa, and Vickers hardness rises to 2450MPa by 1499MPa), while also protecting
The good biocompatibility of pure titanium material and corrosion resistance are stayed.
Brief description of the drawings
Fig. 1 is titanium material Electronic Speculum crystalline phase photo, wherein, (a) is common pure titanium Electronic Speculum crystalline phase photo；(b) it is pure for Ultra-fine Grained
Titanium Electronic Speculum crystalline phase photo；
Fig. 2 changes block diagram for the Vickers hardness of different passage extrusion process；
Fig. 3 is static compression test lower yield strength test stress-strain curve figure；
Fig. 4 is dynamic compressive test lower yield strength test stress-strain curve figure；
Fig. 5 is that differential arc oxidation coating element constitutes collection of illustrative plates, wherein, (a) is common pure titanium；(b) it is differential arc oxidation Ultra-fine Grained
Pure titanium；
Fig. 6 is the surface topography stereoscan photograph of differential arc oxidation coating, wherein, (a) is common pure titanium surface topography
ESEM is seen；(b) seen for the ESEM of the pure titanium surface topography of differential arc oxidation Ultra-fine Grained；
Fig. 7 is the cross-sectional scans electromicroscopic photograph of differential arc oxidation coating, wherein, (a) is the cross-sectional scans of common pure titanium
Electronic Speculum is seen；(b) seen for the cross-sectional scans Electronic Speculum of the pure titanium of differential arc oxidation Ultra-fine Grained；
Fig. 8 is the three-dimensional surface shape scanning figure of differential arc oxidation coating, wherein, (a) is common pure titanium three-dimensional surface shape；
(b) it is the pure titanium three-dimensional surface shape of differential arc oxidation Ultra-fine Grained.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
A kind of preparation method of the pure titanium of differential arc oxidation Ultra-fine Grained, comprises the following steps：
1) the pure titanium of Ultra-fine Grained is prepared
The mould that copper-titanium rod is put into built-in angle passage is extruded repeatedly, specific method be by a diameter of 10mm with
Length (is the circle that the copper rod center that a diameter of 6mm pure titanium rod is placed in into a diameter of 10mm is made for 10cm cylindrical specimens
Cylinder sample, copper rod has been guiding function) it is placed at room temperature in extruding interior angle Φ=120 °, the mould of exterior angle ψ=20 °,
It is about 6mm/s to set universal test compressing head extruding rate, and (rotation is being kept just per experimental sample between extruding twice with Bc paths
90 degree) it is mode of entrance, four-pass is extruded altogether, and experiment material is subjected to ECAP operations.Note material carrying out heat in extruding
Processing, is specially that the Ultra-fine Grained titanium of preparation is tempered into 200 DEG C, air cooling.The lubricant main component of mould is put into extrusion process
For 15%MoS2With 85% graphite.Pure titanium material is separated after extruding successfully test specimen is first polished to by 2000 mesh using SiC sand paper
20%HNO is used afterwards3The reagent of+5%HF+75% water carries out corrosion treatment, and the pure titanium of Ultra-fine Grained is made.
Titanium pure to obtained Ultra-fine Grained carries out performance test, as a result as follows：
To be observed by microexamination the grainiess of pure titanium, referring to Fig. 1, (a) and (b), and carry out hardness and
The experiment of yield strength, referring to Fig. 2,3,4, from figure 2 it can be seen that Vickers hardness (is risen to by the 1499MPa of reset condition
The 2450MPa of 4 passages, improves 65%.As can be seen that static compression test is from the 300MPa of reset condition from Fig. 3,4
4 passage 772MPa are raised to, dynamic compressive test rises to 4 passage 1240MPa from the 900MPa of reset condition, as a result shown ultra-fine
The mechanical strength of brilliant pure titanium is significantly improved.
2) Microarc Oxidation Surface Treatment
The pure titanium of obtained Ultra-fine Grained is cut into the discoid test specimens of diameter 6mm thickness 3mm through line of material.SiC sand paper is polished to
1500 mesh, are cleaned 3 times according still further to the order ultrasonic vibration of acetone, absolute alcohol, deionized water, and common pure titanium control group is also carried out
Corresponding processing.It is placed at microarc oxidation equipment provided Anodic, stainless steel plate is as negative electrode, in phosphate system electrolyte,
5min is handled, it is ultra-fine that differential arc oxidation is made in (differential arc oxidation handles voltage 450V, pulse, frequency 500HZ, cycle period 15%)
Brilliant pure titanium.
Titanium pure to obtained differential arc oxidation Ultra-fine Grained carries out performance test, mainly includes：
Differential arc oxidation coating performance measurement, including：Differential arc oxidation coating composition, the surface topography of differential arc oxidation coating, horizontal stroke
Section is seen, the roughness of differential arc oxidation coating.
1st, differential arc oxidation coating is constituted
The pure titanium experimental group of differential arc oxidation Ultra-fine Grained and common pure titanium control group differential arc oxidation coating element composition are shown in Fig. 5, surpass
The pure titanium face coat of fine grain mainly contains O (47.12%), Ti (35.53%), P (6.98%), Si (10.35%), C
(0.02%), common pure titanium face coat composition is O (47.45%), Ti (35.75%), P (9.61%), Si (7.17%), C
(0.02%) element, test result indicates that, surface composition does not occur substantially after Ultra-fine Grained is handled with common pure titanium through differential arc oxidation
Change.
2nd, the surface topography cross section of differential arc oxidation coating is seen
Referring to Fig. 6, (a) and (b), SEM results show the pure titanium of Ultra-fine Grained and the common pure equal shape in titanium surface after differential arc oxidation
Into loose porous oxide covering.ESEM (5000 times of magnifying powers) shows its surface topography, the pure titanium of Ultra-fine Grained with it is common
Pure titanium differential arc oxidation coating is distributed with crateriform circle or oval micropore.The pure titanium surface oxide layer mesopore rate of Ultra-fine Grained
More than common pure titanium oxide layer.
3rd, cross section is seen
Referring to Fig. 7 (a) and (b), it is shown that the cross-sectional scans electricity of the pure titanium of Ultra-fine Grained and common pure titanium differential arc oxidation coating
Jing Guan.The coating of specimen surface is made up of two parts：Contact the fine and close internal layer of substrate structure and loose porous containing release channel
Outer layer.Experimental group is shown in Table 1 with control group differential arc oxidation coating thickness results：
The Ultra-fine Grained of table 1 and common pure titanium coating thickness, roughness and adhesion
As it can be seen from table 1 7.833 ± 0.771 μm of the average thickness of the pure titanium coating of Ultra-fine Grained, commonly pure titanium coating is flat
Equal 4.775 ± 0.558 μm of thickness.Data fit normal distribution, homogeneity of variance, the two have obvious significant difference (t=9.984,
P<0.05)。
4th, the roughness of differential arc oxidation coating
Referring to Fig. 8 (a) and (b), three-dimensional appearance scanner shows the pure titanium of Ultra-fine Grained and the shape on common pure titanium coating surface
Looks.After two kinds of material differential arc oxidation processing of it can be seen from the figure that, its surface forms rugged rough interfaces.Ultra-fine Grained is pure
The roughness value of titanium face coat is 1.391 ± 0.143 μm, and common pure titanium control group is 1.346 ± 0.091 μm, data fit
Normal distribution, homogeneity of variance, the two no difference of science of statistics (t=0.649, P>0.05), referring to table 1.
5th, the adhesion of differential arc oxidation coating
The adhesion between the latter two material coating and matrix of differential arc oxidation is determined with the automatic scratching instrument of coating adhesion
(table 1).The combination force value of the pure titanium face coat of Ultra-fine Grained is 23.900 ± 1.267N, common pure titanium combination force value for 23.867 ±
1.134N, data fit normal distribution, homogeneity of variance, the two no difference of science of statistics (t=0.048, P>0.05).
Embodiment 2
A kind of preparation method of the pure titanium of differential arc oxidation Ultra-fine Grained, comprises the following steps：
1) the pure titanium of Ultra-fine Grained is prepared
The mould that copper-titanium rod is put into built-in angle passage is extruded repeatedly, specific method be by a diameter of 10mm with
Length (is the circle that the copper rod center that a diameter of 6mm pure titanium rod is placed in into a diameter of 10mm is made for 10cm cylindrical specimens
Cylinder sample) it is placed at room temperature in extruding interior angle Φ=140 °, the mould of exterior angle ψ=20 °, universal test compressing head is set
Extruding rate is about 8mm/s, with Bc paths (keeping positive 90 degree of rotation per experimental sample between extruding twice) for mode of entrance, altogether
Meter 2 passages of extruding, ECAP operations are carried out by experiment material.Note material being heat-treated in extruding, will specially squeeze every time
Copper-titanium rod after pressure processing temper, then air cooling at 150 DEG C.
The lubricant main component that mould is put into extrusion process is 10%MoS2With 90% graphite.Peeled off after extruding successfully
Go out pure titanium material first test specimen is polished to after 2200 mesh using 15%HNO using SiC sand paper3The reagent of+5%HF+80% water enters
Row corrosion treatment, is made the pure titanium of Ultra-fine Grained.
2) Microarc Oxidation Surface Treatment
The pure titanium of obtained Ultra-fine Grained is cut into the discoid test specimens of diameter 8mm thickness 4mm through line of material.SiC sand paper is polished to
2000 mesh, are cleaned 3 times according still further to the order ultrasonic vibration of acetone, absolute alcohol, deionized water, and common pure titanium control group is also carried out
Corresponding processing.It is placed at microarc oxidation equipment provided Anodic, stainless steel plate is as negative electrode, in phosphate system electrolyte,
10min is handled, (differential arc oxidation handles voltage 450V, pulse, frequency 500HZ, cycle period 20%) is made differential arc oxidation and surpassed
The pure titanium of fine grain.
Embodiment 3
A kind of preparation method of the pure titanium of differential arc oxidation Ultra-fine Grained, comprises the following steps：
1) the pure titanium of Ultra-fine Grained is prepared
The mould that copper-titanium rod is put into built-in angle passage is extruded repeatedly, specific method be by a diameter of 10mm with
Length (is the circle that the copper rod center that a diameter of 6mm pure titanium rod is placed in into a diameter of 10mm is made for 10cm cylindrical specimens
Cylinder sample) it is placed at room temperature in extruding interior angle Φ=100 °, the mould of exterior angle ψ=20 °, universal test compressing head is set
Extruding rate is about 5mm/s, with Bc paths (keeping positive 90 degree of rotation per experimental sample between extruding twice) for mode of entrance, altogether
Meter 5 passages of extruding, ECAP operations are carried out by experiment material.Note material being heat-treated in extruding, will specially squeeze every time
Copper-titanium rod after pressure processing temper, then air cooling at 400 DEG C.
The lubricant main component that mould is put into extrusion process is 20%MoS2With 80% graphite.Peeled off after extruding successfully
Go out pure titanium material first test specimen is polished to after 2500 mesh using 25%HNO using SiC sand paper3The reagent of+5%HF+70% water enters
Row corrosion treatment, is made the pure titanium of Ultra-fine Grained.
2) Microarc Oxidation Surface Treatment
The pure titanium of obtained Ultra-fine Grained is cut into the discoid test specimens of diameter 5mm thickness 2mm through line of material.SiC sand paper is polished to
1500 mesh, are cleaned 3 times according still further to the order ultrasonic vibration of acetone, absolute alcohol, deionized water, and common pure titanium control group is also carried out
Corresponding processing.It is placed at microarc oxidation equipment provided Anodic, stainless steel plate is as negative electrode, in phosphate system electrolyte,
4min is handled, it is ultra-fine that differential arc oxidation is made in (differential arc oxidation handles voltage 450V, pulse, frequency 500HZ, cycle period 10%)
Brilliant pure titanium.
Claims (3)
1. a kind of preparation method of the differential arc oxidation mouth cavity planting body pure titanium of Ultra-fine Grained, it is characterised in that comprise the following steps：
1) the pure titanium of Ultra-fine Grained is prepared
At room temperature, copper-titanium rod is put into the mould of built-in angle passage, with omnipotent squeeze test machine using Bc paths as entrance
Mode carries out the processing of 2~5 passage Equal-channel Angular Pressings, and is carried out again after heat treatment elimination internal stress after extrusion process every time
Extrusion process, until extruding is completed, then peels off titanium bar material next time, then polished, corrosion treatment, Ultra-fine Grained is made pure
Titanium；
Wherein, the copper-titanium rod is the cylinder that the copper rod center that a diameter of 6mm pure titanium rod is placed in into a diameter of 10mm is made
Sample；The extruding interior angle of the mould of built-in angle passage be 120 °, extruding exterior angle be 20 °, omnipotent squeeze test compressing head squeeze
Pressure speed is 6mm/s；It is described heat treatment be by the copper after each extrusion process-titanium rod at 200 DEG C temper, Ran Houkong
It is cold；It is described to refer to make titanium bar material turn clockwise 90 ° per between extruding twice by mode of entrance of Bc paths；Equal channel angular
Lubricant is put into during extrusion process in a mold, and the lubricant is by percentage to the quality, by 15% MoS2With 85% graphite
Composition；
Described polishing is that the titanium bar material that will be separated is polished to 2000 mesh with SiC sand paper, and described corrosion treatment is using rotten
Lose agent to carry out, corrosive agent is with volume percentage, including 20%HNO3, 5%HF and 75% water；
2) Microarc Oxidation Surface Treatment
The pure titanium of obtained Ultra-fine Grained is cut into a diameter of 6mm, thickness is 3mm discoid test specimen, then by polishing, cleaning,
Be subsequently placed in it is microarc oxidation equipment provided in anode position, using stainless steel plate as negative electrode, in phosphate system electrolyte,
450V, pulse, 500Hz and cycle period be 15% under conditions of, Microarc Oxidation Surface Treatment 5min, be made differential arc oxidation surpass
The pure titanium of fine grain, 7.833 ± 0.771 μm of the average thickness of the pure titanium of differential arc oxidation Ultra-fine Grained, roughness is 1.391 ± 0.143 μm,
Adhesion is 23.900 ± 1.267N, and tensile strength reaches 791MPa, and Vickers hardness reaches 2450MPa；
Described polishing is that with SiC sand paper discoid test specimen is polished into 1500 mesh；Described cleaning is by the test specimen after polishing
Cleaned successively with acetone, absolute ethyl alcohol and deionized water sonic oscillation.
2. the pure titanium of differential arc oxidation Ultra-fine Grained made from the method described in claim 1, it is characterised in that the differential arc oxidation Ultra-fine Grained
7.833 ± 0.771 μm of the average thickness of pure titanium, roughness is 1.391 ± 0.143 μm, and adhesion is 23.900 ± 1.267N, is resisted
Tensile strength reaches 791MPa, and Vickers hardness reaches 2450MPa.
3. the answering in mouth cavity planting body material is prepared of the pure titanium of differential arc oxidation Ultra-fine Grained made from the method described in claim 1
With.
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| CN106333754B (en) * | 2016-09-21 | 2017-11-17 | 中国人民解放军第四军医大学 | A kind of pure titanium oral cavity micro-implant of Ultra-fine Grained and preparation method thereof |
| CN107313100B (en) * | 2017-06-30 | 2019-07-02 | 宿迁市河海大学研究院 | A kind of preparation method of the high tough corrosion-resistant AZ91 magnesium alloy bulk of yellow |
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