CN108478858A - A kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface - Google Patents

A kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface Download PDF

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Publication number
CN108478858A
CN108478858A CN201810281002.0A CN201810281002A CN108478858A CN 108478858 A CN108478858 A CN 108478858A CN 201810281002 A CN201810281002 A CN 201810281002A CN 108478858 A CN108478858 A CN 108478858A
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titanium implant
hydrophilic surface
preparation
implant
time
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黄文华
严玲玲
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Southern Medical University
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Southern Medical University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/06Titanium or titanium alloys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • C23F3/04Heavy metals
    • C23F3/06Heavy metals with acidic solutions
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/12Materials or treatment for tissue regeneration for dental implants or prostheses

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Organic Chemistry (AREA)
  • Public Health (AREA)
  • Metallurgy (AREA)
  • Dermatology (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Dental Prosthetics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Prostheses (AREA)
  • Materials For Medical Uses (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The present invention proposes a kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface, includes the following steps:Sandblasting polishing treatment is carried out to titanium implant using sand grains;Acid polishing processing is carried out to the titanium implant after sandblasting polishing treatment using pickling solution;Anodized will be carried out in acid polishing treated titanium implant merging electrolyte;Titanium implant after anodized is put into annealing device and is heat-treated.There is urn Topography surface based on titanium implant prepared by this method, the preferably surface texture of simulation bone tissue, more significant biological effect, its super hydrophilic surface layer can increase the contact with wetting fluid, the new bone formation for being conducive to implant-bone interface has good facilitation to planting successfully.

Description

A kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface
Technical field
The present invention relates to a kind of surface treatment method of Medical oral cavity planting body more particularly to a kind of titanium implant nanoscales The preparation method of ultra-hydrophilic surface.
Background technology
Titanium is presently the most common dentistry implant material, with good biocompatibility, mechanical strength And outstanding corrosion resistance, and the relatively low density close to skeleton of density.As dental implant, with bone tissue reality Existing synostosis is one of the major criterion for evaluating Dental implantion success or not.And the surface treatment of planting body is Osseointegrated implants Important influence factor makes the Healing around Titanium Implants time shorten, synosteosis speed is accelerated by being modified to implant surface It is the research emphasis and hot spot in oral implant rehabilitation field now with functional load time advance.In natural bone tissue containing whether there is or not A variety of nano components such as the machine minerals such as collagenous fibres of hydroxyapatite, surface, universal theory think receiving for implant surface Meter level pattern can preferably simulate the mechanism of bone tissue, have more significant biological effect.In addition, the surface of Superhydrophilic The contact with wetting fluid can be increased, promote the new bone apposition around plantation and then improve Integrated implant, duration of load application is made to carry Before.The common surface treatment method of the planting body of business application at present is mostly such as bulky grain sandblasting acid etching (SLA) this list One roughening implant surface processing method, osteogenic action is limited, while facing surface hydrophilicity, close bone, planting body- The problems such as long-time stability of bone interface are undesirable.
Therefore, in view of the shortcomings of the prior art, provide a kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface with gram It is very necessary to take prior art deficiency.
Invention content
The present invention provides a kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface, and this method step is simple, pair sets It is low for requiring, it can increase the contact with wetting fluid on the super hydrophilic surface layer of nanoscale that titanium implant surface is prepared, have Conducive to the new bone formation of Implant-bone interface, there is good facilitation to planting successfully.
The above-mentioned purpose of the present invention is realized by following technological means.
A kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface is provided, is included the following steps:
S1, sandblasting polishing treatment is carried out to titanium implant using sand grains;
S2, acid polishing processing is carried out to the titanium implant after sandblasting polishing treatment using pickling solution;
S3, anodized will be carried out in acid polishing treated titanium implant merging electrolyte;
S4, it the titanium implant after anodized is put into annealing device is heat-treated.
Further, in step S1, sand grains used is the alumina particulate of 20~60 mesh.
Further, in step S1, the sandblasting of sandblasting polishing treatment used distance is 8~25cm, blast time is 15~ 32s。
Further, in step S2, pickling solution used is hydrofluoric acid solution.
Further, in step S2, the etching time of acid polishing processing used is 8~34s.
Further, in step S3, electrolyte used is hydrofluoric acid solution.
Further, in step S3, the voltage of anodized used is 17~32V, and the time is 18~65min, temperature Degree is 15~33 DEG C.
Further, in step S4, the temperature of heat treatment used is 300~600 DEG C, and heat treatment time is 1~8 hour.
Preferably, sandblasting distance is 10~20cm, and blast time is 20~30s;Etching time is 10~30s, pickling solution A concentration of 3%~7%;Anodized voltage is 20~30V, and the time is 20~60min, and temperature is 20~30 DEG C, electrolysis Liquid a concentration of 0.5%~1%;Heat treatment temperature is 350~550 DEG C, and heat treatment time is 3~6 hours.
Preferably, sandblasting distance is 20cm, blast time 20s;Etching time is 20s, pickling solution a concentration of 5%;Sun Pole oxidation processes voltage is 22V, and time 30min, temperature is 20 DEG C, concentration of electrolyte 0.7%;Heat treatment temperature is 450 DEG C, heat treatment time is 4 hours.
The present invention is overcome with the surface treatment method that physical method and electrochemical method are combined at traditional surface Ineffective, the shortcomings that easy ting produce adverse reaction is managed, the titanium implant with urn Topography surface, titanium plantation have been obtained Body have preferably simulation bone tissue surface texture, more significant biological effect, super hydrophilic surface layer can increase with it is wet The contact for moistening liquid, is conducive to the new bone formation of Implant-bone interface, has good facilitation to planting successfully.
Description of the drawings
Using attached drawing, the present invention will be further described, but the content in attached drawing does not constitute any limitation of the invention.
Fig. 1 is the flow chart of the titanium implant surface processing of the present invention;
Fig. 2 is the scanning electron microscope (SEM) photograph that the surface texture before the titanium implant surface processing of the present invention amplifies 500 times;
Fig. 3 is that titanium implant surface treated the surface texture of the present invention amplifies 1000 times of scanning electron microscope (SEM) photograph;
Fig. 4 is the surface hydrophilicity test comparison figure of titanium implant surface before and after the processing, and wherein the left side is untreated samples, The right is sample after processing.
Specific implementation mode
The invention will be further described with the following Examples.
Embodiment 1.
A kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface is provided, as shown in Figure 1, including the following steps:
S1, sandblasting polishing treatment is carried out to titanium implant using the alumina particulate of 20~60 mesh;Sandblasting distance for 8~ 25cm, blast time are 15~32s.
S2, acid polishing processing is carried out to the titanium implant after sandblasting polishing treatment using pickling solution;Etching time be 8~ 34s, pickling solution are hydrofluoric acid solution.
S3, anodized will be carried out in acid polishing treated titanium implant merging electrolyte;At anodic oxidation Reason voltage is 17~32V, and the time is 18~65min, and temperature is 15~33 DEG C, and electrolyte is hydrofluoric acid solution.
S4, it the titanium implant after anodized is put into annealing device is heat-treated.Heat treatment temperature is 300~600 DEG C, heat treatment time is 1~8 hour.
The present embodiment overcomes traditional surface with the surface treatment method that physical method and electrochemical method are combined Treatment effect is bad, the shortcomings that easy ting produce adverse reaction, has obtained the titanium implant with urn Topography surface, the titanium kind Implant have preferably simulation bone tissue surface texture, more significant biological effect, super hydrophilic surface layer can increase with The contact of wetting fluid is conducive to the new bone formation of Implant-bone interface, has good facilitation to planting successfully.
Embodiment 2.
With a specific example, the invention will be further described.
The present embodiment provides a kind of preparation methods of titanium implant nanoscale ultra-hydrophilic surface, as shown in Figure 1, including as follows Step:
S1, sandblasting polishing treatment is carried out to titanium implant using the alumina particulate of 20~60 mesh;Sandblasting distance for 10~ 20cm, blast time are 20~30s.
S2, acid polishing processing is carried out to the titanium implant after sandblasting polishing treatment using pickling solution;Etching time is 10 ~30s, pickling solution are 3%~7% hydrofluoric acid solution.
S3, anodized will be carried out in acid polishing treated titanium implant merging electrolyte;At anodic oxidation Reason voltage is 20~30V, and the time is 20~60min, and temperature is 20~30 DEG C, and electrolyte is 0.5%~1% hydrofluoric acid solution.
S4, it the titanium implant after anodized is put into annealing device is heat-treated.Heat treatment temperature is 350~550 DEG C, heat treatment time is 3~6 hours.
The titanium implant on the urn Topography surface prepared under the conditions of the present embodiment, surface nano-structure is smaller, Distribution is more uniform, and with more significant biological effect, the contact of super hydrophilic surface layer and wetting fluid is more preferable, is conducive to Promote the new bone formation of Implant-bone interface.
Embodiment 3.
With a specific example, the invention will be further described.
The present embodiment provides a kind of preparation methods of titanium implant nanoscale ultra-hydrophilic surface, as shown in Figure 1, including as follows Step:
S1, sandblasting polishing treatment is carried out to titanium implant using the alumina particulate of 20~60 mesh;Sandblasting distance is 20cm, Blast time is 20s.
S2, acid polishing processing is carried out to the titanium implant after sandblasting polishing treatment using pickling solution;Etching time is 20s, pickling solution are 5% hydrofluoric acid solution.
S3, anodized will be carried out in acid polishing treated titanium implant merging electrolyte;At anodic oxidation Reason voltage is 22V, and time 30min, temperature is 20 DEG C, and electrolyte is 0.7% hydrofluoric acid solution.
S4, it the titanium implant after anodized is put into annealing device is heat-treated.Heat treatment temperature is 450 DEG C, heat treatment time is 4 hours.
As shown in Fig. 2, its surface is without urn Topography before titanium implant surface processing, according to method provided in this embodiment Titanium implant its surface nano-structure after surface treatment is smaller, and distribution is more uniform, as shown in Figure 3.To surface treatment Front and back titanium implant does surface hydrophilicity test respectively, and the results are shown in Figure 4, the titanium implant surface before surface treatment and water Between contact angle much larger than surface treatment after titanium implant surface and water between contact angle, after illustrating surface treatment, titanium Implant surface hydrophily is more preferable, and is as can be seen from the figure planted according to the titanium after method provided in this embodiment surface treatment Contact angle between its surface of body and water is almost nil, illustrates the titanium implant surface nanostructure size smaller, distribution is more Uniformly, there is more significant biological effect, the contact of super hydrophilic surface layer and wetting fluid is more preferable, may advantageously facilitate plantation The new bone formation of body-bone interface.
The present invention is overcome with the surface treatment method that physical method and electrochemical method are combined at traditional surface Ineffective, the shortcomings that easy ting produce adverse reaction is managed, the titanium implant with urn Topography surface, titanium plantation have been obtained Body have preferably simulation bone tissue surface texture, more significant biological effect, super hydrophilic surface layer can increase with it is wet The contact for moistening liquid, is conducive to the new bone formation of Implant-bone interface, has good facilitation to planting successfully.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention The limitation of range, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art should manage Solution, technical scheme of the present invention can be modified or replaced equivalently, without departing from technical solution of the present invention essence and Range.

Claims (10)

1. a kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface, which is characterized in that include the following steps:
S1, sandblasting polishing treatment is carried out to titanium implant using sand grains;
S2, acid polishing processing is carried out to the titanium implant after sandblasting polishing treatment using pickling solution;
S3, anodized will be carried out in acid polishing treated titanium implant merging electrolyte;
S4, it the titanium implant after anodized is put into annealing device is heat-treated.
2. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 1, it is characterised in that:The step In rapid S1, sand grains used is the alumina particulate of 20~60 mesh.
3. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 2, it is characterised in that:The step In rapid S1, the sandblasting distance of sandblasting polishing treatment used is 8~25cm, and blast time is 15~32s.
4. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 3, it is characterised in that:The step In rapid S2, pickling solution used is hydrofluoric acid solution.
5. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 4, it is characterised in that:The step In rapid S2, the etching time of acid polishing processing used is 8~34s.
6. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 5, it is characterised in that:The step In rapid S3, electrolyte used is hydrofluoric acid solution.
7. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 6, it is characterised in that:The step In rapid S3, the voltage of anodized used is 17~32V, and the time is 18~65min, and temperature is 15~33 DEG C.
8. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 7, it is characterised in that:The step In rapid S4, the temperature of heat treatment used is 300~600 DEG C, and heat treatment time is 1~8 hour.
9. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 8, it is characterised in that:The spray Sand distance is 10~20cm, and blast time is 20~30s;
The etching time is 10~30s, pickling solution a concentration of 3%~7%;
The anodized voltage is 20~30V, and the time is 20~60min, and temperature is 20~30 DEG C, and concentration of electrolyte is 0.5%~1%;
The heat treatment temperature is 350~550 DEG C, and heat treatment time is 3~6 hours.
10. the preparation method of titanium implant nanoscale ultra-hydrophilic surface according to claim 9, it is characterised in that:It is described Sandblasting distance is 20cm, blast time 20s;
The etching time is 20s, pickling solution a concentration of 5%;
The anodized voltage is 22V, and time 30min, temperature is 20 DEG C, concentration of electrolyte 0.7%;
The heat treatment temperature is 450 DEG C, and heat treatment time is 4 hours.
CN201810281002.0A 2018-04-02 2018-04-02 A kind of preparation method of titanium implant nanoscale ultra-hydrophilic surface Pending CN108478858A (en)

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Cited By (7)

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CN109913919A (en) * 2019-02-18 2019-06-21 江苏大学 A kind of processing method and device preparing micro-nano two-dimensional structure in workpiece surface
CN109957803A (en) * 2019-03-15 2019-07-02 延边伊诺登医疗科技有限公司 A kind of modification anodic titanium surface treatment method for planting body
CN110238709A (en) * 2019-07-04 2019-09-17 尚蒙科技无锡有限公司 A kind of processing method of super-hydrophilic self-cleaning frosting
CN113729998A (en) * 2021-08-04 2021-12-03 佛山市安齿生物科技有限公司 Method for manufacturing dental implant
CN114307201A (en) * 2022-01-06 2022-04-12 中南大学 Liquid energy-saving efficient heating evaporation method, interface material and preparation method
CN115074712A (en) * 2022-07-29 2022-09-20 四川大学 Surface modification treatment method for titanium metal implant material
CN115090905A (en) * 2022-06-08 2022-09-23 佳木斯大学 Preparation method of 3D printed medical nickel-titanium super-hydrophilic complex structure surface

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913919A (en) * 2019-02-18 2019-06-21 江苏大学 A kind of processing method and device preparing micro-nano two-dimensional structure in workpiece surface
CN109913919B (en) * 2019-02-18 2020-11-20 江苏大学 Processing method and device for preparing micro-nano two-dimensional structure on surface of workpiece
CN109957803A (en) * 2019-03-15 2019-07-02 延边伊诺登医疗科技有限公司 A kind of modification anodic titanium surface treatment method for planting body
CN110238709A (en) * 2019-07-04 2019-09-17 尚蒙科技无锡有限公司 A kind of processing method of super-hydrophilic self-cleaning frosting
CN113729998A (en) * 2021-08-04 2021-12-03 佛山市安齿生物科技有限公司 Method for manufacturing dental implant
CN113729998B (en) * 2021-08-04 2023-10-27 广东中科安齿生物科技有限公司 Method for manufacturing dental implant
CN114307201A (en) * 2022-01-06 2022-04-12 中南大学 Liquid energy-saving efficient heating evaporation method, interface material and preparation method
CN114307201B (en) * 2022-01-06 2022-11-08 中南大学 Liquid energy-saving efficient heating evaporation method, interface material and preparation method
CN115090905A (en) * 2022-06-08 2022-09-23 佳木斯大学 Preparation method of 3D printed medical nickel-titanium super-hydrophilic complex structure surface
CN115074712A (en) * 2022-07-29 2022-09-20 四川大学 Surface modification treatment method for titanium metal implant material

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Application publication date: 20180904