CN109234735A - A kind of EBM molding titanium implants and its preparation method and application - Google Patents
A kind of EBM molding titanium implants and its preparation method and application Download PDFInfo
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- CN109234735A CN109234735A CN201811347393.8A CN201811347393A CN109234735A CN 109234735 A CN109234735 A CN 109234735A CN 201811347393 A CN201811347393 A CN 201811347393A CN 109234735 A CN109234735 A CN 109234735A
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23F—NON-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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
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- 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
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- A61L27/06—Titanium or titanium alloys
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
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- A—HUMAN NECESSITIES
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- 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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- 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
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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Abstract
The present invention provides a kind of EBM molding titanium implants and its preparation method and application, belongs to biomedical implant field of material technology.The EBM molding titanium implants preparation method includes post-processing to the molding titanium implants of EBM mode, and the post-processing includes ultrasonic acid etching and anodic oxidation.When the present invention prepares EBM molding titanium implants, EBM titanium implants after molding are surface-treated using ultrasonic acid etching and anodic oxidation etc., residual powder can not only be effectively removed, it prepares simultaneously on surface conducive to cell adherence, the micro-nano multilevel structure of proliferation and differentiation, preparation method of the present invention is easy, and the use of chemical reagent can be effectively reduced, the titanium implants being prepared simultaneously have the composite construction of micro-nano multistage abundant, implant osteogenic activity can be effectively facilitated, effectively enhance the Integrated implant ability of planting body simultaneously, improve plantation success rate, therefore it is with a wide range of applications.
Description
Technical field
The invention belongs to biomedical implant field of material technology, and in particular to a kind of EBM molding titanium implants and its
Preparation method and application.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without answering
It is existing well known to persons skilled in the art that this is considered as recognizing or imply that information composition has become in any form
Technology.
With aging of population process propulsion and it is self, allogenic bone transplantation side effect highlight, clinic is for bone implant
The demand of material increasingly increases.Titanium is due to superiority such as good biocompatibility, corrosion resistance and mechanical properties
Can, it is a kind of internal displacement material with development potentiality, has clinically been widely used for many years.However, titanium material bullet
Property modulus with people's bone differ larger, be also easy to produce stress shielding phenomenon, lead to the inflammation of osteanabrosis and implant, loosen,
Service life is shortened, patient can be made by unnecessary pain.Simultaneously as the physiological structure of every patient is multifarious,
Universal implant specification might not be applicable in each patient, therefore, for patient unique physiological structure and produce
Personalized product have important clinical meaning.
The appearance of increasing material manufacturing (also known as 3D printing) technology brings new opportunity to the design and manufacture of novel implant.Difference
In conventionally manufactured mode, increases material manufacturing technology can carry out personalized customization processing for the special defect structure of sufferer, together
When can manufacture the workpiece with complex external shape and inner porosity more flexiblely.The porous structure of implant can be with
Its elasticity modulus is reduced, " stress shielding " phenomenon is effectively prevent, can internally be grown into using bone tissue, while connectivity is more
Pore structure is conducive to the transmission of nutriment, improves implantation stability and osseointegration character.Electron beam melting deposition
(Electronic Beam Melting, EBM) technology is a kind of to utilize beam energy fusing metal powder and deposition modeling
Increases material manufacturing technology is widely used in the molding of titanium.However, the titanium implants surface after molding EBM is rougher, there are powder
The unfinished sharp flash for melting and being formed, simultaneously because the presence of porous structure, powder residual is easy to be stranded and be trapped in inside hole,
If not removing, it will lead to implant powder abrasion, free danger during long service, cause human poisoning etc. bad anti-
It answers, destroys human normal function.
Summary of the invention
In view of the above shortcomings of the prior art, the present invention provides a kind of EBM molding titanium implants and preparation method thereof and answers
With.When the present invention prepares EBM molding titanium implants, using ultrasonic acid etching and anodic oxidation etc. to EBM titanium implants after molding
It is surface-treated, residual powder can not only be effectively removed, while preparing conducive to cell adherence, proliferation and differentiation on surface
Micro-nano multilevel structure, improve the bone formation performance of implant, with good practical application value.
One of the objects of the present invention is to provide a kind of preparation methods of EBM molding titanium implants.
The second object of the present invention is to provide the EBM molding titanium implants that the above method is prepared.
The third object of the present invention is to provide the application of above-mentioned EBM molding titanium implants.
To achieve the above object, the present invention relates to following technical schemes:
The first aspect of the invention provides a kind of preparation method of EBM molding titanium implants, and the method includes right
The molding titanium implants of EBM mode are post-processed, and the post-processing includes ultrasonic acid etching and anodic oxidation.
Wherein, the ultrasonic acid etching method particularly includes:
Acid corrosion liquid is made in the mixed solution that acid or acid and oxidant is used alone, by the molding titanium implants of EBM mode
It is placed in acid corrosion liquid, while being ultrasonically treated.
Wherein, the acid includes but is not limited to hydrochloric acid, sulfuric acid, hydrofluoric acid, nitric acid, any one or more in oxalic acid；
The oxidant includes but is not limited to hydrogen peroxide；
At 10 DEG C~80 DEG C, the processing time is 1~30min for temperature control；
Supersonic frequency is 40kHz, and power is 100~600W.
The anodized method particularly includes:
Using platinized platinum or graphite as cathode, the titanium implants after ultrasonic acid etching are anode, carry out anode in the electrolytic solution
Oxidation processes；
Wherein, the electrolyte is NH4The mixed solution of F aqueous solution and ethylene glycol；
Further, spacing is 20~40mm between two electrodes, and voltage is 15V~60V, and temperature control is 20 DEG C~60 DEG C,
The processing time is 15~120min.
The second aspect of the invention provides the EBM molding titanium implants that above-mentioned preparation method is prepared.The titanium is planted
Entering body raw material includes Titanium or titanium alloy, and further, the titanium alloy is Ti6Al4V.
The third aspect of the invention provides application of the above-mentioned EBM molding titanium implants in preparation kind bone-grafting material.
Advantageous effects of the invention:
(1) the common micron scale construction preparation method in traditional micro/nano structure preparation method be sandblasting and acid etching,
Middle blasting process dust diffuses, and there are environmental pollutions, unfavorable to the health of operator, while being also possible in material
Residual powder on surface leads to the risk of cause people poisoning or inflammation after implantation human body；And individually using acid etching by micropore area
The blind hole effect in domain etc. influences, acid etching low efficiency, and pollution is larger, and it is more sharp to generate bowl configurations.Preparation method of the present invention
EBM rough morphology after molding is directly utilized, and carries out ultrasonic acid etching and anodic oxidation modification on this basis, eliminates sandblasting
Technique both improves efficiency, also reduces cost and environmental pollution, reduces the risk of graft failure.
(2) due to the implant with porous structure of printing shaping since the blind hole effect of its micro-porous area makes reaction solution
Body is difficult to go deep into carry out ion exchange inside micropore, and the present invention is based on the ultrasounds of microjet principle to have brill seam effect, using super
Heterogeneous reaction speed can be improved in acoustic cavitation shock effect, physical effect etc., and accelerated acid etching liquid is to the blunt of implant surfaces
Change, promotes the powder of porous structure internal residual to overflow, dissolve and the diffusion of product.Simultaneously decrease acid processing time,
Reduce the concentration of required acid solution, for pickling agent recycling, improve resource utilization and reducing environmental pollution and provide
One new approach.
(3) micrometer structure that obtains after ultrasonic acid etching of the present invention can promote the adherency of cell, increase bone with
Inlay resultant force between implant；The nano tubular structure that anodic oxidation is prepared can be improved the hydrophily of material, promote biology
The absorption of active factors.Composite construction with micro-nano multistage can have been influenced the microenvironment of cell, regulation by extensive proof
The behaviors such as cell adherence, proliferation and differentiation enhance the osseointegration character of implant.
To sum up, preparation method of the present invention is easy, and can effectively reduce the use of chemical reagent, while the titanium being prepared is planted
Enter the composite construction that body has micro-nano multistage abundant, implant osteogenic activity, while effectively enhancing kind can be effectively facilitated
The Integrated implant ability of implant improves plantation success rate, therefore is with a wide range of applications.
Detailed description of the invention:
Fig. 1: embodiment 1EBM mode forms porous stud SEM picture (35 ×)；
Fig. 2: embodiment 1EBM mode forms porous stud SEM picture (100 ×)；
Fig. 3: the EBM mode after ultrasonic acid etching-anodized of embodiment 1 forms porous stud SEM picture (35 ×)；
Fig. 4: the EBM mode after ultrasonic acid etching-anodized of embodiment 1 forms porous stud SEM picture (100
×)；
Fig. 5: the EBM mode after ultrasonic acid etching-anodized of embodiment 1 forms porous stud SEM picture (5000
×)；
Fig. 6: the EBM mode after ultrasonic acid etching-anodized of embodiment 1 forms porous stud SEM picture (200000
×)。
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As previously mentioned, the titanium implants surface after molding EBM is rougher in the prior art, there are the unfinished fusing of powder
The sharp flash formed, simultaneously because the presence of porous structure, powder residual is easy to be stranded and be trapped in inside hole, will if not removing
Lead to implant powder abrasion, free danger during long service, causes the adverse reactions such as human poisoning, destroy human body
Normal function.
In view of this, providing a kind of preparation side of EBM molding titanium implants in the specific embodiment of the present invention
Method, which comprises
(1) titanium implants EBM mode forms: using Titanium or titanium alloy spherical powder as raw material, using EBM molding mode
Print implant；
Wherein, beam power 900W, 100 μm of spot diameter, 50 μm of thickness, scanning speed 800mm/s；
(2) different types of acid such as hydrochloric acid, sulfuric acid, hydrofluoric acid, nitric acid, oxalic acid, hydrogen peroxide or oxygen ultrasonic acid etching: are used
Agent progress is one or more to be mixed and made into pickling solution, and molding implant is immersed corrosive liquid.Temperature is 10 DEG C~80 DEG C, processing
Time is 1~30min.Ultrasonic wave, supersonic frequency 40kHz are introduced in acid corrosion process, power is 100~600W.
Wherein, pickling solution is preferably wt.40%HF, wt.37%HCl and water mixed solution, three's volume ratio 1:1:18；
Or,
Preferably wt.98%H2SO4, wt.35%HCl and water mixed solution, three's volume ratio is 0.1:1:10；
Or,
Preferably wt.40%HF, wt.30%H2O2With water mixed solution, three's volume ratio 1:1:10；
Or,
Preferably wt.40%HF, wt.60%HON3With water mixed solution, three's volume ratio 1:1:30.
Using being ultrasonically treated and passing through control supersonic frequency and power, titanium or titanium alloy structure property situation are not being influenced
Under, passivation of the pickling solution to implant surfaces has been substantially speeded up, the powder of porous structure internal residual is promoted to overflow, dissolve and produce
The diffusion of object；The concentration of acid solution needed for also effectively reducing the sour time handled, reduction simultaneously；Meanwhile it has been confirmed by experiments that using upper
Ultrasonic acid etching is stated, the bowl configurations being prepared are smoother, and it is more similar with the Bone resoiption pit of self-assembling formation, therefore more
Be conducive to adherency, proliferation and the differentiation of osteoblast；
(3) anodic oxidation: being anode using platinized platinum or graphite as cathode, molding implant, in NH4F aqueous solution and ethylene glycol
Anodized is carried out in mixed electrolyte.Spacing is 20~40mm between two electrodes, and voltage is 15V~60V, temperature 20
DEG C~60 DEG C, the optimization process time is 15~120min.
Wherein, the electrolyte is specially mass fraction 0.1%NH41:36 is mixed F aqueous solution by volume with ethylene glycol
Solution afterwards.
In still another embodiment of the invention, the EBM molding titanium implants that above-mentioned preparation method is prepared are provided.
The titanium implants raw material includes Titanium or titanium alloy, and further, the titanium alloy is Ti6Al4V.
In still another embodiment of the invention, above-mentioned EBM molding titanium implants are provided in preparation kind bone-grafting material
Application.
Explanation is further explained to the present invention by the following examples, but is not construed as limiting the invention.It should be understood that
These examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.Actual conditions are not specified in the following example
Test method, carry out usually according to normal condition.
Embodiment 1
(1) titanium implants EBM mode forms: the stud model using Solidworks Software on Drawing having a size of Φ 2*3 makes
Porous array unit is added by Boolean calculation mode on stud model with 3-matic software, aperture 0.18mm, unit are set
Shank diameter 0.2mm, porosity 55%.After importing EBM molding equipment, carried out by raw material of titanium alloy ti6al4v spherical powder
Printing.Powder diameter be 45~106 μm, beam power 900W, 100 μm of spot diameter, 50 μm of thickness, scanning speed
800mm/s。
(2) ultrasonic acid etching: preparing mass fraction is 40% hydrofluoric acid and 37% hydrochloric acid, with water 1:1:18 by volume
Molding implant is immersed in acid solution and is corroded by mixing.Temperature is 30 DEG C, etching time 5min.Ultrasound is introduced in acid corrosion process
Wave, supersonic frequency 40kHz, power 500W.
(3) anodic oxidation: being anode by cathode, stud implant of platinized platinum, and electrolyte is mass fraction 0.1%NH4F water
The mixed solution of 1:36, electrode spacing 30mm, voltage 20V, temperature are 20 DEG C by volume for solution and ethylene glycol, electrolysis
Time is 60min.
The titanium alloy implant surfaces powder residue removal that the present embodiment obtains is thorough, and produces with 0.15-0.2mm
Macroporous, 10-100 μm of micron order pit, 0.2-0.5 μm of submicron order hole and 40-60nm nanoscale pipe
The micro-nano multistage composite structure of shape structure.
Embodiment 2
(1) titanium implants EBM mode forms: the stud model using Solidworks Software on Drawing having a size of Φ 2*3 makes
Porous array unit is added by Boolean calculation mode on stud model with 3-matic software, aperture 0.18mm, unit are set
Shank diameter 0.2mm, porosity 55%.After importing EBM molding equipment, printed using titanium spherical powder as raw material.Powder
Expect diameter be 50~110 μm, beam power 900W, 100 μm of spot diameter, 50 μm of thickness, scanning speed 800mm/s.
(2) ultrasonic acid etching: preparing mass fraction is 98% sulfuric acid and 35% hydrochloric acid, with water 0.1:1:10 by volume
Molding implant is immersed in acid solution and is corroded by mixing.Temperature is 40 DEG C, etching time 10min.Ultrasound is introduced in acid corrosion process
Wave, supersonic frequency 40kHz, power 400W.
(3) anodic oxidation: being anode by cathode, stud implant of platinized platinum, and electrolyte is mass fraction 0.1%NH4F water
The mixed solution of 1:36, electrode spacing 30mm, voltage 30V, temperature are 30 DEG C by volume for solution and ethylene glycol, electrolysis
Time is 60min.
Embodiment 3
(1) titanium implants EBM mode forms: the stud model using Solidworks Software on Drawing having a size of Φ 2*3 makes
Porous array unit is added by Boolean calculation mode on stud model with 3-matic software, aperture 0.18mm, unit are set
Shank diameter 0.2mm, porosity 55%.After importing EBM molding equipment, carried out by raw material of titanium alloy ti6al4v spherical powder
Printing.Powder diameter be 45~106 μm, beam power 900W, 100 μm of spot diameter, 50 μm of thickness, scanning speed
800mm/s。
(2) ultrasonic acid etching: preparing mass fraction is 40% hydrofluoric acid and 30% hydrogen peroxide, with water 1:1:10 by volume
Molding implant is immersed in acid solution and is corroded by mixing.Temperature is 40 DEG C, etching time 8min.Ultrasound is introduced in acid corrosion process
Wave, supersonic frequency 40kHz, power 500W.
(3) anodic oxidation: being anode by cathode, stud implant of platinized platinum, and electrolyte is mass fraction 0.1%NH4F water
The mixed solution of 1:36, electrode spacing 40mm, voltage 30V, temperature are 50 DEG C by volume for solution and ethylene glycol, electrolysis
Time is 30min.
Embodiment 4
(1) titanium implants EBM mode forms: the stud model using Solidworks Software on Drawing having a size of Φ 2*3 makes
Porous array unit is added by Boolean calculation mode on stud model with 3-matic software, aperture 0.18mm, unit are set
Shank diameter 0.2mm, porosity 55%.After importing EBM molding equipment, printed using titanium spherical powder as raw material.Powder
Expect diameter be 45~106 μm, beam power 900W, 100 μm of spot diameter, 50 μm of thickness, scanning speed 800mm/s.
(2) ultrasonic acid etching: preparing mass fraction is 40% hydrofluoric acid and 60% nitric acid, and 1:1:30 is mixed by volume with water
It closes, molding implant is immersed in acid solution and is corroded.Temperature is 40 DEG C, etching time 5min.Ultrasonic wave is introduced in acid corrosion process,
Supersonic frequency is 40kHz, power 400W.
(3) anodic oxidation: being anode by cathode, stud implant of platinized platinum, and electrolyte is mass fraction 0.1%NH4F water
The mixed solution of 1:36, electrode spacing 40mm, voltage 30V, temperature are 40 DEG C by volume for solution and ethylene glycol, electrolysis
Time is 40min.
It should be noted that above example is only used to illustrate the technical scheme of the present invention rather than is limited.Although ginseng
It is described the invention in detail according to given example, but those skilled in the art can be as needed to this hair
Bright technical solution is modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. a kind of preparation method of EBM molding titanium implants, which is characterized in that the method includes to the molding titanium of EBM mode
Implant is post-processed, and the post-processing includes ultrasonic acid etching and anodic oxidation.
2. a kind of preparation method as described in claim 1, which is characterized in that the ultrasound acid etching method particularly includes:
Acid corrosion liquid is made in the mixed solution that acid or acid and oxidant is used alone, and the molding titanium implants of EBM mode are placed in
In acid corrosion liquid, while being ultrasonically treated.
3. a kind of preparation method as claimed in claim 2, which is characterized in that the acid includes but is not limited to hydrochloric acid, sulfuric acid, hydrogen
Fluoric acid, nitric acid, any one or more in oxalic acid.
4. a kind of preparation method as claimed in claim 2, which is characterized in that the oxidant includes but is not limited to peroxidating
Hydrogen.
5. a kind of preparation method as claimed in claim 2, which is characterized in that temperature is controlled at 10 DEG C~80 DEG C, handles the time
For 1~30min；Supersonic frequency is 40kHz, and power is 100~600W.
6. a kind of preparation method as described in claim 1, which is characterized in that the anodized method particularly includes:
Using platinized platinum or graphite as cathode, the titanium implants after ultrasonic acid etching are anode, carry out anodic oxidation in the electrolytic solution
Processing.
7. a kind of preparation method as claimed in claim 6, which is characterized in that the electrolyte is NH4F aqueous solution and ethylene glycol
Mixed solution.
8. a kind of preparation method as claimed in claim 6, which is characterized in that spacing is 20~40mm between two electrodes, and voltage is
15V~60V, temperature control are 20 DEG C~60 DEG C, and the processing time is 15~120min.
9. the EBM that any one of the claim 1-8 preparation method is prepared forms titanium implants；Wherein, the titanium implantation
Body raw material includes Titanium or titanium alloy；Preferably, the titanium alloy is Ti6Al4V.
10. application of the EBM molding titanium implants as claimed in claim 9 in preparation kind bone-grafting material.
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| CN113527749A (en) * | 2021-07-15 | 2021-10-22 | 山东大学 | Method for preparing multi-scale porous structure on surface of polyether-ether-ketone |
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| CN115779143A (en) * | 2022-11-11 | 2023-03-14 | 山东大学 | Titanium-based implant and preparation method and application thereof |
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| 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 |
| CN111545750A (en) * | 2020-05-13 | 2020-08-18 | 华中科技大学 | Flow channel powder removing method for high-energy-beam 3D printing heat dissipation cold plate and product |
| CN112387984A (en) * | 2020-10-29 | 2021-02-23 | 山东大学 | Post-treatment device and method for residual powder of 3D printing porous structure |
| CN112387984B (en) * | 2020-10-29 | 2022-04-08 | 山东大学 | Post-treatment device and method for residual powder of 3D printing porous structure |
| CN114681672A (en) * | 2020-12-29 | 2022-07-01 | 中国科学院上海硅酸盐研究所 | Titanium alloy biological function stent and preparation method and application thereof |
| CN112999414A (en) * | 2021-02-07 | 2021-06-22 | 大博医疗科技股份有限公司 | 3D printing titanium alloy and preparation method thereof |
| CN113527749A (en) * | 2021-07-15 | 2021-10-22 | 山东大学 | Method for preparing multi-scale porous structure on surface of polyether-ether-ketone |
| CN113527749B (en) * | 2021-07-15 | 2022-08-02 | 山东大学 | Method for preparing multi-scale porous structure on surface of polyether-ether-ketone |
| CN115779143A (en) * | 2022-11-11 | 2023-03-14 | 山东大学 | Titanium-based implant and preparation method and application thereof |
| CN115779143B (en) * | 2022-11-11 | 2024-02-13 | 山东大学 | Titanium-based implant, and preparation method and application thereof |
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