CN112301399A - Surface treatment method for dental implant - Google Patents

Surface treatment method for dental implant Download PDF

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CN112301399A
CN112301399A CN202010699474.5A CN202010699474A CN112301399A CN 112301399 A CN112301399 A CN 112301399A CN 202010699474 A CN202010699474 A CN 202010699474A CN 112301399 A CN112301399 A CN 112301399A
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titanium
implant
based implant
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张相皞
赵杰
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Jiangsu Yanyuan Elite Medical Technology Co ltd
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    • 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
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C8/00Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools
    • A61C8/0012Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the material or composition, e.g. ceramics, surface layer, metal alloy
    • A61C8/0013Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the material or composition, e.g. ceramics, surface layer, metal alloy with a surface layer, coating
    • 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
    • C25D11/026Anodisation with spark discharge

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Abstract

The invention discloses a surface treatment method of a dental implant, belonging to the technical field of dental implantation. It comprises the following steps: (1) pretreatment: polishing the titanium-based implant to be treated until the surface of the titanium-based implant is smooth; (2) acid pickling treatment: placing the titanium-based implant in acid liquor for acid washing; (3) and (3) drying treatment: cleaning the titanium-based implant and then drying the titanium-based implant; (4) surface anodic oxidation pretreatment: placing the titanium-based implant in surface anodic oxidation electrolyte for surface anodic oxidation; (5) surface micro-arc oxidation treatment: placing the titanium-based implant in a surface micro-arc oxidation electrolyte for surface micro-arc oxidation; (6) and (3) finished product treatment: and washing the titanium-based implant, drying and storing. The surface treatment method provided by the invention has the advantages that the prepared dental implant has higher biocompatibility, the success rate of oral implantation is improved, the treatment time is shortened, the preparation method is simple, and the dental implant has a good application prospect in the field of oral implantation.

Description

Surface treatment method for dental implant
Technical Field
The invention belongs to the technical field of dental implantation, and particularly relates to a surface treatment method of a dental implant.
Background
Pure titanium has good biocompatibility, and thus is widely used in clinical applications as an oral implant material. However, titanium implants still have many problems such as poor bioactivity, lack of osteoinductive effect, low binding strength with surrounding tissues, release of metal ions, long healing time, and poor corrosion resistance. Since the initial implant surface was a machined surface without any treatment and pure titanium implants were widely used in the oral medical field in the 60's of the 20 th century, researchers attempted various surface modification methods to solve the above problems: if the surface topography is optimized, smooth, groove-shaped and thread-shaped surfaces, namely surfaces with different roughness or multiple holes, are formed; such as changing the surface modulus of elasticity; such as implant surface bioactivity, etc.
A common treatment method for implant surfaces is as follows:
acid etching treatment method: the rough surface of the titanium implant is more favorable for the adhesion and proliferation of osteoblasts than the smooth surface, and can promote the osteoblasts to differentiate towards mature phenotype. Therefore, acid etching is a common method for surface roughness treatment, irregular micron-scale roughness can be formed on the surface of the implant, the surface area of the implant is increased, cell attachment and growth are facilitated, the acid-etched pure titanium implant has higher surface free energy, and compared with a titanium implant which is only subjected to mechanical treatment, the acid-etched pure titanium implant can promote osseointegration, enables cells to be better combined with the implant, and can stimulate the formation and attachment of connective tissues and vascular tissues. The type and sequence of the acid used in the acid etching have important influence on the preparation of the rough titanium surface, and researches find that the rough titanium surface obtained by firstly using sulfuric acid and then using hydrochloric acid is optimal and is similar to the surface characteristics of titanium slurry spraying.
Alkali heat treatment: the simplest alkalizing solution at present is the NaOH solution. Some people treat the titanium implant by using NaOH solution, then carry out heat treatment for 1h at 600 ℃, and then place the titanium implant in bionic body fluid for 28d, so that a layer of bone-like apatite is formed on the surface of the titanium implant. In addition, the hydroxyapatite with compact inner layer and high crystallinity can be prepared by utilizing an electrophoretic deposition-alkali thermal method, the hydroxyapatite composite coating with porous outer layer and needle-shaped microstructure can be prepared, and the coating not only can be tightly combined with the titanium implant, but also has the capability of inducing bone.
An anodic oxidation method: the anodic oxidation method is a traditional metal surface treatment method, belongs to an electrochemical treatment method, and has low cost and definite effect. A layer of compact titanium oxide film can be formed on the surface of the titanium subjected to anodic oxidation treatment, the release of metal ions can be effectively inhibited, the corrosion resistance of the metal can be enhanced, and certain bioactivity can be achieved. Research shows that the titanium implant after anodic oxidation treatment not only has firm combination with the bone, but also has tight attachment of soft tissue.
Micro-arc oxidation method: the micro-arc oxidation is also called micro-plasma oxidation, and is a method for generating an oxide ceramic membrane in situ on the surface of metals such as aluminum, magnesium, titanium and the like by introducing a working area from a Faraday area of a common anodic oxidation method to a high-voltage discharge area by adopting higher working voltage. Research shows that the surface of the titanium implant material subjected to micro-arc oxidation treatment has no toxic effect on growth of osteoblasts, is beneficial to growth and proliferation of osteoblasts on the surface, has cell biocompatibility superior to that of a pure titanium implant material, and shows good bone induction capability, so that growth of new bone tissues around the implant is promoted, and the time for osseointegration is shortened. In the micro-arc oxidation process, dielectric breakdown of the titanium surface oxide film occurs under high voltage, spark discharge occurs, and as the breakdown always occurs at a relatively weak part of the film, a uniform oxide film can be finally obtained, the micro-arc oxidation overcomes the defects that the plasma spraying process cannot spray the surface of a workpiece with a complex shape or the thickness is non-uniform. Due to TiO2The ceramic membrane grows in situ from the substrate, has uniform thickness, is tightly combined with the substrate material and is not easy to fall off, thereby improving the wear resistance and corrosion resistance of the titanium implant and effectively inhibiting the release of metal ions.
Micro-arc oxidation is derived from anodic oxidation, but is different from conventional anodic oxidation technology. The biggest difference is that the instantaneous sintering action of the high-temperature and high-pressure area of the microplasma during the micro-arc oxidation causes the amorphous oxide to become a crystalline phase, namely a ceramic phase. In addition, the time required by adopting the anodic oxidation technology is longer, and the micro-arc oxidation technology only needs 3-5min, thereby saving the time and the cost. More importantly, compared with the anodic oxidation surface modification material, the titanium-based micro-arc oxidation film layer can remarkably promote the adhesion of osteoblasts and has good cell compatibility.
An atmospheric heating method: titanium can react with oxygen under natural conditions to form a stable protective oxide film. The film improves the corrosion resistance of titanium and promotes the deposition of a calcium-phosphorus layer on its surface, but because of its thinness (10-20nm), it is very vulnerable to damage and loss of protection. Under the heating condition, titanium reacts with oxygen in the atmosphere to form a compact oxide film, the oxygen is prevented from further reacting with the interior of the titanium, and with the increase of the oxidation temperature, not only the amount of oxides generated on the surface of the titanium is increased, but also the types and the structure types of the oxides are increased, so that a thicker passive film is generated on the surface of the titanium, and the corrosion resistance of the titanium is enhanced. And after the titanium implant is subjected to thermal oxidation treatment in pure oxygen at 800 ℃, the titanium implant has higher osseointegration rate than the mechanically treated implant.
Disclosure of Invention
1. Problems to be solved
In order to solve the problems in the prior art, the invention provides a surface treatment method of a dental implant, which comprises the steps of preparing a porous coating containing calcium and phosphorus by properly pretreating the surface of the implant and utilizing a composite oxidation technology, and nucleating and growing the calcium and the phosphorus on the surface by means of the porous surface characteristics of materials and the influence of calcium and phosphorus elements in a membrane in a simulated physiological environment to form a nano HA bioactive coating, so that the surface shape of the implant is more suitable for the attachment of bone cells, and the biocompatibility of the implant is improved.
2. Technical scheme
In order to solve the problems, the technical scheme provided by the invention is as follows:
a surface treatment method for a dental implant, comprising the steps of:
(1) pretreatment: polishing the titanium-based implant to be treated until the surface of the titanium-based implant is smooth for later use;
(2) acid pickling treatment: placing the pretreated titanium-based implant in the step (1) in acid liquor for acid washing for later use;
(3) and (3) drying treatment: cleaning the titanium-based implant subjected to acid washing in the step (2), and drying for later use;
(4) surface anodic oxidation pretreatment: placing the titanium-based implant dried in the step (3) in surface anodic oxidation electrolyte for surface anodic oxidation for later use;
(5) surface micro-arc oxidation treatment: placing the titanium-based implant subjected to surface anodic oxidation pretreatment in the step (4) in a surface micro-arc oxidation electrolyte for surface micro-arc oxidation for later use;
(6) and (3) finished product treatment: and (5) washing the titanium-based implant subjected to the micro-arc oxidation treatment on the surface in the step (5), drying and storing.
In the above surface treatment method for the dental implant, the specific method of polishing in step (1) is as follows: the titanium-based implant to be treated is roughly ground by using No. 280 metallographic abrasive paper, and then is sequentially ground by using No. 6004, No. 800 and No. 1000 metallographic abrasive paper under the protection of running water until no obvious scratch is formed on the surface of the titanium-based implant.
In the method for treating the surface of the dental implant, the acid solution in the step (2) is composed of hydrofluoric acid and nitric acid, and the volume ratio of the hydrofluoric acid to the nitric acid is 1: 3.
in the surface treatment method of the dental implant, the cleaning solution adopted in the step (3) is deionized water; the drying method in the step (3) adopts an electric hair drier for drying.
In the above method for treating the surface of the dental implant, the specific method for anodizing the surface in the step (4) is as follows: preparing surface anodic oxidation electrolyte, stirring until the surface anodic oxidation electrolyte is fully dissolved, and carrying out electrolytic oxidation by taking the titanium-based implant dried in the step (3) as an anode; the surface anodic oxidation electrolyte comprises an ammonium fluoride solution with the concentration of 0.16mol/L and an ammonium sulfate solution with the concentration of 0.5mol/L, and the volume ratio of the ammonium fluoride solution to the ammonium sulfate solution is 1: 1.
in the above surface treatment method for a dental implant, the specific method of surface micro-arc oxidation in step (5) is as follows: preparing a surface micro-arc oxidation electrolyte, stirring the electrolyte until the electrolyte is fully dissolved, and carrying out electrolytic oxidation by taking the titanium-based implant subjected to surface anodic oxidation treatment in the step (4) as an anode.
In the method for treating the surface of the dental implant, the electrolyte for micro-arc oxidation of the surface in the step (5) comprises a calcium acetate solution with a concentration of 10g/L and a sodium dihydrogen phosphate solution with a concentration of 5g/L, and the volume ratio of the calcium acetate solution to the sodium dihydrogen phosphate solution is 1: 2.
in the method for treating the surface of the dental implant, the device for micro-arc oxidation of the surface in the step (5) comprises a direct current power supply, a stirrer, a cathode sheet, an anode sheet, an electrolytic tank and a cooling tank, wherein the electrolytic tank is arranged in the cooling tank, the cathode sheet and the anode sheet are positioned in the electrolytic tank, the cathode sheet and the anode sheet are respectively connected with the direct current power supply, and the stirrer is arranged in the electrolytic tank.
In the above surface treatment method for a dental implant, the dc power supply in step (5) is an EDI dc voltage stabilization/current stabilization power supply.
In the surface treatment method of the dental implant, the cathode sheet in the step (5) is a cobalt chromium alloy sheet.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
compared with the prior art, the dental implant surface treatment method disclosed by the invention HAs the advantages that after the implant surface is subjected to proper pretreatment, the composite oxidation technology is utilized to prepare the porous coating containing calcium and phosphorus, and in a simulated physiological environment, the calcium and phosphorus are nucleated and grow on the surface by virtue of the porous surface characteristics of the material and the influence of calcium and phosphorus elements in the membrane to form the nano HA bioactive coating, so that the shape of the implant surface is more suitable for the attachment of bone cells, and the biocompatibility of the implant is improved.
Drawings
FIG. 1 is a view showing an apparatus for surface micro-arc oxidation according to example 1 of the present invention;
fig. 2 is a view illustrating the examination of a dental implant manufactured in example 1 of the present invention.
In the figure: 1. a direct current power supply; 2. a stirrer; 3. a cathode sheet; 4. an anode sheet; 5. an electrolytic cell; 6. and (6) cooling the tank.
Detailed Description
The invention is further described with reference to specific embodiments and the accompanying drawings.
Example 1
The surface treatment method of the dental implant of the embodiment comprises the following steps:
(1) pretreatment: polishing the titanium-based implant to be treated until the surface of the titanium-based implant is smooth for later use;
(2) acid pickling treatment: placing the pretreated titanium-based implant in the step (1) in acid liquor for acid washing for later use;
(3) and (3) drying treatment: cleaning the titanium-based implant subjected to acid washing in the step (2), and drying for later use;
(4) surface anodic oxidation pretreatment: placing the titanium-based implant dried in the step (3) in surface anodic oxidation electrolyte for surface anodic oxidation for later use;
(5) surface micro-arc oxidation treatment: placing the titanium-based implant subjected to surface anodic oxidation pretreatment in the step (4) in a surface micro-arc oxidation electrolyte for surface micro-arc oxidation for later use;
(6) and (3) finished product treatment: and (5) washing the titanium-based implant subjected to the micro-arc oxidation treatment on the surface in the step (5), drying and storing.
In the above surface treatment method for the dental implant, the specific method of polishing in step (1) is as follows: the titanium-based implant to be treated is roughly ground by using No. 280 metallographic abrasive paper, and then is sequentially ground by using No. 6004, No. 800 and No. 1000 metallographic abrasive paper under the protection of running water until no obvious scratch is formed on the surface of the titanium-based implant.
In the method for treating the surface of the dental implant, the acid solution in the step (2) is composed of hydrofluoric acid and nitric acid, and the volume ratio of the hydrofluoric acid to the nitric acid is 1: 3.
in the surface treatment method of the dental implant, the cleaning solution adopted in the step (3) is deionized water; the drying method in the step (3) adopts an electric hair drier for drying.
In the above method for treating the surface of the dental implant, the specific method for anodizing the surface in the step (4) is as follows: preparing surface anodic oxidation electrolyte, stirring until the surface anodic oxidation electrolyte is fully dissolved, and carrying out electrolytic oxidation by taking the titanium-based implant dried in the step (3) as an anode; the surface anodic oxidation electrolyte comprises an ammonium fluoride solution with the concentration of 0.16mol/L and an ammonium sulfate solution with the concentration of 0.5mol/L, and the volume ratio of the ammonium fluoride solution to the ammonium sulfate solution is 1: 1.
in the above surface treatment method for a dental implant, the specific method of surface micro-arc oxidation in step (5) is as follows: preparing a surface micro-arc oxidation electrolyte, stirring the electrolyte until the electrolyte is fully dissolved, and carrying out electrolytic oxidation by taking the titanium-based implant subjected to surface anodic oxidation treatment in the step (4) as an anode.
In the method for treating the surface of the dental implant, the electrolyte for micro-arc oxidation of the surface in the step (5) comprises a calcium acetate solution with a concentration of 10g/L and a sodium dihydrogen phosphate solution with a concentration of 5g/L, and the volume ratio of the calcium acetate solution to the sodium dihydrogen phosphate solution is 1: 2.
in the method for treating the surface of the dental implant, as shown in fig. 1, the device for micro-arc oxidation of the surface in the step (5) comprises a dc power supply 1, a stirrer 2, a cathode strip 3, an anode strip 4, an electrolytic bath 5 and a cooling bath 6, wherein the electrolytic bath 5 is arranged inside the cooling bath 6, the cathode strip 3 and the anode strip 4 are positioned inside the electrolytic bath 5, the cathode strip 3 and the anode strip 4 are respectively connected to the dc power supply 1, and the stirrer 2 is arranged inside the electrolytic bath 5.
In the above surface treatment method for a dental implant, the dc power supply 1 in the step (5) is an EDI dc voltage stabilization/current stabilization power supply.
In the surface treatment method of the dental implant, the cathode sheet 4 in the step (5) is a cobalt chromium alloy sheet.
The device information of the present embodiment is shown in table 1:
TABLE 1 device information
Figure BDA0002592493360000051
The raw material and sample information for this example is shown in table 2:
table 2 raw material and sample information
Name of medicine Specification of Manufacturer of the product
Acetic acid calcium salt Analytical purity Beijing reagent Co Ltd
Sodium dihydrogen phosphate Analytical purity Beijing reagent Co Ltd
Phosphoric acid Analytical purity BEIJING CHEMICAL PLANT
Distilled water Self-made
Implant body Iron and Steel Research Institute
Hydrofluoric acid Analytical purity Beijing reagent Co Ltd
Nitric acid Beijing reagent Co Ltd
The aperture adjustment and control of this embodiment is shown in table 3:
TABLE 3 Aperture adjustment and control
Pore diameter Time of day Voltage of Formulation of
1um 5 300v 70g calcium acetate +14g sodium dihydrogen phosphate
3um
10 110v 35g calcium acetate +7g sodium dihydrogen phosphate
5um
20 300v 70g calcium acetate +14g sodium dihydrogen phosphate
15um 25 110v 35g calcium acetate +7g sodium dihydrogen phosphate
20um
10 110v 35g calcium acetate +7g sodium dihydrogen phosphate
The results of the calcium and phosphorus content measurement in this example are shown in FIG. 2.
Comparative example 1
Chinese invention patent, application number: 201811633378.X, published bulletin number: CN109549723A, discloses a surface treatment process and application of dental implant, referring to the specific embodiments of the description thereof;
"the present embodiment provides a surface treatment process of a dental implant, comprising:
and adopting rutile sand with 35 meshes to perform sand blasting treatment on the surface of the implant. The sand blasting process comprises the following steps: the spray gun and the implant form an included angle of 45 degrees, the gun mouth is 8mm away from the implant, and the sand blasting time of each implant is 15 s.
And cleaning the implant subjected to sand blasting, and then putting the implant into acid liquor for acid etching. The acid solution comprises sulfuric acid, hydrochloric acid and water in a volume ratio of 1:1: 2. The acid etching time is 50min, and the acid etching temperature is 65 ℃. After the acid etching is finished, the implant is ultrasonically cleaned twice in absolute ethyl alcohol and deionized water respectively, and each time lasts for 10 min.
And heating and soaking the cleaned implant in a NaOH solution with the concentration of 5mol/L for 24 hours, wherein the soaking temperature is 60 ℃. And cleaning after soaking to obtain the treated implant ".
Comparative example 2
Chinese invention patent, application number: 201710131716.9, publication number: CN106880870A, discloses a treatment method for activating the surface of a titanium-based implant, and refers to the specific embodiment of the specification;
"a titanium base implant surface activation processing method, which comprises the following steps:
the method comprises the following steps: low temperature chemical oxidation
Sequentially polishing the titanium-based implant with 180#, 280#, 360#, 600#, 800# and 1000# sandpaper until the titanium-based implant is smooth, then sequentially and respectively ultrasonically cleaning the titanium-based implant for 20min with 99.5% acetone, 99.7% absolute ethyl alcohol and deionized water, and after the titanium-based implant is cleaned, placing the titanium-based implant in 40ml of mixed solution of hydrogen peroxide and hydrochloric acid for oxidation at the oxidation temperature of 0 ℃ for 24 h; wherein, the mixed solution of hydrogen peroxide and hydrochloric acid is prepared by mixing 20 percent of hydrogen peroxide and 30 percent of hydrochloric acid according to the volume ratio of 0.5: 1, is prepared according to the proportion of 1.
Step two: surface activation
Putting the titanium-based implant subjected to low-temperature oxidation into 50ml of simulated body fluid, adding saturated solution containing calcium and phosphorus into the simulated body fluid, adjusting the pH value to 7.40 by using alkaline solution, and activating the surface of the titanium-based implant for 8 days at the constant temperature of 20 ℃; and taking out the titanium-based implant, cleaning the titanium-based implant by using deionized water, and drying the titanium-based implant for later use.
As can be seen from fig. 1, the titanium-based implant prepared in this example has no cracks, high bonding strength, and uniform morphology, and the titanium-based implant treated in example 1 is subjected to electron microscope scanning.
In order to further verify the beneficial effects of the invention, the titanium-based implant sample prepared in this example was used to perform a bone marrow stromal stem cell complex culture experiment, the specific experimental process is as follows: before planting cells, placing a titanium-based implant sample in an L-DMEM complete culture solution for soaking overnight, then taking out the sample from the culture solution, blowing the sample in a sterile super clean bench for 30min, and moving the sample to a 12-hole culture plate in a sterile environment, wherein one sample is in each hole. Cell suspensions with a cell concentration of 3X 106 cells/ml after digestion were seeded onto the surface of each sample, 20ul per sample. Then, the mixture was subjected to static culture at 37 ℃ in a constant temperature incubator containing 5% CO 2. After composite culture for 1d, taking out a sample, removing culture solution, cleaning the surface of the sample for 3 times by using PBS buffer solution, adding 2.5% glutaraldehyde for fixation for 4 hours at 4 ℃, dehydrating by using gradient alcohol for 10-30 min, naturally drying by using a fume hood, and observing the cell adhesion form under a scanning electron microscope after gold spraying.
The observation of fig. 2 shows that the titanium-based implant of the present embodiment has no cracks, high bonding strength, and uniform morphology, so the titanium-based implant has a large cell adhesion amount, good spreading, compactness, uniformity, growth in the pores, and good bioactivity.
The surface micro-morphology and the cell adhesion morphology of the titanium-based implant processed by other embodiments of the invention are basically the same as those of the embodiment, and are not described in detail.
Comparative example 3
Chinese invention patent, application number: 202010078010.2, publication number: CN111269882A, discloses a surface treatment method of an implant and a bionic implant, and refers to the specific implementation scheme of the specification;
the titanium implant to be treated in this embodiment is a pure titanium implant, and the surface treatment method of the titanium implant includes the following steps:
s100: providing a titanium implant, carrying out anodic oxidation by taking the titanium implant as an anode and pure copper as a cathode, wherein the electrolyte is a mixed solution of 0.15mol/L ammonium fluoride and 0.5mol/L ammonium sulfate, the voltage of anodic oxidation is 22V, and the time is 30 min; forming a titanium dioxide nanotube on the surface of the titanium implant.
S200: ultrasonically cleaning the titanium implant subjected to anodic oxidation by using double distilled water, drying, sterilizing at high temperature and high pressure, and then irradiating under an ultraviolet lamp for 30min to obtain the activated titanium implant.
S210: the abandoned jaw bone cancellous bone is aseptically obtained in orthognathic surgery, and is immediately washed repeatedly for 4 times by using sterile phosphate buffer solution on an ultraclean workbench, centrifuged for 5min at 800r/min, the supernatant is discarded, alpha-MEM culture solution of 10% mass fraction fetal calf serum is adopted to resuspend cells, and the cells and the sheared jaw bone fragment are inoculated in a 25cm2 culture bottle and are placed in an incubator at 37 ℃ and 5% volume fraction CO2 saturation humidity for culture. When the cells grow and converge to 80% of the bottom of the bottle, the cells are digested by 2.5g/L pancreatin and are passaged according to the proportion of 1: 3, which is marked as P1 (the first generation), and the like, and the mesenchymal stem cells of the third generation are taken.
S300: respectively inoculating the third generation of bone marrow mesenchymal stem cells on the surface of the activated titanium implant at an inoculation density of 3 × 105/cm2And obtaining the titanium implant inoculated with the bone marrow mesenchymal stem cells.
S400: and adding an alpha-MEM culture medium containing 10% FBS into the titanium implant inoculated with the bone marrow mesenchymal stem cells, placing the titanium implant in an incubator for 2 days, adding an osteogenic induction liquid for culture, and constructing an extracellular matrix on the surface of the titanium implant after induction for 14 days to obtain an initial product.
S500: carrying out cell removal treatment on the primary product: removing the alpha-MEM culture medium containing 10% FBS on the surface of the primary product, washing with PBS, and adding a cell removal solution for cell removal; sucking off the cell-free solution of the primary product, washing with PBS and deionized water, drying at normal temperature, digesting in digestive enzyme solution, repeatedly washing with PBS to obtain bionic implant, and storing at-20 deg.C.
The cell removal liquid is TritonX-100 solution with the volume fraction of 0.5 percent, and the preparation method comprises the following steps: the concentration of 25 wt% NH3 solution was adjusted to 20mmol/L with PBS solution, and TritonX-100 was added to prepare 0.5% volume fraction TritonX-100 solution ".
Comparative example 4
Chinese invention patent, application number: 201910199562.6, publication number: CN109957803A, disclosing a modified titanium anodic oxide surface treatment method for implant, referring to the specific embodiments of the description thereof;
"As shown in figure 1, a modified anode titanium oxide surface treatment method for an implant comprises the following steps:
1) sand blasting: carrying out sand blasting treatment on the surface of the titanium implant by using hydroxyapatite powder;
2) acid etching: placing the implant subjected to sand blasting treatment into a container containing hydrofluoric acid (HF) for acid etching for 0.5 h;
3) anodic oxidation: connecting the acid-etched implant with the anode of a direct-current power supply, connecting a platinum rod with the cathode of the power supply, putting the implant and the platinum rod into an electrolyte containing hydrofluoric acid (HF), controlling the power supply voltage to be 100V, starting the power supply to oxidize the implant for 1 min;
4) vacuum ultrasonic cleaning: firstly, putting the implant processed in the step 3) into a first cleaning tank of an ultrasonic machine containing an alkaline detergent for first vacuum cleaning, then moving the implant into a second cleaning tank containing the alkaline detergent, carrying out second vacuum cleaning by adopting ultrasonic waves, then moving the implant into a third cleaning tank containing pure water, carrying out third vacuum fine cleaning by adopting the ultrasonic waves, then moving the implant into a fourth cleaning tank containing the pure water, carrying out fourth vacuum cleaning by adopting the ultrasonic waves, then moving the implant into a fifth cleaning tank containing the pure water, carrying out fifth vacuum cleaning by adopting the ultrasonic waves, and finally drying by adopting a vacuum dryer to obtain a finished implant; the ultrasonic vacuum cleaning temperature is 30 ℃, the ultrasonic power is 0.6KW, the ultrasonic frequency is 28KHz, and the cleaning time of the implant in the ultrasonic cleaning tank is 10 min;
the alkaline detergent is calcium hydroxide solution ".
Example 2
The implant prepared by the surface treatment method of the dental implant of example 1 and the implants prepared in comparative examples 1 to 4 were selected and tested (BIC and ITBC values), respectively, and the results are shown in table 4.
TABLE 4 comparison of the test parameters
Figure BDA0002592493360000091
As can be seen from fig. 1, 2 and 4, the surface shape of the implant prepared according to the present invention is more suitable for the adhesion of bone cells than that of comparative examples 1 to 4, and the implant prepared according to the present invention shows the highest cell adhesion as can be seen from the results of the cell adhesion experiment. In addition, histological examination analysis results observed that the implant prepared according to the present invention exhibited more mature bone formation. Therefore, the implant prepared by the invention is an excellent titanium-based implant with biocompatibility.
In conclusion, the dental implant surface treatment method disclosed by the invention HAs the advantages that after the implant surface is subjected to proper pretreatment, the composite oxidation technology is utilized to prepare the porous coating containing calcium and phosphorus, and in a simulated physiological environment, the calcium and phosphorus nucleate and grow on the surface by virtue of the porous surface characteristics of the material and the influence of calcium and phosphorus elements in the film to form the nano HA bioactive coating, so that the shape of the implant surface is more suitable for the attachment of bone cells, and the biocompatibility of the implant is improved.
The present invention and its embodiments have been described above schematically, without limitation, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.

Claims (10)

1. A method for surface treatment of a dental implant, comprising the steps of:
(1) pretreatment: polishing the titanium-based implant to be treated until the surface of the titanium-based implant is smooth for later use;
(2) acid pickling treatment: placing the pretreated titanium-based implant in the step (1) in acid liquor for acid washing for later use;
(3) and (3) drying treatment: cleaning the titanium-based implant subjected to acid washing in the step (2), and drying for later use;
(4) surface anodic oxidation pretreatment: placing the titanium-based implant dried in the step (3) in surface anodic oxidation electrolyte for surface anodic oxidation for later use;
(5) surface micro-arc oxidation treatment: placing the titanium-based implant subjected to surface anodic oxidation pretreatment in the step (4) in a surface micro-arc oxidation electrolyte for surface micro-arc oxidation for later use;
(6) and (3) finished product treatment: and (5) washing the titanium-based implant subjected to the micro-arc oxidation treatment on the surface in the step (5), drying and storing.
2. The surface treatment method for a dental implant according to claim 1, wherein the specific method of grinding in step (1) is as follows: the titanium-based implant to be treated is roughly ground by using No. 280 metallographic abrasive paper, and then is sequentially ground by using No. 6004, No. 800 and No. 1000 metallographic abrasive paper under the protection of running water until no obvious scratch is formed on the surface of the titanium-based implant.
3. A surface treatment method for a dental implant as recited in claim 1, wherein said acid solution in step (2) is composed of hydrofluoric acid and nitric acid, and a volume ratio of said hydrofluoric acid to said nitric acid is 1: 3.
4. a surface treatment method for a dental implant according to claim 1, wherein the cleaning in step (3) is performed using deionized water as a cleaning solution; the drying method in the step (3) adopts an electric hair drier for drying.
5. The surface treatment method for a dental implant according to claim 1, wherein the specific method of surface anodization in step (4) is as follows: preparing surface anodic oxidation electrolyte, stirring until the surface anodic oxidation electrolyte is fully dissolved, and carrying out electrolytic oxidation by taking the titanium-based implant dried in the step (3) as an anode; the surface anodic oxidation electrolyte comprises an ammonium fluoride solution with the concentration of 0.16mol/L and an ammonium sulfate solution with the concentration of 0.5mol/L, and the volume ratio of the ammonium fluoride solution to the ammonium sulfate solution is 1: 1.
6. the surface treatment method for dental implant according to claim 1, wherein the specific method of surface micro-arc oxidation in step (5) is as follows: preparing a surface micro-arc oxidation electrolyte, stirring the electrolyte until the electrolyte is fully dissolved, and carrying out electrolytic oxidation by taking the titanium-based implant subjected to surface anodic oxidation treatment in the step (4) as an anode.
7. The surface treatment method for a dental implant according to claim 6, wherein the surface micro-arc oxidation electrolyte in step (5) comprises a calcium acetate solution with a concentration of 10g/L and a sodium dihydrogen phosphate solution with a concentration of 5g/L, and the volume ratio of the calcium acetate solution to the sodium dihydrogen phosphate solution is 1: 2.
8. the surface treatment method for dental implants according to claim 1, characterized in that said device for surface micro-arc oxidation in step (5) comprises a DC power supply (1), a stirrer (2), a cathode plate (3), an anode plate (4), an electrolytic bath (5) and a cooling bath (6), said electrolytic bath (5) is disposed inside said cooling bath (6), said cathode plate (3) and said anode plate (4) are disposed inside said electrolytic bath (5), said cathode plate (3) and said anode plate (4) are respectively connected to said DC power supply (1), and said stirrer (2) is disposed inside said electrolytic bath (5).
9. A surface treatment method for a dental implant according to claim 8, wherein said dc power supply (1) in step (5) is an EDI dc regulated/stabilized power supply.
10. The surface treatment method for a dental implant according to claim 1, wherein said cathode sheet (4) in step (5) is a cobalt chromium alloy sheet.
CN202010699474.5A 2020-07-20 2020-07-20 Surface treatment method for dental implant Pending CN112301399A (en)

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