CN113186579A - Titanium alloy oral cavity restoration body surface whitening self-cleaning coating and preparation method thereof - Google Patents
Titanium alloy oral cavity restoration body surface whitening self-cleaning coating and preparation method thereof Download PDFInfo
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- 230000002087 whitening effect Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
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- VBGGLSWSRVDWHB-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F VBGGLSWSRVDWHB-UHFFFAOYSA-N 0.000 claims description 4
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- 238000003618 dip coating Methods 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- QTRSWYWKHYAKEO-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(1,1,2,2,2-pentafluoroethoxy)silane Chemical compound FC(F)(F)C(F)(F)O[Si](OC(F)(F)C(F)(F)F)(OC(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F QTRSWYWKHYAKEO-UHFFFAOYSA-N 0.000 claims description 2
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- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 2
- DXODQEHVNYHGGW-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl-tris(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F DXODQEHVNYHGGW-UHFFFAOYSA-N 0.000 claims 1
- QRPMCZNLJXJVSG-UHFFFAOYSA-N trichloro(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)[Si](Cl)(Cl)Cl QRPMCZNLJXJVSG-UHFFFAOYSA-N 0.000 claims 1
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- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/30—Metallic substrate based on refractory metals (Ti, V, Cr, Zr, Nb, Mo, Hf, Ta, W)
- B05D2202/35—Metallic substrate based on refractory metals (Ti, V, Cr, Zr, Nb, Mo, Hf, Ta, W) based on Ti
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Dental Preparations (AREA)
Abstract
The invention provides a titanium alloy oral cavity restoration body surface whitening self-cleaning coating and a preparation method thereof. The titanium alloy dental prosthesis surface coating comprises a white micro-arc oxidation inner layer and a self-cleaning outer layer which are arranged in sequence from inside to outside. In addition, the preparation method of the titanium alloy dental prosthesis surface coating mainly comprises the following steps: firstly, a white micro-arc oxidation inner layer is formed on the surface of a titanium alloy substrate by using a low-energy-consumption micro-arc oxidation technology, and then a self-cleaning outer layer is prepared on the surface of the micro-arc oxidation inner layer. The coating has the advantages of simple preparation method, low cost, strong binding force with a metal matrix, good wear resistance, and the color of the coating is close to the color of teeth, so that the self metal color of the titanium alloy matrix can be effectively shielded, and meanwhile, the surface of the coating is in a hydrophobic state, so that the adhesion of substances such as bacteria, microorganisms and the like can be effectively inhibited, and the surface of the restoration body is endowed with the self-cleaning characteristic.
Description
Technical Field
The invention belongs to the technical field of oral restoration, and relates to a titanium alloy oral restoration body surface whitening self-cleaning coating and a preparation method thereof.
Background
Pure titanium and titanium alloy have the characteristics of good biocompatibility, lower density, excellent corrosion resistance and the like, are suitable for manufacturing dental prostheses such as false teeth, full crowns, supports and the like, are safer and more comfortable compared with the traditional dental materials, but greatly influence the attractiveness due to large color contrast between the titanium alloy and the surface of teeth. At present, methods such as brush coating or dip coating and the like are mainly adopted to prepare polymer whitening coatings such as epoxy resin and the like on the surfaces of dental materials, and although the coatings have certain whitening effect, the coatings have the problems of low hardness, insufficient binding force between the coatings and a substrate, poor biocompatibility, poor wear resistance and the like. Meanwhile, microorganisms such as bacteria in the oral cavity are often attached to the surface of teeth, which is a main factor of common oral diseases such as caries and periodontal tissue inflammation, and the conventional methods prevent the dental caries, dental floss, professional tooth cleaning and the like, but cannot provide a growth environment capable of inhibiting the microorganisms such as bacteria in the oral cavity for a long time. Therefore, it is very necessary to invent a coating which has whitening and self-cleaning functions on the surface of the titanium alloy dental prosthesis.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a simple and low-cost titanium alloy dental prosthesis surface whitening self-cleaning coating and a preparation method thereof.
A titanium alloy dental prosthesis surface whitening self-cleaning coating is characterized by comprising a white micro-arc oxidation inner layer and a self-cleaning outer layer which are arranged from inside to outside in sequence; the micro-arc oxidation inner layer in the coating structure is metallurgically bonded with the titanium alloy substrate, and the multi-scale pore surface of the micro-arc oxidation layer can be used as a riveting and embedding substrate of the self-cleaning coating, so that the bonding force between the self-cleaning coating and the micro-arc oxidation transition layer is improved.
Further, the self-cleaning coating is prepared by adopting perfluorosilane or polytetrafluoroethylene emulsion, wherein the perfluorosilane is at least one of perfluorooctyl trichlorosilane, perfluorodecyl trimethoxy silane, perfluorooctyl triethoxy silane, perfluorodecyl trimethoxy silane and perfluorodecyl triethoxy silane.
A preparation method of a titanium alloy dental prosthesis surface whitening self-cleaning coating is used for preparing the whitening self-cleaning coating, and is characterized by comprising the following steps:
step 1: sequentially polishing and cleaning the surface of the titanium alloy oral cavity restoration body;
step 2: preparing a white micro-arc oxidation inner layer by using a low-energy-consumption micro-arc oxidation technology, soaking a treated sample into an electrolyte, connecting a titanium alloy sample with a power supply anode, connecting a stainless steel electrolytic cell with a power supply cathode, and turning on a power supply to perform micro-arc oxidation treatment to obtain a micro-arc oxidation layer with a white surface;
and step 3: preparing a self-cleaning outer layer, cleaning and drying a sample subjected to micro-arc oxidation, preparing a solution for preparing a self-cleaning coating, coating the solution on the white micro-arc oxidation surface, and drying to obtain the titanium alloy oral restoration whitening self-cleaning coating.
The low-energy-consumption electrolyte comprises 40-60 g/L of hydroxide and 5-20 g/L of phosphate, wherein the hydroxide is at least one of sodium hydroxide or potassium hydroxide, and the phosphate is at least one of sodium tripolyphosphate, sodium hexametaphosphate, trisodium phosphate, sodium pyrophosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate.
Further, the process parameters of the low-energy-consumption micro-arc oxidation treatment comprise: the method is characterized in that pulse voltage is selected in a constant voltage mode, the voltage is 60-90V, the frequency is 50-2000 Hz, the duty ratio is 5-30%, and the processing time is 1-5 min.
The preparation method of the titanium alloy dental restoration surface whitening self-cleaning coating comprises the following steps:
step 1: preparing 10-60% of polytetrafluoroethylene emulsion by mass fraction, or mixing one or more mixed silanes and ethanol in a volume ratio of 1: 10-1: 100;
step 2: coating the mixed solution on the surface of the white micro-arc oxidation layer in a brushing, dip-coating or spraying manner;
and step 3: drying at room temperature, curing at 20-200 ℃ for 1-5 h, and cooling to room temperature along with a furnace, wherein the thickness of the coating is 1-5 mu m.
The invention has the following advantages and beneficial effects:
the invention provides a whitening self-cleaning coating formed on the surface of a titanium alloy dental prosthesis and a preparation method thereof, the coating has strong binding force with a metal matrix and good wear resistance, the color of the coating is close to that of teeth, the self metal color of the titanium alloy matrix can be effectively shielded, and meanwhile, the surface of the coating can effectively inhibit the adhesion of substances such as bacteria, microorganisms and the like, and the self-cleaning effect on the surface of the prosthesis is achieved. In addition, the whitening self-cleaning coating is simple and feasible in preparation process, low in cost and has potential application value.
Drawings
FIG. 1 is a schematic structural view of a whitening self-cleaning coating in an embodiment of the invention;
FIG. 2 is a diagram of a titanium alloy dental prosthesis in an embodiment of the present invention;
FIG. 3 is a diagram of a whitening self-cleaning coating prepared on the surface of a titanium alloy dental restoration in an embodiment of the invention;
fig. 4 is a contact angle of the whitening self-cleaning coating with water in the embodiment of the invention.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Example one
The embodiment provides a surface whitening self-cleaning coating for a titanium alloy oral cavity restoration body and a preparation method thereof, and the method comprises the following steps:
1. preparation of white micro-arc oxidation layer on surface of titanium alloy dental prosthesis
(1) The prepared micro-arc oxidation electrolyte comprises the following components: 50g/L of sodium hydroxide and 15g/L of sodium tripolyphosphate are dissolved by deionized water and are uniformly stirred to prepare the required micro-arc oxidation electrolyte;
(2) and (3) carrying out a micro-arc oxidation process by taking pure titanium as an anode, a stainless steel container as a cathode, and a micro-arc oxidation voltage of 75V, a frequency of 500Hz and a duty ratio of 30% for 2min to obtain a white micro-arc oxidation layer.
2. Preparation of self-cleaning coating on surface of micro-arc oxidation layer
(1) Mixing perfluorooctyl trichlorosilane and ethanol in a volume ratio of 1: 50;
(2) coating the mixed solution on the surface of the micro-arc oxidation layer in a brush coating mode;
(3) air-dried at room temperature and cured at 120 ℃ for 1h, cooled to room temperature and the coating thickness was 3 μm.
Example two
The embodiment provides a surface whitening self-cleaning coating for a titanium alloy oral cavity restoration body and a preparation method thereof, and the method comprises the following steps:
1. preparation of white micro-arc oxidation layer on surface of titanium alloy dental prosthesis
(1) The prepared micro-arc oxidation electrolyte comprises the following components: dissolving 60g/L sodium hydroxide and 10g/L sodium tripolyphosphate by using deionized water, and uniformly stirring to prepare the required micro-arc oxidation electrolyte;
(2) and (3) carrying out a micro-arc oxidation process by taking pure titanium as an anode, a stainless steel container as a cathode, and a micro-arc oxidation voltage of 70V, a frequency of 700Hz and a duty ratio of 30% for 5min to obtain a white micro-arc oxidation layer.
2. Preparation of self-cleaning coating on surface of micro-arc oxidation layer
(1) Preparing polytetrafluoroethylene emulsion with the mass fraction of 10%
(2) The sample was immersed in 10% polytetrafluoroethylene emulsion for 30min
(3) The sample was removed and cured at 100 ℃ for 1h, cooled to room temperature and had a coating thickness of 5 μm.
EXAMPLE III
The embodiment provides a surface whitening self-cleaning coating for a titanium alloy oral cavity restoration body and a preparation method thereof, and the method comprises the following steps:
1. preparation of white micro-arc oxidation layer on surface of titanium alloy dental prosthesis
(1) The prepared micro-arc oxidation electrolyte comprises the following components: 40g/L of sodium hydroxide and 15g/L of sodium hexametaphosphate are dissolved by deionized water and are uniformly stirred to prepare the required micro-arc oxidation electrolyte;
(2) pure titanium is used as an anode, a stainless steel container is used as a cathode, the micro-arc oxidation voltage is 80V, the frequency is 500Hz, the duty ratio is 50%, the micro-arc oxidation process is carried out, the reaction time is 2min, and the white micro-arc oxidation layer is obtained.
2. Preparation of self-cleaning coating on surface of micro-arc oxidation layer
(1) Mixing perfluorooctyl trichlorosilane and ethanol in a volume ratio of 1: 100;
(2) coating the mixed solution on the surface of the micro-arc oxidation layer in a brush coating mode;
(3) air-dried at room temperature and cured at 100 ℃ for 2h, cooled to room temperature and the coating thickness was 2 μm.
As shown in fig. 3, the surface of the sample is white close to the teeth, and has whitening and modifying effects; as shown in FIG. 4, the whitening self-cleaning coating has a hydrophobic effect (the hydrophobic angle is 99.5 degrees and is more than 90 degrees), so that pollutants are difficult to attach to the surface, and the whitening self-cleaning coating has a good self-cleaning effect.
In conclusion, the coating prepared by the method has the color close to that of teeth, can effectively shield the metal color of the titanium alloy matrix, has good whitening effect, can effectively avoid the adhesion of dirt on the surface, has a self-cleaning effect on the surface of the restoration, and has a relatively simple preparation method
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the principles of the invention as set forth herein, and such changes and modifications are to be considered as within the scope of the invention.
Claims (6)
1. A titanium alloy dental prosthesis surface whitening self-cleaning coating is characterized by comprising a white micro-arc oxidation inner layer and a self-cleaning outer layer which are arranged from inside to outside in sequence; the micro-arc oxidation inner layer in the coating structure is metallurgically bonded with the titanium alloy substrate, and the multi-scale pore surface of the micro-arc oxidation layer can be used as a riveting and embedding substrate of the self-cleaning coating, so that the bonding force between the self-cleaning coating and the micro-arc oxidation transition layer is improved.
2. The titanium alloy dental restoration surface self-cleaning coating according to claim 1, wherein said self-cleaning coating is prepared using perfluorosilane or polytetrafluoroethylene emulsion, wherein perfluorosilane is at least one of perfluorooctyltrichlorosilane, perfluorodecyltrichlorosilane, perfluorodecyltrimethoxysilane, perfluorooctyltrimethoxysilane, perfluorooctyltriethoxysilane, perfluorodecyltrimethoxysilane, perfluorodecyltriethoxysilane.
3. A method for preparing a titanium alloy dental prosthesis surface whitening self-cleaning coating, which is used for preparing the whitening self-cleaning coating as described in any one of claims 1-2, and is characterized by comprising the following steps:
step 1: sequentially polishing and cleaning the surface of the titanium alloy oral cavity restoration body;
step 2: preparing a white micro-arc oxidation inner layer by using a low-energy-consumption micro-arc oxidation technology, soaking a treated sample into an electrolyte, connecting a titanium alloy sample with a power supply anode, connecting a stainless steel electrolytic cell with a power supply cathode, and turning on a power supply to perform micro-arc oxidation treatment to obtain a micro-arc oxidation layer with a white surface;
and step 3: preparing a self-cleaning outer layer, cleaning and drying a sample subjected to micro-arc oxidation, preparing a solution for preparing a self-cleaning coating, coating the solution on the white micro-arc oxidation surface, and drying to obtain the titanium alloy oral restoration whitening self-cleaning coating.
4. The method for preparing the titanium alloy oral prosthesis surface whitening self-cleaning coating according to claim 3, wherein the low-energy-consumption electrolyte consists of 40-60 g/L of hydroxide and 5-20 g/L of phosphate, the hydroxide is at least one of sodium hydroxide or potassium hydroxide, and the phosphate is at least one of sodium tripolyphosphate, sodium hexametaphosphate, trisodium phosphate, sodium pyrophosphate, sodium dihydrogen phosphate and disodium hydrogen phosphate.
5. The method for preparing the titanium alloy oral prosthesis surface whitening self-cleaning coating according to claim 3, wherein the process parameters of the low-energy micro-arc oxidation treatment comprise: the method is characterized in that pulse voltage is selected in a constant voltage mode, the voltage is 60-90V, the frequency is 50-2000 Hz, the duty ratio is 5-30%, and the processing time is 1-5 min.
6. The method for preparing the titanium alloy oral prosthesis surface whitening self-cleaning coating according to claim 3, wherein the self-cleaning solution preparation step comprises:
step 1: preparing 10-60% of polytetrafluoroethylene emulsion by mass fraction, or mixing one or more mixed silanes and ethanol in a volume ratio of 1: 10-1: 100;
step 2: coating the mixed solution on the surface of the white micro-arc oxidation layer in a brushing, dip-coating or spraying manner;
and step 3: drying at room temperature, curing at 20-200 ℃ for 1-5 h, and cooling to room temperature along with a furnace, wherein the thickness of the coating is 1-5 mu m.
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Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4050156A (en) * | 1976-06-28 | 1977-09-27 | Daniel Chasanoff | Dental appliance |
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