CN113046812A - Anodic oxidation liquid for titanium alloy dental abutment system and preparation method and application thereof - Google Patents
Anodic oxidation liquid for titanium alloy dental abutment system and preparation method and application thereof Download PDFInfo
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
The invention belongs to the field of metal surface treatment, and discloses an anodic oxidation liquid for a titanium alloy dental abutment system, a preparation method and application thereof, wherein the anodic oxidation liquid comprises hydrofluoric acid, a dispersing agent, inorganic acid, a complexing agent, zinc salt and water, by adjusting the proportion of the anodic oxidation liquid and the anodic oxidation process, controlling parameters and the like in the anodic oxidation process, so that the surface of the titanium alloy dental implant can present various oxidation colors, the color of the obtained dental implant is controllable and adjustable, the color of the anodic oxidation film layer is uniform and consistent, the bonding force with the base material is strong, meanwhile, the anodic oxide film layer can passivate the surface of the base material, enhance the corrosion resistance and the salt spray resistance, form nanotubes with consistent rules on the surface, absorb and inlay a certain amount of zinc ions, and the initial stability and the local antibacterial effect of the abutment system after planting are improved, inflammation is reduced, and the planting success rate is further improved. The preparation method provided by the invention is simple in process and strong in controllability, and is beneficial to large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to an anodic oxidation liquid for a titanium alloy dental abutment system, and a preparation method and application thereof.
Background
At present dental implant base station system owner uses pure titanium and titanium alloy to form through precision finishing, to the base station system, structure and size because of its difference lead to its model numerous, be difficult to distinguish, in order to distinguish easily at the planting process, avoid makeing mistakes, current scheme is that the coating of using laser marking or using different colours at the secret position of base station system carries out the sign, use laser marking inefficiency, and is with high costs, however, use coating to carry out the composition of sign in can leading to the coating and ingest, it is influential to implant person's oral health, and the treatment mode that adopts the sign does not have obvious promotion to the antibacterial effect of base station system.
Disclosure of Invention
The invention provides an anodic oxidation solution for a titanium alloy dental abutment system, a preparation method and application thereof, which are used for solving one or more technical problems in the prior art and providing at least one beneficial choice or creation condition.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
an anodizing solution comprising: hydrofluoric acid, a dispersing agent, organic acid, a complexing agent, zinc salt and water.
Specifically, hydrofluoric acid and organic acid (including citric acid and the like) in the formula can provide a weakly acidic environment and acid radical ions for the anodic oxidation liquid, so that the anodic oxidation liquid has certain conductivity, and the conductivity of the anodic oxidation liquid is easy to control; meanwhile, the titanium dioxide nanotube is easier to form on the surface of the titanium material in a weak acid environment, the nanotube has a certain thickness, can block corrosion factors in the environment, and can bear a certain amount of zinc ions, so that the titanium dioxide nanotube has antibacterial performance.
As a further improvement of the above scheme, the anodic oxidation liquid comprises, in weight percent: 0.1-1% of hydrofluoric acid, 2-60% of a dispersing agent, 0.2-2% of an organic acid, 0.1-0.5% of a complexing agent, 0.5-1% of a zinc salt and 35.5-95% of water.
As a further improvement of the above scheme, the dispersant comprises at least one of polyethylene glycol, ethylene-acrylic acid copolymer or polyethylene homopolymer, preferably polyethylene glycol 400. Specifically, the polyethylene glycol 400 can be well dispersed in the aqueous solution, and the conductivity control in the whole electrolyte is better facilitated.
As a further improvement of the above scheme, the complexing agent comprises at least one of EDTA-2Na, EDTA, tartaric acid, sodium tartrate, or potassium tartrate. Specifically, the complexing agents have a good complexing effect, and can effectively avoid the problems of impurity ion separation in the use process of the electrolyte or turbidity caused by temperature rise and the like.
As a further improvement of the above, the zinc salt includes at least one of zinc nitrate, zinc sulfate, zinc gluconate, zinc chloride, zinc phosphate, zinc hydrogen phosphate, or zinc dihydrogen phosphate. Specifically, zinc salt is taken as an ingestion agent of zinc ions, the zinc ions are taken as an oral antibacterial agent, the zinc ions are adsorbed in the nanotubes generated by anodic oxidation, and after the abutment system is implanted, the nanotubes release a part of the zinc ions and have an antibacterial effect locally in the oral cavity.
The preparation method of the anodic oxidation liquid comprises the following steps: weighing raw material components, sequentially adding hydrofluoric acid, a dispersing agent, inorganic acid, a complexing agent and zinc salt into water, adding the former raw material component into the water and uniformly stirring the mixture, adding the next material into the water, and stirring the mixture after all the raw material components are added. Therefore, the occurrence of the caking phenomenon can be effectively avoided, the raw material components are fully dissolved, and the coloring effect of the obtained anodic oxidation liquid is more stable. The stirring time after all the raw material components are completely put is 5-15min, preferably 10 min.
An anodic oxidation process comprises a pretreatment step, an anodic oxidation step and a post-treatment step of a dental implant abutment system, wherein stainless steel is used as a cathode plate, a titanium alloy dental implant abutment system is clamped by a titanium clamp to be used as an anode plate, and the pretreated titanium alloy dental implant abutment system is soaked in any one of the anodic oxidation solutions; the technological parameters of the anodic oxidation step are as follows: anodic oxidation temperatureAt 10-40 deg.C, anode oxidation current density of 1-5A/dm2The anodic oxidation power supply adopts a direct current power supply (the voltage and the current in use are both controllable), the oxidation voltage is more than 0 and less than or equal to 220V (namely the oxidation voltage is continuously adjustable in the interval), and the anodic oxidation time is 20-60 s.
Further, in the anodic oxidation process, the anodic oxidation liquid needs to be continuously stirred in the using process so as to ensure that the concentration of each component in the anodic oxidation liquid is as uniform as possible. Meanwhile, in the anodic oxidation process, if electrolysis is carried out for a long time, the temperature needs to be controlled to be XX-40 ℃, which is mainly because the solubility of ions in the anodic oxidation liquid and the conductivity of the anodic oxidation liquid are affected by the overhigh temperature (more than 40 ℃) of the anodic oxidation liquid, so that the color of the film layer after anodic oxidation is not uniform.
As a further improvement of the above scheme, the pretreatment step includes ultrasonic degreasing cleaning and ultrasonic water cleaning. The main function of the pretreatment step is oil removal.
As a further improvement of the scheme, the impurity removal step comprises water washing and pure water washing processes. Remove surface impurities and avoid impurity residues. Tap water is not treated, a lot of charged ions, solid impurities, colloids and the like are contained in the tap water, and stains are left after the tap water is cleaned, so that the product cannot be cleaned completely.
The application of the anodic oxidation liquid in metal surface treatment, in particular to the application of the anodic oxidation liquid in surface treatment of titanium alloy and the like.
The invention has the beneficial effects that:
the invention provides an anodic oxidation liquid for a titanium alloy dental abutment system, a preparation method and application thereof, the anodic oxidation liquid obtained by the invention can simply and effectively carry out anodic oxidation coloring treatment on the titanium alloy dental implant abutment system, parameters and the like in the anodic oxidation process are controlled by adjusting the proportion of the anodic oxidation liquid and the anodic oxidation process, so that a plurality of oxidation colors can be presented on the surface of the titanium alloy dental implant, the color of the obtained dental implant is controllable and adjustable, the color of an anodic oxidation film layer is uniform and consistent, the bonding force with a base material is strong, meanwhile, the anodic oxidation film layer can passivate the surface of the base material, the corrosion resistance and the salt spray resistance are enhanced, nanotubes with regular consistency are formed on the surface, a certain amount of zinc ions can be adsorbed and embedded, the initial stability and the local antibacterial effect of the abutment system after being planted are improved, and the inflammation is reduced, thereby improving the planting success rate. The preparation method provided by the invention is simple in process and strong in controllability, and is beneficial to large-scale industrial production.
Drawings
FIG. 1 is a photograph showing a dental implant subjected to an anodic oxidation coloring treatment using the anodic oxidation solution obtained in example 1.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercially available products; the process steps or extraction methods not mentioned in detail are all process steps or extraction methods known to the person skilled in the art.
Example 1
An anodic oxidation liquid comprises the following components in percentage by weight: 0.1% of hydrofluoric acid, 4002% of polyethylene glycol, 0.2% of citric acid, 0.1% of potassium tartrate, 0.5% of zinc nitrate and 95% of water.
Wherein, the hydrofluoric acid is industrial hydrofluoric acid with 40 percent of content, the other products are all commercially available analytical purifiers, and the used water is purified water.
A preparation method of anodic oxidation liquid comprises the following steps: weighing raw material components according to a formula, sequentially adding hydrofluoric acid, polyethylene glycol, citric acid, potassium tartrate and zinc nitrate into water, simultaneously adding the former raw material component into the water and uniformly stirring the mixture, adding the next material into the water, and stirring the mixture for 10min after all the raw material components are completely added.
An anodic oxidation process of anodic oxidation liquid comprises a pretreatment step, an anodic oxidation step and a post-treatment step of a dental implant abutment system, wherein the pretreatment step comprises ultrasonic cleaning, ultrasonic wave and spray rinsing for removing oil; in the step of anodic oxidation, stainless steel is used as a cathode plate, titanium is used as an anode, the used hanger is made of titanium, and the process parameters in the step of anodic oxidation are as follows: the anodic oxidation temperature is 20 ℃, and the anodic oxidation current density is 5A/dm2The anodic oxidation power supply adopts a direct current power supply (the voltage and the current in use are controllable), the oxidation voltage is 0-220V, the precision is 0.01V (namely the oxidation voltage is continuously adjustable within 0-220V), and the anodic oxidation time is 40 s; the impurity removing step comprises a water washing and pure water washing process to remove surface impurities and avoid impurity residues. In the whole anodic oxidation process, the anodic oxidation liquid needs to be stirred magnetically. Removing impurities, and drying at 100 deg.C in an electric oven.
In the anodizing process, different oxidation colors of dental implants obtained under different voltage values (10V, 15V, 20V, 25V, 30V, 35V, 40V, 45V, 50V, 55V, 60V, 65V, 70V and 75V) are obtained by adjusting different voltage values, as shown in fig. 1, and it can be seen from fig. 1 that the color of the dental implant is regularly changed. Meanwhile, when the anodic oxidation parameters are the same, the oxidation color is consistent, and the color of the oxidation film layer is uniform.
Example 2
An anodic oxidation liquid comprises the following components in percentage by weight: 1% of hydrofluoric acid, 40060% of polyethylene glycol, 2% of citric acid, 0.5% of EDTA-2 Na0.5%, 1% of zinc gluconate and 35.5% of water.
Wherein, the hydrofluoric acid is industrial hydrofluoric acid with 40 percent of content, the other products are all commercially available analytical purifiers, and the used water is purified water.
A preparation method of anodic oxidation liquid comprises the following steps: weighing raw material components according to a formula, sequentially adding hydrofluoric acid, polyethylene glycol, citric acid, EDTA-2Na and zinc gluconate into water, meanwhile, in the feeding process, feeding the former raw material component, uniformly stirring, then feeding the next material, and stirring for 10min after all the raw material components are completely fed.
An anodic oxidation process of anodic oxidation liquid comprises a pretreatment step, an anodic oxidation step and a post-treatment step of a dental implant abutment system, wherein the pretreatment step comprises ultrasonic cleaning, ultrasonic wave and spray rinsing for removing oil; in the step of anodic oxidation, stainless steel is used as a cathode plate, titanium is used as an anode, the used hanger is made of titanium, and the process parameters in the step of anodic oxidation are as follows: the anodic oxidation temperature is 20 ℃, and the anodic oxidation current density is 5A/dm2The anodic oxidation power supply adopts a direct current power supply (the voltage and the current in use are controllable), the oxidation voltage is 220V, the precision is 0.01V, and the anodic oxidation time is 20 s; the impurity removing step comprises a water washing and pure water washing process to remove surface impurities and avoid impurity residues. In the whole anodic oxidation process, the anodic oxidation liquid needs to be stirred magnetically. Removing impurities, and drying at 100 deg.C in an electric oven.
Example 3
An anodic oxidation liquid comprises the following components in percentage by weight: 0.5% of hydrofluoric acid, 40030% of polyethylene glycol, 1% of citric acid, 0.25% of EDTA-2Na, 0.75% of zinc hydrogen phosphate and 65% of water.
Wherein, the hydrofluoric acid is industrial hydrofluoric acid with 40 percent of content, the other products are all commercially available analytical purifiers, and the used water is purified water.
A preparation method of anodic oxidation liquid comprises the following steps: weighing raw material components according to a formula, sequentially adding hydrofluoric acid, polyethylene glycol, citric acid, EDTA-2Na and zinc hydrogen phosphate into water, adding the former raw material component into the water and stirring uniformly in the feeding process, then adding the next material, and stirring for 10min after all the raw material components are completely added.
An anodic oxidation process of anodic oxidation liquid comprises a pretreatment step, an anodic oxidation step and a post-treatment step of a dental implant abutment system, wherein the pretreatment step comprises ultrasonic cleaning, ultrasonic wave and spray rinsingWashing and removing oil; in the step of anodic oxidation, stainless steel is used as a cathode plate, titanium is used as an anode, the used hanger is made of titanium, and the process parameters in the step of anodic oxidation are as follows: the anodic oxidation temperature is 20 ℃, and the anodic oxidation current density is 5A/dm2The anodic oxidation power supply adopts a direct current power supply (the voltage and the current in use are controllable), the oxidation voltage is 220V, the precision is 0.01V, and the anodic oxidation time is 60 s; the impurity removing step comprises a water washing and pure water washing process to remove surface impurities and avoid impurity residues. In the whole anodic oxidation process, the anodic oxidation liquid needs to be stirred magnetically. Removing impurities, and drying at 100 deg.C in an electric oven.
Example 4
An anodic oxidation liquid comprises the following components in percentage by weight: 0.2% of hydrofluoric acid, 40050% of polyethylene glycol, 0.5% of citric acid, 0.2% of EDTA-2Na, 0.6% of zinc nitrate and 45% of water.
Wherein, the hydrofluoric acid is industrial hydrofluoric acid with 40 percent of content, the other products are all commercially available analytical purifiers, and the used water is purified water.
A preparation method of anodic oxidation liquid comprises the following steps: weighing raw material components according to a formula, sequentially adding hydrofluoric acid, polyethylene glycol, citric acid, EDTA-2Na and zinc nitrate into water, meanwhile, in the feeding process, feeding the former raw material component, uniformly stirring, then feeding the next material, and stirring for 10min after all the raw material components are completely fed.
An anodic oxidation process of anodic oxidation liquid comprises a pretreatment step, an anodic oxidation step and a post-treatment step of a dental implant abutment system, wherein the pretreatment step comprises ultrasonic cleaning, ultrasonic wave and spray rinsing for removing oil; in the step of anodic oxidation, stainless steel is used as a cathode plate, titanium is used as an anode, the used hanger is made of titanium, and the process parameters in the step of anodic oxidation are as follows: the anodic oxidation temperature is 20 ℃, and the anodic oxidation current density is 5A/dm2The anodic oxidation power supply adopts a direct current power supply (the voltage and the current in use are controllable), the oxidation voltage is 220V, the precision is 0.01V, and the anodic oxidation time is 40 s; the impurity removing step comprises water washing and pure water washingThe process is used for removing surface impurities and avoiding impurity residues. In the whole anodic oxidation process, the anodic oxidation liquid needs to be stirred magnetically. Removing impurities, and drying at 100 deg.C in an electric oven.
Example 5
An anodic oxidation liquid comprises the following components in percentage by weight: 0.5% of hydrofluoric acid, 4002% of polyethylene glycol, 0.3% of citric acid, 0.3% of EDTA-2Na, 0.8% of zinc nitrate and 85% of water.
Wherein, the hydrofluoric acid is industrial hydrofluoric acid with 40 percent of content, the other products are all commercially available analytical purifiers, and the used water is purified water.
A preparation method of anodic oxidation liquid comprises the following steps: weighing raw material components according to a formula, sequentially adding hydrofluoric acid, polyethylene glycol, citric acid, EDTA-2Na and zinc nitrate into water, meanwhile, in the feeding process, feeding the former raw material component, uniformly stirring, then feeding the next material, and stirring for 10min after all the raw material components are completely fed.
An anodic oxidation process of anodic oxidation liquid comprises a pretreatment step, an anodic oxidation step and a post-treatment step of a dental implant abutment system, wherein the pretreatment step comprises ultrasonic cleaning, ultrasonic wave and spray rinsing for removing oil; in the step of anodic oxidation, stainless steel is used as a cathode plate, titanium is used as an anode, the used hanger is made of titanium, and the process parameters in the step of anodic oxidation are as follows: the anodic oxidation temperature is 20 ℃, and the anodic oxidation current density is 5A/dm2The anodic oxidation power supply adopts a direct current power supply (the voltage and the current in use are controllable), the oxidation voltage is 220V, the precision is 0.01V, and the anodic oxidation time is 40 s; the impurity removing step comprises a water washing and pure water washing process to remove surface impurities and avoid impurity residues. In the whole anodic oxidation process, the anodic oxidation liquid needs to be stirred magnetically. Removing impurities, and drying at 100 deg.C in an electric oven.
Comparative example 1
The difference between the comparative example 1 and the example 4 is that EDTA-2Na and zinc nitrate are not added in the preparation process of the anodic oxidation solution of the comparative example 1, in the anodic oxidation process, the pretreatment step adopted before anodic oxidation is carried out ultrasonic oil removal cleaning by using a common metal cleaning agent, and other formulas, preparation methods and anodic oxidation process steps are the same as those in the example 4, so that a titanium alloy anodic oxidation sample is obtained.
Comparative example 2
Comparative example 2 is a titanium alloy sample that was treated with the same pretreatment and post-treatment processes and was not anodized.
Product Performance test 1
The titanium alloy dental implant samples respectively obtained in example 1, comparative example 1 and comparative example 2 are respectively tested by oral streptococcus, the three groups of samples are respectively placed on a culture medium, and after 72-hour bacterial culture, the titanium alloy dental implant obtained in example 1 forms an obvious inhibition zone around the titanium alloy dental implant, and no inhibition zone appears around the samples in comparative example 1 and comparative example 2, which shows that the anodic oxidation solution has an obvious antibacterial effect on the surface of a titanium alloy abutment system.
Product Performance test 2
The titanium alloy dental implant samples obtained in examples 1 to 5 and comparative examples 1 to 2 were tested for corrosion resistance, salt spray resistance, and the like, and the results are shown in table 1 below. Wherein, the corrosion resistance is tested by copper sulfate drop, and the salt spray resistance is tested by acetic acid.
TABLE 1
As can be seen from Table 1, the corrosion resistance and the salt spray resistance of the titanium alloy dental implant samples obtained in examples 1-5 are obviously improved and superior to those obtained in examples 1-2, and compared with examples 1-2, the corrosion resistance of the titanium alloy dental implant samples obtained in examples 1-5 is improved by about 180%, and the acetate salt spray test time is improved by about 150%.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (10)
1. An anodizing solution, comprising: hydrofluoric acid, a dispersing agent, organic acid, a complexing agent, zinc salt and water.
2. The anodizing solution of claim 1, comprising, in weight percent: 0.1-1% of hydrofluoric acid, 2-60% of a dispersing agent, 0.2-2% of an organic acid, 0.1-0.5% of a complexing agent, 0.5-1% of a zinc salt and 35.5-95% of water.
3. The anodizing solution of claim 1, wherein the dispersant comprises at least one of polyethylene glycol, an ethylene-acrylic acid copolymer, or a polyethylene homopolymer.
4. The anodizing solution of claim 1, wherein the complexing agent comprises at least one of EDTA-2Na, EDTA, tartaric acid, sodium tartrate, or potassium tartrate.
5. The anodizing solution of claim 1, wherein the zinc salt comprises at least one of zinc nitrate, zinc sulfate, zinc gluconate, zinc chloride, zinc phosphate, zinc hydrogen phosphate, or zinc dihydrogen phosphate.
6. The method for preparing an anodizing solution according to any one of claims 1 to 5, comprising the steps of: weighing raw material components, sequentially adding hydrofluoric acid, a dispersing agent, an organic acid, a complexing agent and a zinc salt into water, adding the former raw material component into the water and uniformly stirring the mixture, adding the next material into the water, and stirring the mixture after all the raw material components are added.
7. An anodic oxidation process, comprising a pretreatment step, an anodic oxidation step and a post-treatment step for a titanium alloy dental implant abutment system, characterized in that stainless steel is used as a cathode plate, a titanium fixture is used to clamp the titanium alloy dental implant abutment system as an anode plate, and the pretreated titanium alloy dental implant abutment system is immersed in the anodic oxidation solution of any one of claims 1 to 5; the technological parameters of the anodic oxidation step are as follows: the anodic oxidation temperature is 10-40 ℃, and the anodic oxidation current density is 1-5A/dm2The anode oxidation power supply adopts a direct current power supply, the oxidation voltage is more than 0 and less than or equal to 220V, and the anode oxidation time is 20-60 s.
8. The anodic oxidation process according to claim 7, wherein the pretreatment step includes ultrasonic degreasing cleaning and ultrasonic water cleaning.
9. The anodic oxidation process according to claim 7, wherein the post-treatment step includes a water washing and a pure water washing process.
10. Use of an anodizing solution according to any one of claims 1 to 5 in the treatment of a metal surface.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114540911A (en) * | 2020-11-25 | 2022-05-27 | 比亚迪股份有限公司 | Metal part and preparation method thereof |
| CN114540911B (en) * | 2020-11-25 | 2023-11-14 | 比亚迪股份有限公司 | Metal part and preparation method thereof |
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