CN113046748A - Acid etching agent for titanium alloy dental implant and preparation method and application thereof - Google Patents
Acid etching agent for titanium alloy dental implant and preparation method and application thereof Download PDFInfo
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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
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- 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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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
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Abstract
The invention belongs to the technical field of dental implant surface treatment, and discloses an acid etching agent for a titanium alloy dental implant and a preparation method and application thereof. The preparation method provided by the invention is simple in process and strong in controllability, is beneficial to large-scale industrial production, and the acid etching agent obtained by the preparation method can be effectively applied to surface treatment of titanium alloy dental implants and the like, has a wide application prospect, and is worthy of great popularization.
Description
Technical Field
The invention belongs to the technical field of dental implant surface treatment, and particularly relates to an acid etching agent for a titanium alloy dental implant, and a preparation method and application thereof.
Background
Titanium metal is the most commonly used dental implant material at present, has good biocompatibility, mechanical strength and excellent corrosion resistance, and has low density close to the density of human bones. As a dental implant, achieving osseointegration with the surrounding bone tissue is one of the important criteria for evaluating the success of dental implantation. The surface treatment of the dental implant is an important influence factor of the osseointegration of the dental implant, and generally, the surface of the dental implant is modified, so that the healing time of the dental implant bone is shortened, the osseointegration speed is accelerated, and the functional load time is advanced. At present, most of dental implants on the market are modified by combining large-particle sand blasting and acid etching, a primary micron hole is constructed by sand blasting firstly, then the surface is treated by acid etching, the microcosmic appearance after acid etching is controlled by controlling the parameters of acid etching, the acid etching can form a submicron and nanometer structure on the primary micron hole constructed by sand blasting, after the acid etching, the hydrophilicity and the hole on the surface of the dental implant can be obviously changed, the formed nanoscale hole can be effectively combined with osteoblasts, meanwhile, the combination point on a unit area can be increased, and the combination force is enhanced, so that the acid etching is very important for the surface treatment effect of the dental implant.
However, the most used acid corrosion in the market is inorganic acid treatment, and the sulfuric acid, the hydrochloric acid, the nitric acid, the hydrofluoric acid and the like are compounded, so that heating is needed during use, but volatile acids such as the hydrochloric acid, the nitric acid, the hydrofluoric acid and the like have extremely strong volatility in a heating environment, a large amount of white fog can be generated, and the health of operators and the service life of production equipment are seriously affected.
Disclosure of Invention
The invention provides an acid etching agent for a titanium alloy dental implant, a preparation method and application thereof, which are used for solving one or more technical problems in the prior art and at least providing a beneficial choice or creation condition.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
an acid etching agent comprising: sulfuric acid, chlorine-containing inorganic salt, complexing agent, sulfamic acid and water.
Specifically, the sulfuric acid in the formula is used as an inorganic strong acid, has no volatility, can provide extremely high acid value storage for an acid etching agent, and can form a certain pore structure on the surface of a titanium material; sulfamic acid, the chemical property is relatively mild, and the sulfamic acid can replace sulfuric acid to a certain extent as a solid acid, mainly because sulfamic acid is dissolved in water and hydrolyzed to obtain ammonium bisulfate, and then ionized in water to obtain sulfate ions and hydrogen ions, so dangers such as high-temperature splashing caused by the adoption of sulfuric acid when an acid etching agent is prepared can be effectively avoided, and the operation risk of operators is reduced.
As a further improvement of the above scheme, the acid etching agent comprises, by weight: 3-10% of sulfuric acid, 5-50% of chlorine-containing inorganic salt, 0.5-1% of complexing agent, 5-10% of sulfamic acid and 29-85% of water.
Preferably, the acid etching agent comprises, by weight: 5-10% of sulfuric acid, 10-45% of chlorine-containing inorganic salt, 0.5-0.8% of complexing agent, 5-8% of sulfamic acid and 36-79% of water.
As a further improvement of the above aspect, the chlorine-containing inorganic salt is at least one selected from the group consisting of sodium hypochlorite, sodium chlorate, sodium perchlorate, potassium chlorate, sodium chloride, potassium chloride, ammonium chloride, magnesium chloride, and zinc chloride.
As a further improvement of the above aspect, the complexing agent is selected from at least one of citric acid, oxalic acid, tartaric acid, ethylenediaminetetraacetic acid or phytic acid. The complexing agent can effectively prevent ions in the acid etching agent from being separated out on the surface of the implant, so that the smoothness of the surface of the titanium alloy material is improved.
The preparation method of the acid etching agent comprises the following steps: weighing the raw material components according to the formula, slowly adding sulfuric acid into water along the wall of the cup while stirring, and then adding sulfamic acid, complexing agent and chlorine-containing inorganic salt to obtain the acid etching agent. The sulfuric acid should be added first after adding water, and stirring is needed during the addition of the sulfuric acid, so as to avoid splashing of the liquid caused by over-high local temperature.
A surface treatment process of a titanium alloy dental implant comprises the following steps of acid etching treatment: the part of the dental implant needing acid etching treatment is immersed in the acid etching agent for acid etching treatment, wherein the acid etching treatment lasts for about 10min, and the acid etching treatment temperature is about 100 ℃.
As a further improvement of the above scheme, the acid etching treatment step further comprises ultrasonic oil removal treatment, ultrasonic water washing and sand blasting treatment steps before the acid etching treatment step.
As a further improvement of the above scheme, the acid etching treatment step further comprises an ultrasonic cleaning step.
The acid etching agent disclosed by the invention is applied to the surface treatment of the titanium alloy dental implant.
The invention has the beneficial effects that:
the invention provides an acid etching agent for a titanium alloy dental implant and a preparation method and application thereof, and by adjusting the composition and the proportion of the acid etching agent, acid mist in the preparation and use processes of the acid etching agent can be greatly reduced, the influence on the body safety of operators is reduced, the corrosion to equipment in the environment is reduced, the process requirements can be met, the pore structure and distribution on the surface of the implant can be effectively regulated and controlled, a nano structure is formed, and the preparation method is green and environment-friendly. The preparation method provided by the invention is simple in process and strong in controllability, is beneficial to large-scale industrial production, and the acid etching agent obtained by the preparation method can be effectively applied to surface treatment of titanium alloy dental implants and the like, has a wide application prospect, and is worthy of great popularization.
Drawings
FIG. 1 is an SEM photograph of a titanium alloy dental implant sample obtained in example 4;
FIG. 2 is an SEM photograph of a sample of the titanium alloy dental implant obtained in example 5;
FIG. 3 is an SEM photograph of a sample of the titanium alloy dental implant obtained in comparative example 1;
FIG. 4 is an SEM photograph of a sample of the titanium alloy dental implant obtained in comparative example 2;
FIG. 5 is an SEM photograph of a sample of the titanium alloy dental implant obtained in comparative example 3.
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 acid etching agent, which comprises the following components in percentage by weight: 5% of sulfuric acid, 10% of sodium hypochlorite, 0.5% of citric acid, 5% of sulfamic acid and 79% of water.
Wherein, the sulfuric acid is commercial analytical pure concentrated sulfuric acid with the mass concentration of 98 percent; citric acid is analytically pure citric acid monohydrate; sulfamic acid is commercially available analytically pure sulfamic acid.
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 an acid etching agent comprises the following steps: weighing raw material components according to a formula, adding sulfuric acid into water while stirring, and then adding sulfamic acid, citric acid and sodium hypochlorite to obtain the acid etching agent.
A surface treatment process for a dental implant comprises the steps of ultrasonic oil removal treatment, ultrasonic water washing and sand blasting treatment before the step of acid etching treatment, the step of acid etching treatment and the step of ultrasonic cleaning after the step of acid etching treatment.
Firstly, carrying out ultrasonic degreasing treatment (using a commercially available degreasing agent with the concentration of 4% to treat for 5min at normal temperature), 3 times of ultrasonic water washing (cleaning by adopting purified water), drying treatment at 60 ℃ (the drying time is 1h), sand blasting treatment (carrying out sand blasting treatment by using a manual sand blasting machine, wherein sand materials collected by sand blasting are one or more of zirconium dioxide, zirconium silicate and silicon dioxide, the sand blasting distance is 30CM, the sand blasting pressure is 0.5MPa, the sand blasting time is 30s), ultrasonic water washing after sand blasting and other processes; then heating the acid etching agent to about 100 ℃ in a ventilation environment, and immersing the part of the dental implant needing acid etching in the acid etching agent for about 10 min; and finally, carrying out 3 times of ultrasonic cleaning on the implant by using purified water, wherein the cleaning time of each time is 5min, and drying for 1h by using an electric heating furnace at 60 ℃ to obtain the titanium alloy dental implant sample after surface treatment.
Example 2
An acid etching agent, which comprises the following components in percentage by weight: 10% of sulfuric acid, 45% of sodium chlorate, 0.8% of citric acid, 8% of sulfamic acid and 36% of water.
Wherein, the sulfuric acid is commercial analytical pure concentrated sulfuric acid with the mass concentration of 98 percent; citric acid is analytically pure citric acid monohydrate; sulfamic acid is commercially available analytically pure sulfamic acid.
A preparation method of an acid etching agent comprises the following steps: weighing raw material components according to a formula, adding sulfuric acid into water while stirring, and then adding sulfamic acid, citric acid and sodium chlorate to obtain the acid etching agent.
A surface treatment process for a dental implant comprises the steps of ultrasonic oil removal treatment, ultrasonic water washing and sand blasting treatment before the step of acid etching treatment, the step of acid etching treatment and the step of ultrasonic cleaning after the step of acid etching treatment.
Firstly, carrying out ultrasonic degreasing treatment (using a commercially available degreasing agent with the concentration of 4% to treat for 5min at normal temperature), 3 times of ultrasonic water washing (cleaning by adopting purified water), drying treatment at 60 ℃ (the drying time is 1h), sand blasting treatment (carrying out sand blasting treatment by using a manual sand blasting machine, wherein sand materials collected by sand blasting are one or more of zirconium dioxide, zirconium silicate and silicon dioxide, the sand blasting distance is 30CM, the sand blasting pressure is 0.5MPa, the sand blasting time is 30s), ultrasonic water washing after sand blasting and other processes; then heating the acid etching agent to about 100 ℃ in a ventilation environment, and immersing the part of the dental implant needing acid etching in the acid etching agent for about 10 min; and finally, carrying out 3 times of ultrasonic cleaning on the implant by using purified water, wherein the cleaning time of each time is 5min, and drying for 1h by using an electric heating furnace at 60 ℃ to obtain the titanium alloy dental implant sample after surface treatment.
Example 3
An acid etching agent, which comprises the following components in percentage by weight: 12.5% of sulfuric acid, 22.5% of sodium hypochlorite, 0.7% of citric acid, 7% of sulfamic acid and 55% of water.
Wherein, the sulfuric acid is commercial analytical pure concentrated sulfuric acid with the mass concentration of 98 percent; citric acid is analytically pure citric acid monohydrate; sulfamic acid is commercially available analytically pure sulfamic acid.
A preparation method of an acid etching agent comprises the following steps: weighing raw material components according to a formula, adding sulfuric acid into water while stirring, and then adding sulfamic acid, citric acid and sodium hypochlorite to obtain the acid etching agent.
A surface treatment process for a dental implant comprises the steps of ultrasonic oil removal treatment, ultrasonic water washing and sand blasting treatment before the step of acid etching treatment, the step of acid etching treatment and the step of ultrasonic cleaning after the step of acid etching treatment.
Firstly, carrying out ultrasonic degreasing treatment (using a commercially available degreasing agent with the concentration of 4% to treat for 5min at normal temperature), 3 times of ultrasonic water washing (cleaning by adopting purified water), drying treatment at 60 ℃ (the drying time is 1h), sand blasting treatment (carrying out sand blasting treatment by using a manual sand blasting machine, wherein sand materials collected by sand blasting are one or more of zirconium dioxide, zirconium silicate and silicon dioxide, the sand blasting distance is 30CM, the sand blasting pressure is 0.5MPa, the sand blasting time is 30s), ultrasonic water washing after sand blasting and other processes; then heating the acid etching agent to about 100 ℃ in a ventilation environment, and immersing the part of the dental implant needing acid etching in the acid etching agent for about 10 min; and finally, carrying out 3 times of ultrasonic cleaning on the implant by using purified water, wherein the cleaning time of each time is 5min, and drying for 1h by using an electric heating furnace at 60 ℃ to obtain the titanium alloy dental implant sample after surface treatment.
Example 4
An acid etching agent, which comprises the following components in percentage by weight: 15% of sulfuric acid, 15% of sodium hypochlorite, 0.5% of citric acid, 5% of sulfamic acid and 58% of water.
Wherein, the sulfuric acid is commercial analytical pure concentrated sulfuric acid with the mass concentration of 98 percent; citric acid is analytically pure citric acid monohydrate; sulfamic acid is commercially available analytically pure sulfamic acid.
A preparation method of an acid etching agent comprises the following steps: weighing raw material components according to a formula, adding sulfuric acid into water while stirring, and then adding sulfamic acid, citric acid and sodium hypochlorite to obtain the acid etching agent.
A surface treatment process for a dental implant comprises the steps of ultrasonic oil removal treatment, ultrasonic water washing and sand blasting treatment before the step of acid etching treatment, the step of acid etching treatment and the step of ultrasonic cleaning after the step of acid etching treatment.
Firstly, carrying out ultrasonic degreasing treatment (using a commercially available degreasing agent with the concentration of 4% to treat for 5min at normal temperature), 3 times of ultrasonic water washing (cleaning by adopting purified water), drying treatment at 60 ℃ (the drying time is 1h), sand blasting treatment (carrying out sand blasting treatment by using a manual sand blasting machine, wherein sand materials collected by sand blasting are one or more of zirconium dioxide, zirconium silicate and silicon dioxide, the sand blasting distance is 30CM, the sand blasting pressure is 0.5MPa, the sand blasting time is 30s), ultrasonic water washing after sand blasting and other processes; then heating the acid etching agent to about 100 ℃ in a ventilation environment, and immersing the part of the dental implant needing acid etching in the acid etching agent for about 10 min; and finally, carrying out 3 times of ultrasonic cleaning on the implant by using purified water, wherein the cleaning time of each time is 5min, and drying for 1h by using an electric heating furnace at 60 ℃ to obtain the titanium alloy dental implant sample after surface treatment.
Example 5
An acid etching agent, which comprises the following components in percentage by weight: 10% of sulfuric acid, 20% of sodium hypochlorite, 0.6% of citric acid, 8% of sulfamic acid and 58% of water.
Wherein, the sulfuric acid is commercial analytical pure concentrated sulfuric acid with the mass concentration of 98 percent; citric acid is analytically pure citric acid monohydrate; sulfamic acid is commercially available analytically pure sulfamic acid.
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 an acid etching agent comprises the following steps: weighing raw material components according to a formula, adding sulfuric acid into water while stirring, and then adding sulfamic acid, citric acid and sodium hypochlorite to obtain the acid etching agent.
A surface treatment process for a dental implant comprises the steps of ultrasonic oil removal treatment, ultrasonic water washing and sand blasting treatment before the step of acid etching treatment, the step of acid etching treatment and the step of ultrasonic cleaning after the step of acid etching treatment.
Firstly, carrying out ultrasonic degreasing treatment (using a commercially available degreasing agent with the concentration of 4% to treat for 5min at normal temperature), 3 times of ultrasonic water washing (cleaning by adopting purified water), drying treatment at 60 ℃ (the drying time is 1h), sand blasting treatment (carrying out sand blasting treatment by using a manual sand blasting machine, wherein sand materials collected by sand blasting are one or more of zirconium dioxide, zirconium silicate and silicon dioxide, the sand blasting distance is 30CM, the sand blasting pressure is 0.5MPa, the sand blasting time is 30s), ultrasonic water washing after sand blasting and other processes; then heating the acid etching agent to about 100 ℃ in a ventilation environment, and immersing the part of the dental implant needing acid etching in the acid etching agent for about 10 min; and finally, carrying out 3 times of ultrasonic cleaning on the implant by using purified water, wherein the cleaning time of each time is 5min, and drying for 1h by using an electric heating furnace at 60 ℃ to obtain the titanium alloy dental implant sample after surface treatment.
Comparative example 1
The difference between the comparative example 1 and the example 4 is that the acid etching agent of the comparative example 1 mixes sulfuric acid, hydrochloric acid and nitric acid, and the mass ratio of the sulfuric acid to the hydrochloric acid to nitric acid is as follows: 20 wt%, 20 wt% and 2 wt%, the acid etching temperature is 100 ℃, the acid etching time is 10min, and other surface treatment processes are the same as those in example 4, so that the titanium alloy dental implant sample subjected to surface treatment is obtained.
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the acid etching agent of the comparative example 2 comprises 5 mass percent of sulfuric acid, 0.5 mass percent of citric acid, 5 mass percent of sulfamic acid and the balance of water, and the other surface treatment processes are the same as those of the example 4, so that the titanium alloy dental implant sample after surface treatment is obtained.
Comparative example 3
The difference between the comparative example 2 and the example 1 is that the acid etching agent of the comparative example 2 comprises, by mass, 5% of sulfuric acid, 10% of sodium hypochlorite, 0.5% of citric acid and the balance of water, and the other surface treatment processes are the same as those of the example 4, so that a titanium alloy dental implant sample subjected to surface treatment is obtained.
Respectively carrying out scanning electron microscopy on the titanium alloy dental implant samples obtained in examples 4-5 and comparative examples 1-3 to obtain figures 1-5, wherein figure 1 is an SEM picture of the titanium alloy dental implant sample obtained in example 4; FIG. 2 is an SEM photograph of a sample of the titanium alloy dental implant obtained in example 5; FIG. 3 is an SEM photograph of a sample of the titanium alloy dental implant obtained in comparative example 1; FIG. 4 is an SEM photograph of a sample of the titanium alloy dental implant obtained in comparative example 2; FIG. 5 is an SEM photograph of a sample of the titanium alloy dental implant obtained in comparative example 3.
By comparing fig. 1-5, it can be found that the surface microstructures of fig. 1, fig. 2 and fig. 3 are substantially consistent, and both the surface microstructures can form rich 'honeycomb' structures on the surface of the dental implant made of the TC4 titanium alloy material, and the microstructure of the three are substantially consistent; FIG. 4 shows no obvious honeycomb structure on the surface, indicating that inorganic salt containing chlorine is an essential component; figure 5 shows a honeycomb structure, but the structure shows less honeycomb structure than figures 1-3, while the reaction of comparative example 3 is considerably slower during the course of the reaction.
In addition, the inventor also finds that a large amount of acid mist occurs when the acid etching agent of the comparative example 1 is prepared, but the acid etching solution of the examples 1 to 5 does not generate a large amount of acid mist in the preparation process, and does not generate a large amount of acid mist in the process of carrying out acid etching and heating on the titanium alloy dental implant, so that the acid etching agent formula and the surface treatment process can effectively avoid the problem that a large amount of acid mist occurs in the acid etching agent preparation and acid etching processes of the comparative example 1, effectively reduce the influence on the personal health and safety of operators and the corrosion on production equipment in the environment, simultaneously can meet the process requirements and effects, and achieve the purposes of effectively regulating and controlling the pore structure and distribution on the surface of the implant and forming the nano structure, and are green and environment-friendly.
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 acid etching agent, comprising: sulfuric acid, chlorine-containing inorganic salt, complexing agent, sulfamic acid and water.
2. The acid etching agent according to claim 1, comprising, in weight percent: 3-10% of sulfuric acid, 5-50% of chlorine-containing inorganic salt, 0.5-1% of complexing agent, 5-10% of sulfamic acid and 29-85% of water.
3. The acid etching agent according to claim 1, comprising, in weight percent: 5-10% of sulfuric acid, 10-45% of chlorine-containing inorganic salt, 0.5-0.8% of complexing agent, 5-8% of sulfamic acid and 36-79% of water.
4. The acid etching agent according to claim 1, wherein the chlorine-containing inorganic salt is at least one selected from the group consisting of sodium hypochlorite, sodium chlorate, sodium perchlorate, potassium chlorate, sodium chloride, potassium chloride, ammonium chloride, magnesium chloride, and zinc chloride.
5. The pickling agent of claim 1 wherein the complexing agent is selected from at least one of citric acid, oxalic acid, tartaric acid, ethylenediaminetetraacetic acid, or phytic acid.
6. The method for producing an acid etching agent according to any one of claims 1 to 5, comprising the steps of: weighing raw material components according to a formula, adding sulfuric acid into water while stirring, and then adding sulfamic acid, complexing agent and chlorine-containing inorganic salt to obtain the acid etching agent.
7. A surface treatment process of a titanium alloy dental implant is characterized by comprising the following acid etching treatment steps: immersing the part of the dental implant needing acid etching treatment in the acid etching agent of any one of claims 1 to 5 for acid etching treatment, wherein the acid etching treatment lasts for about 10min, and the temperature of the acid etching treatment is about 100 ℃.
8. The surface treatment process according to claim 7, wherein the acid etching treatment step is preceded by ultrasonic degreasing treatment, ultrasonic water washing and sand blasting treatment.
9. The surface treatment process according to claim 7, further comprising an ultrasonic cleaning step after the acid etching treatment step.
10. Use of the acid etching agent of any one of claims 1 to 5 for surface treatment of a titanium alloy dental implant.
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| CN111235577A (en) * | 2020-01-16 | 2020-06-05 | 广东安特齿科有限公司 | Acid etching solution and acid etching treatment method of titanium implant |
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2021
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