Surface treatment method for pure titanium dental implant through alkali heat and acid etching treatment

Abstract

The invention belongs to the technical field of surface treatment methods of pure titanium dental implants, and particularly relates to a surface treatment method of a pure titanium dental implant through alkali heat and acid etching treatment, which comprises the following steps: preparing alkali liquor which contains inorganic alkali and aluminate and / or meta-aluminate; treating the pure titanium dental implant in alkali liquor; preparing acid liquor, wherein the acid liquor contains inorganic acid and organic acid; treating the pure titanium dental implant in an acid solution; and adding a zirconium salt solution into the acid solution for treatment, and then cleaning, drying and heating. The pure titanium dental implant treated by the method has excellent biological activity and wear resistance.

Description

Technical Field

[0001] The invention belongs to the technical field of surface treatment methods for pure titanium dental implants, and specifically relates to a surface treatment method for pure titanium dental implants through alkaline heat and acid etching treatment. Background Art

[0002] Dental implants are surgically implanted into the upper and lower jaws of the human body at the site of tooth loss. After the surgical wound heals, a device to repair dentures is installed on the upper part. The structure of dental implants includes a body, a neck and a base. The body is the part of the implant that is implanted into the human tissue, generally implanted into the mucoperiosteum or soft tissue. The neck is used to connect the body and the base. The base is the part of the dental implant exposed outside the mucosa. The commonly used materials for dental implants are pure titanium, titanium alloys, bioactive ceramics and some composite materials. Titanium and titanium alloys have good corrosion resistance, biocompatibility, mechanical properties and physical and chemical properties, and are the preferred materials for dental implants.

[0003] Compared with titanium alloys, pure titanium implants are more similar to the periodontal soft tissue of natural teeth in soft tissue structure. The thick keratinized epithelium on the interface can effectively protect the periodontal tissue. At the same time, the sulcal epithelium in the adjacent part can also protect the cells in the gingival sulcus to a certain extent. Summary of the invention

[0004] The purpose of the present invention is to provide a surface treatment method of a pure titanium dental implant through alkali heat and acid etching treatment to solve the deficiencies in the related art.

[0005] The technical solution of the present invention is as follows:

[0006] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0007] 1) preparing an alkali solution, wherein the alkali solution contains an inorganic alkali and aluminate and / or metaaluminate;

[0008] 2) placing the pure titanium dental implant to be treated in the alkaline solution, treating it at 55° C.-65° C. for 2-4 hours, and then cleaning and drying it;

[0009] 3) preparing an acid solution, wherein the acid solution contains an inorganic acid and an organic acid;

[0010] 4) placing the pure titanium dental implant treated with alkali solution in the acid solution and treating it at room temperature for 2-4 hours;

[0011] 5) adding a zirconium salt solution to the acid solution, treating for 2-4 hours, washing and drying, and heating at 160° C.-220° C. for 1-3 hours.

[0012] Preferably, the inorganic base is sodium hydroxide or potassium hydroxide, and the aluminate is sodium aluminate or potassium aluminate.

[0013] Preferably, the alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of sodium hydroxide is 0.8-3 mol / L, and the concentration of sodium aluminate is 2-5 mol / L.

[0014] Preferably, the inorganic acid is sulfuric acid.

[0015] Preferably, the organic acid is citric acid or oxalic acid.

[0016] Preferably, the acid solution is a mixed solution of sulfuric acid and citric acid, wherein the concentration of the sulfuric acid is 1.5-3 mol / L, and the concentration of the citric acid is 0.2-1 mol / L.

[0017] Preferably, the zirconium salt is zirconium chloride.

[0018] A pure titanium dental implant is obtained by treating the surface of the pure titanium dental implant by the above-mentioned surface treatment method of alkali heat and acid etching.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] The pure titanium dental implant obtained after the treatment of the present invention has a regular and orderly surface microstructure, and has excellent biological activity and wear resistance; the addition of aluminate / aluminate can not only greatly shorten the time of alkali heat treatment, but also contribute to the formation of a dense oxide film, further improve the hydrophilicity, and combine with the organic acid in the acid solution, so as to better load the zirconium element. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention.

[0022] Figure 1 is a SEM image of the sample of Example 1;

[0023] Figure 2 This is the SEM image of the sample of Comparative Example 1. DETAILED DESCRIPTION

[0024] Exemplary embodiments will be described in detail herein, examples of which are illustrated in the accompanying drawings. When the following description refers to the drawings, unless otherwise indicated, the same numerals in different drawings represent the same or similar elements.

[0025] The terms used in the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The singular forms "a", "the" and "the" used in the present invention and the appended claims are also intended to include plural forms unless the context clearly indicates other meanings. It should also be understood that the term "and / or" used herein refers to and contains any or all possible combinations of one or more associated listed items.

[0026] The following non-limiting examples can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. The following content is only an exemplary description of the scope of the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, which should also fall within the scope of the present invention.

[0027] The present invention is further described below in the form of specific embodiments. The various chemical reagents used in the embodiments of the present invention are obtained through conventional commercial channels unless otherwise specified. Unless otherwise specified, the contents described below are all mass contents. Unless otherwise specified, it is understood that it is carried out at room temperature. The pure titanium dental implants used in the embodiments of the present invention are all the same dental implants.

[0028] A surface treatment method for a pure titanium dental implant comprises the following steps:

[0029] 1) preparing an alkali solution, wherein the alkali solution contains an inorganic alkali and an aluminate and / or aluminate; the inorganic alkali is sodium hydroxide or potassium hydroxide, and the aluminate is sodium aluminate or potassium aluminate;

[0030] 2) placing the pure titanium dental implant to be treated in the alkaline solution prepared in 1), treating at 55° C.-65° C. for 2-4 hours, and then cleaning and drying;

[0031] 3) preparing an acid solution, wherein the acid solution contains an inorganic acid and an organic acid; the inorganic acid is sulfuric acid;

[0032] 4) placing the pure titanium dental implant after the alkali heat treatment in the acid solution prepared in 3) and treating it at room temperature for 2-4 hours;

[0033] 5) adding zirconium salt solution to the acid solution and treating for 2-4 hours; cleaning and drying the pure titanium dental implant, and heating at 160° C.-220° C. for 1-3 hours to obtain a treated pure titanium dental implant.

[0034] In one aspect of an embodiment of the present invention, the alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of sodium hydroxide is 0.8-3 mol / L, and the concentration of sodium aluminate is 2-5 mol / L; preferably, the alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of sodium hydroxide is 1.2-2.5 mol / L, and the concentration of sodium aluminate is 3-4 mol / L.

[0035] In one aspect of the embodiments of the present invention, the organic acid is citric acid or oxalic acid; specifically, the acid solution can be a mixed solution of sulfuric acid and citric acid, wherein the concentration of sulfuric acid is 1.5-3 mol / L, and the concentration of citric acid is 0.2-1 mol / L. Specifically, the acid solution can also be a mixed solution of sulfuric acid and oxalic acid, wherein the concentration of sulfuric acid is 1.5-3 mol / L, and the concentration of oxalic acid is 0.05-0.1 mol / L.

[0036] In one aspect of the embodiment of the present invention, the zirconium salt is zirconium chloride, and the concentration of the zirconium salt solution is 0.1-1 mol / L; preferably, the concentration of the zirconium salt solution is selected from 0.2-0.5 mol / L.

[0037] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0038] 1) preparing an alkali solution, wherein the alkali solution contains an inorganic alkali and aluminate;

[0039] 2) placing the pure titanium dental implant to be treated in the alkaline solution prepared in 1), treating it at 55° C.-65° C. for 2-4 hours, and then washing and drying it;

[0040] 3) preparing an acid solution, wherein the acid solution contains an inorganic acid and an organic acid;

[0041] 4) placing the pure titanium dental implant after the alkali heat treatment in the acid solution prepared in 3) and treating it at room temperature for 2-4 hours;

[0042] 5) adding zirconium salt solution to the acid solution and treating for 2-4 hours; after cleaning and drying the pure titanium dental implant, heating at 160° C.-220° C. for 1-3 hours to obtain a treated pure titanium dental implant.

[0043] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0044] 1) preparing an alkali solution, wherein the alkali solution contains an inorganic alkali and aluminate;

[0045] 2) placing the pure titanium dental implant to be treated in the alkaline solution prepared in 1), treating it at 60° C. for 3 h, and then washing and drying it;

[0046] 3) preparing an acid solution, wherein the acid solution contains an inorganic acid and an organic acid;

[0047] 4) placing the pure titanium dental implant after the alkali heat treatment in the acid solution prepared in 3) and treating it at room temperature for 4 hours;

[0048] 5) adding zirconium salt solution to the acid solution and treating for 2.5 hours; after cleaning and drying, heating at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0049] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0050] 1) preparing an alkali solution, wherein the alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of sodium hydroxide in the alkali solution is 0.8-3 mol / L, and the concentration of sodium aluminate is 2-5 mol / L;

[0051] 2) placing the pure titanium dental implant to be treated in the alkaline solution prepared in 1), treating it at 60° C. for 3 h, and then washing and drying it;

[0052] 3) preparing an acid solution, wherein the acid solution is a mixed solution of sulfuric acid and citric acid, wherein the concentration of sulfuric acid in the acid solution is 1.5-3 mol / L, and the concentration of citric acid is 0.2-1 mol / L;

[0053] 4) placing the pure titanium dental implant after the alkali heat treatment in the acid solution prepared in 3) and treating it at room temperature for 4 hours;

[0054] 5) adding a zirconium chloride solution with a concentration of 0.1-1 mol / L to the acid solution and treating for 2.5 hours; after cleaning and drying, heating at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0055] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0056] 1) preparing an alkali solution, wherein the alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of sodium hydroxide in the alkali solution is 2.5 mol / L, and the concentration of sodium aluminate is 3.5 mol / L;

[0057] 2) placing the pure titanium dental implant to be treated in the alkaline solution prepared in 1), treating it at 60° C. for 3 h, and then washing and drying it;

[0058] 3) preparing an acid solution, wherein the acid solution is a mixed solution of sulfuric acid and citric acid, wherein the concentration of sulfuric acid in the acid solution is 2 mol / L, and the concentration of citric acid is 0.8 mol / L;

[0059] 4) placing the pure titanium dental implant after the alkali heat treatment in the acid solution prepared in 3) and treating it at room temperature for 4 hours;

[0060] 5) adding a zirconium chloride solution with a concentration of 0.5 mol / L to the acid solution and treating for 2.5 hours; after cleaning and drying, heating at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0061] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0062] 1) preparing an alkali solution, wherein the alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of sodium hydroxide in the alkali solution is 2.5 mol / L, and the concentration of sodium aluminate is 3.5 mol / L;

[0063] 2) placing the pure titanium dental implant to be treated in the alkaline solution prepared in 1), treating it at 60° C. for 3 h, and then washing and drying it;

[0064] 3) preparing an acid solution, wherein the acid solution is a mixed solution of sulfuric acid and oxalic acid, wherein the concentration of sulfuric acid in the acid solution is 2 mol / L, and the concentration of oxalic acid is 0.1 mol / L;

[0065] 4) placing the pure titanium dental implant after the alkali heat treatment in the acid solution prepared in 3) and treating it at room temperature for 4 hours;

[0066] 5) adding a zirconium chloride solution with a concentration of 0.5 mol / L to the acid solution and treating for 2.5 hours; after cleaning and drying, heating at 180° C. for 2 hours to obtain a pure titanium dental implant.

[0067] The following non-limiting examples can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. The following content is only an exemplary description of the scope of the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, which should also fall within the scope of the present invention.

[0068] The present invention is further described below in the form of specific embodiments. The various chemical reagents used in the embodiments of the present invention are obtained through conventional commercial channels unless otherwise specified. Unless otherwise specified, the contents described below are all mass contents. Unless otherwise specified, it is understood that it is carried out at room temperature. The pure titanium dental implants used in the embodiments of the present invention are all the same dental implants.

[0069] Embodiment 1

[0070] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0071] 1) preparing an alkali solution; wherein the concentration of sodium hydroxide is 2.5 mol / L, and the concentration of sodium aluminate is 3.5 mol / L;

[0072] 2) placing the pure titanium dental implant to be treated (the dental implant is made of pure titanium material) in the alkaline solution prepared in 1), treating it at 60° C. for 3 hours, and then washing and drying it;

[0073] 3) preparing a mixed solution of sulfuric acid and citric acid; wherein the concentration of the sulfuric acid is 2 mol / L, and the concentration of the citric acid is 0.8 mol / L;

[0074] 4) placing the pure titanium dental implant treated with alkali solution in the acid solution prepared in 3) and treating at room temperature for 4 hours;

[0075] 5) directly adding a zirconium chloride solution with a concentration of 0.5 mol / L into the acid solution and treating for 2.5 hours; cleaning and drying the pure titanium dental implant, and heating at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0076] The surface morphology of the pure titanium dental implant obtained by the treatment in Example 1 is shown in the SEM image. Figure 1 shown.

[0077] Embodiment 2

[0078] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0079] 1) preparing a mixed solution of sodium hydroxide and sodium aluminate; wherein the concentration of sodium hydroxide is 2.5 mol / L, and the concentration of sodium aluminate is 3.5 mol / L;

[0080] 2) placing the pure titanium dental implant to be treated (the dental implant is made of pure titanium material) in the alkaline solution prepared in 1), treating it at 60° C. for 3 hours, and then washing and drying it;

[0081] 3) preparing a mixed solution of sulfuric acid and oxalic acid; wherein the concentration of sulfuric acid is 2 mol / L, and the concentration of oxalic acid is 0.1 mol / L;

[0082] 4) placing the pure titanium dental implant treated with alkali solution in the acid solution prepared in 3) and treating at room temperature for 4 hours;

[0083] 5) directly adding a zirconium chloride solution with a concentration of 0.5 mol / L into the acid solution and treating for 2.5 hours; cleaning and drying the pure titanium dental implant, and heating at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0084] Comparative Example 1

[0085] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0086] 1) preparing a mixed solution of sulfuric acid and citric acid; wherein the concentration of the sulfuric acid is 2 mol / L, and the concentration of the citric acid is 0.8 mol / L;

[0087] 2) placing the pure titanium dental implant to be treated (the dental implant is made of pure titanium material) in the acid solution prepared in 1), treating it at room temperature for 4 hours, and then cleaning and drying it;

[0088] 3) preparing a mixed solution of sodium hydroxide and sodium aluminate; wherein the concentration of sodium hydroxide is 2.5 mol / L, and the concentration of sodium aluminate is 3.5 mol / L;

[0089] 4) placing the pure titanium dental implant in the alkaline solution prepared in 3), treating at 60° C. for 3 h, and then washing and drying;

[0090] 5) adding the pure titanium dental implant treated with alkali solution into a zirconium chloride solution with a concentration of 0.5 mol / L and treating for 2.5 hours, cleaning and drying the pure titanium dental implant, and heating at 180° C. for 2 hours to obtain the treated pure titanium dental implant.

[0091] The SEM image of the surface morphology of the pure titanium dental implant obtained by the treatment of comparative example 1 is as follows: Figure 2 shown.

[0092] Comparative Example 2

[0093] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0094] 1) preparing a sodium hydroxide solution; wherein the concentration of sodium hydroxide is 2.5 mol / L;

[0095] 2) placing the pure titanium dental implant to be treated (the dental implant is made of pure titanium material) in the sodium hydroxide solution prepared in 1), treating it at 60° C. for 3 h, and then washing and drying it;

[0096] 3) preparing a sulfuric acid solution; wherein the concentration of the sulfuric acid is 2 mol / L and the concentration of the citric acid is 0.8 mol / L;

[0097] 4) placing the pure titanium dental implant treated with alkali solution in the acid solution prepared in 3) and treating at room temperature for 4 hours;

[0098] 5) directly adding a zirconium chloride solution with a concentration of 0.5 mol / L into the acid solution and treating for 2.5 hours; after cleaning and drying the pure titanium dental implant, heating it at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0099] Comparative Example 3

[0100] A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, comprising the following steps:

[0101] 1) preparing a mixed solution of sodium hydroxide and sodium aluminate; wherein the concentration of sodium hydroxide is 2.5 mol / L, and the concentration of sodium aluminate is 3.5 mol / L;

[0102] 2) placing the pure titanium dental implant to be treated (the dental implant is made of pure titanium material) in the alkaline solution prepared in 1), treating it at 60° C. for 3 hours, and then washing and drying it;

[0103] 3) preparing a sulfuric acid solution; wherein the concentration of the sulfuric acid is 2 mol / L;

[0104] 4) placing the pure titanium dental implant treated with alkali solution in the sulfuric acid solution prepared in 3) and treating at room temperature for 4 hours;

[0105] 5) directly adding a zirconium chloride solution with a concentration of 0.5 mol / L into the acid solution and treating for 2.5 hours; after cleaning and drying the pure titanium dental implant, heating it at 180° C. for 2 hours to obtain a treated pure titanium dental implant.

[0106] Wear resistance test and surface deposition apatite layer test:

[0107] The wear resistance test used Si3N4 grinding balls to perform dry friction on the surface at a rotation speed of 300 r / min and a load of 300 N. After rubbing for 20 minutes, the wear amount of the samples of Examples 1 and 2 and Comparative Examples 1 to 3 was tested respectively; the values ​​of the wear amount are shown in Table 1.

[0108] Surface deposition of apatite layer test:

[0109] The samples of Examples 1 and 2 and Comparative Examples 1 to 3 were sealed and placed in 50 mL of SBF simulated body fluid at 35°C. The SBF simulated body fluid was replaced every two days. The samples were taken out after 2, 4, 8, 10 and 12 days, respectively, and after drying, the surface morphology was observed using a scanning electron microscope, and the surface composition was analyzed using an infrared spectrometer; the time for forming an apatite layer was recorded; the time for forming an apatite layer of each sample is shown in Table 1.

[0110] Table 1

[0111]

[0112] By comparing the values ​​of Examples 1 and 2 and Comparative Examples 1 to 3, Figure 1 and Figure 2It can be seen that the pure titanium dental implant obtained by the treatment of the present invention has better performance, and the micro-surface formed on the surface of the pure titanium dental implant after alkali heat and acid etching treatment has excellent biological activity and wear resistance; during alkali heat treatment, the addition of sodium aluminate can not only greatly shorten the time of alkali heat treatment, but also contribute to the formation of a dense oxide film, thereby further improving the wear resistance; in addition, the addition of sodium aluminate can also help to improve the hydrophilicity of the surface of the pure titanium dental implant, so that it can be further combined with organic acids during acid etching treatment; citric acid and oxalic acid can undergo a certain complex reaction with zirconium salts, so that zirconium elements can be combined on the surface of the pure titanium dental implant, and zirconium dioxide can be formed after heating to further improve the wear resistance of the pure titanium dental implant; by comparing Example 1 and Comparative Example 3, it can be seen that the addition of organic acid can significantly improve the binding ability with zirconium ions, thereby improving the wear resistance. By comparing Example 1 with Comparative Example 1, it can be seen that changing the order of alkaline heat and acid etching treatment has a great influence on the surface morphology of the pure titanium dental implant. The surface microstructure of the pure titanium dental implant obtained by the treatment of the present invention is more regular and orderly, and is conducive to combining with zirconium salt.

[0113] Those skilled in the art will readily appreciate other embodiments of the invention after considering the specification and practicing the disclosure disclosed herein. The invention is intended to cover any variations, uses or adaptations of the invention that follow the general principles of the invention and include common knowledge or customary techniques in the art not disclosed by the invention; the description and examples are to be regarded as exemplary only.

Claims

1. A surface treatment method of a pure titanium dental implant by alkali heat and acid etching, characterized in that: The following steps are involved: 1) preparing an alkali solution, wherein the alkali solution contains an inorganic alkali and aluminate and / or metaaluminate; 2) placing the pure titanium dental implant to be treated in the alkaline solution, treating it at 55° C.-65° C. for 2-4 hours, and then cleaning and drying it; 3) preparing an acid solution, wherein the acid solution contains an inorganic acid and an organic acid; 4) placing the pure titanium dental implant treated with alkali solution in the acid solution and treating it at room temperature for 2-4 hours; 5) adding a zirconium salt solution to the acid solution, treating for 2-4 hours, washing and drying, and then heating at 160° C.-220° C. for 1-3 hours.

2. The surface treatment method of pure titanium dental implant by alkali heat and acid etching according to claim 1, characterized in that: The inorganic base is sodium hydroxide or potassium hydroxide, and the aluminate is sodium aluminate or potassium aluminate.

3. The surface treatment method of pure titanium dental implant by alkali heat and acid etching according to claim 1 or 2, characterized in that: The alkali solution is a mixed solution of sodium hydroxide and sodium aluminate, wherein the concentration of the sodium hydroxide is 0.8-3 mol / L, and the concentration of the sodium aluminate is 2-5 mol / L.

4. The surface treatment method of pure titanium dental implant by alkali heat and acid etching according to claim 1, characterized in that: The inorganic acid is sulfuric acid.

5. The surface treatment method of pure titanium dental implant by alkali heat and acid etching according to claim 1, characterized in that: The organic acid is citric acid or oxalic acid.

6. The surface treatment method of a pure titanium dental implant by alkali heat and acid etching according to any one of claims 1, 4 or 5, characterized in that: The acid solution is a mixed solution of sulfuric acid and citric acid, wherein the concentration of the sulfuric acid is 1.5-3 mol / L, and the concentration of the citric acid is 0.2-1 mol / L.

7. The surface treatment method of pure titanium dental implant by alkali heat and acid etching according to claim 1, characterized in that: The zirconium salt is zirconium chloride.

8. A pure titanium dental implant, characterized in that: The pure titanium dental implant is obtained by surface treatment by alkali heat and acid etching according to any one of claims 1 to 7.

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