Nanopore titanium material, preparation method thereof and application of nanopore titanium material in preparation of implant titanium abutment

Abstract

The invention belongs to the technical field of biomimetic materials, and particularly relates to a nanopore titanium material, a preparation method thereof and application of the nanopore titanium material in preparation of an implant titanium abutment. According to the method, a titanium material serves as an anode to be placed in an electrolyte, a two-electrode system is adopted for conducting anodic oxidation treatment on the titanium material, the titanium material subjected to anodic oxidation treatment is obtained, the anodic oxidation treatment is conducted through direct-current voltage, and the direct-current voltage is smaller than 40 V; and the titanium material obtained after anodic oxidation treatment is subjected to annealing treatment, the nanopore titanium material is obtained, and the surface of the nanopore titanium material is provided with a titanium oxide coating of a nanopore structure. According to the nanopore titanium material obtained through the preparation method, on the basis that the working intensity of an implant gingival penetrating part abutment is met, the effects of resisting inflammation and promoting soft tissue integration are achieved due to the bionic coating of the nanopore structure, and therefore the effect of improving implant soft tissue integration is further achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of bionic materials, and in particular relates to a nanoporous titanium material and a preparation method thereof, and application of the nanoporous titanium material in preparing a titanium base for an implant. Background Art

[0002] Clinically, titanium is a common material for constructing the gingival contour of implants, whether it is the gingival part of soft tissue level implants or the upper repair base of bone level implants. When an inflammatory reaction caused by microorganisms occurs in this part, it will lead to peri-implant disease. Severe peri-implant disease will also cause irreversible absorption of bone tissue around the implant, namely peri-implantitis, which will eventually lead to implant loosening and failure.

[0003] Studies have shown that compared with rough micro-morphology, smooth titanium can inhibit bacterial adhesion in the early stage of plaque biofilm formation. Therefore, currently, titanium abutments are mostly polished to construct smooth micro-morphology. However, epidemiological surveys show that clinically, about 20% of oral implant patients and about 10% of implant sites still have peri-implantitis. It can be seen that a simple smooth titanium morphology cannot prevent the occurrence of peri-implant disease. How to further optimize the titanium abutment in the gingival part to improve soft tissue integration (STI) is an important issue that needs to be solved urgently.

[0004] Since it was discovered that nanoscale tubular arrays can be constructed on titanium surfaces by anodization, this fine nanomorphology has attracted the attention of many scholars due to its simple and economical manufacturing process and regular and controllable nanoscale dimensions. Recent studies have shown that titanium dioxide nanotubes (TiO2 Nanotubes, TNT) can inhibit inflammatory responses by regulating the polarization direction of macrophages. Compared with smooth titanium surfaces, nanotube-modified titanium surfaces can reduce the immune inflammatory response of macrophages under LPS-induced inflammatory conditions by reducing the release of proinflammatory mediators (TNF-α, MCP-1, NO), indicating that nanostructured surfaces are better tolerated in microenvironments with risks of bacterial contamination.

[0005] Although the nanotube structure can intervene in the soft tissue integration ability around the implant by affecting the inflammatory fiber complex, its special tubular structure significantly reduces the hardness of the material and cannot meet the requirements of implant placement. Summary of the invention

[0006] The purpose of the present invention is to provide a nanoporous titanium material and a preparation method thereof and an application in the preparation of an implant titanium base. The nanoporous titanium material prepared by the present invention has excellent hardness performance and meets the requirements of the implant titanium base; at the same time, it can achieve excellent anti-inflammatory and soft tissue integration-promoting effects.

[0007] To achieve the above object, the present invention provides the following technical solutions:

[0008] The present invention provides a method for preparing a nanoporous titanium material, comprising the following steps:

[0009] Using the titanium material as an anode and placing it in an electrolyte, performing anodic oxidation treatment on the titanium material by means of a two-electrode system to obtain the titanium material after anodic oxidation treatment. The anodic oxidation treatment is carried out using a DC voltage, and the DC voltage < 40V;

[0010] Performing annealing treatment on the titanium material after anodic oxidation treatment to obtain the nanoporous titanium material, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

[0011] Preferably, the electrolyte comprises ammonium fluoride, water and ethylene glycol; the mass percentage content of ammonium fluoride in the electrolyte is 0.1 - 0.5%; the volume percentage content of water in the electrolyte is 1 - 4%.

[0012] Preferably, the DC voltage is 10 - 30V.

[0013] Preferably, the time of the anodic oxidation treatment is 20 - 40 min.

[0014] Preferably, the cathode of the two-electrode system is a carbon rod; the titanium material is a titanium foil.

[0015] Preferably, the temperature of the annealing treatment is 450 - 550 °C, and the holding time is 1 - 3 h.

[0016] Preferably, the heating rate of the annealing treatment is 1 - 5 °C / min.

[0017] Preferably, the average pore diameter of the nanoporous structure is 40 - 80 nm; the thickness of the titanium oxide coating is 1 - 3 μm.

[0018] The present invention provides a nanoporous titanium material prepared by the preparation method described in the above technical solutions, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

[0019] The present invention provides an application of the nanoporous titanium material described in the above technical solutions in the preparation of an implant titanium abutment.

[0020] The present invention provides a method for preparing nanoporous titanium material, comprising the following steps: placing the titanium material as an anode in an electrolyte, subjecting the titanium material to anodic oxidation treatment using a two-electrode system to obtain the titanium material after anodic oxidation treatment, wherein the anodic oxidation treatment is carried out using a DC voltage and the DC voltage < 40V; annealing the titanium material after anodic oxidation treatment to obtain the nanoporous titanium material, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure. By controlling the DC voltage of the anodic oxidation treatment, the present invention obtains a nanoporous structure on the surface of the titanium material through the method of anodic oxidation treatment, and the formed titanium oxide coating with a nanoporous structure can be used as a biomimetic coating; at the same time, the present invention optimizes the microstructure of the titanium material after anodic oxidation treatment through annealing treatment to improve the mechanical properties (hardness) of the nanoporous titanium material. Thus, the nanoporous titanium material obtained by the preparation method provided by the present invention can, on the basis of meeting the working strength of the implant abutment at the gingival-penetrating part, achieve the effect of anti-inflammatory and promoting soft tissue integration due to the biomimetic coating with a nanoporous structure, thereby further realizing the effect of improving the STI of the implant. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 is the surface electron microscope image (×10k) of the nanoporous titanium material prepared in Example 1 of the present invention;

[0022] Figure 2 is the surface electron microscope image (×30k) of the nanoporous titanium material prepared in Example 1 of the present invention;

[0023] Figure 3 is the surface electron microscope image (×100k) of the nanoporous titanium material prepared in Example 1 of the present invention;

[0024] Figure 4 is the AFM-roughness characterization result of the nanoporous titanium material prepared in Example 1 of the present invention;

[0025] Figure 5 is the surface electron microscope image of the nanotube titanium material prepared in Comparative Example 1 of the present invention;

[0026] Figure 6 is the test result of real-time fluorescence quantitative polymerase chain reaction in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0027] The present invention provides a method for preparing nanoporous titanium material, comprising the following steps:

[0028] Placing the titanium material as an anode in an electrolyte, subjecting the titanium material to anodic oxidation treatment using a two-electrode system to obtain the titanium material after anodic oxidation treatment, wherein the anodic oxidation treatment is carried out using a DC voltage and the DC voltage < 40V;

[0029] The anodized titanium material is annealed to obtain the nanoporous titanium material, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

[0030] In the present invention, unless otherwise specified, all preparation raw materials / components are commercially available products well-known to those skilled in the art.

[0031] In the present invention, the titanium material is used as the anode and placed in the electrolyte, and the titanium material is anodized using a two-electrode system to obtain the anodized titanium material. The anodization is carried out using a DC voltage, and the DC voltage < 40V. In the present invention, the titanium material is preferably titanium foil. Before the anodization treatment, the present invention preferably pre-cleans the titanium material, and the pre-cleaning treatment is preferably ultrasonic cleaning successively with acetone, ethanol, and water. The water is preferably deionized water. The present invention has no special requirements for the specific implementation manner of the ultrasonic cleaning, and it is only necessary to ensure that the pre-cleaning treatment removes the oil stains on the surface of the titanium material.

[0032] In the present invention, the cathode of the two-electrode system is preferably a carbon rod. The electrolyte preferably includes ammonium fluoride, water, and ethylene glycol, and the water is preferably deionized water. The mass percentage content of ammonium fluoride in the electrolyte is preferably 0.1 - 0.5%, and it can be 0.3% in the examples. The volume percentage content of water in the electrolyte is preferably 1 - 4%, and it can be 2% in the examples. The DC voltage is preferably 10 - 30V, and it can be 20V in the examples. On the basis of optimizing the DC voltage of the anodization treatment in the present invention, it is also preferred to use hydrogen fluoride to prepare the electrolyte, and at the same time optimize the volume content of water in the electrolyte, so that nanopores can be successfully formed on the surface of the titanium material. The nanopores are pit-like pore structures obtained by anodization treatment on the surface of the titanium material, rather than nanotubes.

[0033] In the present invention, the time of the anodization treatment is preferably 20 - 40 min, more preferably 30 min.

[0034] After obtaining the anodized titanium material, the present invention anneals the anodized titanium material to obtain the nanoporous titanium material, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure. In the present invention, the annealing treatment is preferably carried out in an air atmosphere. The heating rate of the annealing treatment is preferably 1 - 5 °C / min, and it can be 3 °C / min in the examples. The temperature of the annealing treatment is preferably 450 - 550 °C, and it can be 500 °C in the examples. The holding time of the annealing treatment is preferably 1 - 3 h, and it can be 2 h in the examples.

[0035] In the present invention, the average pore diameter of the nanoporous structure is preferably 40 - 80 nm, and may be 60 nm in the examples.

[0036] In the present invention, the thickness of the titanium oxide coating is preferably 1 - 3 μm, and may be 2 μm in the examples.

[0037] The present invention provides a nanoporous titanium material prepared by the preparation method described in the above technical solution, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

[0038] In the present invention, the nanoporous titanium material is a titanium dioxide material.

[0039] In the present invention, the average pore diameter of the nanoporous structure is preferably 40 - 80 nm, and may be 60 nm in the examples.

[0040] In the present invention, the thickness of the titanium oxide coating is preferably 1 - 3 μm, and may be 2 μm in the examples.

[0041] The present invention provides the application of the nanoporous titanium material described in the above technical solution in the preparation of an implant titanium abutment.

[0042] In the present invention, the implant titanium abutment is specifically the titanium abutment of the gingiva-penetrating part.

[0043] In order to further illustrate the present invention, the technical solutions provided by the present invention will be described in detail below in conjunction with examples, but they should not be construed as limiting the protection scope of the present invention.

[0044] Example 1

[0045] This example provides a preparation method of a nanoporous titanium material, which specifically includes the following steps:

[0046] The pure titanium foil (1 cm × 1 cm × 0.2 mm) is ultrasonically cleaned successively with acetone, ethanol and deionized water to remove oil stains.

[0047] The electrolyte is prepared by dissolving deionized water and ammonium fluoride (NH4F) in ethylene glycol. The volume percentage content of deionized water in the electrolysis is 2%, and the mass percentage content of ammonium fluoride (NH4F) is 0.3%. A carbon rod is used as the cathode, and the cleaned pure titanium foil is used as the anode. The anodic oxidation treatment is carried out under the condition of a DC voltage of 20 V for 30 min to obtain the titanium foil after anodic oxidation treatment.

[0048] Then, the titanium foil after anodic oxidation treatment is annealed in an air atmosphere at 500 °C for 2 hours, and the heating rate of the annealing treatment is 4 °C / min, and then it is naturally cooled in the furnace to obtain the titanium foil after annealing treatment.

[0049] The annealed titanium foil was successively ultrasonically cleaned with acetone, ethanol, and deionized water to obtain nanoporous titanium material (TNP).

[0050] The nanoporous titanium material prepared in this example is a titanium dioxide material. The surface of the nanoporous titanium material prepared in this example has a titanium oxide coating with a nanoporous structure, and the average pore diameter of the nanoporous structure is 60 nm.

[0051] Comparative Example 1

[0052] This comparative example provides a method for preparing nanotubular titanium material, which specifically includes the following steps:

[0053] The pure titanium foil (1 cm × 1 cm × 0.2 mm) was successively ultrasonically cleaned with acetone, ethanol, and deionized water to remove oil stains.

[0054] The electrolyte was prepared by dissolving deionized water and ammonium bifluoride (NH4HF2) in ethylene glycol. The volume percentage content of deionized water in the electrolysis was 5%, and the mass percentage content of ammonium bifluoride (NH4HF2) was 0.3%. A carbon rod was used as the cathode, and the cleaned pure titanium foil was used as the anode. The anodization treatment was carried out under a DC voltage of 40 V for 30 min to obtain the titanium foil after anodization treatment.

[0055] Then, the titanium foil after anodization treatment was annealed in an air atmosphere at 500 °C for 2 hours, and the heating rate of the annealing treatment was 4 °C / min, and then it was naturally cooled in the furnace to obtain the annealed titanium foil.

[0056] The annealed titanium foil was successively ultrasonically cleaned with acetone, ethanol, and deionized water to obtain nanotubular titanium material (TNT).

[0057] The nanotubular titanium material prepared in this comparative example is a titanium dioxide material. The surface of the nanotubular titanium material prepared in this comparative example has a titanium oxide coating with a nanotubular structure, and the average pore diameter of the nanotubular structure is 60 nm.

[0058] Test Example

[0059] (1) SEM Test

[0060] Figure 1 is the surface electron micrograph (×10k) of the nanoporous titanium material prepared in Example 1; Figure 2 is the surface electron micrograph (×30k) of the nanoporous titanium material prepared in Example 1; Figure 3 is the surface electron micrograph (×100k) of the nanoporous titanium material prepared in Example 1. From Figure 1 、 Figure 2 and Figure 3As shown, in Example 1, nanoporous titanium material was successfully prepared through anodic oxidation treatment and annealing treatment. The surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

[0061] Figure 5 This is the surface electron microscope image of the nanotubular titanium material prepared in Comparative Example 1. From Figure 5 it can be seen that in Comparative Example 1, by controlling the conditions of anodic oxidation treatment, a nanotubular structure can be successfully prepared.

[0062] (2) AFM test

[0063] The pure titanium foil (Ti) used in Example 1 and the prepared nanoporous titanium material (TNP) were tested for the surface morphology by atomic force microscope (AFM). The test results are as Figure 4 shown. Figure 4 The left figure in is the test result of the surface roughness of the pure titanium foil (Ti) and the nanoporous titanium material (TNP). Figure 4 The middle figure in is the surface morphology image of the pure titanium foil (Ti). Figure 4 The right figure in is the surface morphology image of the nanoporous titanium material (TNP). From Figure 4 it can be seen that the surface roughness of the nanoporous titanium material (TNP) prepared in Example 1 increased significantly. The test data of the surface roughness of the pure titanium foil (Ti) used in Example 1 and the prepared nanoporous titanium material (TNP) are shown in Table 1.

[0064] Table 1 Surface roughness of pure titanium foil and nanoporous titanium material

[0065] Group Ti TNP 1 16 23 2 13.7 24.8 3 12.7 21.5 4 12.6 33.1 5 13.4 23.6 6 5.51 25.7 7 8.66 24.1 8 9.85 46.1 9 7.44 27.1 Average value 11.09555556 27.66666667 Standard deviation 3.21506216 7.23248843

[0066] (3) LDH cytotoxicity test

[0067] The LDH kit was used to detect the cell viability 1 day after cell seeding: Macrophages were seeded at 1×10 5 / well on the surface of the specimens in a 24-well plate. After incubation in an incubator for 24 h, they were rinsed 3 times × 5 min with PBS. 500 μL of diluted LDH release reagent was added to each well. After incubation in the incubator for 1 h, the supernatant was transferred to a 96-well plate, and the prepared LDH detection working solution was added. After incubation at room temperature in the dark for 30 min, the OD value was measured at 490 nm with an enzyme-labeled instrument. The cell viability was calculated using ((OD value of the experimental group - OD value of the blank) / (OD value of the control cells - OD value of the blank)) × 100%. The LDH cytotoxicity test results are shown in Table 2. Table 2 shows the LDH cytotoxicity test results of the pure titanium foil (Ti) used in Example 1 and the prepared nanoporous titanium material (TNP).

[0068] Table 2 LDH cytotoxicity test results

[0069]

[0070]

[0071] (4) Real-time fluorescence quantitative polymerase chain reaction (qRT-PCR)

[0072] Macrophages were seeded at 1×10 5 / well on the surface of the specimens in a 24-well plate. After 3 days of culture, the cells were digested and centrifuged to remove the supernatant. The total RNA of macrophages was extracted using a total RNA extraction kit, and the operation steps were carried out according to the manufacturer's instructions. The purity and concentration of RNA were measured using a NanoDrop 2000 ultraviolet-visible spectrophotometer. Subsequently, cDNA was synthesized according to the instructions of the FastKing RT Kit (containing gDNase). The obtained cDNA was amplified in a real-time fluorescence quantitative PCR system using a MagicSYBR mixture (Beijing ComWin Biotech Co., Ltd., China). On a CFXConnect TM Real-time fluorescence quantitative PCR detection system (Bio-Rad Laboratories, Inc., USA), with GAPDH as the internal reference, the expression level of the target gene mRNA was measured, and the primer sequences are shown in Table 3.

[0073] Table 3 Designed primer sequences

[0074]

[0075]

[0076] The test results of real-time fluorescence quantitative polymerase chain reaction (qRT-PCR) are shown in Table 4 and Figure 6 as follows. Table 4 and Figure 6 are the PCR test results of the pure titanium foil (Ti) used in Example 1 and the prepared nanoporous titanium material (TNP).

[0077] Table 4 PCR test results

[0078]

[0079] From the results in Table 4 and Figure 6 , it can be seen that the expression levels of pro-inflammatory and anti-inflammatory related genes were detected using RT-qPCR, and the results are as Figure 6As shown in Table 4, there was no significant difference in the expression of the M0 marker (CD68) in macrophages cultured on the Ti surface and the TNP surface. However, in macrophages cultured on the TNP surface, the expression of the M1 marker (CD86) was significantly decreased, and this trend was also reflected in the pro-inflammatory cytokines (TNF-α, iNOS, IL-1β). On the contrary, in macrophages cultured on the TNP surface, the expression of the M2 marker (CD206) was increased, and the expression of the anti-inflammatory cytokine TGF-β was also significantly increased.

[0080] (5) Transcriptome sequencing - inflammation-related genes

[0081] Macrophages were seeded at 1×10 5 / well on the surface of specimens in 24-well plates. After 3 days of culture, total RNA of macrophages was extracted using TRIzol reagent according to the manufacturer's protocol. The quality and purity of RNA samples were evaluated by agarose gel electrophoresis, NanoPhotometer spectrophotometer, and Agilent 2100 bioanalyzer. Library construction and sequencing were performed by Shanghai Weihuan Biotechnology Co., Ltd. using Illumina PE150. Clean Reads were accurately aligned with the reference genome using HISAT2 software. Differential gene analysis between the control and NP was performed using DESeq2, with a significant difference criterion of P value < 0.05 and Fold change > 1.5 or < 0.667. Gene Ontology (GO) analysis and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway analysis were performed using the clusterProfiler software.

[0082] Experimental conclusion: Through RNA sequencing, the enrichment analysis results showed that biological processes and cellular components such as "cell projection membrane", "postsynaptic membrane", "focal adhesion", "actin binding", and "collagen trimer" attracted the attention of this invention. These are closely related to the interaction of extracellular matrix-cell membrane-cytoskeleton. It is suggested that the mechanism by which the nanoporous titanium material prepared in Example 1 induces human macrophage polarization may be related to the changes in cell morphology and cytoskeleton. The enrichment analysis results of transcriptome sequencing-inflammation-related genes are shown in Table 5. The genes in Table 5 can be queried in the National Center for Biotechnology Information (NCBI). Table 5 contains some common anti-inflammatory and pro-inflammatory genes. It can be seen from Table 5 that the nanoporous group prepared in Example 1 up-regulated the genes related to inhibiting inflammation and down-regulated the genes related to promoting inflammation.

[0083] Table 5 Enrichment analysis results of transcriptome sequencing-inflammation-related genes

[0084]

[0085]

[0086] (6) Contact angle surface energy test

[0087] The pure titanium foil (Ti) used in Example 1 and the prepared nanoporous titanium material (TNP) were subjected to contact angle and surface energy tests. The test results are shown in Table 6 and Table 7.

[0088] Table 6 Test results of contact angle surface energy of Ti

[0089]

[0090] Table 7 Test results of contact angle surface energy of TNP

[0091]

[0092] (7) Nanoindentation test

[0093] The pure titanium foil (Ti) used in Example 1 and the prepared nanoporous titanium material (TNP) were subjected to nanoindentation tests. The test tool used was a nanoindenter. The two core indicators of nanoindentation tests are: hardness and elastic modulus. The test method is as follows: Use a nanoindenter to press into the surface of the material, and then calculate the hardness value of the material according to the formula (H = Pmax / Ac), where Pmax is the maximum indentation load and Ac is the contact area between the indenter and the material.

[0094] Table 8 gives the hardness data of the pure titanium foil (Ti) and the nanoporous titanium material (TNP), and Table 9 gives the elastic modulus data of the pure titanium foil (Ti) and the nanoporous titanium material (TNP).

[0095] Table 8 Test results of the hardness (unit: GPa) of Ti and TNP

[0096]

[0097]

[0098] Table 9 Test results of the elastic modulus (unit: GPa) of Ti and TNP

[0099] Group Ti TNP 1 24.651075 10.630022 2 25.534692 9.162794 3 25.27606 10.64469 4 24.603748 10.417961 5 25.673361 10.084437 Average value 25.1477872 10.1879808 Standard deviation 0.443864555 0.551108683

[0100] (8) Mechanical property tests

[0101] The nanoporous titanium material (TNP) prepared in Example 1 and the nanotubular titanium material (TNT) prepared in Comparative Example 1 were subjected to nanoindentation tests. The test tool used was a nanoindenter. The two core indicators of nanoindentation tests are: hardness and elastic modulus. The test method is as follows: Use a nanoindenter to press into the surface of the material, and then calculate the hardness value of the material according to the formula (H = Pmax / Ac), where Pmax is the maximum indentation load and Ac is the contact area between the indenter and the material. The test results are shown in Table 10.

[0102] Table 10 Test results of the mechanical properties of the nanoporous titanium material and the nanotubular titanium material

[0103] Group Hardness GPa Elastic modulus GPa TNP 1.59±0.14 10.18±0.55 TNT 0.92±0.27 12.35±1.34

[0104] The operating parameters of the anodization treatment for preparing the nanoporous titanium material (TNP) in Example 1 and the nanotubular titanium material (TNT) in Comparative Example 1 are shown in Table 10. It can be seen from Table 10 that by controlling the DC voltage of the anodization treatment, the present invention can successfully prepare the nanoporous titanium material, and the hardness performance of the prepared nanoporous titanium material is superior to that of the nanotubular titanium material prepared in Comparative Example 1.

[0105] Table 11 Operating parameters of anodic oxidation treatment in Example 1 and Comparative Example 1

[0106]

[0107]

[0108] As can be seen from the above examples, the present invention controls the DC voltage of anodic oxidation treatment, so as to obtain a nanoporous structure on the surface of titanium material by anodic oxidation treatment, and the formed titanium oxide coating with nanoporous structure can be used as a biomimetic coating; at the same time, the present invention optimizes the microstructure of the titanium material after anodic oxidation treatment by annealing treatment, and improves the mechanical properties (hardness) of the nanoporous titanium material. Thus, the nanoporous titanium material obtained by the preparation method provided by the present invention can, on the basis of meeting the working strength of the implant abutment at the gingival penetration site, achieve the effect of anti-inflammatory and promoting soft tissue integration due to the biomimetic coating with nanoporous structure. Therefore, the effect of improving the STI of the implant is further achieved.

[0109] Although the above examples have described the present invention in detail, they are only a part of the embodiments of the present invention, rather than all embodiments. Other embodiments can be obtained according to these embodiments without creative efforts, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A preparation method of a nanoporous titanium material, characterized in that, It includes the following steps: Using titanium material as the anode and placing it in the electrolyte, and adopting a two-electrode system to perform anodic oxidation treatment on the titanium material to obtain the titanium material after anodic oxidation treatment. The anodic oxidation treatment is carried out with a DC voltage, and the DC voltage < 40V; Performing annealing treatment on the titanium material after anodic oxidation treatment to obtain the nanoporous titanium material, and the surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

2. The preparation method according to claim 1, characterized in that, The electrolyte includes ammonium fluoride, water and ethylene glycol; the mass percentage content of ammonium fluoride in the electrolyte is 0.1 - 0.5%; the volume percentage content of water in the electrolyte is 1 - 4%.

3. The preparation method according to claim 1, characterized in that, The DC voltage is 10 - 30V.

4. The preparation method according to any one of claims 1 to 3, characterized in that, The time of the anodic oxidation treatment is 20 - 40 min.

5. The preparation method according to any one of claims 1 to 3, characterized in that, The cathode of the two-electrode system is a carbon rod; the titanium material is titanium foil.

6. The preparation method according to claim 1, wherein, The temperature of the annealing treatment is 450 - 550 °C, and the holding time is 1 - 3 h.

7. The preparation method according to claim 1 or 6, characterized in that The heating rate of the annealing treatment is 1 - 5 °C / min.

8. The preparation method according to claim 1, characterized in that, The average pore diameter of the nanoporous structure is 40 - 80 nm; the thickness of the titanium oxide coating is 1 - 3 μm.

9. The nanoporous titanium material prepared by the preparation method according to any one of claims 1 to 8, characterized in that, The surface of the nanoporous titanium material has a titanium oxide coating with a nanoporous structure.

10. Use of the nanoporous titanium material according to claim 9 in the preparation of an implant titanium abutment.

Images