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CN113476161A - Flexible structure on surface of dental implant and construction method thereof - Google Patents

Flexible structure on surface of dental implant and construction method thereof Download PDF

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CN113476161A
CN113476161A CN202110647526.9A CN202110647526A CN113476161A CN 113476161 A CN113476161 A CN 113476161A CN 202110647526 A CN202110647526 A CN 202110647526A CN 113476161 A CN113476161 A CN 113476161A
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titanium
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华李成
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Ningbo University
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    • A61C8/00Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools
    • A61C8/0012Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the material or composition, e.g. ceramics, surface layer, metal alloy
    • AHUMAN NECESSITIES
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    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C8/00Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools
    • A61C8/0012Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the material or composition, e.g. ceramics, surface layer, metal alloy
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C8/00Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools
    • A61C8/0018Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the shape
    • A61C8/0037Details of the shape
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    • A61C8/00Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools
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    • A61L2430/12Materials or treatment for tissue regeneration for dental implants or prostheses

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Abstract

本发明公开了一种牙种植体表面柔性结构,包括由纳米管线构筑而成的柔性多孔道结构层,纳米管线原位生长于钛基植入体表面,纳米管线的主成分为Na2Ti2O5或Na2Ti3O7。本发明柔性结构中的孔道有利于骨组织长入柔性多孔道结构层,与纳米管线形成纳米管线‑骨组织三维交错形貌的生物复合结构,有利于增强植入体与牙槽骨界面的骨结合强度。本发明柔性结构具有超亲水性能、一定的弹性和极好的抗拉伸性能,在钛基植入体表面增加本发明柔性结构后,钛基植入体表面的摩擦学系数不会增加,不会增加临床医师使用过程中的种植难度。本发明柔性结构的构建方法使用简单的NaOH溶液处理,即在钛基植入体表面原位生长形成纳米管线,可操作性强。

Figure 202110647526

The invention discloses a flexible structure on the surface of a dental implant, comprising a flexible porous channel structure layer constructed of nano-tubes, the nano-tubes are grown on the surface of a titanium-based implant in situ, and the main component of the nano-tubes is Na 2 Ti 2 O 5 or Na 2 Ti 3 O 7 . The pores in the flexible structure of the present invention are conducive to the growth of bone tissue into the flexible porous structure layer, forming a biological composite structure with a three-dimensional staggered morphology of the nanotube-bone tissue with the nanotube, which is beneficial to strengthen the bone at the interface between the implant and the alveolar bone. Bond strength. The flexible structure of the present invention has super-hydrophilic properties, certain elasticity and excellent tensile properties, and after the flexible structure of the present invention is added to the surface of the titanium-based implant, the tribological coefficient of the surface of the titanium-based implant will not increase, It will not increase the difficulty of implantation during use by clinicians. The method for constructing the flexible structure of the present invention uses simple NaOH solution treatment, namely, in-situ growth and formation of nano-pipes on the surface of the titanium-based implant, and has strong operability.

Figure 202110647526

Description

Flexible structure on surface of dental implant and construction method thereof
Technical Field
The invention belongs to the field of oral implantation, and particularly relates to a flexible structure of a dental implant surface and a construction method thereof.
Background
The implant is one of the best methods for repairing the missing tooth at present, the commonly used implant is connected with the bone tissues of the peripheral alveolar bone in a screw-like mechanical locking mode, interface micromotion caused by the connection mode is one of important factors causing the implant to loose and lose efficacy, but an effective method for solving the bottleneck of the interface micromotion failure is not available at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a flexible structure on the surface of a dental implant and a construction method thereof, aiming at the defects of the prior art, the pore of a flexible porous structure layer constructed on the surface of a titanium-based implant is beneficial to bone tissues to grow into the flexible porous structure layer, and the flexible porous structure layer and the nano pipeline form a biological composite structure with a nano pipeline-bone tissue three-dimensional staggered appearance, and the biological composite structure is beneficial to enhancing the bone bonding strength of the interface of the implant and alveolar bone.
The technical scheme adopted by the invention for solving the technical problems is as follows: a flexible structure on the surface of dental implant is composed of a flexible porous structure layer made of nano-pipeline, which is in-situ grown on the surface of Ti-base implant and contains Na as main component2Ti2O5And/or Na2Ti3O7
According to the invention, the flexible porous structure layer is constructed on the surface of the titanium-based implant, after the implant is implanted into the alveolar bone, the flexible porous structure layer can promote the combination of the implant and the alveolar bone, so that bone tissues grow into the flexible porous structure, and a biological composite structure with a nano pipeline-bone tissue three-dimensional staggered appearance, which is formed by compounding the flexible porous structure and the bone tissues, is formed between the implant and the alveolar bone interface, so that a flexible connection structure which is similar to a natural periodontal membrane and has friction buffering and protection performances is formed between the implant and the alveolar bone interface, the interface buffering is realized, the micro-motion failure problem on the surface of the implant is solved, the long-term stability and the service life of the titanium-based implant after being implanted into the alveolar bone are improved, and the service life of a tooth is prolonged.
Preferably, the outer diameter of the nano pipeline is 30-90 nm.
Preferably, the flexible porous structure layer has pores with a micrometer scale, and the pore diameter of the pores is 2-50 μm when viewed from the cross section of the flexible porous structure layer. The pore canal with the diameter of 2-50 mu m is beneficial to the bone tissue to grow into the flexible porous structure layer, and the flexible porous structure layer and the nano pipeline form a nano pipeline-bone tissue three-dimensional staggered biological composite structure.
Preferably, the titanium-based implant is made of pure titanium or titanium alloy.
Preferably, the pure titanium is medical titanium metal TA4, and the titanium alloy is Ti-6Al-4V titanium alloy, Ti-6Al-7Nb titanium alloy or Ti-3Zr-2Sn-3Mo-25Nb titanium alloy.
A construction method of the flexible structure on the surface of the dental implant comprises the steps of carrying out high-temperature treatment on the surface of a titanium-based implant in a closed container by using NaOH solution for at least 1 hour, growing a nano-pipeline on the surface of the titanium-based implant in situ, and constructing a flexible porous structure layer by using the grown nano-pipeline.
According to the construction method of the flexible structure on the surface of the dental implant, the surface of the titanium-based implant is subjected to high-temperature treatment by using NaOH solution, so that NaOH reacts with titanium on the surface of the titanium-based implant, and a nano pipeline grows on the surface of the titanium-based implant in situ. The chemical reaction formula is as follows:
Figure BDA0003109713190000021
Figure BDA0003109713190000022
the construction method of the flexible structure on the surface of the dental implant uses simple NaOH solution treatment, namely, the nano pipeline is formed on the surface of the titanium-based implant by in-situ growth, and the operability is strong.
Preferably, the method for constructing the flexible structure on the surface of the dental implant specifically comprises the following steps:
1) cleaning the titanium-based implant by sequentially adopting acetone, absolute ethyl alcohol and deionized water, and naturally drying;
2) soaking the titanium-based implant in a closed container filled with NaOH solution with the concentration of 0.5-2 mol/L, carrying out surface treatment on the titanium-based implant at 150-240 ℃, wherein the treatment time is 1-24 hours, so that a nano pipeline with the outer diameter of 30-90 nm grows on the surface of the titanium-based implant in situ, and then constructing a flexible porous structure layer with micron-scale pores with the pore diameter of 2-50 mu m by the nano pipeline formed by growth;
3) washing the titanium-based implant treated in the step 2) with deionized water, and naturally drying.
The construction method of the flexible structure on the surface of the dental implant comprises the following cleaning process in the step 1): firstly, ultrasonically cleaning a titanium-based implant by using acetone for at least 2 minutes, then ultrasonically cleaning the titanium-based implant by using absolute ethyl alcohol for at least 2 minutes, and then ultrasonically cleaning the titanium-based implant by using deionized water for at least 2 minutes.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, a flexible porous structure layer is constructed on the surface of the titanium-based implant, pores of the flexible porous structure layer are beneficial to bone tissue to grow into the flexible porous structure layer, and a biological composite structure with a nano-pipeline-bone tissue three-dimensional staggered appearance is formed with the nano-pipeline, and the biological composite structure is beneficial to enhancing the bone bonding strength of the implant and an alveolar bone interface;
(2) the construction method of the flexible structure on the surface of the dental implant uses simple NaOH solution treatment, namely, the nano pipeline is formed on the surface of the titanium-based implant by in-situ growth, and the operability is strong;
(3) the main component of the nano pipeline in the flexible structure is Na2Ti2O5And/or Na2Ti3O7The main element components are titanium, oxygen and sodium, and the coating has no toxicity to human bodies and cells;
(4) surface hydrophilic and hydrophobic property tests show that the flexible structure has super-hydrophilic property, and the super-hydrophilic property can enhance the stretching, adsorption and biological activity of bone cells and quickly promote the interface combination between an implant and alveolar bone;
(5) mechanical tests show that the flexible structure has certain elasticity, can absorb energy by 1.59KJ per square centimeter, and has excellent tensile resistance;
(6) tribology tests show that after the flexible structure is added on the surface of the titanium-based implant, the tribology coefficient of the surface of the titanium-based implant cannot be increased, and the planting difficulty of a clinician in the using process cannot be increased.
Drawings
FIG. 1a is an electron microscope image of a longitudinal section of a flexible porous structure layer in example 2, and FIG. 1b is an enlarged view of a dotted-line frame portion on the right side in FIG. 1 a;
2a, 2b and 2c are electron microscope images of cross sections of the flexible porous channel structure layer in example 2 at different magnifications;
FIG. 3 is a schematic structural diagram of a biological composite structure with a three-dimensional staggered morphology of nanotube wires and bone tissue;
FIG. 4a is an X-ray diffraction pattern of the surface of the flexible multi-channel structure layer constructed in example 2, and FIG. 4b is an X-ray diffraction pattern of the surface of the original titanium-based implant without the flexible multi-channel structure layer;
fig. 5a is a test result of the surface hydrophilicity and hydrophobicity of the flexible porous structure layer constructed in example 2, and fig. 5b is a test result of the surface hydrophilicity and hydrophobicity of the original titanium-based implant without the flexible porous structure layer;
fig. 6a, 6b and 6c show the tensile property test results of the flexible porous channel structure layer of example 2 under different loads.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1: the method selects Ti-6Al-4V titanium alloy as a base material of the titanium-based implant, adopts the construction method of the invention to construct and form a flexible multi-pore structure layer on the surface of the titanium-based implant, and the construction method comprises the following steps: carrying out high-temperature treatment on the surface of the titanium-based implant in a closed container by using NaOH solution, wherein the treatment time is at least 1 hour, growing a nano-pipeline on the surface of the titanium-based implant in situ, and constructing a flexible porous structure layer by the nano-pipeline formed by growth, wherein the construction method specifically comprises the following steps:
1) firstly, ultrasonically cleaning a titanium-based implant for 2 minutes by using acetone, ultrasonically cleaning the titanium-based implant for 2 minutes by using absolute ethyl alcohol, ultrasonically cleaning the titanium-based implant for 2 minutes by using deionized water, and naturally drying the titanium-based implant;
2) soaking the titanium-based implant in a closed container filled with NaOH solution with the concentration of 1.0mol/L, and carrying out surface treatment on the titanium-based implant at 230 ℃ for 6 hours to enable a nano-pipeline with the outer diameter of 30-90 nm to grow on the surface of the titanium-based implant in situ, and constructing a flexible porous structure layer with micron-scale pores with the pore diameter of 2-50 microns by the nano-pipeline formed by growth;
3) washing the titanium-based implant treated in the step 2) with deionized water, and naturally drying.
Through detection, the main component of the flexible multi-pore structure layer formed in the example 1 is Na2Ti2O5
Example 2: the medical titanium TA4 is selected as the base material of the titanium-based implant, and the construction method of the invention is adopted to construct and form the flexible multi-pore structure layer on the surface of the titanium-based implant, and the construction method comprises the following steps: carrying out high-temperature treatment on the surface of the titanium-based implant in a closed container by using NaOH solution, wherein the treatment time is at least 1 hour, growing a nano-pipeline on the surface of the titanium-based implant in situ, and constructing a flexible porous structure layer by the nano-pipeline formed by growth, wherein the construction method specifically comprises the following steps:
1) firstly, ultrasonically cleaning a titanium-based implant for 2 minutes by using acetone, ultrasonically cleaning the titanium-based implant for 2 minutes by using absolute ethyl alcohol, ultrasonically cleaning the titanium-based implant for 2 minutes by using deionized water, and naturally drying the titanium-based implant;
2) soaking the titanium-based implant in a closed container filled with NaOH solution with the concentration of 1.0mol/L, and carrying out surface treatment on the titanium-based implant at 230 ℃ for 12 hours to enable a nano-pipeline with the outer diameter of 30-90 nm to grow on the surface of the titanium-based implant in situ, and constructing a flexible porous structure layer with micron-scale pores with the pore diameter of 2-50 microns by the nano-pipeline formed by growth;
3) washing the titanium-based implant treated in the step 2) with deionized water, and naturally drying.
Electron micrographs of the longitudinal section of the flexible porous structure layer constructed in example 2 are shown in fig. 1a and 1b, and electron micrographs of the cross section of the flexible porous structure layer in example 2 at different magnifications are shown in fig. 2a, 2b, and 2 c. In example 2, after the titanium-based implant is implanted into the alveolar bone, the flexible porous structure layer can promote the combination of the implant and the alveolar bone, so that bone tissue grows into the flexible porous structure, and a biological composite structure with a three-dimensional staggered morphology of a nanotube wire and the bone tissue, which is formed by combining the flexible porous structure and the bone tissue, is formed between the interface of the implant and the alveolar bone, and the structural schematic diagram of the biological composite structure is shown in fig. 3, 1 is the surface of the titanium-based implant, 2 is the surface of the alveolar bone, 3 is the nanotube wire, and 4 is the bone tissue.
The X-ray diffraction pattern of the surface of the flexible porous structure layer constructed in example 2 is shown in fig. 4a (the standard part of the black dots in the figure is a characteristic peak), and the X-ray diffraction pattern of the surface of the original titanium-based implant without the flexible porous structure layer constructed is shown in fig. 4 b. Through detection, the main component of the formed flexible multi-pore structure layer is Na2Ti2O5
The surface hydrophilicity and hydrophobicity test results of the flexible porous structure layer constructed in example 2 are shown in fig. 5a, and the surface hydrophilicity and hydrophobicity test results of the original titanium-based implant without the flexible porous structure layer are shown in fig. 5 b. Surface hydrophilic and hydrophobic property tests show that the flexible structure has super-hydrophilic property, and the super-hydrophilic property can enhance the stretching, adsorption and biological activity of bone cells and quickly promote the interface combination between an implant and alveolar bone.
Mechanical tests show that the flexible porous channel structure layer in example 2 has certain elasticity, can absorb energy by 1.59KJ per square centimeter, and has excellent tensile resistance. Fig. 6a, 6b and 6c show the tensile property test results of the flexible porous channel structure layer of example 2 under different loads. The test method comprises the following steps: different samples of the flexible porous structure layer of example 2 were tensile tested at normal loads of 300 μ N, 400 μ N, 1000 μ N, respectively, using a nano-scratch tester. Tests show that different samples generate cliff type reduction when the tangential force reaches about 400 mu N, and the tensile strength of the flexible porous channel structure layer can reach 600MPa according to the estimation. This higher tensile strength is favorable to improving the osseointegration intensity at implant and alveolar bone interface, forms the flexible connection structure who has friction buffering barrier propterty of similar natural tooth periodontal membrane at implant and alveolar bone interface, solves implant surface micromotion inefficacy problem, improves long-term stability and the active service life of titanium base implant implantation alveolar bone after, extension implant's life. In addition, tribology tests show that after the flexible structure is added on the surface of the titanium-based implant, the tribology coefficient of the surface of the titanium-based implant cannot be increased, and the planting difficulty of a clinician in the using process cannot be increased.

Claims (8)

1.一种牙种植体表面柔性结构,其特征在于,包括由纳米管线构筑而成的柔性多孔道结构层,所述的纳米管线原位生长于钛基植入体表面,所述的纳米管线的主成分为Na2Ti2O5和/或Na2Ti3O71. a dental implant surface flexible structure, is characterized in that, comprises the flexible porous structure layer that is constructed by nanometer pipeline, and described nanometer pipeline grows in situ on the surface of titanium-based implant, and described nanometer pipeline The main components are Na 2 Ti 2 O 5 and/or Na 2 Ti 3 O 7 . 2.根据权利要求1所述的一种牙种植体表面柔性结构,其特征在于,所述的纳米管线的外径为30~90nm。2 . The surface flexible structure of a dental implant according to claim 1 , wherein the outer diameter of the nano-tube is 30-90 nm. 3 . 3.根据权利要求1所述的一种牙种植体表面柔性结构,其特征在于,从所述的柔性多孔道结构层的横截面看,所述的柔性多孔道结构层具有微米尺度的孔道,所述的孔道的孔径为2~50μm。3 . The surface flexible structure of a dental implant according to claim 1 , wherein, viewed from the cross section of the flexible porous channel structure layer, the flexible porous channel structure layer has pores with a micrometer scale, 4 . The pore diameter of the pores is 2-50 μm. 4.根据权利要求1所述的一种牙种植体表面柔性结构,其特征在于,所述的钛基植入体的材质为纯钛或钛合金。4 . The surface flexible structure of a dental implant according to claim 1 , wherein the material of the titanium-based implant is pure titanium or titanium alloy. 5 . 5.根据权利要求4所述的一种牙种植体表面柔性结构,其特征在于,所述的纯钛为医用钛金属TA4,所述的钛合金为Ti-6Al-4V钛合金、Ti-6Al-7Nb钛合金或Ti-3Zr-2Sn-3Mo-25Nb钛合金。5. The surface flexible structure of a dental implant according to claim 4, wherein the pure titanium is medical titanium metal TA4, and the titanium alloy is Ti-6Al-4V titanium alloy, Ti-6Al -7Nb titanium alloy or Ti-3Zr-2Sn-3Mo-25Nb titanium alloy. 6.一种权利要求1-5中任一项所述的牙种植体表面柔性结构的构建方法,其特征在于,使用NaOH溶液在密闭容器中对钛基植入体表面进行高温处理,处理时间至少1小时,在钛基植入体表面原位生长纳米管线,再由生长形成的纳米管线构筑成柔性多孔道结构层。6. A method for constructing a flexible structure on the surface of a dental implant according to any one of claims 1 to 5, wherein the surface of the titanium-based implant is subjected to high-temperature treatment using a NaOH solution in an airtight container, and the treatment time For at least 1 hour, nanowires are grown in situ on the surface of the titanium-based implant, and then a flexible porous structure layer is constructed from the grown nanowires. 7.根据权利要求6所述的牙种植体表面柔性结构的构建方法,其特征在于,具体包括以下步骤:7. The construction method of dental implant surface flexible structure according to claim 6, is characterized in that, specifically comprises the following steps: 1)将钛基植入体依次采用丙酮、无水乙醇、去离子水清洗后,自然干燥;1) After the titanium-based implant is washed with acetone, anhydrous ethanol and deionized water in sequence, it is naturally dried; 2)将钛基植入体浸泡在装有浓度为0.5~2mol/L的NaOH溶液的密闭容器中,在150~240℃对钛基植入体进行表面处理,处理时间为1~24小时,使得钛基植入体表面原位生长外径为30~90nm的纳米管线,再由生长形成的纳米管线构筑成具有孔径为2~50μm的微米尺度的孔道的柔性多孔道结构层;2) Immerse the titanium-based implant in a closed container containing a NaOH solution with a concentration of 0.5-2 mol/L, and perform surface treatment on the titanium-based implant at 150-240 ° C for 1-24 hours, A nano-pipeline with an outer diameter of 30-90 nm is grown in-situ on the surface of the titanium-based implant, and then a flexible porous channel structure layer having micron-scale pores with a pore diameter of 2-50 μm is constructed from the grown nano-pipeline; 3)将经步骤2)处理后的钛基植入体用去离子水清洗,自然干燥。3) Wash the titanium-based implant treated in step 2) with deionized water and dry naturally. 8.根据权利要求7所述的牙种植体表面柔性结构的构建方法,其特征在于,步骤1)中的清洗过程为:先将钛基植入体采用丙酮超声清洗至少2分钟,再采用无水乙醇超声清洗至少2分钟,然后采用去离子水超声清洗至少2分钟。8. The method for constructing a flexible structure on the surface of a dental implant according to claim 7, wherein the cleaning process in step 1) is: first, the titanium-based implant is ultrasonically cleaned with acetone for at least 2 minutes, and then the Ultrasonic cleaning with water ethanol for at least 2 minutes, followed by ultrasonic cleaning with deionized water for at least 2 minutes.
CN202110647526.9A 2021-06-10 2021-06-10 Flexible structure on surface of dental implant and construction method thereof Pending CN113476161A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020143403A1 (en) * 2001-01-02 2002-10-03 Vaidyanathan K. Ranji Compositions and methods for biomedical applications
US20110184529A1 (en) * 2010-01-28 2011-07-28 Johan Forsgren Implants Comprising Titanium and Carbonate and Methods of Producing Implants
CN104233318A (en) * 2014-09-27 2014-12-24 浙江大学 Method for preparing implant surface with multi-scale complex porous structure
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