Medical oral cavity bone increment barrier membrane and preparation method thereof
By designing the magnesium film structure of the support area and the barrier area, and combining with the ceramic coating to regulate the degradation rate, the problems of insufficient mechanical support and mismatch in the degradation period in the existing technology are solved, and the controllable degradation of the magnesium film and the osteogenesis cycle are matched, which is suitable for the industrial production of oral bone incremental barrier membranes.
Patent Information
- Application Number
- CN202510441318.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-09
- Publication Date
- 2025-07-11
AI Technical Summary
The existing oral bone incremental barrier membrane has problems in insufficient mechanical support, degradation cycle mismatch, secondary surgery risks, stress occlusion and prone to collapse, and cannot meet the needs of anatomical mechanics and the synchronous matching of osteogenesis.
A magnesium film is used as the main body to design the support area and barrier area, and retention is enhanced through the claw structure, combined with the ceramic coating to regulate the degradation rate, and an integrated molding technology and micro-arc oxidation treatment are used to form a controllable degradable ceramic coating, and the thickness distribution is optimized to match the bone formation cycle.
It improves the space maintenance ability, reduces the risk of osteogenesis failure, and achieves the matching of the controllable degradation of the magnesium film with the osteogenesis cycle, which is suitable for industrial production.
Smart Images
Figure CN120285285A_ABST
Abstract
Description
Technical Field
[0001] The present disclosure relates to the technical field of biomedical materials, and particularly relates to a medical oral bone augmentation barrier membrane and a preparation method thereof. Background Art
[0002] The success of oral implant restoration depends on sufficient bone mass support. In surgeries such as horizontal bone augmentation and vertical bone augmentation, the barrier membrane plays a core role, mainly used to maintain the bone repair space and block the invasion of soft tissue cells. Currently, the mainstream clinical products include collagen membranes and titanium-reinforced polytetrafluoroethylene non-absorbable membranes, but they have the following limitations:
[0003] The collagen membrane has problems of mechanical defects and uncontrollable degradation: Although the collagen membrane has biocompatibility, its elastic modulus is low (<10 MPa), and it cannot resist the pressure (about 50 N) exerted by the surrounding soft tissues in the bone grafting area during movements such as chewing and laughing, resulting in serious space collapse and poor bone regeneration effect in non-favorable type defects. In addition, its degradation period is affected by the manufacturing process, about 2 - 6 months. Premature degradation is likely to cause soft tissue invasion, and delayed degradation hinders bone remodeling.
[0004] Titanium mesh and titanium-reinforced non-absorbable membranes have problems of secondary surgery and stress shielding: The titanium mesh can maintain the space through high mechanical strength (elastic modulus 110 GPa), but it needs to be removed by secondary surgery 6 months after the operation, and the high exposure rate of the titanium mesh increases the risk of infection. In addition, the elastic modulus of titanium is much higher than that of cortical bone (14 GPa), and long-term retention will cause the stress shielding effect, inhibiting the mechanical adaptive remodeling of new bone. Animal experiments show that the elastic modulus of the newly formed bone in the area covered by the titanium membrane is significantly lower than that of normal bone.
[0005] Magnesium and its alloys are regarded as ideal candidate materials because of their degradability and elastic modulus close to human bone (45 GPa). Currently, magnesium membranes with uniform thickness are mostly used, but the uniform thickness design does not consider the anatomical site differences. High stress areas such as the alveolar ridge crest are prone to collapse due to insufficient strength (finite element analysis shows that the stress concentration exceeds 20 MPa), while the low stress areas are too thick, resulting in material redundancy and accelerating local degradation to produce hydrogen.
[0006] Recently, some studies have tried double-layer composite membranes (such as composite magnesium mesh and absorbable membranes), but the interfacial layers are prone to peeling, and the degradation products of the bonding materials may cause inflammation.
[0007] In summary, there is an urgent need for a new type of barrier membrane, which needs to simultaneously meet the following requirements: thickness matching the anatomical and mechanical needs, degradation period synchronized with the osteogenesis process, and integral structure to avoid composite defects. Summary of the Invention
[0008] To solve the above technical problems, the present disclosure provides a medical oral bone augmentation barrier membrane and a preparation method thereof.
[0009] In a first aspect, the present disclosure provides a medical oral bone augmentation barrier membrane, comprising a magnesium film and a ceramic coating disposed on the surface of the magnesium film;
[0010] The magnesium film includes a support region, a barrier region, and a first transition region connecting the support region and the barrier region, and the barrier region surrounds the support region;
[0011] The support region is approximately fishbone-shaped, including a main bone and a plurality of claw portions, and the plurality of claw portions are distributed on both sides of the main bone and connected to the main bone;
[0012] The thickness of the support region is greater than the thickness of the barrier region, and the thickness of the first transition region decreases from the support region to the barrier region.
[0013] In view of the problems existing in the existing barrier membranes, such as insufficient mechanical support, mismatched degradation periods, risk of secondary surgery, stress shielding, and easy collapse, the present disclosure proposes a novel medical oral bone augmentation barrier membrane. The magnesium film is used as the main body, and the support region and the barrier region are designed. Among them, the support region (mainly referring to the main bone) is distributed in the alveolar ridge crest region to provide mechanical support to stabilize the bone repair material, and the support region also enhances the retention of the bone repair material through the design of the claw portions, reducing osteogenesis failure caused by micro-movement; the barrier region covers the functional barrier region to block the invasion of soft tissues; in addition, the present disclosure also optimizes the thickness distribution through finite element analysis, and conducts gradient design on the thickness of the support region (high stress region) and the barrier region (low stress region), improving the space maintenance ability; further, by setting a ceramic coating on the surface of the magnesium film, initial protection is provided for the magnesium film, and the degradation rates of the magnesium film main body and the ceramic coating are synergistically regulated in the later stage to match the osteogenesis period.
[0014] In the present disclosure, the width of the main bone can be adjusted and designed according to the bone defect region of the patient.
[0015] The following are preferred technical solutions of the present disclosure, but not limitations on the technical solutions provided by the present disclosure. Through the following technical solutions, the technical objectives and beneficial effects of the present disclosure can be better achieved.
[0016] As a preferred technical solution of the present disclosure, the purity of the magnesium material used in the magnesium film is not less than 99.99%.
[0017] As a preferred technical solution of the present disclosure, the thickness of the support area is 0.18 - 0.32 mm, such as 0.18 mm, 0.20 mm, 0.22 mm, 0.24 mm, 0.26 mm, 0.28 mm, 0.30 mm or 0.32 mm, etc.; the thickness of the barrier area is 0.08 - 0.12 mm, such as 0.08 mm, 0.09 mm, 0.10 mm, 0.11 mm or 0.12 mm, etc., but it is not limited to the listed values, and other unlisted values within the above range are equally applicable.
[0018] The slope of the first transition area does not exceed 50°, such as 5°, 10°, 20°, 30°, 40° or 50°, etc., but it is not limited to the listed values, and other unlisted values within this range are equally applicable. Preferably, it does not exceed 30°, and further preferably does not exceed 15°.
[0019] In the present disclosure, the slope of the first transition area should not be too large, otherwise it will cause stress concentration, reduce the material support performance, and increase the clinical shaping difficulty at the same time.
[0020] As a preferred technical solution of the present disclosure, the number of the claw parts is not less than 4, such as 4, 5, 6, 7 or 8, etc., but it is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0021] Preferably, the length of the claw part is 5 - 10 mm, such as 5 mm, 6 mm, 7 mm, 8 mm, 9 mm or 10 mm, etc., but it is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0022] Preferably, the width of the claw part is 3 - 5 mm, such as 3 mm, 3.5 mm, 4 mm, 4.5 mm or 5 mm, etc., but it is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0023] In the present disclosure, the appropriate length and width of the claw part are beneficial to further enhance the retention of the bone repair material and improve the probability of osteogenesis.
[0024] Preferably, the angle between the claw part and the main bone is 60 - 90°, such as 60°, 70°, 80° or 90°, etc., but it is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0025] Preferably, at least 1 fixing hole penetrating the magnesium film is provided in each claw part area.
[0026] Preferably, the fixing hole is circular or oval.
[0027] Preferably, the pore diameter is 0.5-1 mm, such as 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm or 1 mm, etc., but is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0028] Preferably, the distance between two adjacent fixing holes in the same claw area is 2-3 mm, such as 2 mm, 2.2 mm, 2.4 mm, 2.6 mm, 2.8 mm or 3 mm, etc., but is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0029] As a preferred technical solution of the present disclosure, micro-holes penetrating the magnesium film are provided in the barrier area.
[0030] Preferably, the pore diameter of the micro-holes is 2-10 μm, such as 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm, etc., but is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0031] Preferably, the porosity of the barrier area is 15-30%, such as 15%, 20%, 25% or 30%, etc., but is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0032] Preferably, the micro-holes are radially distributed or grid-like distributed on the surface of the barrier area.
[0033] Preferably, the hole spacing between two adjacent micro-holes is 1.5-2 times the pore diameter, such as 1.5 times, 1.6 times, 1.7 times, 1.8 times, 1.9 times or 2 times, etc., but is not limited to the listed values, and other unlisted values within this range are equally applicable.
[0034] In the present disclosure, the setting of the micro-holes in the barrier area can accelerate the penetration of body fluids. However, its size and distribution need to be designed. If the size is too small and the arrangement is too dense, it will affect the exchange between metabolic substances and nutrients in the local regeneration environment; if the size is too large and the arrangement is too sparse, it will lead to the migration of soft tissue cells and affect the bone regeneration environment.
[0035] As a preferred technical solution of the present disclosure, the magnesium film further includes a strengthening area arranged around the barrier area. The strengthening area is connected to the barrier area through a second transition area, and the thickness of the strengthening area is greater than the thickness of the barrier area. The thickness of the second transition area decreases from the strengthening area to the barrier area.
[0036] Preferably, the thickness of the strengthening area is 0.18 - 0.32 mm, such as 0.18 mm, 0.20 mm, 0.22 mm, 0.24 mm, 0.26 mm, 0.28 mm, 0.30 mm or 0.32 mm, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0037] Preferably, the slope of the second transition area does not exceed 50°, such as 5°, 10°, 20°, 30°, 40° or 50°, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable. Preferably, it does not exceed 30°, and more preferably does not exceed 15°.
[0038] Preferably, the width of the strengthening area is 1 - 2 mm, such as 1 mm, 1.2 mm, 1.4 mm, 1.6 mm, 1.8 mm or 2 mm, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0039] In the present disclosure, the design of the strengthening area helps to further maintain the stability of the local regeneration space.
[0040] As a preferred technical solution of the present disclosure, the composition of the ceramic coating includes MgO, Ca3(PO4)2 and SiO2.
[0041] Preferably, in the ceramic coating, the molar ratio of Ca / P is 1.5 - 1.8, such as 1.5, 1.6, 1.7 or 1.8, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0042] Preferably, in the ceramic coating, the content of SiO2 is 5 - 10 wt%, such as 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt% or 10 wt%, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0043] Preferably, the thickness of the ceramic coating is 10 - 30 μm, such as 10 μm, 15 μm, 20 μm, 25 μm or 30 μm, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0044] In the present disclosure, by controlling the thickness of the ceramic coating, the degradation period of the medical oral bone augmentation barrier membrane is regulated to match the bone regeneration period (6 ± 1 months).
[0045] In a second aspect, the present disclosure provides a method for preparing a medical oral bone augmentation barrier membrane as described in the first aspect, including:
[0046] (1) Hot-roll the magnesium plate to the set thickness of the support area, then cut out the contour of the support area on its surface, and then form the first transition area and the barrier area through stamping to obtain the magnesium film.
[0047] (2) Perform micro-arc oxidation treatment on the magnesium film obtained in step (1) to form a ceramic coating on its surface, that is, obtain the medical oral bone augmentation barrier membrane.
[0048] The present disclosure uses an integrated molding technology to prepare the magnesium film body, and uses micro-arc oxidation treatment to form a controllable degradation ceramic coating on its surface. The preparation method is simple and efficient, and is suitable for industrial production.
[0049] Furthermore, when the barrier area has micropores or the barrier area is connected with a reinforcing area, those skilled in the art can fabricate the micropores and the reinforcing area according to the actual situation.
[0050] As a preferred technical solution of the present disclosure, the preparation method further includes: after the micro-arc oxidation treatment, performing vacuum annealing treatment; or, after the micro-arc oxidation treatment, performing growth factor impregnation.
[0051] Preferably, the temperature of the vacuum annealing treatment is 200 - 250 °C, such as 200 °C, 210 °C, 220 °C, 230 °C, 240 °C or 250 °C, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0052] Preferably, the time of the vacuum annealing treatment is 1 - 2 h, such as 1 h, 1.2 h, 1.4 h, 1.6 h, 1.8 h or 2 h, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0053] As a preferred technical solution of the present disclosure, the components of the electrolyte used in the micro-arc oxidation treatment in step (2) include Na2SiO3, KF, NaOH and Ca(H2PO4)2.
[0054] Preferably, in the electrolyte, the concentration of Na2SiO3 is 5 - 10 g / L, such as 5 g / L, 6 g / L, 7 g / L, 8 g / L, 9 g / L or 10 g / L, etc.; the concentration of KF is 2 - 5 g / L, such as 2 g / L, 3 g / L, 4 g / L or 5 g / L, etc.; the concentration of Ca(H2PO4)2 is 1 - 3 g / L, such as 1 g / L, 2 g / L or 3 g / L, etc., but not limited to the listed values, and other unlisted values within the above range are equally applicable.
[0055] Preferably, the pH of the electrolyte is 10 - 12, such as 10, 10.5, 11, 11.5 or 12, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0056] In the present disclosure, the composition of the electrolyte used in micro-arc oxidation treatment is not limited to the above one kind, and the specific composition can be adjusted according to the final design requirements.
[0057] Preferably, the voltage of the micro-arc oxidation treatment is 300 - 400V, such as 300V, 320V, 340V, 360V, 380V or 400V, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0058] Preferably, the frequency of the micro-arc oxidation treatment is 500 - 1000Hz, such as 500Hz, 600Hz, 700Hz, 800Hz, 900Hz or 1000Hz, etc., but not limited to the listed values, and other unlisted values within this range are equally applicable.
[0059] Preferably, the time of the micro-arc oxidation treatment is 5 - 15min, such as 5min, 7min, 10min, 13min or 15min, etc., not limited to the listed values, and other unlisted values within this range are equally applicable.
[0060] In the third aspect, the present disclosure provides an application of the medical oral bone augmentation barrier membrane as described in the first aspect or the medical oral bone augmentation barrier membrane prepared by the preparation method as described in the second aspect. The main bone of the support area is located in the alveolar ridge crest area; the barrier area is used to cover the functional barrier area and is in contact with the buccal and lingual sides.
[0061] The contour of the medical oral bone augmentation barrier membrane described in the present disclosure is customized according to the defect morphology during the application process, and the overall coverage extends more than 3mm into the healthy bone tissue.
[0062] The technical solutions provided by the embodiments of the present disclosure have the following advantages compared with the prior art:
[0063] (1) In view of the problems existing in the existing barrier membranes, such as insufficient mechanical support, mismatched degradation period, risk of secondary surgery, stress shielding, easy collapse, etc., the present disclosure proposes a novel medical oral bone augmentation barrier membrane, which uses a magnesium membrane as the main body and designs a support area and a barrier area. Among them, the support area is distributed in the alveolar ridge crest area, providing mechanical support and stabilizing the bone repair material, and the barrier area covers the functional barrier area, blocking the invasion of soft tissues; further, the support area also enhances the retention of the bone repair material through the design of the claw structure, reducing the osteogenesis failure caused by micromotion.
[0064] (2) The present disclosure also optimizes the thickness distribution through finite element analysis, and conducts a gradient design on the thickness of the support area (high stress area) and the barrier area (low stress area), improving the space maintenance ability.
[0065] (3) The present disclosure also provides initial protection for the magnesium film by providing a ceramic coating on the surface of the magnesium film, and realizes the coordinated regulation of the degradation rates of the magnesium film body and the ceramic coating in the later stage, matching the osteogenic cycle.
[0066] (4) The preparation method described in the present disclosure uses an integrated molding technology to prepare the magnesium film body, and uses micro-arc oxidation treatment to form a controllable degradation ceramic coating on its surface. The preparation method is simple and efficient and is suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS
[0067] The accompanying drawings herein are incorporated into the specification and constitute a part of this specification, showing embodiments consistent with the present disclosure, and are used together with the specification to explain the principles of the present disclosure.
[0068] In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.
[0069] Figure 1 It is a top-plan view structural schematic diagram of the magnesium film in the medical oral bone augmentation barrier film according to Embodiment 1 of the present disclosure;
[0070] Figure 2 It is a front-sectional view structural schematic diagram of the medical oral bone augmentation barrier film according to Embodiment 1 of the present disclosure;
[0071] Figure 3 It is a top-plan view structural schematic diagram of the magnesium film in the medical oral bone augmentation barrier film according to Embodiment 2 of the present disclosure;
[0072] Figure 4 It is a top-plan view structural schematic diagram of the magnesium film in the medical oral bone augmentation barrier film according to Embodiment 3 of the present disclosure.
[0073] Among them, 1. magnesium film; 1-1. support area; 1-2. barrier area; 1-3. first transition area; 1-4. main bone; 1-5. claw part; 1-6. fixing hole; 1-7. strengthening area; 1-8. second transition area; 1-9. micropores; 2. ceramic coating. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0074] In order to be able to more clearly understand the above-mentioned objects, features, and advantages of the present disclosure, the following will further describe the solutions of the present disclosure. It should be noted that, without conflict, the embodiments of the present disclosure and the features in the embodiments can be combined with each other.
[0075] In the following description, numerous specific details are set forth to provide a thorough understanding of the present disclosure, but the present disclosure may be practiced in other ways different from those described herein; obviously, the embodiments in the specification are only a part of the embodiments of the present disclosure, rather than all of the embodiments.
[0076] Example 1 (basic type)
[0077] This example provides a medical oral bone augmentation barrier membrane and a preparation method thereof. The medical oral bone augmentation barrier membrane includes a magnesium membrane 1 and a ceramic coating 2 provided on the surface of the magnesium membrane 1;
[0078] The magnesium membrane 1 includes a support area 1-1, a barrier area 1-2, and a first transition area 1-3 connecting the support area 1-1 and the barrier area 1-2. The barrier area 1-2 surrounds the support area 1-1;
[0079] The support area 1-1 is in a near fishbone shape, including a main bone 1-4 and 4 claw parts 1-5. The 4 claw parts 1-5 are distributed on both sides of the main bone 1-4 and are connected to the main bone 1-4;
[0080] The thickness of the support area 1-1 is greater than the thickness of the barrier area 1-2, and the thickness of the first transition area 1-3 decreases from the support area 1-1 to the barrier area 1-2;
[0081] The thickness of the support area 1-1 is 0.2 mm, and the thickness of the barrier area 1-2 is 0.1 mm;
[0082] The slope of the first transition area 1-3 is 10°.
[0083] Further, the length of each claw part 1-5 is 8 mm, the width is 4 mm, and the included angle between the claw part 1-5 and the main bone 1-4 is 60°;
[0084] Further, 2 fixing holes 1-6 are provided on each claw part 1-5. The fixing holes 1-6 are circular, with a hole diameter of 0.7 mm, and the spacing between adjacent two fixing holes 1-6 is 2.5 mm.
[0085] Further, the composition of the ceramic coating 2 includes MgO, Ca3(PO4)2, and SiO2. Among them, the Ca / P molar ratio is 1.67, the SiO2 content is 8 wt%, and the thickness of the ceramic coating 2 is 22 μm.
[0086] Among them, the schematic top view plane structure of the magnesium membrane 1 in the medical oral bone augmentation barrier membrane is as Figure 1 shown; the schematic front view cross-sectional structure of the medical oral bone augmentation barrier membrane is as Figure 2 shown (cut along the midline of the main bone 1-4).
[0087] The preparation method includes:
[0088] (1) Roll a magnesium plate with a purity of 99.99% to 0.2 mm at 300 °C, then cut out the contour of the support area 1-1 on its surface, and then form the first transition area 1-3 and the barrier area 1-2 by stamping. Then, punch fixing holes 1-6 on the claw parts 1-5 of the support area 1-1 to obtain the magnesium film 1;
[0089] (2) Perform micro-arc oxidation treatment on the magnesium film 1 obtained in step (1) to form a 22-μm ceramic coating 2 on its surface, thereby obtaining a medical oral bone augmentation barrier membrane;
[0090] Among them, the parameters of the micro-arc oxidation treatment are as follows:
[0091] Electrolyte: 8 g / L of Na2SiO3, 3 g / L of KF, 2 g / L of Ca(H2PO4)2, NaOH (adjust the pH to 11.5);
[0092] Voltage: 350 V, frequency: 700 Hz, treatment time: 10 min.
[0093] Example 2 (high-support type)
[0094] This example provides a medical oral bone augmentation barrier membrane and its preparation method. The medical oral bone augmentation barrier membrane includes a magnesium film 1 and a ceramic coating 2 provided on the surface of the magnesium film 1;
[0095] The magnesium film 1 includes a support area 1-1, a barrier area 1-2, and a first transition area 1-3 connecting the support area 1-1 and the barrier area 1-2. The barrier area 1-2 surrounds the support area 1-1;
[0096] The support area 1-1 is nearly fishbone-shaped, including a main bone 1-4 and 8 claw parts 1-5. The 8 claw parts 1-5 are distributed on both sides of the main bone 1-4 and are connected to the main bone 1-4;
[0097] The thickness of the support area 1-1 is greater than the thickness of the barrier area 1-2, and the thickness of the first transition area 1-3 decreases from the support area 1-1 to the barrier area 1-2;
[0098] The thickness of the support area 1-1 is 0.3 mm, and the thickness of the barrier area 1-2 is 0.1 mm;
[0099] The slope of the first transition area 1-3 is 15°.
[0100] Further, the length of each of the claw portions 1-5 is 5 mm, the width is 3 mm, and the angle between the claw portions 1-5 and the main bone 1-4 is 60°;
[0101] Further, one fixing hole 1-6 is provided on each of the claw portions 1-5. The fixing hole 1-6 is circular and has a pore diameter of 0.5 mm.
[0102] Further, the magnesium film 1 further includes a strengthening region 1-7 disposed around the barrier region 1-2. The strengthening region 1-7 is connected to the barrier region 1-2 through a second transition region 1-8, and the thickness of the strengthening region 1-7 is greater than the thickness of the barrier region 1-2. The thickness of the second transition region 1-8 decreases from the strengthening region 1-7 to the barrier region 1-2;
[0103] The thickness of the strengthening region 1-7 is 0.3 mm and the width is 2 mm;
[0104] The slope of the second transition region 1-8 is 15°;
[0105] Further, the composition of the ceramic coating 2 includes MgO, Ca3(PO4)2, and SiO2. Among them, the Ca / P molar ratio is 1.67, the SiO2 content is 10 wt%, and the thickness of the ceramic coating 2 is 26 μm.
[0106] Among them, the schematic top view plane structure of the magnesium film 1 in the medical oral bone augmentation barrier membrane is as Figure 3 shown.
[0107] The preparation method includes:
[0108] (1) Roll a magnesium plate with a purity of 99.99% to 0.3 mm, then cut out the contours of the support region 1-1, the barrier region 1-2, and the strengthening region 1-7 on its surface, and then form the first transition region 1-3, the barrier region 1-2, and the second transition region 1-8 by stamping. Then, punch the fixing holes 1-6 on the claw portions 1-5 of the support region 1-1 to obtain the magnesium film 1;
[0109] (2) Perform micro-arc oxidation treatment on the magnesium film 1 obtained in step (1) to form a 26-μm ceramic coating 2 on its surface, that is, obtain the medical oral bone augmentation barrier membrane;
[0110] Among them, the parameters of the micro-arc oxidation treatment are as follows:
[0111] Electrolyte: Na2SiO3 8 g / L, KF 3 g / L, Ca(H2PO4)2 2 g / L, NaOH (adjust the pH to 11.5);
[0112] Voltage: 400 V, frequency: 600 Hz, treatment time: 15 min.
[0113] Example 3 (Fast Osteogenesis Type)
[0114] This example provides a medical oral bone augmentation barrier membrane and a preparation method thereof. The medical oral bone augmentation barrier membrane includes a magnesium film 1 and a ceramic coating 2 provided on the surface of the magnesium film 1;
[0115] The magnesium film 1 includes a support area 1-1, a barrier area 1-2, and a first transition area 1-3 connecting the support area 1-1 and the barrier area 1-2. The barrier area 1-2 surrounds the support area 1-1;
[0116] The support area 1-1 is nearly fishbone-shaped, including a main bone 1-4 and 4 claw parts 1-5. The 4 claw parts 1-5 are distributed on both sides of the main bone 1-4 and are connected to the main bone 1-4;
[0117] The thickness of the support area 1-1 is greater than the thickness of the barrier area 1-2, and the thickness of the first transition area 1-3 decreases from the support area 1-1 to the barrier area 1-2;
[0118] The thickness of the support area 1-1 is 0.2 mm, and the thickness of the barrier area 1-2 is 0.1 mm;
[0119] The slope of the first transition area 1-3 is 12°.
[0120] Furthermore, the length of each claw part 1-5 is 10 mm, the width is 5 mm, and the included angle between the claw part 1-5 and the main bone 1-4 is 60°;
[0121] Furthermore, 1 fixing hole 1-6 is provided on each claw part 1-5. The fixing hole 1-6 is circular, and the aperture is 1 mm.
[0122] Micropores 1-9 penetrating through the magnesium film 1 are provided in the barrier area 1-2. The aperture of the micropores 1-9 is 6 μm, the porosity is 25%, the micropores 1-9 are distributed in a grid pattern, and the hole spacing between adjacent two micropores 1-9 is 12 μm;
[0123] Furthermore, the composition of the ceramic coating 2 includes MgO, Ca3(PO4)2, and SiO2. Among them, the Ca / P molar ratio is 1.67, the SiO2 content is 10 wt%, and the thickness of the ceramic coating 2 is 30 μm.
[0124] Among them, the schematic top view structure diagram of the magnesium film 1 in the medical oral bone augmentation barrier membrane is as Figure 4 shown.
[0125] The preparation method includes:
[0126] (1) Roll a magnesium plate with a purity of 99.999% to 0.2 mm at 300 °C, then cut out the contour of the support area 1-1 on its surface, and then form the first transition area 1-3 and the barrier area 1-2 by stamping. Then, make micropores 1-9, and punch fixing holes 1-6 on the claw part 1-5 of the support area 1-1 to obtain the magnesium film 1;
[0127] (2) Perform micro-arc oxidation treatment on the magnesium film 1 obtained in step (1) to form a 30-μm ceramic coating 2 on its surface, and then impregnate it with BMP-2 growth factor (concentration: 0.15 mg / mL) for 30 min to obtain the medical oral bone augmentation barrier membrane;
[0128] Among them, the parameters of the micro-arc oxidation treatment are as follows:
[0129] Electrolyte: 8 g / L of Na2SiO3, 3 g / L of KF, 2 g / L of Ca(H2PO4)2, NaOH (adjust the pH to 11.5);
[0130] Voltage: 350 V, frequency: 700 Hz, treatment time: 10 min.
[0131] Example 4
[0132] This comparative example provides a medical oral bone augmentation barrier membrane. Referring to Example 1, the only difference is that the slope of the first transition area 1-3 is 60°.
[0133] Comparative Example 1
[0134] This comparative example provides a medical oral bone augmentation barrier membrane. Referring to Example 1, the only difference is that the magnesium film 1 is a sheet-like magnesium film 1 with a uniform thickness of 0.1 mm.
[0135] Comparative Example 2
[0136] This comparative example provides a medical oral bone augmentation barrier membrane. Referring to Example 1, the only difference is that the magnesium film 1 is a sheet-like magnesium film 1 with a uniform thickness of 0.2 mm.
[0137] Comparative Example 3
[0138] This comparative example provides a medical oral bone augmentation barrier membrane, including a reticular titanium film (obtained by 3D printing), and a collagen film (purchased from Geistlich) provided on the surface of the reticular titanium film;
[0139] The thickness of the reticular titanium film is 0.2 mm, and the thickness of the collagen film is 0.3 mm.
[0140] Comparative Example 4
[0141] This comparative example provides a medical oral bone augmentation barrier membrane. Referring to Example 1, the only difference is that: the surface of the magnesium film 1 does not have a ceramic coating 2.
[0142] I. In vitro degradation test
[0143] The medical oral bone augmentation barrier membranes obtained in Examples 1-4 and Comparative Examples 1-4 were respectively immersed in simulated body fluid (SBF solution, 37 °C) for 6 months, and then their weight loss rates were measured. The test results are shown in Table 1.
[0144] II. Collapse resistance test
[0145] The average width of the bone defect area was set to 7.9 ± 1.3 mm, and the height was 4.4 ± 1.1 mm. According to the defect morphology, medical oral bone augmentation barrier membranes were customized from the materials of Examples 1-4 and Comparative Examples 1-4. After filling the bone defect area with bone powder (demineralized bovine bone mineral), a vertical load was applied until the membrane collapsed, and the collapse resistance was recorded. The test results are shown in Table 1.
[0146] Table 1
[0147] Weight loss rate Collapse resistance (g) Example 1 52％ 169 Example 2 37％ 341 Example 3 Complete degradation 171 Example 4 49％ 146 Comparative Example 1 82％ 71 Comparative Example 2 26％ 419 Comparative Example 3 The collagen membrane was completely degraded, and the titanium membrane was not degraded 272 Comparative Example 4 Complete degradation 153
[0148] As can be seen from Table 1, the medical oral bone augmentation barrier membranes obtained in Examples 1-3 are not only applicable to various situations, but also significantly superior to Comparative Example 1 in terms of mechanical properties, degradation matching degree and osteogenic effect, demonstrating the synergistic advantages of structural design, gradient thickness design and surface modification. Among them, in Example 2, due to the design of the support area thickness and the strengthening area, the support effect is better; in Example 3, due to the setting of micropores in the barrier area and the impregnation of growth factors, while promoting osteogenesis, the material degradation is accelerated;
[0149] Compared with Example 1, in Example 4, the slope of the first transition area is too large, resulting in stress concentration, reducing the material support performance (i.e., lower collapse resistance), and at the same time increasing the clinical shaping difficulty.
[0150] Compared with Example 1, Comparative Example 1 used a magnesium film with a uniform thickness (0.1 mm), with a lower collapse resistance and faster degradation.
[0151] Compared with Example 1, Comparative Example 2 used a magnesium film with a uniform thickness (0.2 mm), and the degradation rate was too slow.
[0152] Compared with Example 1, Comparative Example 3 used an existing composite membrane (titanium film + collagen film). Although it has a higher collapse resistance, the titanium film is non-degradable and requires a second operation for removal.
[0153] Compared with Example 1, in Comparative Example 4, the magnesium film was not micro-arc oxidized to form a ceramic coating, and it was completely degraded within the degradation period, unable to match the osteogenic cycle.
[0154] The above are only specific embodiments of the present disclosure, enabling those skilled in the art to understand or implement the present disclosure. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present disclosure. Therefore, the present disclosure will not be limited to these embodiments described herein, but rather will be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A medical oral bone augmentation barrier membrane, characterized in that, It includes a magnesium film and a ceramic coating provided on the surface of the magnesium film; The magnesium film includes a support area, a barrier area, and a first transition area connecting the support area and the barrier area, and the barrier area surrounds the support area; The support area is nearly fishbone-shaped, including a main bone and a plurality of claw parts, and the plurality of claw parts are distributed on both sides of the main bone and connected to the main bone; The thickness of the support area is greater than the thickness of the barrier area, and the thickness of the first transition area decreases from the support area to the barrier area.
2. The medical oral bone augmentation barrier membrane according to claim 1, wherein The thickness of the support area is 0.18 - 0.32 mm, and the thickness of the barrier area is 0.08 - 0.12 mm; Preferably, the slope of the first transition area does not exceed 50°, preferably does not exceed 30°.
3. The medical oral bone augmentation barrier membrane according to claim 1 or 2, characterized in that, The number of the claw parts is not less than 4; Preferably, the length of the claw part is 5 - 10 mm; Preferably, the width of the claw part is 3 - 5 mm; Preferably, the included angle between the claw part and the main bone is 60 - 90°; 4. The medical oral bone augmentation barrier membrane according to any one of claims 1-3, characterized in that, At least one fixing hole penetrating the magnesium film is provided in each claw part area; Preferably, the fixing hole is circular or oval; Preferably, the aperture of the fixing hole is 0.5 - 1 mm; Preferably, the distance between two adjacent fixing holes in the same claw part area is 2 - 3 mm.
5. The medical oral bone augmentation barrier membrane according to any one of claims 1-4, characterized in that, Micropores penetrating the magnesium film are provided in the barrier area; Preferably, the aperture of the micropore is 2 - 10 μm; Preferably, the porosity of the barrier area is 15 - 30%; Preferably, the micropores are radially distributed or grid-like distributed on the surface of the barrier area; Preferably, the hole spacing between two adjacent micropores is 1.5 - 2 times the aperture.
6. The medical oral bone augmentation barrier membrane according to any one of claims 1-5, characterized in that, The magnesium film further includes a strengthening area provided around the barrier area, the strengthening area is connected to the barrier area through a second transition area, and the thickness of the strengthening area is greater than the thickness of the barrier area, and the thickness of the second transition area decreases from the strengthening area to the barrier area; Preferably, the thickness of the strengthening area is 0.18 - 0.32 mm; Preferably, the slope of the second transition area does not exceed 50°, preferably does not exceed 30°; Preferably, the width of the strengthening area is 1 - 2 mm.
7. The medical oral bone augmentation barrier membrane according to any one of claims 1-6, characterized in that, The composition of the ceramic coating includes MgO, Ca3(PO4)2, and SiO2; Preferably, in the ceramic coating, the molar ratio of Ca / P is 1.5 - 1.8; Preferably, in the ceramic coating, the content of SiO2 is 5 - 10 wt%; Preferably, the thickness of the ceramic coating is 10 - 30 μm.
8. A method for preparing a medical oral bone augmentation barrier membrane according to any one of claims 1-7, characterized in that, It includes: (1) Hot-roll a magnesium plate to the set thickness of the support area, then cut out the contour of the support area on its surface, and then form the first transition area and the barrier area through stamping to obtain a magnesium film; (2) Perform micro-arc oxidation treatment on the magnesium film obtained in step (1) to form a ceramic coating on its surface, thereby obtaining a medical oral bone augmentation barrier membrane.
9. The preparation method according to claim 8, wherein, The preparation method further includes: after the micro-arc oxidation treatment in step (2), perform vacuum annealing treatment; Preferably, the temperature of the vacuum annealing treatment is 200 - 250 °C; Preferably, the time of the vacuum annealing treatment is 1 - 2 h.
10. The preparation method according to claim 8 or 9, characterized in that, The components of the electrolyte used in the micro-arc oxidation treatment described in step (2) include Na2SiO3, KF, NaOH, and Ca(H2PO4)2; Preferably, in the electrolyte, the concentration of Na2SiO3 is 5-10 g / L, the concentration of KF is 2-5 g / L, and the concentration of Ca(H2PO4)2 is 1-3 g / L; Preferably, the pH of the electrolyte is 10-12; Preferably, the voltage of the micro-arc oxidation treatment is 300-400 V; Preferably, the frequency of the micro-arc oxidation treatment is 500-1000 Hz; Preferably, the time of the micro-arc oxidation treatment is 5-15 min.