Oral guided bone regeneration isolation composite membrane as well as preparation method and application thereof

Abstract

The invention provides an oral cavity guided bone regeneration isolation composite membrane as well as a preparation method and application thereof, and belongs to the technical field of biomedical materials and processing thereof. The oral cavity barrier film with excellent performance is produced by combining the Zn-Mg alloy and the Mg-Zn alloy and utilizing an accumulative roll-bonding process under the limitation of a certain reduction rate and repetition times of accumulative roll-bonding, and the oral cavity barrier film has wide application prospects and market potential. The material not only can effectively promote the regeneration of oral cavity bone formation tissues, has good antibacterial performance, but also enhances the mechanical properties of the material, and can meet the requirements of clinical dental implant. In addition, the preparation method is easy for industrial production, low in cost and environment-friendly, and shows remarkable economic benefits and social benefits. The oral cavity GBR barrier membrane obtained by the preparation method has great breakthrough and application value in the field of biomedical materials.

Description

Technical Field

[0001] The present invention relates to the technical field of biomedical materials and their processing, and more specifically, the present invention relates to an oral guided bone regeneration isolation composite membrane, a preparation method thereof, and an application thereof. Background Art

[0002] Guided bone regeneration (GBR) technology is a modern surgical treatment method for promoting bone regeneration. This technology is mainly used when there is insufficient bone mass or bone defect in dental implantation. By using a barrier membrane to isolate the bone defect area and prevent the invasion of rapidly growing soft tissues, favorable conditions are created for the regeneration of bone tissue. As a key material in GBR technology, the performance of the barrier membrane directly affects the treatment effect. An ideal GBR isolation membrane not only needs to have good biocompatibility, but also should possess appropriate mechanical strength, degradation rate, osteogenic promotion, and antibacterial properties.

[0003] The currently used GBR isolation membrane materials can be divided into absorbable membranes and non-absorbable membranes. Although existing GBR isolation membrane materials such as expanded polytetrafluoroethylene (e-PTFE) and collagen membranes meet clinical needs to a certain extent, they still have some limitations. For example, e-PTFE cannot be absorbed by the membrane and requires a second operation for resection; while the collagen membrane, although absorbable, may lack sufficient mechanical support and long-term barrier effect in some cases. Therefore, developing a new type of barrier membrane material to overcome the deficiencies of existing materials is one of the important directions in current medical research on oral problems.

[0004] Magnesium metal (Mg) has excellent biocompatibility and antibacterial effects and is widely used in oral medical implant materials. However, due to its overly active chemical properties, its degradation rate in the body is too fast, making it difficult to achieve the desired shielding effect. Zinc metal (Zn) is an essential trace element for the human body, has good mechanical properties, a relatively appropriate corrosion degradation rate, can effectively bond implants and alveolar bone, and has good adhesiveness. However, the comprehensive mechanical properties, degradation behavior, and biocompatibility of pure zinc still need to be further improved.

[0005] The prior art discloses a medical degradable zinc alloy thin sheet for guided bone regeneration. Zinc forms an alloy with lithium and silver, strontium, magnesium, or bismuth, and a 0.05 - 0.5 mm zinc alloy thin sheet is obtained through steps of smelting, casting, homogenization annealing, extrusion, rolling, and leveling. However, the alloy in this prior art has zinc as the main body, with poor biocompatibility and osteogenic promotion, and its mechanical properties still need to be improved.

[0006] Therefore, developing an oral guided bone regeneration isolation composite membrane with excellent biocompatibility, osteogenic promotion, antibacterial properties, and good mechanical properties has important research significance and application value. Summary of the Invention

[0007] The present invention aims to overcome the deficiencies of the prior art and provides a preparation method of an oral guided bone regeneration isolation composite membrane. The developed oral guided bone regeneration isolation composite membrane has excellent biocompatibility, osteogenic performance, antibacterial performance and good mechanical properties, and is an ideal biomedical material.

[0008] Another object of the present invention is to provide an oral guided bone regeneration isolation composite membrane prepared by the above preparation method.

[0009] Another object of the present invention is to provide an application of the above oral guided bone regeneration isolation composite membrane.

[0010] To achieve the above objects, the present invention adopts the following technical solutions:

[0011] The present invention protects a preparation method of an oral guided bone regeneration isolation composite membrane, comprising the following steps:

[0012] S1. Melting metal particles in an inert atmosphere to obtain a binary alloy liquid: Zn-Mg and Mg-Zn;

[0013] S2. Casting the alloy liquid into a blank and then performing cold rolling to roll Zn-Mg plates and Mg-Zn plates;

[0014] S3. Cumulatively stacking and rolling the two alloy plates described in S2 for 4 to 8 times to obtain an alloy thin plate;

[0015] S4. Performing annealing treatment on the alloy thin plate;

[0016] Wherein, the metal particles are a mixture of metallic magnesium and metallic zinc;

[0017] In step S3, the reduction rate of each pass of the cumulative stacking and rolling is 50-75%;

[0018] In the Zn-Mg, the mass fraction of Mg is 0.5-2.0 wt.%, and in the Mg-Zn alloy, the mass fraction of Zn is 0.5-2.0 wt.%.

[0019] The present invention utilizes a magnesium-zinc alloy, which has good biocompatibility. The cumulative stacking and rolling process prepares Zn-Mg plates and Zn-Mg plates into an oral guided bone regeneration isolation composite membrane, which has excellent biocompatibility, osteogenic performance and antibacterial performance.

[0020] The combined use of Zn and Mg can produce good effects, further improving the biocompatibility, osteogenic ability and antibacterial properties of GBR membrane materials. Zn-Mg alloys can release free radical Zn and Mg ions, which can stimulate the activity of osteocytes and accelerate the bone treatment process. By adjusting the composition and structure of the alloy, its degradation rate can be precisely controlled to match the bone regeneration process and provide continuous isolation.

[0021] Accumulative Roll Bonding (ARB) is a severe plastic deformation technology used to refine the grain structure of metals and improve the mechanical properties of materials. Through repeated pressing and cold rolling, the grains can be refined and the structure of the material can be uniformly changed, thereby improving the mechanical properties and bioactivity of the material. Using the accumulative roll bonding process in the preparation of GBR barrier membranes can significantly improve the mechanical strength of magnesium-zinc alloys. This process can refine the grains and enhance the structure of the material, providing sufficient support in the oral environment, effectively isolating soft tissues, and ensuring the stability of the bone regeneration space. It can also further optimize the surface structure and composition distribution of the alloy, improve its compatibility with surrounding tissues, and reduce inflammatory reactions. In addition, by adjusting the number of accumulative roll bonding repetitions and the reduction ratio per pass, the accumulative roll bonding process can enhance the mechanical properties, making it more in line with the application requirements of oral GBR barrier membranes.

[0022] Preferably, the accumulative roll bonding includes the following steps: rolling two alloy plates into cold-rolled plates, cutting the cold-rolled plates into two pieces from the middle after each rolling, laminating them, and then performing cold rolling.

[0023] Preferably, the melting temperature in step S1 is 680 - 750 °C.

[0024] Preferably, the reduction ratio per pass of the cold rolling in step S2 is 50 - 75%.

[0025] Reasonable parameters for achieving tight cold rolling combination without cracking can be obtained within this range.

[0026] Preferably, the thickness of the Zn-Mg plate and the Mg-Zn plate is 1 mm.

[0027] Preferably, the Zn-Mg plate and the Mg-Zn plate are 100 mm long and 100 mm wide.

[0028] Preferably, the reduction ratio of the accumulative roll bonding for each pass in step S3 is 55 - 75%.

[0029] Preferably, the annealing temperature in step S4 is 250 - 350 °C.

[0030] Preferably, the holding time of the annealing in step S4 is 10 - 60 min.

[0031] Preferably, the metal particles are of analytical grade purity, with a purity ≥ 99.9%.

[0032] The present invention also protects an oral guided bone regeneration isolation composite membrane prepared by the above preparation method.

[0033] The application of the above oral guided bone regeneration isolation composite membrane in biomedical materials is also within the scope of protection of the present invention.

[0034] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0035] The present invention provides a preparation method for an oral guided bone regeneration isolation composite membrane. By combining Zn-Mg alloy and Mg-Zn alloy and using the accumulative roll-bonding process, under the limitation of a certain reduction ratio and repetition times of accumulative roll-bonding, an oral barrier membrane with excellent performance is produced, which has broad application prospects and market potential. This material can not only effectively promote the regeneration of oral osteogenic tissue, has good antibacterial properties, but also enhances the mechanical properties of the material, and can meet the needs of clinical dental implantation. In addition, this preparation method is easy for industrial production, has low cost and is environmentally friendly, showing significant economic and social benefits. The oral GBR barrier membrane obtained by this preparation method has made a major breakthrough and has application value in the field of biomedical materials. Description of the Drawings

[0036] Figure 1 Schematic flow chart of the preparation method of the oral guided bone regeneration isolation composite membrane for the embodiment. Detailed Description of the Invention

[0037] In order to describe the technical solution of the present invention more clearly and completely, the following further details the present invention through specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention, and various changes can be made within the scope defined by the rights of the present invention.

[0038] Unless otherwise specified, the reagents and materials used in the following examples are all commercially available.

[0039] 1. Test Indexes

[0040] (1) In the osteogenic performance experiment, the improvement rate of ALP activity and the improvement rate of OCN expression level of MC3T3-E1 cells on the barrier membrane were tested:

[0041] Cell Culture

[0042] Cell resuscitation: Take out MC3T3-E1 cells from liquid nitrogen, quickly thaw them in a 37°C water bath, and transfer them to α-MEM medium containing 10% FBS. Cell passage: When the cells reach 80-90% confluence, wash them with PBS, digest them with 0.25% trypsin, and passage them at a ratio of 1:3.

[0043] Material preparation

[0044] Treatment of Zn-Mg oral barrier composite membrane: Cut the membrane into a size suitable for the culture plate, sterilize it with ultraviolet light for 30 minutes, and soak it in PBS overnight. Cell seeding: Seed MC3T3-E1 cells onto the membrane at a density of 1×10 4 cells / cm 2 , and place them in an incubator at 37°C and 5% CO2.

[0045] ALP activity detection

[0046] Cell treatment: After culturing for 7 days and 14 days, take out the samples, wash them with PBS, and add lysis buffer (such as RIPA buffer) to lyse the cells. ALP activity assay: Use an ALP detection kit, operate according to the instructions, measure the absorbance at 405 nm, and calculate the ALP activity.

[0047] OCN expression level detection

[0048] RNA extraction: After culturing for 7 days and 14 days, extract total RNA with TRIzol reagent and measure the concentration and purity. cDNA synthesis: Reverse transcribe RNA into cDNA using a reverse transcription kit. qPCR detection: Design primers for OCN and internal reference genes (such as GAPDH), perform qPCR, and calculate the OCN expression level.

[0049] Data analysis

[0050] ALP activity increase rate: Compare the ALP activities of the experimental group and the control group and calculate the increase rate.

[0051] OCN expression level increase rate: Compare the OCN expression levels of the experimental group and the control group and calculate the increase rate.

[0052] (2) In the antibacterial performance experiment, measure the inhibition zone diameter of Staphylococcus aureus and Escherichia coli, and the cell growth inhibition rate:

[0053] Bacterial solution preparation: Bacterial strain activation: Inoculate Staphylococcus aureus and Escherichia coli into LB liquid medium respectively and culture them at 37°C with shaking for 12-16 hours. Bacterial solution dilution: Dilute the bacterial solution with PBS buffer to about 10 6 CFU / mL (OD600

[0054] ≈0.1).

[0055] Inhibition zone diameter test (agar diffusion method): Preparation of agar plate: Pour LB agar medium into a sterile petri dish and let it cool and solidify. Coating of bacterial solution: Take 100 μL of the diluted bacterial solution and evenly coat it on the agar plate. Placement of sample:

[0056] Gently place the sterilized Zn-Mg oral barrier membrane discs on the agar plate coated with the bacterial solution, with 1 - 2 discs placed on each plate. Incubation: Invert the plates and place them in an incubator at 37 °C for 24 hours.

[0057] Measurement of inhibition zone: After incubation, use a vernier caliper or an inhibition zone measuring instrument to measure the diameter of the clear inhibition zone around the membrane disc (unit: mm), and record the data.

[0058] Cell growth inhibition rate test (liquid medium method)

[0059] Inoculation of bacterial solution: Add 5 mL of LB liquid medium to a sterile test tube and inoculate 100 μL of the diluted bacterial solution (10 6 CFU / mL).

[0060] Addition of sample: Add the sterilized Zn-Mg oral barrier composite membrane discs to the test tube, and set up a control group without adding the sample at the same time.

[0061] Incubation: Place the test tube in a constant temperature shaking incubator at 37 °C for 24 hours.

[0062] Measurement of OD value: After incubation, take 1 mL of the bacterial solution to measure the OD600 value and record the data.

[0063] Calculation of inhibition rate:

[0064] Inhibition rate = (OD600 of control group - OD600 of experimental group) / OD600 of control group × 100%

[0065] (3) In the biocompatibility experiment, measure the absorbance rate of MC3T3-E1 cells in the MTS test on the barrier membrane:

[0066] Cell culture: Cell resuscitation: Take out MC3T3-E1 cells from liquid nitrogen, quickly thaw them in a 37 °C water bath, and transfer them to α-MEM medium containing 10% FBS. Cell passage: When the cells reach 80 - 90% confluence, wash them with PBS, digest them with 0.25% trypsin, and passage them at a ratio of 1:3.

[0067] Sample preparation: Barrier membrane treatment: Cut the Zn-Mg oral barrier membrane into a size suitable for the culture plate, sterilize it with ultraviolet light for 30 minutes, and soak it in PBS overnight. Cell seeding: Seed MC3T3-E1 cells onto the barrier membrane at a density of 1×10 4 cells / cm 2, Incubate in an incubator at 37°C with 5% CO2.

[0068] MTS assay: Selection of incubation time points: Conduct MTS assays on days 1, 3, and 7 of incubation respectively. Prepare the MTS

[0069] working solution: Mix the MTS reagent with the culture medium at a ratio of 1:5 according to the instructions (e.g., 100 μL of MTS reagent + 500 μL of culture medium). Change the culture medium: Take out the culture plate, aspirate the old culture medium, and gently wash the cells 1 - 2 times with PBS. Add the MTS working solution: Add 100 μL of the MTS working solution to each well to ensure complete coverage of the cells. Incubation: Return the culture plate to the incubator at 37°C with 5% CO2 and incubate for 2 - 4 hours. Measure the absorbance: After the incubation is completed, measure the absorbance value (OD value) at 490 nm using a microplate reader.

[0070] Data analysis: Record the data: Record the OD values at each time point.

[0071] (4) Flexural strength (MPa) ASTM D790 / ISO 178;

[0072] (5) Compressive strength (MPa) ASTM D695 / ISO 604;

[0073] (6) Elastic modulus (GPa) ASTM E111 / ISO 527.

[0074] 2. Experimental methods

[0075] Example 1

[0076] S1 Use Zn - 1.0 wt.% Mg alloy and Mg - 1.0 wt.% Zn alloy as raw materials, and carry out melting under argon protection to ensure that the alloy is not oxidized during the melting process. The melting temperature is controlled at 750°C.

[0077] S2 Pour the melted alloy liquid into billets, and then perform cold rolling. The reduction rate for each pass of cold rolling is 60%. Roll them into Zn - Mg plates and Zn - Mg plates with a thickness of 1 mm respectively.

[0078] S3 Adopt the accumulative roll - bonding technology. Cut the rolled plates into two plates with the same original size, and repeat the shearing, stacking, and rolling operations. The reduction rate for each pass reaches 60%, and the number of repetitions of accumulative roll - bonding is 6 passes.

[0079] S4 Anneal the cold - rolled thin plates, with the temperature controlled at 300°C and the time being 30 min.

[0080] Example 2

[0081] S1 Use Zn-0.5wt.% Mg alloy and Mg-1.0wt.% Zn alloy as raw materials and carry out smelting under argon protection to ensure that the alloy is not oxidized during the smelting process. The smelting temperature is controlled at 700 °C.

[0082] S2 Pour the smelted alloy liquid into billets, and then carry out cold rolling. The reduction rate of each pass of cold rolling is 60%, and Zn-Mg plates and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0083] S3 Adopt the accumulative roll-bonding technology, cut the rolled plates into two plates with the same size as the original, and repeat the shearing, laminating and rolling operations. The reduction rate of each pass reaches 60%, and the number of repetitions of accumulative roll-bonding is 6 passes.

[0084] S4 Anneal the cold-rolled thin plates, control the temperature at 300 °C and the time at 30 min.

[0085] Example 3

[0086] S1 Use Zn-1.0wt.% Mg alloy and Mg-0.5wt.% Zn alloy as raw materials and carry out smelting under argon protection to ensure that the alloy is not oxidized during the smelting process. The smelting temperature is controlled at 700 °C.

[0087] S2 Pour the smelted alloy liquid into billets, and then carry out cold rolling. The reduction rate of each pass of cold rolling is 60%, and Zn-Mg plates and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0088] S3 Adopt the accumulative roll-bonding technology, cut the rolled plates into two plates with the same size as the original, and repeat the shearing, laminating and rolling operations. The reduction rate of each pass reaches 60%, and the number of repetitions of accumulative roll-bonding is 6 passes.

[0089] S4 Anneal the cold-rolled thin plates, control the temperature at 300 °C and the time at 30 min.

[0090] Example 4

[0091] S1 Use Zn-1.0wt.% Mg alloy and Mg-1.0wt.% Zn alloy as raw materials and carry out smelting under argon protection to ensure that the alloy is not oxidized during the smelting process. The smelting temperature is controlled at 700 °C.

[0092] S2 Pour the smelted alloy liquid into billets, and then carry out cold rolling. The reduction rate of each pass of cold rolling is 60%, and Zn-Mg plates and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0093] In S3, accumulative roll-bonding technology is adopted. The rolled sheet is cut into two sheets with the same size as the original, and the shearing, laminating and rolling operations are repeated. The reduction per pass reaches 60%, and the number of repetitions of accumulative roll-bonding is 6 passes.

[0094] In S4, the cold-rolled thin sheet is annealed, with the temperature controlled at 300 °C and the time being 30 min.

[0095] Example 5

[0096] In S1, Zn-1.0wt.%Mg alloy and Mg-1.0wt.%Zn alloy are used as raw materials and melted under argon protection to ensure that the alloy is not oxidized during melting. The melting temperature is controlled at 700 °C.

[0097] In S2, the melted alloy liquid is cast into billets, and then cold-rolled. The reduction per pass of cold rolling is 60%, and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0098] In S3, accumulative roll-bonding technology is adopted. The rolled sheet is cut into two sheets with the same size as the original, and the shearing, laminating and rolling operations are repeated. The reduction per pass reaches 75%, and the number of repetitions of accumulative roll-bonding is 6 passes.

[0099] In S4, the cold-rolled thin sheet is annealed, with the temperature controlled at 300 °C and the time being 30 min.

[0100] Example 6

[0101] In S1, Zn-1.0wt.%Mg alloy and Mg-1.0wt.%Zn alloy are used as raw materials and melted under argon protection to ensure that the alloy is not oxidized during melting. The melting temperature is controlled at 700 °C.

[0102] In S2, the melted alloy liquid is cast into billets, and then cold-rolled. The reduction per pass of cold rolling is 60%, and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0103] In S3, accumulative roll-bonding technology is adopted. The rolled sheet is cut into two sheets with the same size as the original, and the shearing, laminating and rolling operations are repeated. The reduction per pass reaches 50%, and the number of repetitions of accumulative roll-bonding is 6 passes.

[0104] In S4, the cold-rolled thin sheet is annealed, with the temperature controlled at 300 °C and the time being 30 min.

[0105] Example 7

[0106] S1 Use Zn-1.0wt.% Mg alloy and Mg-1.0wt.% Zn alloy as raw materials, and carry out melting under argon protection to ensure that the alloy is not oxidized during the melting process. The melting temperature is controlled at 700 °C.

[0107] S2 Pour the molten alloy liquid into billets, and then carry out cold rolling. The reduction rate per pass of cold rolling is 60%, and Zn-Mg plates and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0108] S3 Adopt the accumulative roll bonding technology, cut the rolled plates into two plates with the same size as the original, and repeat the shearing, overlapping and rolling operations. The reduction rate per pass reaches 55%, and the number of repetitions of accumulative roll bonding is 6 passes.

[0109] S4 Carry out annealing treatment on the cold-rolled thin plates, with the temperature controlled at 300 °C and the time being 30 min.

[0110] Example 8

[0111] S1 Use Zn-1.0wt.% Mg alloy and Mg-1.0wt.% Zn alloy as raw materials, and carry out melting under argon protection to ensure that the alloy is not oxidized during the melting process. The melting temperature is controlled at 700 °C.

[0112] S2 Pour the molten alloy liquid into billets, and then carry out cold rolling. The reduction rate per pass of cold rolling is 60%, and Zn-Mg plates and Zn-Mg plates with a thickness of 1 mm are respectively rolled.

[0113] S3 Adopt the accumulative roll bonding technology, cut the rolled plates into two plates with the same size as the original, and repeat the shearing, overlapping and rolling operations. The reduction rate per pass reaches 60%, and the number of repetitions of accumulative roll bonding is 4 passes.

[0114] S4 Carry out annealing treatment on the cold-rolled thin plates, with the temperature controlled at 300 °C and the time being 30 min.

[0115] Example 9

[0116] S1 Use Zn-1.0wt.% Mg alloy and Mg-1.0wt.% Zn alloy as raw materials, and carry out melting under argon protection to ensure that the alloy is not oxidized during the melting process. The melting temperature is controlled at 700 °C.

[0117] S2 Pour the molten alloy liquid into billets, and then carry out cold rolling. The reduction rate per pass of cold rolling is 60%, and Zn-Mg and Zn-Mg thin plates with a thickness of 1 mm are respectively rolled.

[0118] In S3, accumulative roll-bonding technology is adopted. The rolled sheet is cut into two sheets with the same size as the original, and the operations of shearing and overlapping and rolling are repeated. The reduction ratio per pass reaches 60%, and the number of repetitions of accumulative roll-bonding is 8 passes.

[0119] In S4, the cold-rolled thin sheet is annealed, the temperature is controlled at 300 °C, and the time is 30 min.

[0120] Comparative Example 1

[0121] The experimental method is the same as that of Example 1, except that in step S1, Zn-0.3wt.% Mg alloy and Mg-0.3wt.% Zn alloy are used.

[0122] Comparative Example 2

[0123] The experimental method is the same as that of Example 1, except that in step S1, Zn-2.5wt.% Mg alloy and Mg-2.5wt.% Zn alloy are used.

[0124] Comparative Example 3

[0125] The experimental method is the same as that of Example 1, except that the number of repetitions of the accumulative roll-bonding described in step S3 is 3 times.

[0126] Comparative Example 4

[0127] The experimental method is the same as that of Example 1, except that the number of repetitions of the accumulative roll-bonding described in step S3 is 9 times.

[0128] Comparative Example 5

[0129] The experimental method is the same as that of Example 1, except that the reduction ratio of the accumulative roll-bonding per pass described in step S3 is 45%.

[0130] Comparative Example 6

[0131] The experimental method is the same as that of Example 1, except that the reduction ratio of the accumulative roll-bonding per pass described in step S3 is 80%.

[0132] 3. Test Results

[0133] Table 1 Biological Test Performance of Examples and Comparative Examples

[0134]

[0135]

[0136] Table 2 Mechanical Test Performance of Examples and Comparative Examples

[0137] Flexural strength (MPa) Compressive strength (MPa) Elastic modulus (GPa) Example 1 320 370 48 Example 2 280 330 46 Example 3 290 340 46.5 Example 4 300 350 47 Example 5 310 360 47.5 Example 6 250 300 44 Example 7 260 310 44.5 Example 8 270 320 45.5 Example 9 260 310 45 Comparative Example 1 200 250 40 Comparative Example 2 220 270 39 Comparative Example 3 180 230 38 Comparative Example 4 240 290 41 Comparative Example 5 150 200 35 Comparative Example 6 220 270 39

[0138] According to the data of Examples 1-9 in Table 1, the osteogenic promotion performance, antibacterial performance, and biocompatibility of the prepared oral guided bone regeneration isolation composite membrane all have advantages, that is, it has excellent biocompatibility, osteogenic promotion performance, and antibacterial performance. According to the mechanical property test results in Table 2, the flexural strength, compressive strength, and elastic modulus of Examples 1-9 all have advantages, and the mechanical properties are improved, among which Example 1 is the optimal preparation condition.

[0139] The alloy content of Comparative Example 1 and Comparative Example 2 exceeds the range, and the osteogenic promotion performance, antibacterial performance, biocompatibility, and mechanical properties all decrease significantly.

[0140] In Comparative Example 3, when the cumulative cold rolling pass number is too small (3 times), its biological performance is not good because the cumulative cold rolling pass number is insufficient, the grain refinement is insufficient, the surface activity of the material is low, and Mg 2+ and Zn 2+ ions cannot be effectively released, affecting osteogenic promotion and antibacterial properties; in terms of mechanical properties, insufficient cumulative cold rolling pass number leads to insufficient grain refinement, and the strength and toughness of the material are low, and the flexural strength, compressive strength, and elastic modulus are significantly reduced.

[0141] In Comparative Example 4, when the cumulative cold rolling pass number is too large (9 times), its biological performance is not good because the cumulative cold rolling pass number is too large, excessive internal stress accumulates in the material, microcracks or structural inhomogeneity may occur, affecting ion release and biocompatibility; in terms of mechanical properties, excessive cumulative cold rolling pass number leads to excessive internal stress accumulation in the material, microcracks or structural inhomogeneity may occur, and the flexural strength, compressive strength, and elastic modulus are significantly reduced.

[0142] In Comparative Example 5, when the reduction ratio is too low (45%), its biological performance is not good because the reduction ratio is insufficient, the material density is insufficient, and the release rates of Mg 2+ and Zn 2+ ions are slow, affecting osteogenic promotion and antibacterial properties; in terms of mechanical properties, insufficient reduction ratio leads to insufficient material density, and the flexural strength, compressive strength, and elastic modulus are significantly reduced.

[0143] In Comparative Example 6, when the reduction ratio is too high (80%), its biological performance is not good because the reduction ratio is too high, excessive internal stress accumulates in the material, microcracks or structural inhomogeneity may occur, affecting ion release and biocompatibility; in terms of mechanical properties, excessive reduction ratio leads to excessive internal stress accumulation in the material, microcracks or structural inhomogeneity may occur, and the flexural strength, compressive strength, and elastic modulus are significantly reduced.

[0144] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, rather than limitations on the implementation manners of the present invention. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the claims of the present invention.

Claims

1. A method for preparing an isolation composite membrane for oral guided bone regeneration, characterized in that: The following steps are involved: S1. The metal particles are melted in an inert atmosphere to obtain binary alloy liquids: Zn-Mg and Mg-Zn; S2. The alloy liquid is cast into a billet and then cold rolled to produce Zn-Mg plate and Mg-Zn plate; S3. Repeat the cumulative rolling of the two alloy plates in S2 4 to 8 times to obtain an alloy sheet; S4. annealing the alloy sheet; Wherein, the metal particles are a mixture of metal magnesium and metal zinc; In step S3, the cumulative rolling reduction rate of each pass is 50-75%; The mass fraction of Mg in the Zn-Mg is 0.5-2.0 wt. %, and the mass fraction of Zn in the Mg-Zn alloy is 0.5-2.0 wt. %.

2. The preparation method according to claim 1, characterized in that: The cumulative lamination includes the following steps: rolling two alloy plates into cold-rolled plates, cutting the cold-rolled plates into two pieces from the middle after each rolling, laminating them, and then cold-rolling them.

3. The preparation method according to claim 1, characterized in that: The smelting temperature in step S1 is 680-750°C.

4. The preparation method according to claim 1, characterized in that: The reduction rate of each cold rolling pass in step S2 is 50-75%.

5. The preparation method according to claim 1, characterized in that: The cumulative rolling reduction rate of each pass in step S3 is 55-75%.

6. The preparation method according to claim 1, characterized in that: The annealing temperature in step S4 is 250-350°C.

7. The preparation method according to claim 1, characterized in that: The annealing holding time in step S4 is 10 to 60 minutes.

8. The preparation method according to claim 1, characterized in that: The purity of the metal particles is ≥99.9%.

9. An oral guided bone regeneration isolation composite membrane, characterized in that: The invention is prepared by the preparation method according to any one of claims 1 to 8.

10. Use of the oral guided bone regeneration isolation composite membrane according to claim 9 as a biomedical material.

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