CN116898604B - Preparation method of medical degradable integral membrane and integral membrane - Google Patents

Abstract

The present disclosure provides a method for preparing a medical degradable integral membrane, the method for preparing the medical degradable integral membrane comprising powder preparation, sintering molding, processing molding, surface treatment and ultrasonic cleaning. According to the method, the degradable membrane with the porous structure and meeting the thickness requirement can be obtained, the strength of the membrane is high, the membrane is sufficiently applied to the alveolar bone absorption of a large area, the porous structure is simultaneously used for preventing the filling bone cement in the periodontal pocket from overflowing, the manufacturing cost is low, and the medical popularization and application are facilitated.

Description

Preparation method of medical degradable integral membrane and integral membrane

Technical Field

The application relates to the field of medical instruments, in particular to a preparation method of a medical degradable integral membrane, an integral membrane and a periodontal tissue regeneration method.

Background

In periodontal tissue regeneration treatment surgery, a membrane material is used as a barrier to prevent gingival connective tissue from contacting the implant root surface, and periodontal ligament cells having the ability to form new adhesion are guided to occupy the implant root surface in a limited manner, thereby forming new cementum on the root surface that has been exposed in the periodontal pocket. The non-degradable membranes commonly used in the prior art mainly comprise PTFE (polytetrafluoroethylene membrane), titanium mesh and titanium reinforced expanded polytetrafluoroethylene membrane, however, secondary operation is needed for taking out, and reinfection and wound cracking are easy to occur. In order to solve the problem, research and development personnel use magnesium alloy materials to prepare degradable film materials, and the degradable film materials have lower strength and cannot be applied to large-area alveolar bone absorption. In addition, the membrane material has higher manufacturing cost and is not beneficial to clinical application and popularization.

Disclosure of Invention

The application provides a preparation method of a medical degradable integral membrane, the integral membrane and a periodontal tissue regeneration method.

Specifically, the application is realized by the following technical scheme:

in a first aspect, an embodiment of the present application provides a method for preparing a medical degradable integral film, including:

preparing powder, namely mixing inorganic bone material with magnesium powder/magnesium alloy powder by doping pore-forming agent;

sintering and molding, namely placing the prepared powder into a sintering furnace, and sintering and molding the powder into a porous blank;

machining and forming, namely cutting the porous blank into a membrane;

performing surface treatment, namely performing micro-arc oxidation treatment on the surface of the membrane;

and (5) ultrasonic cleaning, and removing the residual on the surface of the membrane.

In some embodiments, the forming comprises: cutting, namely cutting the porous blank into a membrane; and grinding, namely grinding the surface of the membrane.

In some embodiments, the forming comprises: cold rolling, namely placing the porous blank into a rolling mill to be cold rolled into a diaphragm; and (3) heat treatment, and annealing heat treatment is carried out on the membrane.

In some embodiments, the powder preparation comprises: preparing a high-purity inorganic bone material; pretreating the inorganic bone material; mixing the pretreated inorganic bone material with a pore-forming agent; and/or, the powder preparation comprises: preparing magnesium powder/magnesium alloy powder; pretreating the magnesium powder/magnesium alloy powder; and mixing the pretreated magnesium powder/magnesium alloy powder with a pore-forming agent.

In some embodiments, after the sintering forming, the forming process is preceded by: evaluating the physical and mechanical properties of the porous blank; and if the physical and mechanical properties are not evaluated to be qualified, re-regulating the mixing proportion of the powder preparation.

In some embodiments, after the forming, further comprising: performing biocompatibility evaluation on the porous blank; and if the biocompatibility evaluation is unqualified, re-regulating the mixing proportion of the powder preparation.

In some embodiments, after the ultrasonic cleaning, further comprising: plating the surface of the membrane with aluminum, titanium, nickel or tantalum.

In some embodiments, the grinding comprises: friction stir processing and/or surface mechanical abrasion treatment.

In a second aspect, an embodiment of the present application provides a medical degradable integral membrane for periodontal tissue regeneration, which is made by the medical degradable integral membrane preparation method in the first aspect, and the medical degradable integral membrane comprises:

the membrane array forms a plurality of micropores, and the micropores are formed by the pore-forming agent;

the thickness of the membrane is 0.05-0.1mm.

In a third aspect, an embodiment of the present application provides a periodontal tissue regeneration method, including:

filling bone cement in the periodontal pocket;

disposing the medical degradable integral membrane of the second aspect on bone cement in the periodontal pocket;

teeth are implanted on the integral membrane within the periodontal pocket.

According to various embodiments of the present disclosure, a porous blank is formed by sintering a mixed powder doped with a pore-forming agent, and a membrane meeting thickness requirements is formed by processing the porous blank, wherein the powder comprises magnesium powder/magnesium alloy and a bone material, the bone material improves the strength of the membrane so as to be sufficiently applied to large-area alveolar bone absorption, and the porous structure improves the strength of the membrane on one hand and simultaneously prevents overflow of filling bone cement in a periodontal pocket; in addition, a protective ceramic coating is constructed on the surface of the membrane through a surface treatment process, so that the corrosion resistance of the integral membrane is improved; the impurities on the surface of the diaphragm are removed by an ultrasonic cleaning process, so that periodontal tissue infection is avoided.

It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application as claimed.

Detailed Description

The present disclosure will now be discussed with reference to several embodiments. It should be understood that these embodiments are discussed only in order to enable a person of ordinary skill in the art to better understand and thus practice the present disclosure, and are not meant to imply any limitation on the scope of the present disclosure.

As used herein, the term "comprising" and variants thereof are to be interpreted as meaning "including but not limited to" open-ended terms. The term "based on" is to be interpreted as "based at least in part on". The terms "embodiment" and "one embodiment" are to be interpreted as "at least one embodiment. The term "another embodiment" is to be interpreted as "at least one other embodiment". The terms "first," "second," and the like, may refer to different or the same object. Other explicit and implicit definitions are also possible below.

As described above, in the periodontal tissue regeneration treatment surgery, the film material used in the prior art cannot satisfy both the conditions of being degradable and being strong enough. The technical problem is solved by the embodiment of the disclosure, and specifically, the medical degradable integrated membrane provided by the embodiment of the disclosure mainly comprises a membrane, the membrane with the thickness of 0.05-0.1mm can be manufactured by the preparation method provided by the embodiment of the disclosure, and a plurality of micropores are formed in the membrane in an array manner, so that enough membrane strength can be still ensured under the condition of such a thin membrane thickness, and meanwhile, the micropores of the array are used for preventing filled bone cement from overflowing.

When the medical degradable integral membrane disclosed by the embodiment of the disclosure is used for periodontal tissue regeneration treatment operation, bone cement is filled in a periodontal pocket, the medical degradable integral membrane is paved in the periodontal pocket and covered on the bone cement, then implant teeth are implanted on the integral membrane in the periodontal pocket, and finally wound suturing is carried out. Over time, the integral membrane serves as a barrier to resist removal of gingival connective tissue from the implant, directing newly grown periodontal ligament cells to adhere to the implant root surface, while the integral membrane eventually is gradually degraded.

In order to prepare the medical degradable integral membrane, the thickness of the prepared integral membrane reaches 0.05-0.1mm, and the membrane also has enough strength and a microporous structure, the embodiment of the disclosure provides a novel membrane preparation method, which generally comprises the steps of powder preparation, sintering molding, processing molding, surface treatment and ultrasonic cleaning, wherein the powder preparation step is to mix inorganic bone materials with magnesium powder/magnesium alloy powder by doping pore-forming agents, the sintering molding step is to place the prepared powder into a porous blank by sintering in a sintering furnace, the porous blank is cut into a membrane by the processing molding step, the surface of the membrane is subjected to micro-arc oxidation treatment by the surface treatment step, and the surface residues of the membrane are removed by the ultrasonic cleaning step.

In one embodiment, the bone material is prepared in advance, and illustratively, a high-purity inorganic bone material is provided, the inorganic bone material is pretreated, the bone material is subjected to the pretreatment to reach the target granularity, and then the bone material and the pore-forming agent are uniformly mixed. The bone material is, for example, calcium sulfate which has degradability, the calcium sulfate powder with the particle size of 25 nanometers is obtained by pretreatment of a grinder, and the small-particle-size powder has strong bonding force, so that the strength of the membrane is improved, and the surface roughness of the membrane is reduced; the pore-forming agent is sodium chloride particles, for example.

In one embodiment, magnesium powder or magnesium alloy powder is prepared in advance, and illustratively, the magnesium powder or magnesium alloy powder is pretreated, the magnesium powder or magnesium alloy powder reaches the target granularity through pretreatment, and then the magnesium powder or magnesium alloy powder is uniformly mixed with the chisel. Wherein, the magnesium powder or magnesium alloy has degradability, so that the integrated film is taken out without secondary operation. Illustratively, in the pretreatment, magnesium powder or magnesium alloy material is ground to obtain magnesium powder with the particle size of 50 nanometers and zinc powder with the particle size of 25 nanometers, and the small-particle-size powder has strong bonding force with each other, so that the strength of the diaphragm is improved, and the surface roughness of the diaphragm is reduced.

In one embodiment, the inorganic bone material doped with the pore-forming agent may be mixed with the magnesium alloy powder doped with the pore-forming agent, or the pretreated inorganic evaluation material, magnesium powder/magnesium alloy powder, and pore-forming agent may be mixed simultaneously to prepare the powder material. For example, the magnesium powder or magnesium alloy powder can be subjected to heat treatment by adopting a vacuum tube furnace, the powder material with proper granularity is screened by adopting a vibrating screen, and the powder mixing is realized by adopting a three-dimensional mixer and a mixing ball mill.

In one embodiment, the porous blank is produced by sintering the powder using a vacuum or atmosphere protected hot press sintering furnace, and the porous blank may be plate-shaped or block-shaped. In the hot press sintering furnace, for example, a hot press temperature of 650 ℃ is set, a hot press time is maintained for 30 minutes, and a hot press pressure of 30MPa.

In one embodiment, the forming step may be accomplished by a cutting process, illustratively, by direct cutting of the porous blank into a film having a thickness of up to 0.05-0.1mm using a planing, milling or the like process.

In one embodiment, the cut-formed membrane may be surface ground to improve the surface flatness of the membrane, and exemplary grinding may employ friction stir processing to create grain surfaces by altering the microstructure of the metal and alloy surfaces to improve the surface strength of the integral membrane. The grinding may also be, for example, a surface mechanical abrasion treatment by which the surface grains of the membrane are refined to the nanometer level, thereby improving the surface strength of the membrane.

In one embodiment, the forming step may be accomplished by a cold rolling process, for example, using a rolling mill to cold roll the porous blank into a film sheet having a thickness of 0.05-0.1mm, the cold rolling process may increase the strength and toughness of the film sheet, and then modulating the overall properties of the film sheet by annealing heat treatment.

In one embodiment, the physical and mechanical properties are evaluated to ensure that the mechanical properties of the prepared integral membrane are qualified, and the mixing proportion of powder preparation can be regulated again if the evaluation is not qualified. Exemplary, the tensile strength of the integral membrane is required to reach 300-350MPa.

In one embodiment, the biocompatibility of the porous blank can be evaluated, the biocompatibility evaluation can be directly performed after the porous blank is processed and formed into a membrane, or can be performed after the surface treatment, and if the biocompatibility evaluation is unqualified, the mixing proportion of powder preparation can be regulated again, or the surface treatment process can be optimized. Exemplary biocompatibility assessments include in vitro cytotoxicity, skin sensitization, intradermal reaction, acute systemic toxicity, pyrogen test, sub-chronic systemic toxicity genotoxicity, implantation test, and the like.

In one embodiment, the surface micro-arc oxidation treatment builds a protective ceramic coating on the alloy surface, providing a thermally conductive, electrically insulating hard surface, and the ceramic coating surface also has excellent corrosion resistance, which is a property sought in biodegradable implant applications.

In one embodiment, ultrasonic cleaning employs surface plating, and materials such as aluminum, titanium, nickel or tantalum are plated on the surface of the membrane by means of electrodeposition, magnetron sputtering or the like to improve corrosion resistance and adhesion.

The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the application.

Claims (8)

1. The preparation method of the medical degradable integrated film is characterized by comprising the following steps of:

preparing powder, namely mixing inorganic bone material with magnesium powder/magnesium alloy powder by doping pore-forming agent;

sintering and molding, namely placing the prepared powder into a sintering furnace, and sintering and molding the powder into a porous blank;

machining and forming, namely cutting the porous blank into a membrane;

performing surface treatment, namely performing micro-arc oxidation treatment on the surface of the membrane;

ultrasonic cleaning to remove the residual on the surface of the membrane;

wherein the powder preparation comprises:

preparing a high-purity inorganic bone material;

pretreating the inorganic bone material to enable the inorganic bone material to reach a target granularity;

mixing the pretreated inorganic bone material with a pore-forming agent;

and the powder preparation comprises:

preparing magnesium powder/magnesium alloy powder;

pretreating the magnesium powder/magnesium alloy powder to enable the magnesium powder/magnesium alloy powder to reach a target granularity;

and mixing the pretreated magnesium powder/magnesium alloy powder with a pore-forming agent.

2. The method of manufacturing according to claim 1, wherein the forming comprises:

cutting, namely cutting the porous blank into a membrane;

and grinding, namely grinding the surface of the membrane.

3. The method of manufacturing according to claim 1, wherein the forming comprises:

cold rolling, namely placing the porous blank into a rolling mill to be cold rolled into a diaphragm;

and (3) heat treatment, and annealing heat treatment is carried out on the membrane.

4. The method according to claim 1, characterized in that after the sintering molding, the method further comprises, before the working molding:

evaluating the physical and mechanical properties of the porous blank;

and if the physical and mechanical properties are not evaluated to be qualified, re-regulating the mixing proportion of the powder preparation.

5. The method of manufacturing according to claim 1, further comprising, after the forming:

performing biocompatibility evaluation on the porous blank;

and if the biocompatibility evaluation is unqualified, re-regulating the mixing proportion of the powder preparation.

6. The method according to claim 1, characterized by further comprising, after the ultrasonic cleaning:

plating the surface of the membrane with aluminum, titanium, nickel or tantalum.

7. The method of preparing according to claim 2, wherein the grinding comprises: friction stir processing and/or surface mechanical abrasion treatment.

8. A medical degradable integral membrane for periodontal tissue regeneration, characterized by being prepared by the medical degradable integral membrane preparation method of any one of claims 1 to 7, comprising:

the membrane array forms a plurality of micropores, and the micropores are formed by the pore-forming agent;

the thickness of the membrane is 0.05-0.1mm.