CN111905154B - Root canal file with antibacterial function and preparation method thereof - Google Patents

Root canal file with antibacterial function and preparation method thereof Download PDF

Info

Publication number
CN111905154B
CN111905154B CN201910378174.4A CN201910378174A CN111905154B CN 111905154 B CN111905154 B CN 111905154B CN 201910378174 A CN201910378174 A CN 201910378174A CN 111905154 B CN111905154 B CN 111905154B
Authority
CN
China
Prior art keywords
root canal
coating
sublimation
copper
magnesium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910378174.4A
Other languages
Chinese (zh)
Other versions
CN111905154A (en
Inventor
季洋
于晓明
杨柯
杨华哲
谭丽丽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Metal Research of CAS
Original Assignee
Institute of Metal Research of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Metal Research of CAS filed Critical Institute of Metal Research of CAS
Priority to CN201910378174.4A priority Critical patent/CN111905154B/en
Publication of CN111905154A publication Critical patent/CN111905154A/en
Application granted granted Critical
Publication of CN111905154B publication Critical patent/CN111905154B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L31/16—Biologically active materials, e.g. therapeutic substances
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/02—Inorganic materials
    • A61L31/022—Metals or alloys
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A61L31/082—Inorganic materials
    • A61L31/088—Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L31/148—Materials at least partially resorbable by the body
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/087—Coating with metal alloys or metal elements only
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104—Silver, e.g. silver sulfadiazine
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents

Abstract

The root canal file is made of stainless steel and titanium alloy which are clinically applied, and a thread part of the root canal file is coated with a magnesium-silver-copper coating.

Description

Root canal file with antibacterial function and preparation method thereof
Technical Field
The invention relates to a root canal file and a preparation method thereof, and particularly provides a root canal file with an antibacterial function for root canal treatment of an oral cavity.
Background
Root canal therapy is the preferred and effective method for treating endodontic and periapical diseases. In recent years, with the development of endodontic theory knowledge, treatment techniques, related applied materials and equipment, the success rate has been significantly improved, but there are many cases of failure. The main cause of failure is root canal infection. The causes of infection are mainly three: one, due to the complexity of the root canal anatomy and the diversity of microbial species, existing mechanical and chemical preparation methods have difficulty in completely eliminating the infection within the root canal; secondly, pathogenic bacteria directly spread to periapical tissues through dentinal debris or root canal preparation instruments such as root canal files which go beyond the apical foramen, causing infection; third, foreign body reaction during the root canal treatment, paper tips, cotton twigs, contaminated gutta-percha tips and food debris may fall into the root tips, causing foreign body reaction. And once infection occurs, it is difficult to control, placing additional burden on both the physician and the patient.
A root canal file is a medical instrument used for thoroughly clearing an infection source in a root canal in root canal treatment, and is a necessity for root canal treatment. The most commonly used root canal files in clinic are made of stainless steel files and nickel titanium alloys. Due to the complexity of the root canal anatomy and the diversity of microbial species, existing mechanical and chemical preparation methods have difficulty in completely eliminating the infection within the root canal. About 40% of the inner wall of the oval root canal is dead zones which cannot be reached by the root canal file, some special anatomical structures are difficult to completely clean, and the root canal disinfectant is difficult to permeate into the dead zones. In addition, the current root canal filling techniques also fail to achieve a tight seal without leakage. Therefore, microorganisms remain, multiply or re-invade in the complicated root canal system, which can cause the change of the ecological environment of the microorganisms in the root canal, and the treatment fails due to the secondary infection of the root canal.
Currently, the bactericidal action of silver ions is widely used by people, and silver can kill 650 different pathogens. Unlike antibiotics, it is effective against various bacteria, fungi/yeasts, viruses, mycoplasma, parasites, etc., without distinction. Silver has strong bactericidal capacity and is harmless to people and livestock, so more than half of airlines adopt silver to purify drinking water, and swimming pools of many countries adopt silver ion sterilization, which enters the field of electric appliances such as washing machines and the like. Silver ion sterilization will also play a great role in the medical field. The use of copper ions for sterilization has a long history. Research reports that the Ti-Cu alloy formed by adding 5% of Cu element into pure titanium has obvious sterilization function, and shows stronger anti-inflammatory action and certain biomedical function of promoting osteogenesis in an implantation experiment in an animal body.
The invention patent 201610099989.5 describes a magnesium-copper coating for bone implantation and a preparation method thereof, the magnesium-copper coating is used for bone implantation materials by combining evaporation and chemical vapor deposition, and has no requirement on the wear resistance of the coating, so that the surface of the coating is loose and the wear resistance is poor. The invention patent CN102438669A discloses a magnesium alloy coating for bone implantation, however, the content of copper is strictly controlled as impurity element, thus the copper element has no antibacterial effect. Patent CN104513922A discloses a medical metal material with antibacterial function and capable of being degraded by body fluid, however, the copper content is low (less than or equal to 3wt percent), and the antibacterial effect is questionable. Utility model patent 201420015137X has recorded a degradable magnesium alloy root canal file, though including fluorine coating in magnesium alloy root canal file main part periphery, but magnesium alloy self intensity is not enough, the function of root canal file that can't go. To the service environment of root canal file, certain wear-resisting performance need be resisted to the magnesium-based coating, needs release antibacterial element again simultaneously before the operation process finishes, therefore above-mentioned prior art all can't satisfy root canal file's requirement.
Disclosure of Invention
In order to solve the infection problem in the root canal treatment, the invention provides a root canal file with an antibacterial function and a preparation method thereof.
The technical scheme of the invention is as follows:
the root canal file with the antibacterial function is made of stainless steel and titanium alloy, and the surface of the root canal file is coated with a magnesium-copper-silver coating.
The root canal file with the antibacterial function has the advantages that the thickness of the magnesium-silver-copper coating is 0.1-200 mu m, and the mass ratio of silver to copper in the coating is as follows: 0% < Ag less than 10%, 0% < Cu less than 10% (preferably 1% < Ag less than 5%, 2% < Cu less than 7%), and the balance Mg.
The invention relates to a preparation method of a root canal file with an antibacterial function, which is characterized in that three raw materials of magnesium, silver and copper are sublimed and deposited on the surface of a substrate together by a vacuum sublimation method to form a magnesium-silver-copper coating.
The invention relates to a preparation method of a root canal file with an antibacterial function, which adopts a vacuum sublimation method, controls the deposition temperature and is a gradient structure that crystal grains are gradually reduced from the inside to the outside of a coating.
According to the preparation method of the root canal file with the antibacterial function, the vacuum sublimation method is adopted, the coating sample support is made of copper, the cooling water pipeline is arranged on the back of the coating sample support, and the coating can be rapidly cooled, so that the coating has an amorphous structure.
The invention relates to a preparation method of a root canal file with an antibacterial function, which adopts a vacuum sublimation method and controls the temperature of a sublimation source to control a coating to form a multilayer structure with different components.
The invention relates to a preparation method of a root canal file with an antibacterial function, wherein a matrix is a medical root canal file.
According to the preparation method of the root canal file with the antibacterial function, the raw materials are pure magnesium particles with purity being equal to or greater than 99.99%, pure copper particles with purity being equal to or greater than 99.99% and pure silver particles with purity being equal to or greater than 99.99%.
The invention relates to a preparation method of a root canal file with antibacterial function, wherein the vacuum degree of a vacuum sublimation method is 10- 3Pa-1Pa, the sublimation temperature of pure magnesium is 300-450 ℃, the sublimation temperature of pure copper is 950-1300 ℃, and the sublimation temperature of pure silver is 750-1050 ℃. The deposition temperature was-100 ℃ and 300 ℃.
The preparation method of the root canal scrubber comprises the following steps:
(1) ultrasonically cleaning the threaded part of the root canal file with absolute ethyl alcohol and deionized water in sequence, drying with dry nitrogen, and sending into a deposition chamber;
(2) respectively placing the raw material particles into respective sublimation furnaces, and vacuumizing to 10 DEG-5Pa, ensuring an anaerobic environment;
(3) the deposition chamber is heated to the deposition temperature, each sublimation furnace is heated to the sublimation temperature of the corresponding raw material to sublimate the raw material, the raw material is sublimated to be gaseous deposition on the surface of the root canal file according to a certain proportion, and the reaction is completed and then is cooled to the room temperature along with the furnace.
The invention has the beneficial effects that:
1. the invention provides a root canal file with an antibacterial function and a preparation method thereof. With the use of the root canal file, the magnesium-silver-copper coating naturally falls off and is kept in the root canal, thereby playing a role of long-acting intrinsic antibiosis, reducing the possibility of postoperative infection and greatly improving the success rate of the operation.
2. The method for preparing the coating can coat the magnesium-copper-silver coating with a certain thickness and a gradient structure on the surfaces of various materials, is suitable for various surfaces, does not need to carry out special treatment on the surfaces of the materials, and has wide application range.
3. The method for preparing the coating can obtain a better compact coating, thereby improving the wear resistance; magnesium and silver can play the alloying strengthening role of copper, and through regulating and controlling the surface components of the coating, the wear resistance and the shedding performance are unified, so that the root canal file scraping effect and the coating shedding antibacterial effect are matched.
4. The method for preparing the coating can obtain an amorphous surface, thereby obtaining the coating with high corrosion resistance and high wear resistance.
5. The magnesium metal coated on the surface of the root canal file has good biocompatibility. Magnesium and water can be degraded to produce a substance that is soluble in water and can be absorbed by the human body. Meanwhile, the degraded magnesium also has the function of promoting bone formation, can improve alveolar bone mass and has the function of stabilizing teeth after root canal treatment.
Drawings
Fig. 1 is a schematic structural view of a vacuum sublimation apparatus in embodiment 1.
Fig. 2 is a coated file of example 2.
Reference numerals:
1-a deposition chamber; 2-a substrate; 3-a vacuum system; 4-magnesium sublimation furnace; 5-copper sublimation furnace; 6-silver sublimation furnace; 7-magnesium-copper-silver coating.
Detailed Description
As shown in FIG. 1, the main part of the vacuum sublimation apparatus used in the method of the present invention is a deposition chamber, and the attached systems include a vacuum system. The deposition matrix is placed at the position of the matrix 2 in the figure, and the raw materials are respectively placed at the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Under the specific vacuum condition and working condition, heating magnesium, copper and silver for sublimation and depositing on the substrate. To ensure uniform coating, the substrate may be rotated in the direction indicated by the arrow.
Example 1
Will notThe stainless steel root canal file is arranged at the position of the basal body 2 in the furnace body 1 of the deposition chamber, and magnesium, copper and silver particles are respectively arranged at the positions of the magnesium sublimation furnace 4, the copper sublimation furnace 5 and the silver sublimation furnace 6. Cu content of 2%, Ag content of 1%, drawing ultimate vacuum (10)-5Pa) is added. Setting the sublimation temperatures of Mg, Cu and Ag at 300 deg.C, 950 deg.C and 750 deg.C, respectively, and the working pressure at 1 × 10-3Pa, the deposition temperature is 300 ℃, the deposition time is 30min, and the thickness of the deposited metal magnesium-silver-copper layer is 0.1 μm. To determine the osteoinductive effect of the coating, an alkaline phosphatase (ALP) test was performed, and after 1, 4, and 7 days of incubation, the coating groups were darker than the matrix groups, indicating that the coating groups had a higher alkaline phosphatase activity than the matrix groups, indicating that the coating had osteoinductive effect.
Example 2
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 3%, Ag content of 2%, and drawing ultimate vacuum (10)-5Pa) is added. Setting the sublimation temperatures of Mg, Cu and Ag at 350 deg.C, 1000 deg.C and 850 deg.C, respectively, and the working pressure at 1 × 10-2Pa, the temperature of the substrate is 200 ℃, the deposition time is 1h, and the thickness of the deposited metal magnesium-silver-copper layer is 2 mu m. The substrate was turned on and the entire substrate surface was completely coated with the coating as shown in fig. 2.
Example 3
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 5%, Ag content of 3%, drawing ultimate vacuum (10)-5Pa) is added. Setting sublimation temperatures of Mg, Cu and Ag at 380 deg.C, 1150 deg.C and 930 deg.C, respectively, and working pressure at 1 × 10-1Pa, the deposition temperature is 100 ℃, the deposition time is 2h, and the thickness of the deposited metal magnesium-silver-copper layer is 50 μm. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface. And determining that the coating is magnesium, silver and copper through X-ray diffraction analysis and scanning electron microscope energy spectrum analysis.
Example 4
The titanium alloy root canal file is arranged in the position of a basal body 2 in a furnace body 1 of a deposition chamber,magnesium, copper and silver particles are respectively placed in a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 6%, Ag content of 4%, drawing ultimate vacuum (10)-5Pa) is added. Setting the sublimation temperature of magnesium, copper and silver as 420 ℃, 1250 ℃, 1000 ℃, the working pressure as 1Pa, the deposition temperature as 50 ℃, the deposition time as 1.5h, the thickness of the deposited magnesium-silver-copper layer as 100 μm, firstly depositing silver, and then codepositing magnesium and copper. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface. And determining the coating to be a multilayer structure with an inner layer of silver and an outer layer of magnesium and copper through X-ray diffraction analysis and scanning electron microscope energy spectrum analysis.
Example 5
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 7%, Ag content of 5%, drawing ultimate vacuum (10)-5Pa) is added. Setting the sublimation temperature of magnesium, copper and silver as 450 ℃, 1300 ℃ and 1050 ℃, the working pressure as 1Pa, the deposition temperature as 50 ℃, the deposition time as 2h, and the thickness of the deposited magnesium-silver-copper layer as 150 μm. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface.
Example 6
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 7%, Ag content of 5%, drawing ultimate vacuum (10)-5Pa) is added. Setting the sublimation temperature of magnesium, copper and silver as 450 ℃, 1300 ℃ and 1050 ℃, the working pressure as 1Pa, the deposition temperature as 50 ℃, the deposition time as 2.5h, and the thickness of the deposited magnesium-silver-copper layer as 200 μm. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface.
Example 7
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 5%, Ag content of 3%, drawing ultimate vacuum (10)-5Pa) is added. Setting sublimation temperatures of magnesium, copper and silver at 410 deg.C and 1200 deg.C respectively1020 ℃, the working pressure is 1Pa, the deposition temperature is 50 ℃, the deposition time is 2h, and the thickness of the deposited metal magnesium-silver-copper layer is 180 mu m. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface.
The samples are subjected to quantitative antibacterial performance detection according to relevant standard regulations such as ' JISZ2801-2000 ' antibacterial processed product-antibacterial property test method and antibacterial effect ', GB/T2591-2003 ' antibacterial plastic antibacterial performance test method and antibacterial effect '. As a result, the sterilization rate of the sample after the action on common infectious bacteria (enterococcus faecalis) is 99%.
Example 8
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 5%, Ag content of 3%, drawing ultimate vacuum (10)-5Pa) is added. Magnesium, silver and copper are deposited in sequence, and the coating is of a three-layer structure. Setting the sublimation temperatures of Mg, Cu and Ag at 410 deg.C, 1200 deg.C and 1020 deg.C, respectively, and the working pressure at 5 × 10-1Pa, the deposition temperature is 0 ℃, the deposition time is 2h, and the thickness of the deposited metal magnesium-silver-copper layer is 100 mu m. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface.
Example 9
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 5%, Ag content of 3%, drawing ultimate vacuum (10)-5Pa) is added. Silver, magnesium and copper are deposited in sequence, and the coating is of a three-layer structure. Setting the sublimation temperature of magnesium, copper and silver as 410 deg.C, 1200 deg.C and 1020 deg.C, the working pressure as 1Pa, the deposition temperature as-50 deg.C, the deposition time as 1h, and the thickness of the deposited magnesium-silver-copper layer as 120 μm. And starting the substrate to rotate, and completely coating the coating on the whole substrate surface.
Example 10
The titanium alloy root canal file is placed in the position of a substrate 2 in a deposition chamber furnace body 1, and magnesium, copper and silver particles are respectively placed in the positions of a magnesium sublimation furnace 4, a copper sublimation furnace 5 and a silver sublimation furnace 6. Cu content of 5%, Ag content of 3%, and ultimate vacuum pumping(10-5Pa) is added. Magnesium, copper and silver are deposited in sequence, and the coating is of a three-layer structure. Setting the sublimation temperatures of Mg, Cu and Ag at 410 deg.C, 1200 deg.C and 1020 deg.C, respectively, and the working pressure at 1 × 10-1Pa, the deposition temperature is-100 ℃, the deposition time is 2h, and the thickness of the deposited magnesium-silver-copper layer is 150 mu m. XRD and XPS analysis show that the coating is amorphous.
The results of the examples show that the invention adopts the vacuum sublimation method to prepare the magnesium-copper-silver coating with bone-promoting and antibacterial effects on the surface of the root canal file. The technology can provide effective coverage of the magnesium-copper-silver coating, and can increase the content of alveolar bone while endowing the root canal file with antibacterial capability so as to improve the postoperative stability of teeth.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (4)

1. The utility model provides a root canal file with antibacterial function which characterized in that: the root canal file is made of stainless steel and titanium alloy, the surface of the root canal file is coated with a magnesium-copper-silver coating, and the content of each element in the magnesium-copper-silver coating is as follows by weight percent: ag is more than 0 percent and less than or equal to 10 percent, Cu is more than 2 percent and less than or equal to 10 percent, and the balance is Mg, and the coating is prepared by a vacuum sublimation method:
controlling the deposition temperature to enable the coating to have a gradient structure with the grains gradually decreasing from the inside to the outside;
or the coating sample support is made of copper, and the back part of the coating sample support is provided with a cooling water pipeline, so that the coating has an amorphous structure;
or controlling the temperature of the sublimation source to control the coating to form a multilayer structure with different components;
the specific process parameters are as follows: the sublimation temperature of the pure magnesium is 300-450 ℃, the sublimation temperature of the pure copper is 950-1300 ℃, and the sublimation temperature of the pure silver is 750-1050 ℃; the deposition temperature was-100 ℃ and 300 ℃.
2. The root canal file having an antibacterial function according to claim 1, wherein: the raw materials are pure magnesium particles with the purity of not less than 99.99 percent, pure copper particles with the purity of not less than 99.99 percent and pure silver particles with the purity of not less than 99.99 percent.
3. The root canal file having an antibacterial function according to claim 1, wherein: the working pressure of the vacuum sublimation method is 10-3Pa-1Pa。
4. The root canal file with antibacterial function according to claim 1, characterized by comprising the following steps:
(1) ultrasonically cleaning the threaded part of the root canal file with absolute ethyl alcohol and deionized water in sequence, drying with dry nitrogen, and sending into a deposition chamber;
(2) respectively putting the raw material particles into respective sublimation furnaces, and vacuumizing to 10 DEG-5Pa, ensuring an anaerobic environment;
(3) the deposition chamber is heated to the deposition temperature, each sublimation furnace is heated to the sublimation temperature of the corresponding raw material to sublimate the raw material, the raw material is sublimated to be gaseous deposition on the surface of the root canal file according to a certain proportion, and the reaction is completed and then is cooled to the room temperature along with the furnace.
CN201910378174.4A 2019-05-08 2019-05-08 Root canal file with antibacterial function and preparation method thereof Active CN111905154B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910378174.4A CN111905154B (en) 2019-05-08 2019-05-08 Root canal file with antibacterial function and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910378174.4A CN111905154B (en) 2019-05-08 2019-05-08 Root canal file with antibacterial function and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111905154A CN111905154A (en) 2020-11-10
CN111905154B true CN111905154B (en) 2022-03-11

Family

ID=73241946

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910378174.4A Active CN111905154B (en) 2019-05-08 2019-05-08 Root canal file with antibacterial function and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111905154B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1082625A (en) * 1992-05-19 1994-02-23 韦斯泰姆技术有限公司 The anti-microbial coating that medicine equipment is used
CN1995442A (en) * 2006-02-28 2007-07-11 姜培齐 Method for producing surface antibiotic product using physical gas phase deposition technology
EP1975132A1 (en) * 2005-12-12 2008-10-01 Qinhuangdao Yipeng Special Glass Co., Ltd Antibacterial sol-gel coating solution, method for preparing antibacterial sol-gel coating solution, antibacterial articles, and method and equipments for preparing antibacterial articles
US20120071807A1 (en) * 2010-09-16 2012-03-22 Webtec Converting, Llc. Silver-Silicone Antimicrobial Dressing
CN105420657A (en) * 2008-12-17 2016-03-23 高标国际有限公司 Anti-microbial coating and metal product containing same
CN108904893A (en) * 2018-07-24 2018-11-30 南方科技大学 A kind of composite coating and its preparation method and application having both antibacterial and biocompatibility
CN109652766A (en) * 2017-10-10 2019-04-19 中国科学院金属研究所 A kind of medical embedded material magnesium-silver-copper coating and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1082625A (en) * 1992-05-19 1994-02-23 韦斯泰姆技术有限公司 The anti-microbial coating that medicine equipment is used
EP1975132A1 (en) * 2005-12-12 2008-10-01 Qinhuangdao Yipeng Special Glass Co., Ltd Antibacterial sol-gel coating solution, method for preparing antibacterial sol-gel coating solution, antibacterial articles, and method and equipments for preparing antibacterial articles
CN1995442A (en) * 2006-02-28 2007-07-11 姜培齐 Method for producing surface antibiotic product using physical gas phase deposition technology
CN105420657A (en) * 2008-12-17 2016-03-23 高标国际有限公司 Anti-microbial coating and metal product containing same
US20120071807A1 (en) * 2010-09-16 2012-03-22 Webtec Converting, Llc. Silver-Silicone Antimicrobial Dressing
CN109652766A (en) * 2017-10-10 2019-04-19 中国科学院金属研究所 A kind of medical embedded material magnesium-silver-copper coating and preparation method thereof
CN108904893A (en) * 2018-07-24 2018-11-30 南方科技大学 A kind of composite coating and its preparation method and application having both antibacterial and biocompatibility

Also Published As

Publication number Publication date
CN111905154A (en) 2020-11-10

Similar Documents

Publication Publication Date Title
Mihailescu et al. Structural, compositional, mechanical characterization and biological assessment of bovine-derived hydroxyapatite coatings reinforced with MgF2 or MgO for implants functionalization
Zhang et al. Sr/ZnO doped titania nanotube array: an effective surface system with excellent osteoinductivity and self-antibacterial activity
CN102341132B (en) Antibacterial surface and method of fabrication
CN108853604B (en) Method for rapidly eliminating bacterial biofilm on surface of bone implant by utilizing near infrared
CN103834945B (en) A kind of titanium oxide composite coating and preparation method thereof
CN101869725B (en) Antibacterial bioactivity composite coating comprising nano Ag particles and preparation method
CN106860911A (en) A kind of surface of metal titanium antimicrobial composite coating and preparation method thereof
Huang et al. Cytocompatibility and antibacterial properties of zirconia coatings with different silver contents on titanium
CN107661544A (en) Antibacterial facilitates porous orthopaedics implant of bone complex function and preparation method thereof
CN108795289A (en) A kind of nanosizing titanium area load Si, Cu-TiO2The preparation method of antibacterial bioactivity film layer
Shimabukuro et al. Investigation of antibacterial effect of copper introduced titanium surface by electrochemical treatment against facultative anaerobic bacteria
Si et al. A heterogeneous TiO2/SrTiO3 coating on titanium alloy with excellent photocatalytic antibacterial, osteogenesis and tribocorrosion properties
CN107829123B (en) Aluminum alloy with double-layer coating on surface and preparation method and application thereof
CN101791433B (en) Molecular sieve antibacterial coating with pure titanium or titanium alloy surface and preparation method thereof
Liu et al. A study on bactericidal properties of Ag coated carbon nanotubes
CN109652769A (en) A kind of medical embedded material magnesium-silver coating and preparation method thereof
CN111905154B (en) Root canal file with antibacterial function and preparation method thereof
CN104001207A (en) Medical titanium surface composite coating and preparation method thereof
CN111020669B (en) Medical S-TiO on titanium metal surface2-xMethod for producing thin film
CN103877618B (en) A kind of method preparing argentiferous titanium deoxid film in medical titanium or titanium alloy surface
Gao et al. Plasma sprayed rutile titania-nanosilver antibacterial coatings
CN109652766B (en) Magnesium-silver-copper coating for medical implant material and preparation method thereof
CN110965024B (en) Biomedical material and preparation method thereof
CN108300897A (en) A kind of low modulus argentiferous Anti-infection medical titanium alloy
CN104878351A (en) Method for preparing titanium-silver alloy layer on surface of nickel-titanium alloy

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant