CN118064829A - Efficient antibacterial bone-promoting nano composite silicon nitride coating, preparation method and application - Google Patents
Efficient antibacterial bone-promoting nano composite silicon nitride coating, preparation method and application Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 65
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000000576 coating method Methods 0.000 title claims abstract description 63
- 239000011248 coating agent Substances 0.000 title claims abstract description 54
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 25
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000010410 layer Substances 0.000 claims abstract description 52
- 239000007943 implant Substances 0.000 claims abstract description 50
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000151 deposition Methods 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 210000000988 bone and bone Anatomy 0.000 claims abstract description 14
- 230000008021 deposition Effects 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
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- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 11
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- 238000007733 ion plating Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
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- 239000002344 surface layer Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 241000894006 Bacteria Species 0.000 claims description 2
- 230000011164 ossification Effects 0.000 abstract description 8
- 238000001727 in vivo Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 35
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 23
- 229910052719 titanium Inorganic materials 0.000 description 21
- 239000002253 acid Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 238000004381 surface treatment Methods 0.000 description 6
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- 238000005530 etching Methods 0.000 description 5
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- 238000010883 osseointegration Methods 0.000 description 4
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- 239000002609 medium Substances 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
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- 238000010603 microCT Methods 0.000 description 2
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- 230000000451 tissue damage Effects 0.000 description 2
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- 102000007469 Actins Human genes 0.000 description 1
- 108010085238 Actins Proteins 0.000 description 1
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- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 208000010392 Bone Fractures Diseases 0.000 description 1
- 206010017076 Fracture Diseases 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 229910006360 Si—O—N Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
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- 239000004053 dental implant Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
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- 239000004576 sand Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 210000003518 stress fiber Anatomy 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- PMTRSEDNJGMXLN-UHFFFAOYSA-N titanium zirconium Chemical compound [Ti].[Zr] PMTRSEDNJGMXLN-UHFFFAOYSA-N 0.000 description 1
- 210000000689 upper leg Anatomy 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
The invention discloses a high-efficiency antibacterial nano composite silicon nitride coating for promoting bones, a preparation method and application thereof, wherein an implant is taken as a matrix, and the implant comprises an ion intermixing layer, a bonding layer, a transition layer and a silicon nitride layer from bottom to top in sequence; the preparation method comprises the following steps: (1) Bombarding and cleaning the surface of the implant by using high-energy particles, and forming an ion mixing layer on the surface of the implant; (2) Depositing a bonding layer on the surface layer of the ion-mixed layer by using a magnetron sputtering ion plating deposition technology; (3) Keeping the current of the silicon target constant, and obtaining a transition layer by adjusting the flow of nitrogen and the pressure in the cavity; (4) Controlling the flow of nitrogen by using the glow intensity, and depositing to obtain a silicon nitride layer; the obtained nano composite silicon nitride coating can be applied to the field of oral implants. The coating of the invention obviously improves the osteogenesis and antibacterial performance of the implant, and provides reliable guarantee for long-term use of the implant in vivo.
Description
Technical Field
The invention relates to the field of functional coatings, in particular to a high-efficiency antibacterial nano composite silicon nitride coating for promoting bones, a preparation method and application thereof.
Background
Dental implants are a common method of dealing with the problem of missing teeth. Early osseointegration and rapid bone formation at the bone-implant interface are critical to the clinical success of the oral implant. The osseointegrative ability of the implant is related to its surface chemistry and morphology, so the osteogenic ability of the implant can be improved by surface treatment. Commercially available sand blasting and acid etching (SLA) can alter implant surface morphology, increase roughness and surface area, and enhance mechanical fixation, promote biofilm formation, and ultimately benefit osseointegration. However, high roughness presents a number of problems including bacterial attachment, soft tissue damage, cleaning difficulties, and delayed bone healing.
Compared with the commercial surface morphology modification, the surface chemical composition and structure of the implant are reasonably designed, so that not only can the bone integration of the implant be effectively enhanced, but also the antimicrobial performance of the implant can be improved. Silicon nitride is a biomedical material with excellent mechanical strength, biocompatibility and biochemical stability. Si 3N4 has excellent osteogenic and antimicrobial properties because of its own specific chemical bonding which makes its surface susceptible to the formation of hydrophilic functional groups. However, the inherent brittleness of Si 3N4 presents high fracture risk and difficulties for manufacturing and surgery. In summary, the biomedical advantages of Si 3N4 are combined with the mechanical advantages of metals, and by preparing Si 3N4 coatings on the metal surface, an advantageous approach is achieved.
Disclosure of Invention
The invention aims to: the invention aims to provide a nano composite silicon nitride coating which has high efficiency and can be used for resisting bacteria and promoting bones, and also provides a preparation method and application of the nano composite silicon nitride coating.
The technical scheme is as follows: the invention provides a high-efficiency antibacterial bone-promoting nano composite silicon nitride coating, which takes an implant as a matrix and sequentially comprises an ion-mixing layer, a bonding layer, a transition layer and a silicon nitride layer from bottom to top.
Further, the thickness of the ion-mixing layer is 10-300nm, the thickness of the bonding layer is 50-500nm, the thickness of the transition layer is 10-300nm, and the thickness of the silicon nitride layer is 500-2000nm.
The preparation method of the high-efficiency antibacterial bone-promoting nano composite silicon nitride coating comprises the following steps:
(1) Bombarding and cleaning the surface of the implant by using high-energy particles, and forming an ion mixing layer on the surface of the implant;
(2) Depositing a bonding layer on the surface layer of the ion-mixed layer by using a magnetron sputtering ion plating deposition technology;
(3) Keeping the current of the silicon target constant, and obtaining a transition layer by adjusting the flow of nitrogen and the pressure in the cavity;
(4) And controlling the flow of nitrogen by using glow intensity, and depositing to obtain a silicon nitride layer, thus obtaining the high-efficiency antibacterial bone-promoting nano composite silicon nitride coating.
Further, in the step (1), the high-energy particles are Ar and Si; the implant is made of pure titanium, titanium alloy, titanium zirconium alloy or zirconium oxide.
Further, in the step (2), the magnetron sputtering ion plating deposition technology adopts a high-purity silicon target; the bias voltage of the substrate is 60-150V in the sputtering process, and the power of the silicon target is 200-3000W; the sputtering atmosphere is a mixed gas of argon and nitrogen, and the deposition pressure is 0.1-1.0Pa; the nitrogen component in the sputtering process is controlled by a spectrometer.
Further, in the step (3), the set value of the pressure in the cavity is 0.1-1.0Pa.
Further, in the step (4), the glow intensity is used for controlling the flow rate of nitrogen, and the range of the glow intensity is 35% -75%.
The high-efficiency antibacterial bone-promoting nano composite silicon nitride coating is applied to the field of oral implants.
The principle of the invention: the method comprises the steps of firstly treating the surface of an implant, bombarding and cleaning the surface of the implant by high-energy particles to form an ion intermixing layer, then depositing silicon with a certain thickness on the surface layer of the ion intermixing layer by using a magnetron sputtering ion plating deposition technology to form a bonding layer, secondly designing and preparing a transition layer, keeping the current of a silicon target unchanged, gradually changing the pressure in a cavity by adjusting the flow of nitrogen to obtain the transition layer, finally preparing a silicon nitride layer, controlling the flow of nitrogen by glow intensity, and depositing to obtain the silicon nitride layer. Through the steps, the nano composite silicon nitride coating with excellent osteogenesis and antibacterial properties is obtained.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages:
(1) The invention improves the osseointegration and antibacterial performance of the implant by a reasonable surface treatment process so as to achieve the purposes of promoting the osteogenesis of the implant and reducing the infection risk. The magnetron sputtering ion plating deposition technology can accurately regulate and control the chemical composition and thickness of the coating, and ensure stable performance; aiming at the special requirements of the oral implant, the nano composite silicon nitride coating suitable for the oral environment is designed and prepared; can be widely applied to the oral implant, improves the osteogenesis performance of the implant, has excellent antibacterial performance, is hopeful to improve the clinical success rate in the oral implant surgery, reduces the infection risk, and brings new technical progress for the field of oral restoration.
(2) The present invention presents significant professional advantages in several respects over the currently prevailing oral implant surface treatment methods: although the traditional sand blasting and acid etching treatments achieve certain achievement in improving the surface roughness, the problems accompanying the traditional sand blasting and acid etching treatments, such as bacterial adhesion, soft tissue damage, cleaning difficulty and the like, limit the application of the traditional sand blasting and acid etching treatments in the field of oral restoration; in comparison, the invention adopts the magnetron sputtering ion plating deposition technology, can realize the accurate regulation and control of surface treatment, ensures the uniformity and consistency of the surface and improves the controllability and the reliability of the coating.
(3) The silicon nitride (Si 3N4) coating introduced by the technology has excellent osteogenic and antibacterial properties, which brings an innovative solution to the field of surface treatment of oral implants. Compared with the infection risk possibly caused by the traditional method, the antibacterial property of the silicon nitride effectively reduces bacterial attachment and provides a safer and more reliable choice for the oral cavity repair operation. In general, the present invention surpasses the current state of the art in terms of precise control of surface treatment, osteogenesis and antibacterial properties, and is expected to bring significant professional progress in the design and application of oral implants.
Drawings
FIG. 1 is a schematic illustration of a nanocomposite silicon nitride coating according to the present invention;
FIG. 2 is a graph showing the surface morphology, composition and wettability of pure titanium and silicon nitride coatings of example 1;
FIG. 3 is a fine spectrum of XPS component full spectrum (a) and Ti (b), si (c) and N (d) of pure titanium and silicon nitride coating in example 1;
FIG. 4 shows the number of gram-negative bacilli colonies on the surface of pure titanium and silicon nitride coatings after 24 hours in the medium of example 1;
FIG. 5 shows the adhesion and spreading of human bone marrow mesenchymal stem cells on the surface of pure titanium and silicon nitride coating in example 1;
FIG. 6 is a graph showing the number of Staphylococcus aureus colonies on the surface of SAL treated pure titanium samples and silicon nitride coatings after 24 hours in the medium of example 2;
FIG. 7 is an in vivo osteogenic Micro-CT and three-dimensional reconstruction of SAL treated pure titanium samples and silicon nitride coatings of example 2;
FIG. 8 is an in vivo osteogenic histological observation of SAL treated pure titanium specimens and silicon nitride coatings of example 2;
FIG. 9 shows the results of the coating bond strength test of example 2 of the present invention, (a): detecting the binding force of the silicon nitride coating by using a scratch method; (b): the Rockwell indentation method detects the coating bond strength.
Detailed Description
The invention will be further described with reference to specific examples and figures.
As shown in fig. 1, the high-efficiency antibacterial bone-promoting nano composite silicon nitride coating provided by the invention takes an implant A as a matrix, and the nano composite silicon nitride coating F sequentially comprises an ion intermixing layer B, a bonding layer C, a transition layer D and a silicon nitride layer E from bottom to top, wherein the thickness of the ion intermixing layer B is 10-300nm, the thickness of the bonding layer C is 50-500nm, the thickness of the transition layer D is 10-300nm, and the thickness of the silicon nitride layer E is 500-2000nm.
Example 1: the preparation method of the nano composite silicon nitride coating provided by the embodiment specifically comprises the following steps:
And adopting an unbalanced direct current magnetron sputtering deposition system, wherein the target material is a silicon target with the purity of 99.9 percent. A flat mirror-polished commercial pure titanium sample (. Phi.15 mm. Times.1.5 mm) was ultrasonically cleaned in ethanol for 20 minutes and then fixed on a triaxial clamp. When the bottom gas pressure was lower than 3×10 -3 Pa, the sample was etched and pre-cleaned in Ar + for 10 minutes with a substrate bias of-400V and a frequency of 250kHz to obtain an ion intermixing layer. In the subsequent deposition phase, ar was introduced at a flow rate of 40sccm to sputter the target, the deposited working pressure was 0.8Pa, and the sample was held at a bias of-60V for 4 minutes to obtain a bonding layer. The subsequent nitrogen and silicon deposition was carried out at a bias voltage of-70V, during which the direct current of the silicon target was 3A, the nitrogen gas was controlled by the glow intensity and set to 65%, and the deposition time was 180 minutes, yielding a silicon nitride composite coating having a thickness of 500 nm.
As shown in fig. 2, the silicon nitride coating (Si 3N4 -Ti) did not change its original roughness to the surface of the pure titanium (Ti) substrate, and it was known from EDS analysis to prepare silicon nitride as a silicon rich coating. From fig. 2, it can be seen that the silicon nitride coating has a significantly improved hydrophilicity compared to the original pure titanium substrate, which is advantageous for the proliferation of subsequent cells and for the osteogenesis.
As shown in FIG. 3, the surface composition of the sample was analyzed by means of X-ray photoelectron spectroscopy, two peaks at 458.4-458.7eV corresponding to characteristic Ti 2p3/2 and Ti 2p1/2 peaks of Ti 4+, and Si-O, si-N and Si-Si bonds were detected in the fine spectrum of Si 2p, respectively. In addition, the N1 s spectrum consists of Si-O-N and Si-N bonds.
Further carrying out antibacterial comparison on the pure titanium matrix and the silicon nitride coating. FIG. 4 shows the number of gram-negative bacillus colonies on the surface of pure titanium and silicon nitride coating after 24 hours in the culture medium, and the number of the colonies of the silicon nitride coating can be obviously reduced compared with that of the pure titanium matrix, which shows that the silicon nitride coating has excellent antibacterial effect.
Further comparison of in vitro cell adhesion for pure titanium substrates and silicon nitride coatings, FIG. 5 shows the adhesion and spreading of human bone marrow mesenchymal stem cells on the surface of pure titanium and silicon nitride coatings, which have a larger spreading area than pure titanium substrates and more actin stress fibers.
Example 2: the preparation method of the nano composite silicon nitride coating provided by the embodiment specifically comprises the following steps: and adopting an unbalanced direct current magnetron sputtering deposition system, wherein the target material is a silicon target with the purity of 99.9 percent. After the titanium rod is bombarded for 30s by using large-particle alumina sand grains, the titanium sheet is acid etched for 1 hour at 60 ℃ by using a mixed acid solution containing 18% hydrochloric acid and 49% sulfuric acid, and the titanium sheet is ultrasonically cleaned and sterilized to be used as a control group (SLA-Ti). And fixing the titanium rod which is not subjected to acid etching treatment on a triaxial clamp of a cavity of the magnetron sputtering equipment to prepare the silicon nitride coating. The coating preparation process parameters were the same as in example 1, and the silicon nitride coating was prepared as an experimental group (Si 3N4 -Ti).
The bonding strength of the silicon nitride coating to the titanium substrate was measured by a scratch method, and the scratch test result is shown in fig. 6 (a), wherein the maximum bonding force is 17.47±1.49N when the coating is peeled off (marked with white ellipses) according to ASTM C1624-22.
The results of detecting the bonding strength of the coating by using a Rockwell indentation method are shown as (b) in fig. 6, and the crack around the indentation and the peeling of the coating are not seen, which belong to class 0 in the ISO26443:2008 standard, and the good bonding performance between the silicon nitride coating and the titanium substrate is proved.
FIG. 7 is a graph of the comparison of the number of Staphylococcus aureus colonies on the surface of SLA-Ti samples and Si 3N4 -Ti samples after 24 hours in the medium. Compared with the SLA-Ti sample, the Si 3N4 -Ti sample with the silicon nitride coating on the surface has obviously less colony number, and has excellent antibacterial performance.
Further in vivo femur end osteogenesis performance tests were performed on SLA-Ti samples and Si 3N4 -Ti in mice, and Micro-CT and three-dimensional reconstruction are shown in FIG. 8. At 4 weeks, only a small number of bone trabeculae formed around the SLA-Ti group implant, while more bone trabeculae had been produced around the Si 3N4 -Ti implant; while at 8 weeks, the Si 3N4 group implant had now been made of a large number of bone fragments Liang Baoguo. This indicates that the Si 3N4 coating can produce faster, earlier osseointegration than SLA-Ti.
Further in vivo implant histological observations were made on SLA-Ti implants and Si 3N4 -Ti implants, as shown in FIG. 9. At 4 weeks, the new bone generated by the SLA-Ti implant has less contact with the implant and is discontinuous; in contrast, new bone produced around the Si 3N4 -Ti implant has wrapped around the implant surface and is more continuous. At 8 weeks, the SLA-Ti implant produced more and thicker bone trabeculae on the surface than at 4 weeks, and the contact with the implant was slightly increased, while the Si 3N4 -Ti peri-implant had substantially completely wrapped the implant surface, and there were a large number of newly-grown bone trabeculae around the implant, the bone trabeculae were interwoven with each other and connected into a mesh.
Claims (10)
1. The nanometer composite silicon nitride coating for promoting bone with high efficiency and bacteria resistance is characterized in that the nanometer composite silicon nitride coating (F) sequentially comprises an ion intermixing layer (B), a bonding layer (C), a transition layer (D) and a silicon nitride layer (E) from bottom to top.
2. The nanocomposite silicon nitride coating according to claim 1, wherein the thickness of the ion-intermixed layer (B) is 10-300nm.
3. Nanocomposite silicon nitride coating according to claim 1, characterized in that the thickness of the bonding layer (C) is 50-500nm.
4. Nanocomposite silicon nitride coating according to claim 1, characterized in that the thickness of the transition layer (D) is 10-300nm.
5. Nanocomposite silicon nitride coating according to claim 1, characterized in that the thickness of the silicon nitride layer (E) is 500-2000nm.
6. A method of preparing a highly effective antimicrobial bone-promoting nanocomposite silicon nitride coating according to claim 1, comprising the steps of:
(1) Bombarding and cleaning the surface of the implant (A) by using high-energy particles, and forming an ion-mixing layer (B) on the surface of the implant;
(2) Depositing a bonding layer (C) on the surface layer of the ion-mixed layer (B) by using a magnetron sputtering ion plating deposition technology;
(3) Keeping the current of the silicon target constant, and obtaining a transition layer (D) by adjusting the flow of nitrogen and the pressure in the cavity;
(4) And (3) controlling the flow of nitrogen by using glow intensity, and depositing to obtain a silicon nitride layer (E) to obtain the high-efficiency antibacterial bone-promoting nano composite silicon nitride coating (F).
7. The method of claim 6, wherein in step (2), the magnetron sputtering ion plating deposition technique employs a high purity silicon target; the bias voltage of the substrate is 60-150V in the sputtering process, and the power of the silicon target is 200-3000W; the sputtering atmosphere is a mixed gas of argon and nitrogen, and the deposition pressure is 0.1-1.0Pa; the nitrogen component in the sputtering process is controlled by a spectrometer.
8. The method according to claim 6, wherein in the step (3), the set value of the pressure in the chamber is 0.1 to 1.0Pa.
9. The method of claim 6, wherein in step (4), the glow intensity is in the range of 35% to 75%.
10. Use of the high-efficiency antimicrobial bone-promoting nanocomposite silicon nitride coating of claim 1 in the field of oral implants.
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