CN106913905B - Cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial performance and preparation method and application thereof - Google Patents
Cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial performance and preparation method and application thereof Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- 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
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- A—HUMAN NECESSITIES
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- 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
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- 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
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/606—Coatings
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- 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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/06—Coatings containing a mixture of two or more compounds
Abstract
The invention relates to a cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial performance, and a preparation method and application thereof. According to the invention, a proper amount of cerium dioxide is doped, so that the material can have good antibacterial activity. The biological coating provided by the invention has excellent biological activity and biocompatibility, and has degradation resistance and antibacterial property, solves the defect problems in the prior art, and promotes the development of the field of hard tissue repair and replacement materials.
Description
Technical Field
The invention relates to a cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial performance, a preparation method and application thereof, in particular to a cerium dioxide doped calcium silicate-based coating which is sprayed on the surface of a metal base material such as pure titanium, titanium alloy and the like by adopting a plasma spraying technology, a preparation method and application thereof, and belongs to the technical field of medical biological coatings.
Background
The main reasons for the failure of the orthopedic implant during the operation include the poor osseointegration between the implant and the adjacent bone tissue, the mismatch of mechanical properties between the implant and the surrounding bone tissue, and the infection of the implant during the operation. Wherein the infection of the implant body becomes one of the most serious problems in the orthopedic implant operation. According to literature reports, the infection rates of the implant in fracture fixation, joint replacement and femoral and knee joint repair operations reach 2%, 5% and 14% respectively, and the infection related to the implant brings great inconvenience to postoperative healing of patients. In order to prevent implant-related infections, it is desirable to provide the implant itself with anti-infective properties. Therefore, the preparation of antibacterial coatings on the surface of implant materials is receiving much attention.
Titanium, titanium alloy and the like are clinically common bone implant materials, and the calcium silicate coating prepared on the surface of the bone implant material by using a plasma spraying method can endow the bone implant material with good biocompatibility and enhance the combination between the bone implant material and bone tissues. The calcium silicate coating material shows good biological activity and biocompatibility in vitro experiments, and has higher bonding strength with a metal substrate; the coating has the capability of inducing osteogenesis in vivo animal experiments, and has stronger binding capability with surrounding bone tissues. However, the degradation speed of the coating under the erosion of physiological body fluid is too high, and the long-acting stability of the coating needs to be improved; and the coating has no antibacterial property and poor postoperative anti-infection capability.
In conclusion, the research on the biological coating which not only has excellent biological activity and biocompatibility, but also has degradation resistance and antibacterial property has profound significance for promoting the repair of hard tissues and the development of the field of replacing materials.
Disclosure of Invention
The invention aims to solve the problems of defects in the prior art and provides a biological coating which not only has excellent biological activity and biocompatibility, but also has degradation resistance and antibacterial property and a preparation method thereof.
The invention aims to provide a cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial performance, wherein the cerium dioxide doped calcium silicate coating is formed by spraying cerium dioxide doped calcium silicate-based powder on the surface of a base material through a plasma spraying technology.
The biological coating has obvious antibacterial effect on staphylococcus aureus and escherichia coliThe antibacterial rate reaches more than 99 percent; and the mass loss per unit area after being soaked in a solution equivalent to the physiological environment of a human body for 21 days is less than 5mg/cm2Has good degradation resistance and can be used as a repair and replacement material for hard tissues. The rare earth Ce ions have good antibacterial activity and strong killing effect on gram-positive bacteria and gram-negative bacteria, and the material can be endowed with good antibacterial activity by doping a proper amount of cerium dioxide. The biological coating provided by the invention has excellent biological activity and biocompatibility, and has degradation resistance and antibacterial property, solves the defect problems in the prior art, and promotes the development of the field of hard tissue repair and replacement materials.
As a preferable scheme, the mass fraction of the cerium dioxide in the cerium dioxide doped calcium silicate-based powder is 10-50%, excessive doping of the cerium dioxide can cause release of more cerium ions and easily cause cytotoxicity, and excessive doping can cause insignificant improvement of antibacterial effect and chemical stability. The powder consists of particles with the particle size of 10-200 microns, and the particles in the size range have enough fluidity, so that the particles are favorably deposited on the surface of a matrix, and the bonding strength of the coating is improved. More preferably, the mass fraction of the cerium dioxide in the cerium dioxide doped calcium silicate-based powder is 15-30%.
Preferably, the base material is pure titanium, a titanium alloy, stainless steel or a cobalt chromium molybdenum (CoCrMo) alloy. Such materials may provide better strength, toughness, and excellent processability.
Another object of the present invention is to provide a method for preparing the cerium oxide-doped calcium silicate coating, the method comprising: the method comprises the steps of taking cerium dioxide doped calcium silicate-based powder as a raw material, and spraying the raw material on the surface of a substrate subjected to surface treatment by adopting a plasma spraying technology to obtain the cerium dioxide doped calcium silicate coating.
The preparation method adopts a plasma spraying process, and the cerium dioxide doped calcium silicate-based powder is sprayed on the surface of the treated substrate to prepare the coating, so that the preparation method has the advantages of simple operation, high efficiency, good repeatability, suitability for large-scale production and the like.
As a preferable scheme, the ceria-doped calcium silicate-based powder is prepared by a solid-phase sintering method, and specifically comprises the following steps: according to the weight ratio of 10-50: 25-45: 42-75, mixing and ball-milling cerium dioxide powder, silicon dioxide powder and calcium carbonate powder, keeping the temperature of 1100-1450 ℃ for 1-3 hours to obtain mixed powder, and sieving and drying the mixed powder to obtain the cerium dioxide doped calcium silicate-based powder.
As a preferable scheme, the conditions of the plasma spraying process are as follows: the flow rate of Ar of the plasma gas is 30-50 slpm; plasma gas H2The flow rate is 6-18 slpm; the flow rate of Ar of the powder carrier gas is 1.5-5 slpm; the spraying distance is 80-330 mm; the spraying power is 30-55 kilowatts; the powder feeding rate is 8.0-30 g/min. The slpm refers to standard liters per minute. By selecting proper process conditions, the combination strength between the substrate and the coating can be improved while the bioactivity and biocompatibility of the biological coating are ensured.
Preferably, the base material is pure titanium, titanium alloy, stainless steel or cobalt-chromium-molybdenum alloy. The surface treatment of the base material is that the surface of the base material is subjected to sand blasting or sand paper polishing treatment, then is subjected to ultrasonic cleaning and drying to obtain the base material, and the pressure intensity of the sand blasting treatment is preferably 0.1-0.8 MPa. In this way, the bonding strength of the coating to the substrate can be improved.
The invention also aims to provide application of the cerium dioxide doped calcium silicate coating in preparing a repair and replacement material for hard tissues. The biological coating of the invention not only has excellent biological activity and biocompatibility, but also has degradation resistance and antibacterial property, solves the defect problems in the prior art, and promotes the development of the field of hard tissue repair and replacement materials.
Drawings
Fig. 1 is an XRD pattern of the cerium oxide-doped calcium silicate-based powder of example 1 before and after forming a coating layer, in which: the a spectrum is an XRD spectrum of the powder before the coating is formed; b is the XRD pattern of the coating after the coating is formed;
FIG. 2 is a scanning electron micrograph of the coating of example 1;
FIG. 3 is a schematic representation of the ceria-doped calcium silicate-based coating and CaSiO3Graph plotting the soaking time of the coating in Tris-HCl buffer solution versus the mass loss per unit area of the coating, in which: curve a is CaSiO3The relation curve of the soaking time of the coating in a Tris-HCl buffer solution and the mass loss of the coating in unit area; the curve b is a relation curve of the soaking time of the cerium dioxide doped calcium silicate-based coating in a Tris-HCl buffer solution and the mass loss of the coating in unit area; FIG. 4 is a graph of the antimicrobial effect of the cerium oxide doped calcium silicate based coating of example 1 on Staphylococcus aureus, where: the picture a shows visible bacteria after the bacteria react with Ti-6Al-4V for 24 hours; b photo is of visible bacteria after 24h of interaction with ceria doped calcium silicate based coating;
FIG. 5 is a graph of the antimicrobial effect of the ceria-doped calcium silicate-based coating of example 1 on E.coli. In the figure: the picture a shows visible bacteria after the bacteria react with Ti-6Al-4V for 24 hours; the b picture is the visible bacteria after 24h of interaction with the ceria-doped calcium silicate-based coating.
Detailed Description
The present invention is further described below in conjunction with the following embodiments, which are intended to illustrate and not to limit the present invention.
The invention provides a cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial performance, which is a coating formed by spraying cerium dioxide doped calcium silicate-based powder on the surface of a base material such as pure titanium, titanium alloy, stainless steel or CoCrMo alloy. The invention adopts a plasma spraying process to spray the powder on the surface of the treated base material to prepare the coating. The mass fraction of cerium dioxide in the powder is 10-50%, and the powder is composed of particles with the particle size of 10-200 microns, and the preferred particle size is 60-150 microns. The thickness of the cerium dioxide doped calcium silicate coating is dozens of micrometers to hundreds of micrometers. If the thickness of the coating is too thin, the coating is completely degraded in a short period of time, so that complete bonding of the coating to the bone tissue cannot be achieved; if the thickness of the coating is too thick, the bonding strength of the coating to the substrate is significantly reduced, and there is a risk that the coating peels off from the surface of the substrate.
The biological coating provided by the invention has excellent biological activity and biocompatibility, and has degradation resistance and antibacterial property, solves the defect problems in the prior art, and promotes the development of the field of hard tissue repair and replacement materials.
The invention also provides a preparation method of the cerium dioxide doped calcium silicate coating with good degradation resistance and antibacterial property, which is formed by spraying cerium dioxide doped calcium silicate based powder on the surface of the treated alloy base material by adopting a plasma spraying process.
In the preparation method, the plasma spraying process conditions are as follows: the flow rate of Ar of the plasma gas is 30-50 slpm; plasma gas H2The flow rate is 6-18 slpm; the flow rate of Ar of the powder carrier gas is 1.5-5 slpm; the spraying distance is 80-330 mm; the spraying power is 30-55 kW; the powder feeding rate is 8.0-30 g.min-1. The slpm refers to standard liters per minute. The plasma spraying process has the advantages of high coating deposition efficiency, controllable coating thickness, capability of preparing coatings of different shapes and convenience for industrialization.
In the invention, the cerium dioxide doped calcium silicate-based powder can be prepared by a solid-phase sintering method. As an example, for example, the ratio of 10 to 50: 25-45: 42-75, mixing cerium dioxide powder, silicon dioxide powder and calcium carbonate powder, and carrying out ball milling in a planetary ball mill, wherein the ball milling speed is 70-170 r/min, and the ball milling time is 60-180 min. And (3) keeping the temperature of 1100-1450 ℃ for 1-3 hours to obtain mixed powder, sieving the powder by using a sieve of 80-200 (for example 80), and drying at 100-120 ℃ to obtain the cerium dioxide doped calcium silicate-based powder.
The base material of the invention can be pure titanium, titanium alloy, stainless steel or CoCrMo alloy. The surface treatment of the base material is that the surface of the base material is subjected to sand blasting or sand paper polishing treatment, ultrasonic cleaning and drying to obtain the base material. The pressure intensity of the sand blasting treatment is preferably 0.1-0.8 MPa.
As proved by experiments: the inventionThe biological coating has obvious antibacterial effect on staphylococcus aureus and escherichia coli, and the antibacterial rate reaches more than 99%; and the mass loss per unit area after being soaked in a solution equivalent to the physiological environment of a human body for 21 days is less than 5mg/cm2Has good degradation resistance and can be used as a repair and replacement material for hard tissues. In addition, research finds that the compatibility of cerium oxide particles in various cell types is good, and the biological toxic effect of cerium oxide is extremely limited under the condition of reasonably controlling the particle size and the concentration.
Compared with the prior art, the invention has the following beneficial effects:
1) the biological coating provided by the invention not only has excellent biological activity and biocompatibility, but also has degradation resistance and antibacterial property;
2) the preparation method has the advantages of simple operation, high efficiency, good repeatability, suitability for large-scale production and the like.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Examples
A. Preparation of cerium dioxide doped calcium silicate based powder by solid phase reaction method
Mixing cerium dioxide powder, silicon dioxide powder, calcium carbonate powder and zirconia grinding balls according to the mass ratio of 10:45:75:260, putting the mixture into a polytetrafluoroethylene grinding tank, and carrying out ball milling in a planetary ball mill, wherein the ball milling speed is 400r/min, and the ball milling time is 300 min. Keeping the temperature of 1300 ℃ for 1 hour to obtain mixed powder, sieving the powder with a 80-mesh sieve, and drying at 100-120 ℃ for later use;
B. preparation of coatings by plasma spraying
Carrying out sand blasting or sand paper polishing treatment on the surface of pure titanium or Ti-6Al-4V alloy, carrying out ultrasonic treatment for 1-2 times in an absolute ethanol solution for 3-5 minutes each time, and then drying for 1-2 hours at 100-120 ℃ for later use; the pressure intensity of the sand blasting treatment is 0.1-0.5 MPa. Spraying the powder on the surface of the treated pure titanium or Ti-6Al-4V alloy by adopting a plasma spraying process, wherein the plasma spraying process has the following conditions: ar flow rate of plasma gas is 40slpm, and plasma gas H2The flow rate is 10slpm, the flow rate of Ar of the powder carrier gas is 3slpm, the spraying distance is 100mm, the spraying power is 40kW, and the powder feeding rate is 24 g.min-1. The slpm refers to standard liters per minute.
The XRD patterns of the ceria-doped calcium silicate-based powder and the coating shown in fig. 1 can be seen: the composition structure of the coating and the powder is not obviously changed, but the coating after spraying has partial non-crystallization phenomenon, which is caused by that part of molten phase is not crystallized in time in the process of rapid cooling.
As can be seen from FIG. 2, the coating has a rough surface topography, and the coating material with the rough surface is favorable for being combined with bone tissues in a human body.
C. Degradation resistance test of Ceria-doped calcium silicate-based coating
Mixing a ceria-doped calcium silicate-based coating with a pure phase of CaSiO3The coatings were immersed in Tris-HCl buffer solutions, respectively, and the mass loss per unit area of the coatings was compared with time.
The results are shown in FIG. 3, from which it can be seen that: day 1 of soaking, CaSiO3The mass loss of the coating per unit area reaches 4mg/cm2While the coating after doping with cerium oxide is only 0.5mg/cm2Significantly lower than the former; after being soaked for 21 days, the mass loss of the doped coating per unit area is less than 5mg/cm2And CaSiO3The coating is more than 10mg/cm2. By comparison, it can be seen that: doping ceria into the calcium silicate-based ceramic may improve the degradability of the calcium silicate-based coating.
D. Antibacterial property test of cerium oxide-doped calcium silicate-based coating
Quantitatively detecting the antibacterial property of the material by adopting a flat plate counting method: taking staphylococcus aureus and escherichia coli as strains for tests; inoculating the strain on the surface of nutrient agar, and culturing in a constant temperature box for 18 h; diluting to 2 × 10 with reference to bacteria standard turbidimetric tube8Bacteria/ml, 10-fold serial dilution to 10-2Concentration bacterial liquid; pure Ti (reference) with the thickness of 30mm multiplied by 10mm multiplied by 2mm and cerium dioxide doped calcium silicate base coating which are sterilized at high temperature are respectively dripped with 50 mul of bacterial liquid, and are stuck with a preservative film sterilized by alcohol, and the temperature is kept at 37 ℃ for 24 h. Respectively putting the samples into test tubes containing 5ml of PBS, carrying out vortex oscillation for 30s, sequentially taking 0.5ml of liquid in the test tubes, and carrying out 10 times of operation-1And 10-2Diluting, inoculating 0.2ml of each solution into nutrient agar, and culturing for 48 h.
Fig. 4 and 5 are graphs showing the antibacterial effect of the cerium dioxide doped calcium silicate-based coating on staphylococcus aureus and escherichia coli, and compared with a control piece, the sprayed coating has an obvious antibacterial effect, and the antibacterial rate reaches more than 99%.
Claims (4)
1. The preparation method of the cerium dioxide doped calcium silicate coating is characterized in that the cerium dioxide doped calcium silicate coating is formed by spraying cerium dioxide doped calcium silicate-based powder on the surface of a base material by a plasma spraying technology; the antibacterial rate of the coating to staphylococcus aureus and escherichia coli reaches more than 99%, and the preparation method comprises the following steps: the method comprises the following steps of (1) spraying cerium dioxide doped calcium silicate-based powder serving as a raw material on the surface of a base material by adopting a plasma spraying technology to obtain a cerium dioxide doped calcium silicate coating; the plasma spraying process conditions were as follows: the flow rate of Ar of the plasma gas is 30-50 slpm; plasma gas H2The flow rate is 6-18 slpm; the flow rate of Ar of the powder carrier gas is 1.5-5 slpm; the spraying distance is 80-330 mm; the spraying power is 30-55 kilowatts; the powder feeding rate is 8.0-30 g/min.
2. The method according to claim 1, wherein the ceria-doped calcium silicate-based powder comprises 10 to 50% by mass of ceria, and the powder comprises particles having a particle size of 10 to 200 μm.
3. The preparation method according to claim 2, wherein the ceria-doped calcium silicate-based powder is prepared by a solid-phase sintering method, and specifically comprises: according to the weight ratio of 10-50: 25-45: 42-75, mixing and ball-milling cerium dioxide powder, silicon dioxide powder and calcium carbonate powder, keeping the temperature of 1100-1450 ℃ for 1-3 hours to obtain mixed powder, and sieving and drying the mixed powder to obtain the cerium dioxide doped calcium silicate-based powder.
4. The method according to any one of claims 1 to 3, wherein the base material is pure titanium, a titanium alloy, stainless steel, or a cobalt-chromium-molybdenum alloy.
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| CN115029752B (en) * | 2022-06-28 | 2023-07-18 | 郑州大学 | Preparation method of composite coating suitable for bone implantation of magnesium or magnesium alloy |
| CN115558426A (en) * | 2022-09-23 | 2023-01-03 | 无锡兴华衡辉科技有限公司 | Method for grinding chip surface, suspension grinding and polishing liquid for grinding chip surface and preparation method thereof |
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