CN102380127A - Preparation method and application of antibacterial glass coating of antibacterial bone fracture plate - Google Patents
Preparation method and application of antibacterial glass coating of antibacterial bone fracture plate Download PDFInfo
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Abstract
The invention relates to a preparation method and application of an antibacterial glass coating of an antibacterial bone fracture plate. The method comprises the following steps: preparing sterile ion-containing borate bioactive glass, crushing the glass, and screening into glass powder with a certain size; adding a liquid-phase solvent, adhesive and stabilizer to the glass powder to prepare uniform glass slurry; coating the glass slurry to the surface of a titanium or titanium alloy bone fracture plate by utilizing a mechanical immersion method or a low temperature spraying method, drying with infrared ray or heat, and curing the slurry to the surface of the bone fracture plate; and volatilizing the solvent and the additives by virtue of high temperature sintering treatment, re-melting the residual glass powder to form molten glass, and adhering to the surface of the bone fracture plate to form the antibacterial glass coating capable of resisting bacteria and promoting tissue growth. The preparation method has the advantages of simple production process, easiness in operation, low cost and scale production; and the antibacterial glass coating has the functions of effective antibacterial performance and bioactivity in promotion of bone cell growth.
Description
Technical field
The invention belongs to technical field of bioengineering, be specifically related to a kind of method for preparing and application thereof of antibiotic blade plate antibiotic glass coating.
Background technology
Pure titanium and titanium alloy (Ti6Al4V) are because its excellent mechanical property and biocompatibility are used as load-bearing embedded material, for example blade plate widely.The shortcoming of this type of material is and the direct bonding of human body bone, and because the existence of v element makes it have certain toxicity.Simultaneously, be example with the blade plate, the main method of treatment fracture is at present implanted blade plate exactly, thereby carries out internal fixation of fracture.Yet there is the situation of a large amount of postoperative infection in internal fixation of fracture, and according to bibliographical information, its infection rate is about 5 % ~ 20 %.Wherein the plate nail infects serious consequences such as more can causing screw loosening, brings huge misery to sufferer.It is thus clear that, be example with present blade plate, there is obvious defects in the implantation equipment of many types.They do not have antibiotic property usually, need the oral antibiotic medicine, and effect is not good enough.Therefore, people press for its improvement.
The present invention be based upon on the basis of existing antibiotic borate antibacterial glass coating (number of patent application: 201010209082.2, the date of application: 2010.06.24), carried out thematic in-depth, made it to be more suitable for large-scale production.A kind of method for preparing of borate antibacterial glass coating of biologically active has been described in this patent application.Wherein describe this composition and antibiotic ionic kind and the content that contains the borate glass of antibiotic ionic biologically active in detail; Provide the method for preparing of three kinds of antibacterial glass coatings, be respectively sedimentation, spraying process and czochralski method; Antimicrobial coating has been carried out cell experiment and zoopery, and the result shows that this antibiotic bioactive borate glass has good antibacterial property and the performance that stimulates the osteocyte growth.In order to satisfy large-scale production; The present invention confirms as titanium or titanium alloy with the base material of coating; And to czochralski method in the above-mentioned patent and spraying process, done necessary replenishing and innovation, be suitable for the production with scale with activation; Formed main contents of the present invention thus, necessary fully technological parameter required in actual production is provided.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing and application thereof of antibiotic blade plate antibiotic glass coating of ability large-scale production biologically active.
The method for preparing of the antibiotic blade plate antibiotic glass coating that the present invention proposes, concrete steps are following:
(1) preparation of glass powder
In borosilicate glass, add and contain antibiotic ionic salt, after ground and mixed is even, adopt high-temperature melting method to make glass blocks; Again gained is contained antibiotic ionic glass blocks quenching, pulverize, screening obtains the glass powder that particle diameter is 0.05-50 μ m; The glass network former of said borosilicate glass is by B
2O
3, do not contain or contain on a small quantity SiO
2/ or contain P
2O
5Form, wherein B
2O
3Content is greater than SiO
2Or P
2O
5Content, the sum of the molar ratio of glass network former, accounting for glass composition total amount is 30-90mol%; Network outer body contains CaO, and also contains Na
2O, K
2O alkali metal oxide and MgO, the SrO alkaline earth oxide; It is 5-80mol% that total molar ratio of network-modifying ion oxide accounts for glass composition total amount; The 0.l wt%-15 wt% that antibiotic ionic addition is the borate glass quality;
(2) glass paste preparation
Annex solution phase solvent, binding agent and stabilizing agent in the glass powder of gained in step (1) are processed uniform glass paste, and gained glass paste viscosity is 10
0-10
4DPa
S; The addition of liquid phase solvent is 1-4 mL in every gram glass powder; The mass ratio of glass powder and binding agent is 1:0.001-1:0.05; The mass ratio of glass powder and stabilizing agent is 1:0.01-1:0.5;
(3) blade plate pretreatment
Before applying blade plate is cleaned through ultrasonic water successively, alkaline solution soaks, deionized water rinsing;
(4) coating of antibiotic glass coating and sintering
(a) pretreated blade plate in the step (3) is immersed in the glass paste that obtains in the step (2), adopts mechanical driving device, regulate the speed that lifts, lift blade plate, glass paste is coated in the surface of pure blade plate with certain speed;
Perhaps (b) is with the glass slip of the preparation in the step (2); Be filled into by in the mechanical hand-guided low temperature gas spray gun charging basket; Under the certain pressure of compressed air, certain air-flow to step (3) in pretreated blade plate; Carry out the cold nebulization slip and apply, make blade plate surface coverage one deck glass paste;
Blade plate through after step (a) or the step (b) gets into delivery track successively; Through infrared lamp arrangement drying baker is dry continuously, get into tunnel type Muffle furnace kiln then, carry out the high temperature sintering heat treatment; The glass dust that is positioned at titanium alloy blade plate surface is by remelting; Be tiled on the metal surface, the cooling back forms the antibiotic glass coating, and the thickness of antibiotic glass coating is the 2-50 micron; The said rate of pulling is 0.5-25 mm/s; The injection temperation of described low temperature gas spray gun is 10-35 ℃; Described compressed-air actuated pressure is 0.05-1.0 MPs; Described compressed air require is 30-550 L/min; Said infrared drying temperature is 50-90 ℃, time 2-10 min; Said high-temperature heat treatment temperature is 600-800 ℃, time 2-30 min;
Wherein: said blade plate be in pure titanium bone plate, titanium alloy blade plate, orthopaedics steel blade plate, niobium titanium alloy blade plate or the niobium tantalum alloy blade plate any.
Among the present invention, the said antibiotic ion of step (1) is an one to multiple kind in silver ion, copper ion or the zinc ion.
Among the present invention, the high-temperature fusion temperature is 1000-1350 ℃ described in the step (1), and the time is 0.5-8 hour.
Among the present invention, contain antibiotic ionic glass blocks in the step (1) and pulverize, in small, broken bits through the coarse crushing of horizontal type ball mill, ball milling successively, pulverize through jet mill again, the vibrosieve sub-sieve, obtaining grain size is the granule of 0.05-50 μ m.
Among the present invention, liquid phase solvent is deionized water or dehydrated alcohol described in the step (2), and said binding agent is carboxymethyl cellulose or carboxymethyl starch sodium, and said stabilizing agent is a bentonite.
Among the present invention, ultrasonic water scavenging period is 10-30 min in the step (3), and used alkaline solution is that concentration is the NaOH solution of 5 mol/L, and the NaOH solution soaking time is 5-10 min.
Among the present invention, the bond strength of the antibacterial glass coating that obtains and titanium alloy blade plate be 8-14 MPa.
The antibacterial glass coating of gained of the present invention obtains fixedly the time to use at repair of bone fractures, the fixing position of the injury of the bone, and can suppress growing of antibacterial, and can be antibiotic, can also promote the growth of osteocyte.
The whole coating of the present invention, drying and heat treatment process are accomplished on circular pipeline; Can be through the viscosity and the rate of pulling of glass paste; Perhaps the pressure of gas and flow and spray time are regulated the thickness of gained coating in the cold nebulization, thereby regulate antibiotic ionic content in the coating.Regulate the bond strength of gained coating and implantation equipment through heat treated temperature and time.Regulate antibiotic ionic rate of release in the gained coating through the composition of sterilize ionic incorporation or glass carrier, thus biological activity and the antibiotic cycle and the effect of the coating of regulating.Through the composition of glass dust, the ratio of various oxides can be regulated the biological activity and the biological degradability of antibacterial glass coating, and to the stimulation of osteocyte growth.
The present invention adopts the method for ion antibacterial, in conjunction with traditional implantation equipment excellent mechanical property and good biological activity and the special construction of borate glass, and antibiotic ion; Silver ion for example, its antimicrobial efficiency is high, little to human harm, the advantage of has a broad antifungal spectrum, and process equipment is simple; Operation is with low cost easily, can effectively reduce in the operation by bacterial disease; Be applied to bone simultaneously and repair on the implant, tangible promotion osteocyte growth effect is arranged.
Description of drawings
Fig. 1 scribbles the blade plate sketch map of antimicrobial coating: a) front view; B) side view.
The SEM figure of Fig. 2 coating and substrate bonded face.
Fig. 3 scribbles the surperficial XRD spectrum of borate antibacterial glass coating blade plate.
The zinc ion release profiles of Fig. 4 Different Zinc content borate antibacterial glass coating.
The Micro-CT sheet that Fig. 5 silver ion blade plate is drawn materials after 6 weeks is in vivo observed: a) simple titanium plate; B) BG coated titanium plate; C) BG-0.5Ag coated titanium plate; D) BG-1Ag coated titanium plate.
Label among the figure: 1 is the blade plate substrate, and 2 is antibacterial glass coating.
The specific embodiment
Further specify the present invention through embodiment below.
Embodiment 1: the preparation and the vitro characterization of cupric borate antibacterial glass blade plate coating
(1) preparation of the borate glass of copper content 0.25%
Take by weighing the 1.888g natrium carbonicum calcinatum, 12.311g Anhydrous potassium carbonate, 6.921g basic magnesium carbonate, 10.698g calcium carbonate, 13.149g strontium carbonate, 9.632g silicon dioxide, 39.652g boric acid, 5.558g sodium dihydrogen phosphate, 0.192g copper sulfate.After the grinding, fully mix, obtain original ingredient.Original ingredient as for insulation 120 min in inherent 1150 ℃ of the platinum crucible, is poured on the fining glass liquid of gained on the steel plate of preheating after the taking-up and obtains glass blocks.The gained glass blocks is in small, broken bits through the coarse crushing of horizontal type ball mill, ball milling successively, to pulverize through jet mill again, the vibrosieve sub-sieve obtains the glass powder of particle diameter at the 0.05-20 micron.
(2) preparation of coating
Measure the 100ml deionized water as in the 200ml plastic containers, put into agitator, the beginning mechanical agitation; When stirring, add 0.15g sodium carboxymethyl cellulose, resulting glass powder in 1.5g bentonite and the 150g step (1) successively; Then mechanical agitation/ultra-sonic dispersion/mechanical agitation hockets, and each 20min forms the uniform sizing material with certain viscosity.The pure titanium bone plate that will pass through after ultrasonic cleaning and the saturated NaOH solution-treated (each 10min) is immersed in the glass paste that step (2) obtains with the fine rule suspension, adopts mechanical driving device, regulates the speed that lifts; To carry on the 0.5mm/s speed; To apply the blade plate of slurry then, be suspended on the delivery track, get into 50 ℃ of infrared drying oven inner drying 5min that continuous infrared lamp is arranged; Again by delivery track; Get into tunnel type Muffle furnace kiln, 600 ℃ of flat-temperature zone operation 2min in Muffle furnace are behind the cooling area through the Muffle furnace kiln; Take tunnel type Muffle furnace kiln out of by delivery track, the antibiotic glass coating that obtains being evenly distributed behind the quenching is wrapped in titanium alloy blade plate surface (see figure 1).
(3) coating physical property
Choose suitable position, the blade plate of applying coating is therefrom sawed-off, choose cross section then, through scanning electron microscope (Scanning Electron Microscopy, SEM, Hitachi S2360N, Tokyo Japan) carries out pattern to it and characterizes.The result shows: the thickness of coating～20 micron, and the structure of antibacterial glass coating is tight, and thickness is even, does not have tangible interface between blade plate and the antibacterial glass coating, has inter-level diffusion to take place, and good transition (see figure 2) is arranged between the two.
With XRD (X-ray Diffraction, Rigaku, D/max 2550VB3+/PC, USA) crystalline phase to face coat characterizes.The result shows: the XRD figure spectrum is shown as the steamed bread peak, and the thing of institute's applying coating is the glassy state (see figure 3) mutually.
With the mechanical property of stretching experiment testing coating, test is produced on the Z150 type stretching-machine in moral and is carried out.Adopting polyacrylic resin glue is r garden shape faying face with the radius, coating sample is bonded on the handle of 2 customizations.Draw speed 1mm/min carries out along with tensile, and pulling force constantly rises and takes place until coating stripping.Peel strength can be calculated as follows and obtain:
Wherein:
is peel strength (MPa); F is the maximum pull value (N) in the extension test; R is that radius (mm) is closed in sample and polyacrylic resin gluing.
Experimental result: coating has higher binding strength, and the coating of mensuration and the adhesion of blade plate are 11.0 MPa.
Embodiment 2: contain antibiotic ionic release of zinc-borate glass antimicrobial coating and anti-microbial property
According to embodiment 1 described method; In glass formula; Change copper sulfate into zinc sulfate; Add 0.472g, 0.944g, 1.416g, 1.888g zinc sulfate respectively, make three kinds of borate glasses that zinc content is different respectively, and and then to make the zinc ion mass percent be 0.5%, 1.0%, 1.5%, 2.0% the blade plate that contains the zinc-borate glass antimicrobial coating.
With the coating block for preparing respectively with every 1cm
2The ratio of the corresponding 100 ml solution of surface area be soaked in the SBF solution (the Kokubo method pH=7.25), places 37 ℃ of calorstats, at 1d, 2d, 4d takes out sample behind the 7d.Through inductive coupling plasma emission spectrograph (inductively coupled plasma optical emission spectroscopy, ICP-OES, Optima 2100DV; PerkinElmer, Shelton CT) detects the zinc ion concentration in the soak.Time to soak is abscissa, and the concentration of zinc ion is that vertical coordinate is drawn a diagram.
The result shows that the zinc ion release profiles of Different Zinc content has shapes similar, but the initial high more glass blocks of zinc content, and the zinc ion concentration of its release is high more.Every kind of sheet glass all has zinc ion rate of release faster in 48 hours of beginning most, in the subsequent time, slow down gradually then.The concentration of silver ions that its accumulative total of (0.5,1.0,1.5,2.0 wt %) borate glass of four kinds of zinc content discharges has all reached the concentration (least concentration of Zn ion bacteria growing inhibiting is 0.2-0.3 μ g/mL) that can suppress most bacterial growths.The relation of the initial nearly direct ratio of zinc content in the concentration of zinc ion releasing and the glass, the visible zinc ion concentration (see figure 4) that can come adjustment release through the content of regulating zinc in the initial glass.
With antibiotic glass coating block (5 * 5 * 2mm that makes
3) be immersed in 75% the ethanol 24 hours respectively, use the deionized water clean surface afterwards 3 times.Then according to 1.25 cm
2The ratio of the corresponding 1 mL solution of surface area, these coating blocks are immersed in DMEM, and (the Eagle culture medium by the Dulbecco improvement contains identical nutritional labeling with MEM; But concentration exceeds 2 ~ 4 times; Be applied to the fast cell of growth) or α-MEM (alpha type Eagle culture medium is compared with DMEM, and its nutritional labeling is more) in; Be stored in the calorstat (37 ℃, 5% CO
2).After 24 hours, the glass blocks in the culture medium is removed, to the hyclone (FBS) that wherein replenishes 10 %, the streptomycin sulfate of the mycillin of 100 U/mL and 100 μ g/mL has obtained the coating block lixiviating solution simultaneously.
Other puts escherichia coli ATCC25922, and staphylococcus aureus ATCC25923 commentaries on classics before test is planted on blood agar plate, hatches 18h for 35 ℃, and difference picking escherichia coli and a staphylococcus aureus 2-3 bacterium colony are in meat soup on blood plate then, and 35 ℃ of ovum are educated 2h.Get a certain amount of bacterium liquid with micro sample adding appliance and add successively by low concentration in the lixiviating solution of high concentration arrangement, the result observes, and the minimum lixiviating solution concentration of no naked eyes visible growth is its bacteriostasis property to this bacterium (MIC).A certain amount of bacterium liquid of dilution by a certain percentage is inoculated on 2 blood plates, is coated with 35 ℃ and hatches 18h.Calculate the bacterium colony number on the blood plate, take the mean and calculate initial inoculation bacterium amount.0.1% the minimum lixiviating solution concentration that the bacterium colony number is lower than initial inoculation bacterium amount is its (going out) bacterium ability (MBC) of killing to this bacterium.
The result shows, the bacteriostasis property of the antimicrobial coating of antibiotic borate glass is stronger than the parent glass ability of sterilizing, and do not mix that zinc or zinc content are less not to have antibacterial ability basically.The coating of zinc content 2% is all relatively good to the antibacterial and bactericidal effect of escherichia coli and staphylococcus aureus, and zinc content 1% and 1.5% coating are apparent in view to colibacillary fungistatic effect, but just weaker to the killing effect of staphylococcus aureus.Along with the increase of zinc content, sterilization effect significantly increases (seeing table 1).
The sterilization effect of the different zinc content borate antibacterial glass coatings of table 1
Embodiment 3: the antibacterial action in animal body of argentiferous borate antibacterial glass coating and stimulation of bone growth performance
According to embodiment 1 described method; In glass formula; Change copper sulfate into silver sulfate; Add 0g, 0.269g, 0.595g silver sulfate respectively, make three kinds of borate glasses that silver content is different respectively, and and then make the blade plate that the silver ion mass percent is 0.0%, 0.5%, 1.0% argentiferous borate antibacterial glass coating.
Use simple titanium bone plate (not being coated with glass), the antimicrobial coating blade plate of the antibiotic borate glass of argentiferous (BG coated titanium plate) and argentiferous 0.5% (BG-0.5Ag coated titanium plate), 1.0% (BG-1Ag coated titanium plate) does not carry out interior animal experiment.Laboratory animal is a new zealand white rabbit, and body weight is 2 ~ 3kg, and each organizes used laboratory animal quantity is 10.With animal weigh the back, anesthesia after.With the tibial tubercle is starting point, before tibia outside the long otch of side-draw 3cm, successively separate; Cut periosteum; Appear cortical bone, at the local sawed-off tibia apart from tibial tubercle 0.5cm, fibula is not sawed-off; Carry out the reduction of the fracture then, and with the 5 hole 2.0cm fixing fracture end of titanium plate and 4 pieces of 2.0mm screws of applying coating.Sew up the incision and inject the bacterium liquid that 0.1mL contains staphylococcus aureus (ATCC25923) at the fracture of tibia end.Postoperative continues single cage raises, and puts to death animal through the excessive pentobarbital sodium of intravenous injection after 6 weeks.
Laboratory animal is carried out the Micro-CT image analysis: postoperative is after 6 weeks; Choose representative Micro-CT sheet (see figure 5) in each treatment group, as can be seen from the figure simple titanium plate treatment group and BG coated titanium plate treatment group, it is low that bone connects degree; Stable inadequately, the osteolysis situation is serious.BG-0. 5Ag coated titanium plate treatment group is compared to preceding two groups, and bone connects, skeletal stability all gets a promotion, and the osteolysis situation reduces.BG-1Ag coated titanium plate treatment group, osteogenesis in order.Explain that argentiferous antibacterial glass coating has anti-microbial property in good stimulation of bone growth performance and the body.
Microbiology index-antibacterial culturing and identification of strains: 6 weeks of postoperative are when drawing materials; Take out fracture end titanium panel area tissue or pus, collect rapidly in the sterile test tube, deliver to microbial room; At first sample is seeded on the blood agar plate; Hatch 24 h at 37 ℃ of calorstats, then same lot sample originally is inoculated in the brain-heart infusion medium simultaneously, hatched 7 days at 37 ℃ of calorstats.The bacterial clump of turning out is carried out the experiment of coagulase tube, and adopt full automatic microorganism evaluation/antibiotics susceptibility test system that the antibacterial of turning out is carried out identification of strains.
The result shows: simple 10 rabbit secretions of titanium plate treatment group are all turned out antibacterial, and verified be staphylococcus aureus; There is the secretions of 8 rabbits to turn out antibacterial in 10 rabbits of BG coated titanium plate treatment group, and turns out to be staphylococcus aureus through the blue Albert'stain Albert of G; There is the secretions of 3 rabbits to turn out antibacterial in 10 rabbits of BG-0.5Ag coated titanium plate treatment group, and turns out to be staphylococcus aureus through the blue Albert'stain Albert of G; All do not turn out bacterial growth (seeing table 2) in the secretions of 10 rabbits of BG-1Ag coated titanium plate treatment group.Explain that argentiferous antibacterial glass coating has anti-microbial property in the good body, and along with the increase of silver content, antibiotic new can being strengthened.
The antimicrobial coating blade plate of the different silver content borate glasses of table 2 is antibacterial effect in animal body
| Experimental group | Infect quantity | Do not infect quantity |
| Simple titanium plate | 10 | 0 |
| BG coated titanium plate | 8 | 2 |
| BG-0.5Ag coated titanium plate | 3 | 7 |
| BG-1Ag |
0 | 10 |
The above-mentioned description to embodiment is can understand and use the present invention for ease of the those of ordinary skill of this technical field.The personnel of skilled obviously can easily make various modifications to these embodiment; And a General Principle in this explanation is applied among other embodiment; For example can use the same method antibiotic outstanding being coated on the orthopedic steel plate; On the niobium titanium alloy blade plate, on the niobium tantalum alloy blade plate, and needn't pass through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (7)
1. the method for preparing of an antibiotic blade plate antibiotic glass coating is characterized in that concrete steps are following:
(1) preparation of glass powder
In borosilicate glass, add and contain antibiotic ionic salt, after ground and mixed is even, adopt high-temperature melting method to make glass blocks; Again gained is contained antibiotic ionic glass blocks quenching, pulverize, screening obtains the glass powder that particle diameter is 0.05-50 μ m; The glass network former of said borosilicate glass is by B
2O
3, do not contain or contain on a small quantity SiO
2/ or contain P
2O
5Form, wherein B
2O
3Content is greater than SiO
2Or P
2O
5Content, the sum of the molar ratio of glass network former, accounting for glass composition total amount is 30-90mol%; Network outer body contains CaO, and also contains Na
2O, K
2O alkali metal oxide and MgO, the SrO alkaline earth oxide; It is 5-80mol% that total molar ratio of network-modifying ion oxide accounts for glass composition total amount; The 0.l wt%-15 wt% that antibiotic ionic addition is the borate glass quality;
(2) glass paste preparation
Annex solution phase solvent, binding agent and stabilizing agent in the glass powder of gained in step (1) are processed uniform glass paste, and gained glass paste viscosity is 10
0-10
4DPa
S; The addition of liquid phase solvent is 1-4 mL in every gram glass powder; The mass ratio of glass powder and binding agent is 1:0.001-1:0.05; The mass ratio of glass powder and stabilizing agent is 1:0.01-1:0.5;
(3) blade plate pretreatment
Before applying blade plate is cleaned through ultrasonic water successively, alkaline solution soaks, deionized water rinsing;
(4) coating of antibiotic glass coating and sintering
(a) pretreated blade plate in the step (3) is immersed in the glass paste that obtains in the step (2), adopts mechanical driving device, regulate the speed that lifts, lift blade plate or bone screw, glass paste is coated in the surface of blade plate with certain speed;
Perhaps (b) is with the glass slip of the preparation in the step (2); Be filled into by in the mechanical hand-guided low temperature gas spray gun; Under the certain pressure of compressed air, certain air-flow to step (3) in pretreated blade plate; The slip of spraying applies, and makes blade plate surface coverage one deck glass paste;
Blade plate through after step (a) or the step (b) gets into delivery track successively; Through infrared lamp arrangement drying baker is dry continuously, get into tunnel type Muffle furnace kiln then, carry out the high temperature sintering heat treatment; The glass dust that is positioned at titanium alloy blade plate surface is by remelting; Be tiled on the metal surface, the cooling back forms the antibiotic glass coating, and the thickness of antibiotic glass coating is the 2-50 micron; The said rate of pulling is 0.5-25 mm/s; The injection temperation of described low temperature gas spray gun is 10-35 ℃; Described compressed-air actuated pressure is 0.05-1.0 MPs; Described compressed air require is 30-550 L/min; Said infrared drying temperature is 50-90 ℃, time 2-10 min; Said high-temperature heat treatment temperature is 500-800 ℃, time 2-30 min;
Wherein: said blade plate be in pure titanium bone plate, titanium alloy blade plate, orthopaedics steel blade plate, niobium titanium alloy blade plate or the niobium tantalum alloy blade plate any.
2. method for preparing according to claim 1 is characterized in that the said antibiotic ion of step (1) is an one to multiple kind in silver ion, copper ion or the zinc ion.
3. method for preparing according to claim 1 is characterized in that the high-temperature fusion temperature is 1000-1350 ℃ described in the step (1), and the time is 0.5-8 hour.
4. method for preparing according to claim 1; It is characterized in that containing in the step (1) antibiotic ionic glass blocks pulverize, in small, broken bits through the coarse crushing of horizontal type ball mill, ball milling successively; Pulverize through jet mill again, the vibrosieve sub-sieve, obtaining grain size is the granule of 0.05-50 μ m.
5. method for preparing according to claim 1 is characterized in that liquid phase solvent is deionized water or dehydrated alcohol described in the step (2), and said binding agent is carboxymethyl cellulose or carboxymethyl starch sodium, and said stabilizing agent is a bentonite.
6. method for preparing according to claim 1 is characterized in that ultrasonic water scavenging period is 10-30 min in the step (3), and used alkaline solution is that concentration is the NaOH solution of 5 mol/L, and the NaOH solution soaking time is 5-10 min.
7. the application of antibacterial glass coating as claimed in claim 1 in repair of bone fractures is fixing.
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| US11039620B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
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