CN103242550A - Method for preparing anti-infectious medical material by plasma technology - Google Patents
Method for preparing anti-infectious medical material by plasma technology Download PDFInfo
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Abstract
The invention discloses a method for preparing an anti-infectious medical material by a plasma technology. The method comprises: in a vacuum condition, firstly, immersing a medical high-molecular material in argon plasma, then injecting nitrogen plasma and silver plasma on to a medical material surface, and finally obtaining the medical high-molecular material with surface anti- infectivity. The method is simple in operation, does not affect physical and chemical structures of material noumenon, and the high-molecular material after treated, has a stable surface structure, and has a long-acting and wide spectrum anti-infectious performance.
Description
Technical field
The present invention relates to modified polymer material, relate to the method that adopts plasma technology to prepare the medical use anti-infection macromolecular material particularly.
Background technology
At present on the market or the various flexible materialss that use of hospital; comprise wound medical polymer film, burn medical polymer film etc.; they are commonly used to protect the damaged tissue position to avoid extraneous injury again, create a good microenvironment to damaged tissue, to promote the healing of wound.If these materials do not possess anti-infective performance, tend to cause the damaged tissue infection or inflammatory phenomena occurs, postpone or hinder healing or the regeneration of damaged tissue.For example, when the burn protective membrane was the polyethylene non-woven fabrics, the external world that burns except its protection of needs in the use also needed it can kill or suppress the bacterium that wound has infected not by infected by microbes, creates a good regeneration microenvironment to tissue of burn.
Current, the method of giving the film antiseptic-germicide mainly concentrates on and adds antiseptic-germicides such as silver, zinc in the bulk material, steel and manufacture method thereof as patent CN99800249.6 product having enhanced antibacterial action, it is by an amount of silver that adds in stainless steel, there are in silver particles, silver oxide and the silver-colored sulfide one or more on stainless surface in right amount, obtain the good stainless steel plate of germ resistance height and processibility and erosion resistance.If but use this method to be used for film or non-woven fabrics, can increase preparation technology's difficulty of film or non-woven fabrics, cost is higher simultaneously.Report about the material surface modifying aspect has, preparation method's (application number 200910308258.7) of people's such as Tian Xiubo slow-release type skeleton-type Ti/Cu-Zn metal level antibacterial film adopts magnetron sputtering technique to deposit slow-release type skeleton-type TiN/Cu-Zn metal level at frosting, thereby give the frosting anti-microbial property, the magnetron sputtering technique that this patent adopts forms coating on the surface, this coating is often comparatively stable at block frosting, but the film surface in softness often comes off easily, this patent is not modified the molecular structure of material and is given the material anti-microbial property simultaneously, mainly utilize zinc or copper to give the antibacterial surface performance and only obtain its anti-microbial property by additional substance at outside surface, therefore, this technology is difficult to give flexible thin-film material's durable antibacterial performance.Liu Xuan bravely waits the surface modifying method (application number 201110106021.8) of a kind of medical titanium metallic substance of people with in the ion implantation medical titanium metallic substance of silver/nitrogen binary, after this invention is injected titanium metal material with nitrogen plasma, generate titanium alloy, do not make material generate the nitrogenous organic chemistry group with anti-infective performance, injecting nitrogen plasma simultaneously mainly is in order to improve mechanical property and corrosion resistance nature, anti-microbial property and the biocompatibility requirement that can comprise anti-infection property do not have help, and anti-microbial property only derives from the injection of silver-colored plasma body.In addition, people such as Liu Xianghuai, Wang Xi improves the method for artificial cardiac valve material blood compatibility and safety in utilization, and (publication number is: CN1385142A), with the ion implantation heart valve leaflet surface of making to RESEARCH OF PYROCARBON of N+, this method has only improved the blood compatibility of material, do not solve material surface anti-infective performance and and the tissue between biocompatibility issues; People such as Zhang Yiming, Chen Yu has invented the surface modifying method of medical grade silicon rubber, and (publication number is: CN101880402A), this method is injected into silastic surface with carbon ion, reach histocompatibility by improving its surface hydrophilicity, do not solve the silastic surface infection problems; For another example, people such as Zhao Jie, Liu Qianxiang has reported and has prepared the method for silver-enriched antibacterial film at medical RESEARCH OF PYROCARBON and TiN film (publication number is: CN1827840), this method is only silver ions to be injected on RESEARCH OF PYROCARBON and the TiN film to reach antibacterial effect, RESEARCH OF PYROCARBON and TiN film belong to inorganic and metal_based material, the chemical structure on medical macromolecular materials surface is not modified in this invention, thereby improves its surface anti infection performance.
Therefore, a kind of technology need be provided, it can modify the chemical structure of medical macromolecular materials surface macromolecular chain by generating anti-infective chemical structures such as nitrogenous functional group, make macromolecular chain itself have anti-infection ability, the silver-colored plasma body of collaborative injection makes that with the anti-infective performance on the medical molecular material of further improvement surface the anti-microbial property of macromolecular material is more lasting simultaneously.
Summary of the invention
The technical problem to be solved in the present invention provides the method that adopts plasma technology to prepare the medical use anti-infection macromolecular material; This method is at first medical macromolecular materials to be immersed in cleaning material surface in the argon plasma under vacuum condition, then nitrogen plasma is injected into the medical macromolecular materials surface, finally obtains having the surface anti infection medical macromolecular materials; Present method is simple to operate, does not influence the physical chemistry structure of material body, and the polymer surface Stability Analysis of Structures that obtains after the processing has anti-infective performance long-acting, wide spectrum.
For solving the problems of the technologies described above, the invention provides the method that adopts plasma technology to prepare the medical use anti-infection macromolecular material, may further comprise the steps:
(1) be 1.0 * 10 at the sealed vacuum degree
-2～1.0 * 10
-5Under the Pa condition, medical macromolecular materials were placed argon plasma 0.001～2 hour;
(2) nitrogen plasma is injected into the medical macromolecular materials surface, reacts with macromolecular chain, generate nitrogenous functional group, obtain the medical use anti-infection macromolecular material;
Wherein, described nitrogen plasma is N
2And/or NH
3The nitrogen plasma of plasma body generation takes place;
The implantation dosage of nitrogen plasma is 1.0 * 10
15～5.0 * 10
22Ions/cm
2, injecting the degree of depth is 0.001～3 μ m.
Among the present invention, the molecular structure generation chemical reaction of nitrogen plasma and macromolecular material, generate a large amount of nitrogenous organic groups at polymer surface, these nitrogenous organic groups have anti-infective performance, make macromolecular material to growth and the breeding of bacterium restraining effect be arranged, also help the growth and breeding of cell and tissue simultaneously.
In actually operating, those skilled in the art can control the implantation dosage of nitrogen plasma and the injection degree of depth according to prior art.Because the instrument difference of using, each service data difference does not limit herein.
Usually, setting the argon flow amount that feeds is 2SCCM～40SCCM.The effect of argon plasma is the generation that helps nitrogen plasma, and argon plasma constantly bombards macromolecular material simultaneously, makes macromolecular material have more C=C key to produce, and more is conducive to the generation of nitrogen-containing functional group.Final experimental result is had promoter action to the flow of argon gas but influence is little, therefore argon flow amount do not limited.
After polymer surface injects nitrogen plasma, namely can obtain anti-infectious macromolecular material; But preferably, described step (2) also comprises silver as electrode, with silver-colored plasma body injection medical macromolecular materials surface; The implantation dosage of silver plasma body is 1.0 * 10
13～5.0 * 10
19Ions/cm
2, injecting the degree of depth is 0.001～3 μ m.Injecting the silver-colored plasma body that reinjects outside the nitrogen plasma, making the medical material surface not only to the restraining effect of growth and the breeding of bacterium, even bacterium is being had killing action.
Usually use 99.9% simple substance silver as negative electrode, described silver-colored plasma body refers to the silver-colored plasma body that 99.9% silver-colored simple substance forms.
The injection of nitrogen plasma and silver-colored plasma body order does not limit, and injects silver-colored plasma body after can injecting nitrogen plasma earlier, injects nitrogen plasma after can injecting silver-colored plasma body earlier yet, can inject nitrogen plasma and silver-colored plasma body simultaneously yet.
Described medical macromolecular materials comprise film, woven and the non-woven fabrics that polyethylene, polypropylene, tetrafluoroethylene, polyvinylidene difluoride (PVDF), polyvinyl acetate (PVA), poly(lactic acid), polyhydroxyalkanoate, polyethylene terephthalate, Mierocrystalline cellulose etc. are made.
Described anti-infection property refers to that the medical use anti-infection polymer surface reaches more than 90% the anti-infective rate of bacterium; Bacterial species comprises intestinal bacteria, streptococcus aureus, staphylococcus epidermidis, Pseudomonas aeruginosa, Candida albicans, streptococcus pneumoniae, klebsiella, blackish green coccus.
The present invention has following beneficial effect:
1, the present invention utilizes N
2And/or NH
3Plasma body injects nitrogen plasma to medical macromolecular materials, and nitrogenous organo-functional group is produced in nitrogen plasma and medical macromolecular materials surface reaction, makes material have growth and the breeding effect that suppresses bacterium.
2, the present invention also utilizes silver-colored plasma body to inject silver ions to medical macromolecular materials surfaces, not only to the restraining effect of growth and the breeding of bacterium, even to bacterium killing action is arranged, and has further improved the anti-infective performance of medical macromolecular materials.
3, the present invention is simple to operate, does not influence the physical chemistry structure of material body.
4, the medical use anti-infection polymer surface Stability Analysis of Structures that obtains after the present invention's processing has anti-infective performance long-acting, wide spectrum.
Description of drawings
The Antiinfection polyethylene non-woven fabrics that Fig. 1 makes for embodiment 1;
The growth and breeding situation map of the Antiinfection polyethylene non-woven fabrics that Fig. 2 makes for embodiment 1 and the material streptococcus aureus of handling without the inventive method;
Fig. 3 is the Antiinfection polyethylene nonwoven surface silver that utilizes the embodiment 1 of XPS to make, the depth profile that nitrogen plasma injects;
Fig. 4 is the surface chemical structure figure of the Antiinfection polyethylene non-woven fabrics that embodiment 1 is made that utilizes that XPS obtains.
Fig. 5 is grown in the growth and breeding situation of polyethylene nonwoven surface cultivation after 24 hours that embodiment 2 makes for intestinal bacteria.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further specified.
Embodiment 1
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) be that 1.0mm, size are positioned on the sample table for 5.0cm * 10.0cm medical polyethylene non-woven fabrics with thickness, as electrode, silver electrode is contained on the plasma cathode arc of plasma apparatus with 99.9% silver medal, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 1 * 10
-5During Pa, feed the argon gas of 20.0SCCM, open the radio frequency plasma body source, power is 1000W, generates argon plasma, allows the polyethylene non-woven fabrics soak in argon plasma 1 minute;
(3) argon flow amount is adjusted to 5.0SCCM, feed the nitrogen of 20.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 300 μ s, and frequency is 30Hz, voltage is-5kv, nitrogen plasma is injected the polyethylene nonwoven surface, inject the degree of depth and can reach 1.2 μ m, implantation dosage reaches 1 * 10
15Ions/cm
2The time, turn off nitrogen;
(4) keep argon flow amount 5.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 300 μ s, frequency is 30Hz, and electric current is 1.0A, and silver-colored plasma body is injected the polyethylene nonwoven surface, inject the degree of depth and can reach 1.2 μ m, the silver ions implantation dosage reaches 1 * 10
17Ions/cm
2The time, turn off cathode arc and radio-frequency plasma power supply;
(5) take out the polyethylene non-woven fabrics, obtain the Antiinfection polyethylene non-woven fabrics.
Fig. 1 is the Antiinfection polyethylene non-woven fabrics that embodiment 1 makes.
The polyethylene non-woven fabrics that embodiment 1 makes is tested, as shown in Figure 2, almost be can't see streptococcus aureus on the polyethylene non-woven fabrics that embodiment 1 makes as can be seen, it is 1 * 10 to concentration
4The antibiotic rate of the streptococcus aureus of CFU/ml is 99.9%.
Fig. 3 is the polyethylene nonwoven surface silver that utilizes the embodiment 1 of XPS to make, the depth profile that nitrogen injects; The injection degree of depth of silver, nitrogen reaches 1.2 μ m respectively as can be seen, and silver element and nitrogen element are injected into the upper layer of polyethylene non-woven fabrics, and are not only to rest on outside surface.
Fig. 4 is the surface chemical structure figure of the polyethylene non-woven fabrics that embodiment 1 is made that utilizes that XPS obtains; N-C, N ≡ C, N-C=O have been formed as can be seen on the surface of polyethylene non-woven fabrics.
Embodiment 2
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) be that 0.5mm, size are positioned on the sample table for 10.0cm * 10.0cm medical polyethylene non-woven fabrics with thickness, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 8 * 10
-4During Pa, feed the argon gas of 10.0SCCM, open the radio frequency plasma body source, power is 1000W, generates argon plasma, allows the polyethylene non-woven fabrics soak in argon plasma 50 minutes;
(3) argon flow amount is adjusted to 3.0SCCM, and the nitrogen of feeding 20.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 300 μ s, and frequency is 30Hz, voltage is-0.5kv, nitrogen plasma is injected the polyethylene nonwoven surface, inject the degree of depth and can reach 0.001 μ m, implantation dosage reaches 5 * 10
22Ions/cm
2The time, turn off nitrogen and radio-frequency plasma power supply;
(4) take out the polyethylene non-woven fabrics, obtain the Antiinfection polyethylene non-woven fabrics.
Fig. 5 is the growth and breeding situations of intestinal bacteria after the Antiinfection polyethylene nonwoven surface that embodiment 2 makes is cultivated 24 hours; From figure, can obviously find out the polyethylene non-woven fabrics quantity of the intestinal bacteria quantity on the Antiinfection polyethylene non-woven fabrics after processing before handle.
Embodiment 3
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) with thickness be the polypropylene film of 0.05mm fixedly on the treatment bench, 99.9% silver medal as electrode, is contained on the cathode arc of plasma apparatus, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 1 * 10
-3During Pa, feed the argon gas of 10.0SCCM, open the radio frequency plasma body source, power is 800W, generates argon plasma, allows polypropylene film soak in argon plasma 10 minutes;
(3) argon flow amount is adjusted to 3.0SCCM, and the nitrogen of feeding 10.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 300 μ s, and frequency is 30Hz, voltage is-20kv, nitrogen plasma is injected polypropylene film, inject the degree of depth and can reach 3 μ m, implantation dosage reaches 1 * 10
22Ions/cm
2The time, turn off nitrogen;
(4) keep argon flow amount 3.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 300 μ s, and frequency is 30Hz, and electric current is 1.0A, and silver-colored plasma body is injected polypropylene film, injects the degree of depth and can reach 3 μ m, and the silver ions implantation dosage reaches 1 * 10
19Ions/cm
2The time, turn off cathode arc and radio-frequency plasma power supply;
(5) take out polypropylene film, obtain anti-infective polypropylene film.
Embodiment 4
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) with thickness be the polyvinyl acetate (PVA) film of 0.02mm fixedly on the treatment bench, 99.9% silver medal as electrode, is contained on the cathode arc of plasma apparatus, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 5 * 10
-4During Pa, feed the argon gas of 5.0SCCM, open the radio frequency plasma body source, power is 1200W, generates argon plasma, allows the polyvinyl acetate (PVA) film soak in argon plasma 100 minutes;
(3) keep argon flow amount 5.0SCCM, feed the nitrogen of 10.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 300 μ s, and frequency is 30Hz, voltage is-2kv, nitrogen plasma is injected the polyvinyl acetate (PVA) film, inject the degree of depth and can reach 0.5 μ m, implantation dosage reaches 1 * 10
17Ions/cm
2The time, turn off nitrogen;
(4) keep argon flow amount 5.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 300 μ s, and frequency is 30Hz, and electric current is 1.0A, and silver-colored plasma body is injected the polyvinyl acetate (PVA) film, injects the degree of depth and can reach 0.5 μ m, and the silver ions implantation dosage reaches 5 * 10
19Ions/cm
2The time, turn off cathode arc and radio-frequency plasma power supply;
(5) take out the polyvinyl acetate (PVA) film, obtain anti-infective polyvinyl acetate (PVA) film.
Embodiment 5
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) with thickness be 0.05mm, size on the sample table that 10.0cm * 10.0cm poly(lactic acid) non-woven fabrics is positioned over, as electrode, silver electrode is contained on the plasma cathode arc of plasma apparatus with 99.9% silver medal, sealing equipment vacuum chamber then, and vacuumizing;
(2) when vacuum tightness be 1 * 10
-5During Pa, feed the argon gas of 10.0SCCM, open the radio frequency plasma body source, power is 1000W, generates argon plasma, allows the poly(lactic acid) non-woven fabrics soak in argon plasma 0.06 minute;
(3) argon flow amount is adjusted to 5.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 200 μ s, and frequency is 40Hz, electric current is 1.0A, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 200 μ s, and frequency is 40Hz, voltage is-30kv, the silver-colored plasma body that generates is injected the poly(lactic acid) nonwoven surface, inject the degree of depth and can reach 2 μ m, the silver ions implantation dosage reaches 1 * 10
13Ions/cm
2The time, turn off cathode arc;
(4) keep argon flow amount 5.0SCCM, feed the NH of 30.0SCCM
3, generate nitrogen plasma, nitrogen plasma is injected the poly(lactic acid) nonwoven surface, inject the degree of depth and can reach 3 μ m, implantation dosage reaches 1 * 10
20Ions/cm
2The time, turn off nitrogen and radio-frequency plasma power supply;
(5) take out the poly(lactic acid) non-woven fabrics, obtain anti-infective poly(lactic acid) non-woven fabrics.
Embodiment 6
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) be that 0.05mm, size are positioned on the sample table for 10.0cm * 10.0cm polyethylene terephthalate non-woven fabrics with thickness, with 99.9% silver medal as electrode, on the plasma cathode arc, sealing equipment vacuum chamber then, and vacuumizing;
(2) when vacuum tightness be 1 * 10
-5During Pa, feed the argon gas of 10.0SCCM, open the radio frequency plasma body source, power is 1000W, generates argon plasma, allows the polyethylene terephthalate non-woven fabrics soak in argon plasma 5 minutes;
(3) argon flow amount is adjusted to 5.0SCCM, and the nitrogen of feeding 30.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 200 μ s, and frequency is 40Hz, voltage is-30kv, nitrogen plasma is injected the polyethylene terephthalate nonwoven surface, inject the degree of depth and can reach 0.3 μ m, implantation dosage reaches 1 * 10
20Ions/cm
2The time, turn off nitrogen;
(4) keep argon flow amount 5.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 200 μ s, frequency is 40Hz, electric current is 1.0A, the silver-colored plasma body that will generate again injects the polyethylene terephthalate nonwoven surface, injects the degree of depth and can reach 0.001 μ m, and the silver ions implantation dosage reaches 1 * 10
14Ions/cm
2The time, turn off cathode arc and radio-frequency plasma power supply;
(5) take out the polyethylene terephthalate non-woven fabrics, obtain anti-infective polyethylene terephthalate non-woven fabrics.
Embodiment 7
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) be that 0.2mm, size are positioned on the sample table for 10.0cm * 10.0cm cellulosic textile fabric with thickness, as electrode, silver electrode is contained on the plasma cathode arc with 99.9% silver medal, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 8 * 10
-3During Pa, feed the argon gas of 5.0SCCM, open the radio frequency plasma body source, power is 1500W, generates argon plasma, allows cellulosic textile fabric soak in argon plasma 120 minutes;
(3) argon flow amount is adjusted to 5.0SCCM, feeds the nitrogen of 10.0SCCM, generate nitrogen plasma; Open silver-colored plasma cathode arc, the cathode arc pulsewidth is 200 μ s, frequency is 40Hz, and electric current is 1.0A, opens the pulsed negative bias on the sample table simultaneously, pulsewidth is 250 μ s, frequency is 30Hz, and voltage is-10kV that nitrogen plasma and silver-colored plasma body are injected the cellulosic textile fabric surface, inject the degree of depth and can reach 1 μ m, when the nitrogen implantation dosage reaches 5 * 10
18Ions/cm
2The time, turn off nitrogen, when the silver ions implantation dosage reaches 5 * 10
19Ions/cm
2After, turn off cathode arc and radio-frequency plasma power supply;
(4) take out this cellulosic textile fabric, obtain the plain yarn fabric of anti-infectious fiber.
Embodiment 8
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) be that the polytetrafluoroethylene film of 0.1mm is fixed on the treatment bench with thickness, 99.9% silver medal as electrode, is contained on the cathode arc of plasma apparatus, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 2 * 10
-3During Pa, feed the argon gas of 40.0SCCM, open the radio frequency plasma body source, power is 800W, generates argon plasma, allows polytetrafluoroethylene film soak in argon plasma 10 minutes;
(3) argon flow amount is adjusted to 3.0SCCM, and the nitrogen of feeding 20.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 300 μ s, and frequency is 30Hz, voltage is-20kv, nitrogen plasma is injected polytetrafluoroethylene film, inject the degree of depth and can reach 3 μ m, implantation dosage reaches 1 * 10
22Ions/cm
2The time, turn off nitrogen;
(4) keep argon flow amount 3.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 300 μ s, and frequency is 30Hz, and electric current is 1.0A, and silver-colored plasma body is injected polytetrafluoroethylene film, injects the degree of depth and can reach 1.8 μ m, and the silver ions implantation dosage reaches 1 * 10
19Ions/cm
2The time, turn off cathode arc and radio-frequency plasma power supply;
(5) take out polytetrafluoroethylene film, obtain anti-infective polytetrafluoroethylene film.
Embodiment 9
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) with thickness be the polyvinylidene difluoride (PVDF) non-woven thin-film of 0.05mm fixedly on the treatment bench, sealing equipment vacuum chamber then, and vacuumize;
(2) when vacuum tightness be 1 * 10
-2During Pa, feed the argon gas of 40.0SCCM, open the radio frequency plasma body source, power is 800W, generates argon plasma, allows polyvinylidene difluoride film soak in argon plasma 10 minutes;
(3) argon flow amount is adjusted to 3.0SCCM, and the nitrogen of feeding 20.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 300 μ s, and frequency is 30Hz, voltage is-10kv, nitrogen plasma is injected polyvinylidene difluoride film, inject the degree of depth and can reach 2 μ m, implantation dosage reaches 1 * 10
22Ions/cm
2The time, turn off nitrogen;
(4) take out polyvinylidene difluoride film, obtain anti-infective polyvinylidene difluoride film.
Embodiment 10
Adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, may further comprise the steps:
(1) be that 0.5mm, size are positioned on the sample table for 10.0cm * 10.0cm polyhydroxyalkanoate non-woven fabrics with thickness, with 99.9% silver medal as electrode, on the plasma cathode arc, sealing equipment vacuum chamber then, and vacuumizing;
(2) when vacuum tightness be 1 * 10
-5During Pa, feed the argon gas of 5.0SCCM, open the radio frequency plasma body source, power is 500W, generates argon plasma, allows the polyhydroxyalkanoate non-woven fabrics soak in argon plasma 1 minute;
(3) argon flow amount is adjusted to 5.0SCCM, and ammonia and the 15.0SCCM nitrogen of feeding 15.0SCCM, generate nitrogen plasma, open the pulsed negative bias on the sample table simultaneously, pulsewidth is 200 μ s, and frequency is 40Hz, voltage is-30kv, nitrogen plasma is injected the polyhydroxyalkanoate nonwoven surface, inject the degree of depth and can reach 3 μ m, implantation dosage reaches 1 * 10
17Ions/cm
2The time, turn off nitrogen;
(4) keep argon flow amount 5.0SCCM, open silver-colored plasma cathode arc, the cathode arc pulsewidth is 200 μ s, frequency is 40Hz, and electric current is 1.0A, and the silver-colored plasma body that will generate again injects the polyhydroxyalkanoate nonwoven surface, inject the degree of depth and can reach 1.0 μ m, the silver ions implantation dosage reaches 1 * 10
13Ions/cm
2The time, turn off cathode arc and radio-frequency plasma power supply;
(5) take out the polyhydroxyalkanoate non-woven fabrics, obtain anti-infective polyhydroxyalkanoate non-woven fabrics.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that apparent variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (3)
1. adopt plasma technology to prepare the method for medical use anti-infection macromolecular material, it is characterized in that, may further comprise the steps:
(1) be 1.0 * 10 at the sealed vacuum degree
-2～1.0 * 10
-5Under the Pa condition, medical macromolecular materials were placed argon plasma 0.001～2 hour;
(2) nitrogen plasma is injected into the medical macromolecular materials surface, reacts with macromolecular chain, generate nitrogenous functional group, obtain the medical use anti-infection macromolecular material;
Wherein, described nitrogen plasma is N
2And/or NH
3The nitrogen plasma of plasma body generation takes place;
The implantation dosage of nitrogen plasma is 1.0 * 10
15～5.0 * 10
22Ions/cm
2, injecting the degree of depth is 0.001～3 μ m.
2. employing plasma technology according to claim 1 prepares the method for medical use anti-infection macromolecular material, it is characterized in that, described step (2) comprises that also silver as electrode, injects the medical macromolecular materials surface with silver-colored plasma body; The implantation dosage of silver plasma body is 1.0 * 10
13～5.0 * 10
19Ions/cm
2, injecting the degree of depth is 0.001～3 μ m.
3. employing plasma technology according to claim 1 and 2 prepares the method for medical use anti-infection macromolecular material, it is characterized in that described medical macromolecular materials comprise film, woven and the non-woven fabrics that polyethylene, polypropylene, tetrafluoroethylene, polyvinylidene difluoride (PVDF), polyvinyl acetate (PVA), poly(lactic acid), polyhydroxyalkanoate, polyethylene terephthalate, Mierocrystalline cellulose etc. are made.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103526175A (en) * | 2013-11-06 | 2014-01-22 | 武汉科技大学 | Antibacterial hard stainless steel tool and preparation method thereof |
| CN104817711A (en) * | 2015-04-14 | 2015-08-05 | 中国人民解放军第三军医大学第二附属医院 | Antibacterial property modification method of silicone rubber |
| CN109999224A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院理化技术研究所 | A kind of antibacterial and biocompatibility bone implant material and its preparation method and application |
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| US20070050007A1 (en) * | 2005-08-18 | 2007-03-01 | Boston Scientific Scimed, Inc. | Surface modification of ePTFE and implants using the same |
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| US20070050007A1 (en) * | 2005-08-18 | 2007-03-01 | Boston Scientific Scimed, Inc. | Surface modification of ePTFE and implants using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103526175A (en) * | 2013-11-06 | 2014-01-22 | 武汉科技大学 | Antibacterial hard stainless steel tool and preparation method thereof |
| CN104817711A (en) * | 2015-04-14 | 2015-08-05 | 中国人民解放军第三军医大学第二附属医院 | Antibacterial property modification method of silicone rubber |
| CN104817711B (en) * | 2015-04-14 | 2018-03-02 | 中国人民解放军第三军医大学第二附属医院 | The antibiotic property method of modifying of silicon rubber |
| CN109999224A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院理化技术研究所 | A kind of antibacterial and biocompatibility bone implant material and its preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103242550B (en) | 2014-11-26 |
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