CN112048906A - Antibacterial silver-containing fiber with excellent biocompatibility and preparation method thereof - Google Patents
Antibacterial silver-containing fiber with excellent biocompatibility and preparation method thereof Download PDFInfo
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- CN112048906A CN112048906A CN201911232133.0A CN201911232133A CN112048906A CN 112048906 A CN112048906 A CN 112048906A CN 201911232133 A CN201911232133 A CN 201911232133A CN 112048906 A CN112048906 A CN 112048906A
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
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Abstract
The invention relates to a preparation method of an antibacterial silver-containing fiber with excellent biocompatibility, which comprises the following steps: (1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt; (2) mounting the pretreated seaweed filament bundle on a feeding roller for magnetron sputtering; (3) and closing the vacuum sputtering coating chamber and vacuumizing. (4) And introducing gas, starting a processing power supply and a target table power supply, and processing the alginate fiber filaments to obtain the antibacterial silver-containing fiber with excellent biocompatibility. The fiber is treated, so that the structure on the surface of the fiber has certain flowing property, the deposition and the attachment of silver atoms are facilitated, the working efficiency is greatly improved, and the production cost is reduced.
Description
Technical Field
The invention belongs to the field of textile materials, and particularly relates to an antibacterial silver-containing fiber with excellent biocompatibility and a preparation method thereof.
Background
Common medical auxiliary material includes fabrics such as gauze, medical sponge, common medical auxiliary material uses the cellulose material preparation mostly among the prior art to form, but the cellulose material is owing to lack certain bacterinertness, and self defects such as hygroscopicity is not good and be difficult to degradation nature, make it as medical dressing in-process, need regular change, and do not have obvious promotion effect to wound healing, and in medical dressing change-process, cause wound secondary damage to patient's wound easily, especially, the wound area is great, like patient such as burn, the change of medical dressing can cause huge injury to the wounded.
In the prior art, researches on antibacterial materials are increasingly paid attention, for example, in 'preparation and performance research of antibacterial alginate fiber' of a master thesis of Liangpeng, the antibacterial alginate fiber is prepared by adding nano silver particles into a sodium alginate spinning solution, and the fiber has excellent antibacterial performance and can be used as a medical auxiliary material; the master thesis of Zhaoxihui 'alginate in-situ preparation of nano silver/alginate fiber and performance thereof' discloses that nano silver/alginate fiber is obtained by hydrothermal and microwave heating methods through in-situ polymerization on the surface of alginate fiber, and the fiber has excellent antibacterial performance and can be used as biomedical materials. However, the addition of nano silver particles into the spinning solution has the technical problems of high cost, low durability of antibacterial performance, broken filaments in spinning and the like, which are only obtained by the spinning process and are difficult to overcome, and for the in-situ polymerization method, the hydrothermal reaction conditions are relatively severe, and the treatment solution contains various particles, which can bring great damage to the mechanical properties of the fibers.
The magnetron sputtering technique is to use metal as a target, use high-energy particles to impact the target, bombard the target by the principle, and deposit atoms on a base material under the action of a magnetic field. The metal layer deposited by the method has the advantages of uniform and compact structure, excellent performance, high adhesion fastness of the film and a substrate material, high deposition speed, easy sputtering of any substance, no change of the property of the substrate, no environmental pollution and the like, and is widely applied in the fields of machinery, electronics, ceramics and the like. The polymer material is taken as a major branch of materials, and the flexibility of the matrix of the polymer material improves the difficulty of magnetron sputtering surface coating, and related patents are less, such as a method for depositing metal or hard decorative films on plastic substrates (application No. 200910112273.4) and a method for plating chromium on plastics (application No. 200910153277.7).
The invention aims to provide an antibacterial fiber with good biocompatibility, excellent antibacterial performance and good durability, the fiber can be widely applied to the field of medical biology, and in order to prepare the antibacterial fiber, a magnetron sputtering method is used, so that the prepared fiber has the advantages of uniform surface sputtering, less mechanical property loss and low cost.
Disclosure of Invention
The invention relates to an antibacterial silver-containing fiber with excellent biocompatibility and a preparation method thereof, wherein the antibacterial silver-containing fiber is mainly prepared by a magnetron sputtering method, alginic acid fiber is selected as a base material, and the alginate fiber is extracted from natural seaweed, so that the antibacterial silver-containing fiber has excellent biocompatibility and large water absorption capacity and is beneficial to wound healing.
Specifically, the invention provides an antibacterial silver-containing fiber with excellent biocompatibility, which is characterized in that the silver-containing fiber is an alginic acid fiber, and silver is attached to the surface of the fiber.
The silver-containing fiber can maintain bacteriostatic performance for more than 7 days, preferably more than 30 days, more preferably more than 180 days, and more preferably more than 360 days.
The bacteriostatic properties were such that the bacteria were unable to reproduce, i.e. no new colonies were formed in the medium test.
The silver-containing fiber has excellent water absorption, and the specific water absorption is more than 17 g/g.
The invention also provides a preparation method of the antibacterial silver-containing fiber with excellent biocompatibility, which is characterized in that the fiber is silvered by using a magnetron sputtering method, and the fiber is an alginic acid fiber filament bundle.
The method also comprises the step of carrying out pretreatment on the alginate fiber filament bundle, wherein the pretreatment is carried out by an organic solution containing sodium salt.
Specifically, the preparation method comprises the following steps:
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
(2) mounting the pretreated seaweed filament bundle on a feeding roller for magnetron sputtering;
(3) and closing the vacuum sputtering coating chamber and vacuumizing.
(4) And introducing gas, starting a processing power supply and a target table power supply, and processing the alginate fiber filaments to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The organic solution is one or more of acetone, ethanol and methanol.
The concentration of the sodium salt is 0.1-1 g/L.
The pretreatment time in the step (1) is 1-30 seconds.
The sodium salt is one or more of sodium sulfate, sodium chloride and sodium carbonate.
When the magnetron sputtering silver plating is carried out, the current of the target table power supply is 0.001-15A.
The temperature of the magnetron sputtering silver plating is controlled at 25-70 ℃, preferably 25-50 ℃, and more preferably 30-40 ℃.
When the magnetron sputtering silver plating is carried out, the vacuum chamber needs to be pumped to the background vacuum degree, and the vacuum degree is 1 multiplied by 102-1×10-2Pa。
The target material is silver.
And (4) the sputtering gas in the step (4) is argon.
The speed of processing the alginate fiber filaments in the step (4) is 7-15 m/min.
In the process of processing the alginate fiber filament, the filament is not subjected to pretreatment operation, and when the surface of the fiber is sputtered with silver to a certain thickness, the required time is greatly increased relative to the required time of the pretreated fiber filament. Magnetron sputtering is considered to impact a treated substrate by utilizing high-energy atoms, and the existence of the substances has adverse effect on the sputtering deposition of silver atoms due to the calcium ions and the like in alginate fibers. The pretreated alginate fiber is treated by an organic solvent and sodium salt, the calcium ions and the sodium ions on the surface layer of the fiber have ion exchange effect, the calcium ions on the surface of the fiber are partially replaced, so that the structure of the surface of the fiber is changed, and a thin gel layer exists on the surface of the fiber.
Another technical problem to be solved by the pretreatment of the fibres is to increase the treatment speed, which is usually 0.6-3m/min for fabric treatment in the prior art, but by this solution the treatment speed can reach 7-15m/min, preferably 10-15 m/min.
The magnetron sputtering machine used in the invention is an elliptical magnetron sputtering silver plating machine, a plurality of rectangular plane large-area magnetron sputtering sources are respectively arranged on the peripheral wall of an elliptical cylindrical vacuum chamber, and a winding device which enables a fiber bundle to perform winding motion is arranged at the central position of the vacuum chamber opposite to the sputtering sources, so that silver atoms sputtered by the magnetron sputtering sources are uniformly deposited on the surface of the fiber.
Specifically, the elliptical magnetron sputtering silver plating machine is provided with two large-diameter winding silver plating rollers which rotate in opposite directions, so that silver can be plated on both sides of the fiber bundle, the silver attachment amount is increased, the silver plating uniformity is improved, and the silver plating efficiency is improved.
The diameter of the winding silver plating roller is 40-80 cm.
Furthermore, a winding device on the fiber of the elliptical magnetron sputtering silver plating machine is provided with a mechanism for automatically adjusting the tension.
Furthermore, in order to control the silver plating temperature, the two winding silver plating rollers are provided with water cooling devices, and the two small-diameter rollers are respectively an unwinding roller and a winding roller of the ribbon fiber fabric.
The antibacterial silver-containing fiber with excellent biocompatibility and the preparation method thereof provided by the invention have the following beneficial effects.
(1) The fiber is treated by using the organic solution of sodium salt, so that the structure of the surface of the fiber is changed to a certain extent, and the fiber has certain flowing property, and is beneficial to deposition and attachment of silver atoms in the treatment of magnetron sputtering. In addition, the used treatment solvent is an organic solvent such as ethanol, methanol, acetone and the like, which is very volatile and can be easily removed in a vacuum environment of magnetron sputtering, so that the drying of the treated alginate fibers is ensured, and the physical form stability of the fibers can be ensured.
(2) In the invention, the seaweed fiber after the pretreatment is subjected to magnetron sputtering treatment, and silver atoms are more easily attached to the treated fiber, so that the treatment speed can be greatly improved.
(3) The magnetron sputtering equipment adopted by the invention is provided with the two large-diameter winding silver-plating rollers, and the two surfaces of the fiber bundle can be plated with silver by rotating in opposite directions, so that the silver plating amount is obviously improved.
(4) The invention adopts magnetron sputtering equipment to carry out silver plating, and compared with the scheme of adding nano silver into the spinning solution, the invention can reduce the using amount of silver and improve the antibacterial effect, including the bactericidal rate and the bacteriostatic effective time.
(5) The calcium alginate adopted by the invention is used as a base material, and the metal silver is used for plating, so that the obtained fiber has excellent conductivity, can be used as an additive material of antistatic fiber, and can also be used as a conductive component in electronic construction.
Drawings
FIG. 1 is an SEM image of untreated alginate fibers in FIG. 1; wherein the image (b) is an SEM image of example 1.
FIG. 2 EDX analysis of the fiber of example 1.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
In order to further illustrate the concept of the present invention in detail, the present invention provides the following examples
Example 1
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
wherein the organic solution of sodium salt is 0.2% ethanol solution of sodium chloride, and the treatment time is 20 s.
(2) And (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(3) And closing the vacuum sputtering coating chamber and vacuumizing.
(4) Argon is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 8m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 10A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
Example 2
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
wherein the organic solution of sodium salt is 0.2% ethanol solution of sodium chloride, and the treatment time is 30 s.
(2) And (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(3) And closing the vacuum sputtering coating chamber and vacuumizing.
(4) Argon is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 5m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 10A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
Example 3
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
wherein the organic solution of sodium salt is 1% ethanol solution of sodium chloride, and the treatment time is 30 s.
(2) And (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(3) And closing the vacuum sputtering coating chamber and vacuumizing.
(4) Argon gas is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 15m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 10A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
Example 4
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
wherein the organic solution of sodium salt is 1% ethanol solution of sodium chloride, and the treatment time is 10 s.
(2) And (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(3) And closing the vacuum sputtering coating chamber and vacuumizing.
(4) Argon gas is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 15m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 10A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
Example 5
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
wherein the organic solution of sodium salt is 0.2% ethanol solution of sodium chloride, and the treatment time is 30 s.
(2) And (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(3) And closing the vacuum sputtering coating chamber and vacuumizing.
(4) Argon is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 8m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 5A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
Example 6
The silver-containing fiber prepared in any one of examples 1 to 5 is blended with other fibers to prepare a yarn or fabric.
Comparative example 1
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) and (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(2) And closing the vacuum sputtering coating chamber and vacuumizing.
(3) Argon is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 8m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 10A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
Comparative example 2
A method for preparing antibacterial silver-containing fiber with excellent biocompatibility comprises the following steps,
(1) and (3) mounting the pretreated seaweed filament bundle on a delivery roller of magnetron sputtering, passing the fiber bundle through a winding silver-plating roller, automatically adjusting a tension mechanism, and finally taking up the fiber bundle to the winding roller.
(2) And closing the vacuum sputtering coating chamber and vacuumizing.
(3) Argon gas is introduced, the processing power supply and the target platform power supply are started, the speed of fiber processing is controlled to be 2m/min, and the alginic acid fiber filaments are processed to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
The current of the target table power supply is 10A, and the temperature of the sputtering silver plating is controlled to be 30-40 ℃.
The fibers prepared in examples 1 to 5 and comparative examples 1 and 2 were subjected to the antibacterial durability test, and the test results were as follows:
| example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | |
| 7 days | 99.9 | 99.9 | 99.9 | 99.9 | 99.9 | 99.9 | 99.9 |
| 30 days | 99.9 | 99.9 | 99.9 | 99.9 | 99.9 | 99.9 | 99.9 |
| 180 days | 99.9 | 99.9 | 99.9 | 95.8 | 97.4 | 78.6 | 87.6 |
Therefore, all the silver-plated alginate fibers have good antibacterial performance, but as time goes on, the silver is oxidized, the antibacterial performance is weakened, and the fibers with low silver content have the condition of weakening the antibacterial performance at the earliest.
The fibers prepared in examples 1 to 5 and comparative examples 1 and 2 were subjected to the breaking strength test, and the test results are as follows.
From the mechanical properties, the alginate fiber after pretreatment has reduced mechanical properties because part of calcium is replaced by sodium ions, but after silver plating, the mechanical properties are improved, and the mechanical properties of the fiber after the treatment are similar to those of the fiber without pretreatment.
It should be noted that the methods disclosed in the examples of the present invention are not intended to limit the scope of the present invention, and reference should be made to the following claims for specific protection.
Claims (9)
1. A preparation method of antibacterial silver-containing fiber with excellent biocompatibility is characterized in that: the preparation method comprises the following steps:
(1) pretreating alginate fiber filament bundles, wherein the pretreatment step is to pass alginate fibers through an organic solution of sodium salt;
(2) mounting the pretreated seaweed filament bundle on a feeding roller for magnetron sputtering;
(3) and closing the vacuum sputtering coating chamber and vacuumizing.
(4) And introducing gas, starting a processing power supply and a target table power supply, and processing the alginate fiber filaments to obtain the antibacterial silver-containing fiber with excellent biocompatibility.
2. A method for preparing the antibacterial silver-containing fiber having excellent biocompatibility as set forth in claim 1, wherein: the organic solution is one or more of acetone, ethanol and methanol; the concentration of the sodium salt is 0.1-1 g/L; the sodium salt is one or more of sodium sulfate, sodium chloride and sodium carbonate.
3. A method for preparing the antibacterial silver-containing fiber having excellent biocompatibility as set forth in claim 1, wherein: in the step (3), the current of the power supply of the target table is 0.001-15A; the temperature is controlled at 25-70 deg.C, preferably 25-50 deg.C, and more preferably 30-40 deg.C.
4. A method for preparing the antibacterial silver-containing fiber having excellent biocompatibility as set forth in claim 1, wherein: in the step (3), the vacuum chamber needs to be pumped to the background vacuum degree, and the vacuum degree is 1 multiplied by 102-1×10-2Pa。
5. A method for preparing the antibacterial silver-containing fiber having excellent biocompatibility as set forth in claim 1, wherein: the sputtering gas in the step (4) is argon; the speed of processing the alginate fiber filaments in the step (4) is 7-15 m/min.
6. A magnetron sputtering machine for carrying out the method for producing the antibacterial silver-containing fiber having excellent biocompatibility according to claim 1, characterized in that: the fiber bundle silver plating machine is characterized in that a plurality of rectangular plane large-area magnetron sputtering sources are respectively arranged on the peripheral wall of an oval cylindrical vacuum chamber, a winding device which enables the fiber bundle to perform winding motion is arranged in the central position of the vacuum chamber opposite to the sputtering sources, so that silver atoms sputtered by the magnetron sputtering sources are uniformly deposited on the surface of the fiber, two large-diameter winding silver plating rollers are arranged on the oval magnetron sputtering silver plating machine and rotate in opposite directions, and therefore silver can be plated on both sides of the fiber bundle, the attachment amount of silver is increased, the uniformity of silver plating is improved, and the silver plating efficiency is improved.
7. A fiber obtained by the method for producing an antibacterial silver-containing fiber having excellent biocompatibility as recited in any one of claims 1 to 5, wherein: the silver-containing fiber is alginic acid fiber, and the silver is attached to the surface of the fiber.
8. A fiber obtained by the method for preparing an antibacterial silver-containing fiber having excellent biocompatibility according to any one of claim 7, wherein: the silver-containing fiber can maintain the performance of bacteriostasis, and the time for maintaining the bacteriostasis fiber is more than 7 days, preferably more than 20 days, and more preferably more than 30 days.
9. A fiber obtained by the method for preparing an antibacterial silver-containing fiber having excellent biocompatibility according to any one of claim 7, wherein: the silver-containing fiber has excellent water absorption, and the specific water absorption is 17 g/g.
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