CN106702730A - Method for preparing nano-metal antibacterial fibers by adopting physical deposition process - Google Patents
Method for preparing nano-metal antibacterial fibers by adopting physical deposition process Download PDFInfo
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- CN106702730A CN106702730A CN201611063549.0A CN201611063549A CN106702730A CN 106702730 A CN106702730 A CN 106702730A CN 201611063549 A CN201611063549 A CN 201611063549A CN 106702730 A CN106702730 A CN 106702730A
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- physical deposition
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Physical Vapour Deposition (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a method for preparing nano-metal antibacterial fibers by adopting a physical deposition process. High-pressure superfine water flow is injected to a multilayer fiber mesh, so that fibers are intertwisted into a coil, and coiled fibers are obtained; the coiled fibers are put in a vacuum chamber, argon is introduced to the vacuum chamber, and a metal target material is sputtered under negative pressure by adopting magnetron sputtering coating equipment. The method has the advantages of no wastewater discharge during preparation, long service life, no volatility, no environmental pollution, wide-spectrum and high-efficiency antibiosis, difficulty in drug resistance generation and the like.
Description
Technical field
The invention belongs to anti-biotic material preparing technical field, and in particular to one kind prepares nm of gold using physical deposition process
The method for belonging to anti-bacterial fibre.
Background technology
Antibacterial material generally can be divided into organic antibacterial material and the major class of inorganic antibacterial material two.Usual organic antibacterial material root
More than 20 major classes are divided into according to its chemical molecular structure, as the relatively simple aldehyde radical aqueous solution class of structure and structure are complex
Isothiazole and imidazoles etc., they the characteristics of be all that, with certain volatility and toxicity, temperature tolerance is poor, typically at 200 DEG C
Within, long-term use has the phenomenons such as dissolution, precipitation, and easily skin and eyes etc. are caused to stimulate and corroded, or even also depositing of having
Controlled concentration must be paid close attention in the potential danger of carcinogenic and bad blood, therefore in use；Inorganic antibacterial material is primarily referred to as weight
Metal ion Ag+、Zn2+、Cu2+Or with silicate or phosphate containing these ions be the antibacterial material of carrier.It is antibacterial with organic
Material is compared, and it has a preferable heat-resisting and security, and bacteriostasis are strong, good endurance the features such as, wherein especially with Ag+'s
Sterilization ability is concerned, and it has strong killing to various malignant bacterias such as Escherichia coli, staphylococcus aureus etc.
Go out effect.
Current antibacterial silver fiber technology of preparing mainly has chemical plating, fused mass directly spinning, physical technique.The wherein maximum of chemical plating
Have the disadvantage that in production process the sewage containing heavy metal ion can be produced, the restriction that will be environmentally protected, this technology just by
Gradually it is eliminated；The disadvantage of fused mass directly spinning is that silver particles dispersing uniformity is poor, spinning technique control difficulty is big, bacteriostasis property not
Stabilization；Physical technique is the state-of-the-art process for treating surface in the current world, realizes Metallization effects the most on textile material surface
It is preferable.
How under test current domestic technical matters is, and most enterprise does not possess the bar of batch production silver plated fiber also
Part, the factory of rare several production silver plated fiber, mostly using Electroless Silver Plating.Low production efficiency, high cost, pollution are tight
Weight, production process is always by the strict limitation of environmental administration.It is raw and foreign countries are to the relative secrecy of silver plated fiber production Technology
High cost is produced, though so in the market has silver plated fiber to occur, its quality level and large-scale production cannot satisfy social needs.
The content of the invention
To make up the deficiencies in the prior art, the present invention provides a kind of environmental protection, the use physical deposition process of low cost
The method for preparing nano-metal antibacterial fiber.
The present invention is achieved through the following technical solutions：
A kind of method that use physical deposition process prepares nano-metal antibacterial fiber, it is characterized in that：Including following step
Suddenly：
（1）The fine water flow jet of high pressure is online to multi-layer fiber, make fiber mutually entangled, it is wound into obtaining coiled material
Fiber；
（2）Coiled material fiber is placed in vacuum chamber, negative pressure is evacuated in vacuum chamber, then to argon gas is passed through in vacuum chamber, used
Magnetic-controlled sputtering coating equipment splash-proofing sputtering metal target, the voltage between the two poles of the earth of sputtering zone is 300-500V, and DC current is 5-8A, is splashed
The time is penetrated for 1-1.5min, anode is provided with anode film ion gun, what coiled material fiber was produced before sputter by anode film ion gun
Ion beam is processed；The target source of the magnetic-controlled sputtering coating equipment uses rectangular plane magnetic control target and coaxial cylindrical magnetic control target
With reference to.
Further, the method that a kind of use physical deposition process of the invention prepares nano-metal antibacterial fiber, step
（1）In the coiled material fiber grammes per square metre that obtains be 40 g/m2。
Further, the method that a kind of use physical deposition process of the invention prepares nano-metal antibacterial fiber, step
（2）Being evacuated to negative pressure in middle vacuum chamber is（1-10）×10-3Pa, being passed through the working vacuum after argon gas is（1-2）×10-1Pa。
Further, the method that a kind of use physical deposition process of the invention prepares nano-metal antibacterial fiber, anode
Film ion gun is using focusing discharge mode, voltage 2000V, electric current 2.5A.
Further, the method that a kind of use physical deposition process of the invention prepares nano-metal antibacterial fiber, it is described
Magnetic-controlled sputtering coating equipment is configured with cryogenic pump system in vacuum chamber, places and is imitated by the cryogenic condensation on its surface in a vacuum chamber
Should, the residual gas of rapid trapping vacuum system.Compare the time that can be greatly shortened and vacuumize with legacy equipment（Can shorten
The pumpdown time of 60-90%）, obtain clean vacuum environment, vacuum can improve half order of magnitude, improve production efficiency.
Preferably, the method that a kind of use physical deposition process of the invention prepares nano-metal antibacterial fiber,
The winding of coiled material fiber, unreel winding operating winding is realized using direct current generator Direct Torque, it is magnetic powder clutched relative to traditional
Device also has well adapting to property to thin material, narrow material and extensibility material；Winding side is provided with the auxiliary of individual motor driving
Power carry-over pinch rolls, it is ensured that Winding Tension Controlling reaches precision higher, fully ensure that the breadth of material and the uniformity of grammes per square metre.
Preferably, the winding of coiled material fiber and unreel position and be mounted with that the segmentation of controlling angle can be realized outside machine
Nip rolls, can implement regulation and control immediately, it is ensured that material in vacuum winding coating process is carried out according to practically necessary flattening effect
The smooth quality of material.
The beneficial effects of the invention are as follows：
（1）The present invention can carry out type selecting to different classes of, specification chopped fiber, design chopped fiber boundling state and crosslinking degree,
The technological parameters such as control tension force, grammes per square metre, gas porosity, form the web-like base material of special requirement, it is ensured that the uniformity of Product processing, one
Cause property and continuity, accomplish scale production.
（2）Present invention use plasma processing technique, low pressure, low-voltage, line high, it is low that anode film ion gun is produced
Energy, the ion beam of big line can effectively remove the organic pollution and oxide layer of substrate surface, increase adhesion of thin film,
Avoid causing to damage when bombarding base material simultaneously, plasma processing is carried out to fiber base material under vacuum conditions, make fiber surface
The free free radical of generation, improves fiber surface activity；Solve plasma processing and physical vapour deposition (PVD) simultaneous techniques, it is to avoid
The recontamination of base material, while improve production efficiency, solves the technical barrier of adhesive force between general fibre and metal, has
Interface binding power between effect reinforcing fiber surface and metal.
（3）Continuously be sent in vacuum chamber fibrous matrix by winding method by the present invention, recycles high vacuum magnetic control to splash
The technology of penetrating makes fiber surface deposit the metal levels such as silver, copper, zinc with antibacterial effect.Distribution of Magnetic Field in magnetron sputtering is to target
Utilization rate important.In order to improve the utilization rate and production efficiency of target, Distribution of Magnetic Field and a series of knots are redesigned
Structure is designed, and the magnetic line of force at magnetic control target edge forms a large amount of Ions Bombardments, directly in the through substrate surface of divergent shape in substrate surface
Intervene substrate surface spatter film forming.
（4）Process of the present invention does not have discharge of wastewater, long service life, non-volatility, environmentally safe, with wide
The advantages of composing high-efficiency antimicrobial, be not likely to produce the resistance to the action of a drug.Itself and fiber composite are made high-performance bacteriostatic fiber composite, can be
Silver ion is slowly released in for a long time, effective concentration of silver ions is kept for a long time, so that with anti-microbial property stabilization, sterilization is made
It is long with the time, the features such as easy to use.Ensure uniformity, the coherence and continuity of Product processing, accomplish scale production.
Specific embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
Embodiment 1
A kind of method that use physical deposition process prepares nano-metal antibacterial fiber, comprises the following steps：
（1）The fine water flow jet of high pressure is online to multi-layer fiber, make fiber mutually entangled, so that fleece is able to
Reinforce and possess certain strength, flexibility tangle, the original feature of fiber is not influenceed, do not damage fiber, without adhesive reinforce, it is resistance to
Wash, obtain coiled material fiber, grammes per square metre is controlled in 40 g/m2；
（2）Coiled material fiber is placed in vacuum chamber, it is 1 × 10 that negative pressure is evacuated in vacuum chamber-3Pa, then leads to in vacuum chamber
Enter argon gas, keep working vacuum 1 × 10-1Pa, using magnetic-controlled sputtering coating equipment splash-proofing sputtering metal target, the magnetic control of the present embodiment splashes
Penetrate filming equipment to be applied in cylindrical magnetic controlled sputtering target the structural principle of rectangular plane magnetic control target, the magnetic controlled sputtering target of design
Referred to as cylinder, plane-type magnetic controlled sputtering target, it has the equal of the advantage of both planar rectangular target and concentric cylinder target, i.e. plated film concurrently
Even property is good, and target utilization is higher, and the voltage between the two poles of the earth of sputtering zone is 300V, and DC current is 5A, and sputtering time is
1min, two interpolars produce electric discharge, argon gas is formed cation Ar+As electron carrier, flown from anode to the silver-colored target surface of negative electrode
OK.Because the vertical magnetic field on silver-colored target surface is acted on, electronics is set to be spun up at a high speed into cycloid, and touched with metallic silver target on negative electrode
Hit, target makes the metallic atom or molecule on silver-colored target surface, dash coat adhere on the surface of the fabric in the presence of collision energy.By
The impact energy of Ar+ is away from the crystal energy of metallic atom in sputtering, anode film ion gun is produced in addition low energy, big line
Ion beam can effectively remove the organic pollution and oxide layer of substrate surface, ion gun using focusing on discharge mode work,
Voltage 2000v, electric current 2.5A, are that the attachment fastness of Ag atoms in this fibrous webs is preferable, and itself can also carry out surface
Migration and spread, depth of penetration occurs and enters base material body phase, be a kind of practicality fine film technique very high, and film phase purity
Higher than other processes.
The present embodiment uses DC control system in the drive device of matrix material lining home roll, and is equipped with high-resolution volume
Code device, to ensure to realize the stabilization of wound membrane speed in winding process and eliminate the influence of the change of voltage ripple of power network and load,
Make material film plating uniform.
The winding of the matrix material of the present embodiment, unreel winding matrix is all realized using direct current generator Direct Torque Control
The operating winding of material, also has to thin material, narrow material and extensibility material relative to traditional magnetic powder cluth and well adapts to
Property.The auxiliary tension force carry-over pinch rolls of individual motor driving are provided with winding side, it is ensured that Winding Tension Controlling reaches precision higher.Fill
The breadth of code insurance card material and the uniformity of grammes per square metre.
The winding of the present embodiment matrix material reel system and unreel position and be equipped with being directly realized by outside machine and turn
The segmentation nip rolls of angle control, can implement instant in vacuum winding coating process is carried out according to practically necessary flattening effect
Regulation and control.Ensure the smooth quality of material.The all not similar outfits of equipment currently on the market.
The present embodiment filming equipment is configured with cryogenic pump system in vacuum workshop, places and passes through its surface in a vacuum chamber
Cryogenic condensation effect, the residual gas of rapid trapping vacuum system.Comparing with legacy equipment can greatly shorten what is vacuumized
Time（The pumpdown time of 60-90% can be shortened）, obtain clean vacuum environment（Vacuum can improve half order of magnitude, improve
Production efficiency.
The present embodiment equipped with a set of fast and reliable combined type fine pumping system, with the speed of evacuation is fast, exhaust
The premium properties that amount is big, vacuum is high.The operation of reel system and vacuum system is automatically controlled using man-machine interface and PLC, this
15 ㎏ of the plated film yield/H of embodiment.
Embodiment 2
A kind of method that use physical deposition process prepares nano-metal antibacterial fiber, comprises the following steps：
（1）The fine water flow jet of high pressure is online to multi-layer fiber, make fiber mutually entangled, so that fleece is able to
Reinforce and possess certain strength, flexibility tangle, the original feature of fiber is not influenceed, do not damage fiber, without adhesive reinforce, it is resistance to
Wash, obtain coiled material fiber, grammes per square metre is controlled in 40 g/m2；
（2）Coiled material fiber is placed in vacuum chamber, it is 10 × 10 that negative pressure is evacuated in vacuum chamber-3Pa, then leads to in vacuum chamber
Enter argon gas, keep working vacuum 2 × 10-1Pa, using magnetic-controlled sputtering coating equipment splash-proofing sputtering metal target, the magnetic control of the present embodiment splashes
Penetrate filming equipment to be applied in cylindrical magnetic controlled sputtering target the structural principle of rectangular plane magnetic control target, the magnetic controlled sputtering target of design
Referred to as cylinder, plane-type magnetic controlled sputtering target, it has the equal of the advantage of both planar rectangular target and concentric cylinder target, i.e. plated film concurrently
Even property is good, and target utilization is higher, and the voltage between the two poles of the earth of sputtering zone is 500V, and DC current is 8A, and sputtering time is
1.2min, two interpolars produce electric discharge, argon gas is formed cation Ar+As electron carrier, from silver-colored target surface from anode to negative electrode
Flight.Because the vertical magnetic field on silver-colored target surface is acted on, electronics is set to be spun up at a high speed into cycloid, and touched with metallic silver target on negative electrode
Hit, target makes the metallic atom or molecule on silver-colored target surface, dash coat adhere on the surface of the fabric in the presence of collision energy.By
The impact energy of Ar+ is away from the crystal energy of metallic atom in sputtering, anode film ion gun is produced in addition low energy, big line
Ion beam can effectively remove the organic pollution and oxide layer of substrate surface, ion gun using focusing on discharge mode work,
Voltage 2000v, electric current 2.5A.
Embodiment 3
A kind of method that use physical deposition process prepares nano-metal antibacterial fiber, comprises the following steps：
（1）The fine water flow jet of high pressure is online to multi-layer fiber, make fiber mutually entangled, so that fleece is able to
Reinforce and possess certain strength, flexibility tangle, the original feature of fiber is not influenceed, do not damage fiber, without adhesive reinforce, it is resistance to
Wash, obtain coiled material fiber, grammes per square metre is controlled in 40 g/m2；
（2）Coiled material fiber is placed in vacuum chamber, it is 5 × 10 that negative pressure is evacuated in vacuum chamber-3Pa, then leads to in vacuum chamber
Enter argon gas, keep working vacuum 1.5 × 10-1Pa, using magnetic-controlled sputtering coating equipment splash-proofing sputtering metal target, the magnetic control of the present embodiment
Sputtering coating equipment is applied to the structural principle of rectangular plane magnetic control target in cylindrical magnetic controlled sputtering target, the magnetron sputtering of design
Target is referred to as cylinder, plane-type magnetic controlled sputtering target, and it has the advantage of both planar rectangular target and concentric cylinder target, i.e. plated film concurrently
Uniformity is good, and target utilization is higher, and the voltage between the two poles of the earth of sputtering zone is 400V, and DC current is 6A, and sputtering time is
1.5min, two interpolars produce electric discharge, argon gas is formed cation Ar+As electron carrier, from silver-colored target surface from anode to negative electrode
Flight.Because the vertical magnetic field on silver-colored target surface is acted on, electronics is set to be spun up at a high speed into cycloid, and touched with metallic silver target on negative electrode
Hit, target makes the metallic atom or molecule on silver-colored target surface, dash coat adhere on the surface of the fabric in the presence of collision energy.By
The impact energy of Ar+ is away from the crystal energy of metallic atom in sputtering, anode film ion gun is produced in addition low energy, big line
Ion beam can effectively remove the organic pollution and oxide layer of substrate surface, ion gun using focusing on discharge mode work,
Voltage 2000v, electric current 2.5A.
Claims (7)
1. a kind of method that use physical deposition process prepares nano-metal antibacterial fiber, it is characterised in that：Comprise the following steps：
（1）The fine water flow jet of high pressure is online to multi-layer fiber, make fiber mutually entangled, it is wound into obtaining coiled material
Fiber；
（2）Coiled material fiber is placed in vacuum chamber, negative pressure is evacuated in vacuum chamber, then to argon gas is passed through in vacuum chamber, used
Magnetic-controlled sputtering coating equipment splash-proofing sputtering metal target, the voltage between the two poles of the earth of sputtering zone is 300-500V, and DC current is 5-8A, is splashed
The time is penetrated for 1-1.5min, anode is provided with anode film ion gun, what coiled material fiber was produced before sputter by anode film ion gun
Ion beam is processed；The target source of the magnetic-controlled sputtering coating equipment uses rectangular plane magnetic control target and coaxial cylindrical magnetic control target
With reference to.
2. the method that a kind of use physical deposition process according to claim 1 prepares nano-metal antibacterial fiber, it is special
Levy and be：Step（2）Being evacuated to negative pressure in middle vacuum chamber is（1-10）×10-3Pa, being passed through the working vacuum after argon gas is（1-2）×
10-1Pa。
3. the method that a kind of use physical deposition process according to claim 1 and 2 prepares nano-metal antibacterial fiber, its
It is characterised by：Anode film ion gun is using focusing discharge mode, voltage 2000V, electric current 2.5A.
4. the method that a kind of use physical deposition process according to claim 1 and 2 prepares nano-metal antibacterial fiber, its
It is characterised by：Coiled material fiber grammes per square metre is 40g/m2。
5. the method that a kind of use physical deposition process according to claim 1 prepares nano-metal antibacterial fiber, it is special
Levy and be：The winding of coiled material fiber, unreel winding operating winding is realized using direct current generator Direct Torque, winding side is provided with solely
Vertical motor-driven auxiliary tension force carry-over pinch rolls.
6. a kind of method that use physical deposition process prepares nano-metal antibacterial fiber according to claim 5, its feature
It is：The winding of the coiled material fiber and unreel position and be mounted with that the segmentation nip rolls of controlling angle can be realized outside machine.
7. a kind of method that use physical deposition process prepares nano-metal antibacterial fiber according to claim 1, its feature
It is：The magnetic-controlled sputtering coating equipment is configured with cryogenic pump system in vacuum chamber.
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| CN201611063549.0A CN106702730B (en) | 2016-11-28 | 2016-11-28 | A method of nano-metal antibacterial fiber is prepared using physical deposition process |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999815A (en) * | 2006-12-20 | 2007-07-18 | 周菊先 | Loading pressure sputtering mfg. process of antobiosis textile material and its products |
| CN101275215A (en) * | 2008-04-17 | 2008-10-01 | 苏州工业园区鸿锦纳米有限公司 | Antibacterial substrate having silver film, manufacturing method thereof and preparing device therefor |
| CN101660125A (en) * | 2009-09-18 | 2010-03-03 | 邵楠 | Technology for plating nano-metal on fiber |
| CN101744402A (en) * | 2008-12-19 | 2010-06-23 | 北京振涛国际钛金技术有限公司 | Antibacterial deodorant shoe plated with nanosilver by physical vapor deposition method |
| CN103284771A (en) * | 2013-05-22 | 2013-09-11 | 韩永俊 | Antibacterial medical suture and production method thereof |
-
2016
- 2016-11-28 CN CN201611063549.0A patent/CN106702730B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999815A (en) * | 2006-12-20 | 2007-07-18 | 周菊先 | Loading pressure sputtering mfg. process of antobiosis textile material and its products |
| CN101275215A (en) * | 2008-04-17 | 2008-10-01 | 苏州工业园区鸿锦纳米有限公司 | Antibacterial substrate having silver film, manufacturing method thereof and preparing device therefor |
| CN101744402A (en) * | 2008-12-19 | 2010-06-23 | 北京振涛国际钛金技术有限公司 | Antibacterial deodorant shoe plated with nanosilver by physical vapor deposition method |
| CN101660125A (en) * | 2009-09-18 | 2010-03-03 | 邵楠 | Technology for plating nano-metal on fiber |
| CN103284771A (en) * | 2013-05-22 | 2013-09-11 | 韩永俊 | Antibacterial medical suture and production method thereof |
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| CN106702730B (en) | 2019-04-12 |
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Address after: 274700 West Zhangbo Village, Huangji Township, Yuncheng County, Heze City, Shandong Province Patentee after: Heze Tianyuan electronic Polytron Technologies Inc Address before: 274700 West Zhangbo Village, Huangji Township, Yuncheng County, Heze City, Shandong Province Patentee before: Yuncheng Tianyuan Electronic Technology Co., Ltd. |
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