CN113844140A - Nano-zinc oxide antibacterial non-woven fabric, medical mask and preparation devices and preparation methods of nano-zinc oxide antibacterial non-woven fabric and medical mask - Google Patents
Nano-zinc oxide antibacterial non-woven fabric, medical mask and preparation devices and preparation methods of nano-zinc oxide antibacterial non-woven fabric and medical mask Download PDFInfo
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- CN113844140A CN113844140A CN202110978175.XA CN202110978175A CN113844140A CN 113844140 A CN113844140 A CN 113844140A CN 202110978175 A CN202110978175 A CN 202110978175A CN 113844140 A CN113844140 A CN 113844140A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/022—Non-woven fabric
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/02—Layered materials
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/10—Impermeable to liquids, e.g. waterproof; Liquid-repellent
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/12—Hygroscopic; Water retaining
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/14—Air permeable, i.e. capable of being penetrated by gases
- A41D31/145—Air permeable, i.e. capable of being penetrated by gases using layered materials
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2500/00—Materials for garments
- A41D2500/30—Non-woven
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
- B32B2037/246—Vapour deposition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/20—All layers being fibrous or filamentary
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0253—Polyolefin fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
- B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/724—Permeability to gases, adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2571/00—Protective equipment
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Abstract
The invention discloses a nano zinc oxide antibacterial non-woven fabric, a medical mask, a preparation device and a preparation method thereof, wherein a nano zinc oxide film is sputtered on non-woven fabric fibers by utilizing a magnetron sputtering technology, and the nano zinc oxide antibacterial non-woven fabric is applied to a mask product by utilizing the antibacterial characteristic of nano zinc oxide, and the mask comprises the following components from outside to inside: a water-repellent non-woven fabric layer, a nano zinc oxide antibacterial non-woven fabric layer, an electret polypropylene non-woven fabric layer and a hydrophilic super-soft non-woven fabric layer. The manufactured mask has lasting antibiosis and higher haze protection efficiency, the antibiosis rate of the mask reaches 99.9%, and the mask can resist the bacterium for 6-8 hours, so that the frequency of replacing the mask by a user is greatly reduced, and the safety guarantee of the user is improved.
Description
Technical Field
The invention relates to the technical field of medical material antibacterial modification, in particular to a nano zinc oxide antibacterial non-woven fabric, a medical mask, a preparation device and a preparation method thereof.
Background
At present, the medical mask in China has three standards, which are respectively: YY/T0969-2013 medical mask for disposable use, YY0469-2011 medical surgical mask, and GB19083-2010 medical protective mask technical requirements, wherein the medical surgical mask mainly aims at the crowd who have invasive operation and other processes by clinical medical staff; and the medical protective mask mainly aims at the medical working environment with high exposure risk.
At present, the demand of the common people is more great for the disposable medical mask. The disposable medical mask has the requirements for obstructing and filtering pathogenic microorganism particles in air, namely bacterial aerosol with the particle size of 5 mu m is obstructed, the filtering efficiency reaches 28.3ml/min, the bacterial filtering efficiency is more than or equal to 95 percent, and the resistance is 8/Lmin and less than or equal to 49 Pa.
The medical surgical mask has the requirements for blocking and filtering pathogenic microorganism particles in air, namely staphylococcus aureus aerosol with the particle size of 3 +/-0.3 mu m and NaCL aerosol with the particle size of (0.24 +/-0.06), the filtering efficiency reaches (30 +/-2) L/min, the bacterial filtering efficiency is more than or equal to 95 percent, meanwhile, the particle filtering efficiency is more than or equal to 30 percent, the resistance is 8/Lmin, the inspiration resistance is less than or equal to 49Pa, the expiration resistance is less than or equal to 29.4Pa, and the blood permeability is as follows: synthetic blood is impermeable to 120 mmHg.
The medical protective mask has the requirements for blocking and filtering pathogenic microorganism particles in air, namely blocking particle aerosol with the particle size of (0.24 +/-0.06) mu mNaCL; when the gas flow reaches 85 +/-2L/min, the filtration efficiency is more than or equal to 95 percent (grade 1), the filtration efficiency is more than or equal to 99 percent (grade 2), and the filtration efficiency is more than or equal to 99.97 (grade 3); the resistance condition is that the resistance is less than or equal to 343.2Pa when the air flow is 85 +/-2/Lmin; the hemodialysis condition was 80mmHg impermeable to the synthetic blood.
At present, the reference of haze protection efficiency in China is GB2626-2006 respiratory protection articles-self-absorption filter type particulate matter prevention respirator, the haze protection of the mask according to the GB2626-2006 standard is divided into 3 grades of KN90/KN95/KN100, and the protection efficiency is respectively 90%, 95% and more than 99.97%.
The medical mask used in the market generally comprises an outer layer, a middle layer and an inner layer, wherein the outer layer is a non-woven fabric layer for preventing spray, the middle layer is an electrostatic adsorption filter layer, and the inner layer is non-woven fabric or natural gauze made of skin-friendly moisture-absorbing materials. In the use, the outer layer of the mask can obstruct and adsorb large dust pollutants, and the middle layer can adsorb and obstruct tiny particles such as bacteria and germs through the electrostatic action. But wear for a long time, the gauze mask inlayer causes the reduction of gauze mask adsorption filtration efficiency because the moist gas of lasting exhalation probably breeds the bacterium, also can cause the microorganism of adsorbing on the gauze mask to breed simultaneously, causes adverse effect to wearer's health. Therefore, the continuous wearing time of the traditional medical mask is generally not more than 4 hours. The disposable use and frequent replacement of the mask cause a great deal of resource consumption and are not favorable for the continuous work of medical staff.
In order to solve the above problems, researchers have used some means to attach nano zinc oxide to a non-woven fabric, and use its antibacterial property to improve the antibacterial property of the mask.
At present, the combination mode of the nano zinc oxide and the non-woven fabric is generally as follows:
1) the nano zinc oxide particles are directly combined into the non-woven fabric substrate. Chinese patent publication No. CN210407181 discloses a patent for using the antibacterial property of nano zinc oxide for a mask structure layer, wherein the nano zinc oxide is directly added to a polypropylene substrate to be made into a non-woven fabric through a melt-blowing process. When the nano zinc oxide is directly added into the non-woven fabric base material for melt-blowing, partial nano zinc oxide particles are wrapped inside fibers of the melt-blown non-woven fabric, so that the effects of the nano zinc oxide such as antibiosis and antivirus cannot be achieved, and the antibacterial and protective effects are reduced.
2) The antibacterial solution is prepared from antibacterial components such as nano zinc oxide and the like, and is attached to the non-woven fabric by adopting the processes of dipping or spraying and drying. Chinese patent publication nos. CN111172749A and CN107513865B disclose that nano zinc oxide particles are used as disinfectant of inorganic antibacterial agent, and the antibacterial disinfectant is used to treat the non-woven fabric by dipping and spraying, and then the non-woven fabric is dried by drying or naturally airing to obtain the antibacterial non-woven fabric. The mode of adding nano zinc oxide particles to prepare the antibacterial disinfectant and then impregnating or spraying is adopted, the problem that fibers are mutually adhered due to the fact that drying and drying processes are long in time consumption and other components in the disinfectant in a solid state in an original state are solved, air resistance is increased, meanwhile, the zinc oxide is not high in firmness of the non-woven fabric fibers in a loading mode of direct impregnation or spraying, and is easy to fall off and inhaled by a user when the zinc oxide is breathed, so that adverse effects are caused.
Therefore, the method for applying the antibacterial performance of the nano zinc oxide to the mask needs to be optimized urgently, and the mask has good antibacterial and antiviral performance and haze filtering performance and has lasting antibacterial time.
Sputtering is a widely used coating technique, which is commonly referred to as magnetron sputtering, and belongs to a high-speed low-temperature sputtering method. The process requires a vacuum degree of 1 × 10-3About Torr, i.e. 1.3X 10-3Vacuum of PaArgon (Ar) as inert gas is filled in the state, high-voltage direct current is applied between the plastic substrate (anode) and the metal target (cathode), electrons generated by glow discharge (glow discharge) excite the inert gas to generate plasma, and the plasma bombs out atoms of the metal target to be deposited on the plastic substrate.
The magnetron sputtering technology is mature at present and applied to the fields of semiconductors, photoelectric materials, displays and the like, but the application of the magnetron sputtering technology in the field of antibacterial modification of medical fabrics such as nano zinc oxide non-woven fabrics and the like is not disclosed in the technology. Different from the above-mentioned field of application: because the non-woven fabric is made of fibers, the fibers are mutually staggered to form a structure which is provided with pores and macroscopically shows a plane, and the microstructure of the non-woven fabric is a multilayer structure, if the air pressure is higher, the density generated by argon positive ions is too high, so that the density of generated sputtering atoms is too high, the number of atoms deposited on the fibers on the layer close to one side of the target is redundant, the fibers on the layer far away from the target are not uniform, and the sputtering thickness on the fibers is not uniform, so that lower air pressure needs to be manufactured, and sputtering atoms can be uniformly deposited on different distances. However, if the pressure is too low, for example, the vacuum degree of the vacuum equipment can reach 1.013X 10-10Pa, if 10 is used-10The Pa-level working air pressure can put higher demands on the sealing performance and energy consumption of the cavity, the cost is too high, and the yield caused by reducing the pressure to the too low air pressure is not high and is not practical.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a device for preparing a nano zinc oxide antibacterial non-woven fabric, and the nano zinc oxide antibacterial non-woven fabric prepared by the device solves the problems that nano zinc oxide particles on the nano zinc oxide antibacterial non-woven fabric in the prior art are poor in adhesion firmness, fibers are mutually adhered, the nano zinc oxide particles are wrapped inside fibers of the non-woven fabric, and the like.
In order to achieve the purpose, the invention adopts the technical scheme that: the utility model provides a preparation equipment of antibiotic non-woven fabrics of nanometer zinc oxide, includes spatters the chamber of plating, its characterized in that: the front end and the rear end of the sputtering cavity are respectively connected with a pre-pumping cavity in a sealing manner, the two pre-pumping cavities are communicated with the sputtering cavity, conveying mechanisms are distributed in the pre-pumping cavity and the sputtering cavity, an objective table is arranged on the conveying mechanisms, pumping mechanisms are arranged on the pre-pumping cavity and the sputtering cavity, and the sputtering cavity is communicated with an argon source through a pipeline.
The objective table is made of aluminum alloy, and is matched with the conveying belts distributed in the pre-pumping cavity and the sputtering cavity through a gear transmission piece to form the circular reciprocating motion of the pre-pumping cavity at the front end towards the sputtering cavity and the pre-pumping cavity at the rear end in sequence. The air pumping mechanism on the pre-pumping cavity sequentially comprises an air valve, a Rough pump and a rotary pump from the cavity of the pre-pumping cavity to the outside; the air pumping mechanism is arranged on the sputtering cavity and sequentially comprises a turbine pump, an air valve, a Rough pump and a rotary pump from the cavity to the outside; the sputtering cavity and the argon source are controlled by an air valve. The pre-pumping cavity has the main purpose that when the sputtering cavity works, the pre-pumping cavity can pre-pump air, so that the time for pumping the sputtering cavity is shortened.
The second purpose of the invention is that: the invention also provides a preparation method of the nano zinc oxide antibacterial non-woven fabric, which is characterized by comprising the following steps: a sputtering target source is arranged in the sputtering cavity, a zinc oxide target with the purity of 4N is placed on the sputtering target source, when the non-woven fabric is conveyed into the sputtering cavity, the door of the sputtering cavity can be closed to start air extraction, and when the background vacuum degree in the sputtering cavity reaches 6 multiplied by 10-6When the pressure is Torr, argon gas is filled as sputtering working gas, the pressure is kept at 0.3-0.5Pa, and the power density value (electric power/area of the surface of the zinc oxide target material bombarded by the plasma) is controlled at 1.8w/cm2～7.1w/cm2Argon gas is used to form Ar-plasma; when Ar & lt- & gt is accelerated to impact on a zinc oxide target, the Ar & lt- & gt can bombard and splash zinc oxide, and deposit and attach on the fiber surface of non-woven fabric to form a nano-scale zinc oxide film; after sputtering, the sputtering cavity is opened to send the non-woven fabric out of the pre-pumping cavity at the rear end.
If the vacuum degree of the sputtering chamber is too low, oxygen molecules in the air can oxidize non-woven fabrics (base materials), nitrogen molecules can consume sputtered atoms, the sputtering efficiency is reduced, and if the vacuum degree is too high, the requirement on a vacuum pump is increased and the energy consumption is increased; furthermore, the magnitude of the operating pressure in the sputtering chamber also has an effect on the lifetime of the Ar-and the sputtering rate; in addition, when the sputtering power density value is lower, the microstructure of the zinc oxide film layer formed on the surface of the substrate is the growth of crystal grains in two-dimensional directions, the flatness of the surface of the film layer is higher, when the sputtering power density is increased, sputtered atoms, ions and other particles are deposited on the substrate at high speed and high energy, sufficient time cannot be obtained for migration on the surface of the substrate, and the microstructure of the film layer can present a three-dimensional island-shaped microstructure, so that the roughness and the thickness of the surface of the film layer are increased. The rough surface film (film layer) of the fiber is beneficial to improving the antibacterial performance, and the rough surface area of the film layer is larger than that of the film layer, so that bacteria and carriers thereof are easy to capture and kill, and the antibacterial rate is further improved. However, when the power density is too high, the thickness of the deposited zinc oxide film is increased to several micrometers, the diameter range of fibers of the melt-blown non-woven fabric is 0.5-10 micrometers, and when the film thickness is too high, the size of the fibers attached with the zinc oxide film is increased, the porosity formed among the fibers is reduced, and the airflow resistance is increased; meanwhile, when the thickness of the zinc oxide film is increased to a few micrometers, the adhesion of the zinc oxide film on the fiber is reduced due to the larger thickness of the film, and the film is more easily broken to form particles and fall off when being bent (when the mask is used), so that the use is influenced.
Furthermore, the area ratio of the non-woven fabric to the zinc oxide target is 0.6-1.0, and the distance between the non-woven fabric and the zinc oxide target is set to be 5-7 cm. When the area of the non-woven fabric (substrate) is not more than the area of the zinc oxide target (the area ratio is not more than 1), the non-woven fabric can be completely positioned in the motion path range of atoms sputtered from the zinc oxide target during sputtering, sputtered atoms can be deposited on the substrate, so that the target can be effectively utilized, but the area ratio cannot be too small, and when the area ratio is too small, although all areas of the non-woven fabric can be deposited by the sputtered atoms, the sputtered atoms can be deposited on an objective table, waste is caused, and the objective table is polluted; when the area ratio of the non-woven fabric to the target material is larger than 1, namely the area of the non-woven fabric is larger than that of the target material, the edge of the non-woven fabric is out of the movement path range of atoms sputtered by the zinc oxide target material, and the target material cannot be deposited in the area, so that a zinc oxide film blank is caused.
Under a proper area ratio, when the non-woven fabric is far away from a zinc oxide target material in sputtering, the target material atoms can still be ensured to have enough energy to move to non-woven fabric fibers (base materials) by matching with a larger power density so as to be deposited on the non-woven fabric fibers (base materials) to form a zinc oxide film, and when the power density is too high, the film layer is locally too thick, local nano zinc oxide is excessively attached, and the attachment is not firm, so that the problem that more particles fall off in the using process of the mask is caused; similarly, when the non-woven fabrics is close to the zinc oxide target material, the target material can be deposited on the whole area of the substrate by matching with a small power density, but if the distance between the non-woven fabrics and the zinc oxide target material is too close, the probability of the target material atoms in the local deposition of the substrate is increased, the deposited film layer is too thick locally, the nano zinc oxide is not firm in adhesion, and more nano zinc oxide particles fall off in the mask bending use process.
Further, the method comprises a sputtering preparation step, wherein the non-woven fabric is placed on a conveying object stage before the pre-pumping cavity, the pre-pumping cavity is opened, the non-woven fabric is fed into the pre-pumping cavity, and the pressure of the pre-pumping cavity is pumped to 10 DEG-4After the Torr is carried out, the non-woven fabrics wait in the pre-pumping cavity, and once the sputtered non-woven fabrics are sent out from the sputtering cavity, the sputtering cavity can be opened to allow the non-woven fabrics to be subsequently plated to enter.
Furthermore, the thickness of the zinc oxide film is 20-2000 nm. If the thickness of the zinc oxide film is less than 20nm, the antibacterial property is not good, but if the thickness of the zinc oxide film reaches several micrometers, when the zinc oxide film is attached to a non-woven fabric with the fiber diameter ranging from 0.5 to 10 micrometers, the size of the fiber attached with the zinc oxide film is increased, the porosity formed among the fibers is reduced, the airflow resistance is increased, and the air permeability of the mask is reduced; meanwhile, when the thickness of the zinc oxide film is increased to a few micrometers, the adhesion of the zinc oxide film on the fiber is reduced due to the larger thickness of the film, the film is more easily broken to form particles and fall off when being bent (when the mask is used), and the antibacterial durability effect is reduced.
The invention has the third purpose: the invention also provides a nano zinc oxide antibacterial non-woven fabric, which comprises a non-woven fabric body and is characterized in that: the non-woven fabric body is sputtered with a zinc oxide film.
Furthermore, the thickness of the zinc oxide film is 20-2000 nm.
The nanometer zinc oxide antibacterial non-woven fabric solves the problems that nanometer zinc oxide particles in the nanometer zinc oxide antibacterial non-woven fabric in the prior art are poor in adhesion firmness, fibers are mutually adhered, the nanometer zinc oxide particles are wrapped inside the fibers of the non-woven fabric, and the like.
The invention aims at four: the invention also provides a medical mask made of the nano zinc oxide antibacterial non-woven fabric, which sequentially comprises a water-repellent spun-bonded non-woven fabric layer, a nano zinc oxide antibacterial non-woven fabric layer, an electret polypropylene spun-bonded non-woven fabric layer and a hydrophilic super-soft spun-bonded non-woven fabric layer from outside to inside, wherein the nano zinc oxide antibacterial non-woven fabric layer comprises a non-woven fabric body, and a zinc oxide film is sputtered on the non-woven fabric body.
Furthermore, the thickness of the zinc oxide film is 20-2000 nm.
By adopting the scheme, the medical mask has the advantages of good air permeability, lasting antibacterial time, good filtering performance and the like.
The invention is further described below with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic view of a vacuum sputtering apparatus according to the present invention;
FIG. 2 is a scanning electron microscope image of a nonwoven fabric fiber sputtered with a nano zinc oxide coating in an embodiment of the present invention, wherein M is a schematic cross-sectional structure of the fiber, and N is a structural view of an axial covering film of the fiber;
fig. 3 is a schematic view of the mask product of the present invention;
FIG. 4 is a scanning electron microscope image of example 1 (FIG. a) -4 (FIG. b) -5 (FIG. c) -6 (FIG. d) sputtering zinc oxide film on the nonwoven fabric fiber;
FIG. 5 is a comparison of the antibacterial performance test of example 5 and a control group;
FIG. 6 is a schematic diagram of a particle shedding testing apparatus in performance testing;
in fig. 1: 1-sputtering a plating cavity; 2-pre-pumping the cavity; 3-an objective table; 4-a transport mechanism;
in fig. 2: 210-non-woven fiber cross section; 220-sputtered nano zinc oxide;
in fig. 3: 1-water repellent spun-bonded nonwoven fabric; 2-nano zinc oxide antibacterial non-woven fabric; 3-electret polypropylene spunbond nonwoven fabric; 4-hydrophilic super-soft non-woven fabric.
Detailed Description
The embodiments of the present invention were prepared using the following sputtering apparatus.
As shown in fig. 1, the sputtering device comprises a workbench, a front end (feed end) and a rear end (discharge end) of the workbench are both provided with a pre-pumping cavity 2, a sputtering cavity 1 is arranged on an intermediate station of the workbench, the sputtering cavity 1 can be set 1 according to actual conditions, 2 or more cavities are formed, the pre-pumping cavity 2 and the sputtering cavity 1 are communicated with each other, a conveying mechanism 4 is further arranged on the workbench, a non-woven fabric is enabled to be pre-pumped along the front end along the same way, the middle sputtering cavity 1 is formed, the rear end is pre-pumped with the cavity 2 to pass through, the conveying mechanism 4 comprises a conveying belt and an objective table 3 located on the conveying belt, the objective table is made of aluminum alloy, and the objective table 3 and the conveying belt are matched through a gear transmission piece to move circularly along the direction.
The pre-pumping cavity 2 and the sputtering cavity 1 are respectively connected with a pumping mechanism, and the pumping mechanism of the pre-pumping cavity 2 sequentially comprises an air valve, a Rough pump and a rotary pump from the cavity to the outside; the air pumping mechanism on the sputtering cavity 1 sequentially comprises a turbine pump, an air valve, a Roots pump and a rotary pump from the cavity to the outside; the sputtering cavity 1 is also provided with a pipeline communicated with an argon source, and the opening and closing of the sputtering cavity and the argon source are controlled by an air valve. The main purpose of the pre-suction chamber 2 is: when the sputtering cavity 1 works, namely the air valve and various pumps of the sputtering device keep working continuously, the use of the pre-pumping cavity 2 greatly shortens the pumping time of the sputtering cavity 1, so that the air pressure in the sputtering cavity 1 can quickly reach the required air pressure, and the materials can be continuously fed to the sputtering device. Therefore, the zinc oxide film formed on the surface of the prepared nano zinc oxide antibacterial non-woven fabric fiber is not easy to fall off, the continuous feeding production is realized, and the production efficiency is improved.
The specific examples of the sputtering apparatus for sputtering a nano zinc oxide film on a nonwoven fabric are shown below.
1. Preparing nano zinc oxide antibacterial non-woven fabric
Selecting and cutting a piece of non-woven fabric;
vacuumizing the sputtering cavity until the air pressure is controlled at 6 x 10-6Torr, when the non-woven fabric reaches the sputtering cavity, argon gas as working gas is filled into the sputtering cavity, so that the working pressure is kept at 0.3-0.5 Pa; starting a direct current power supply to supply a direct current power with a certain power to the magnetron sputtering target to form argon plasma; the zinc oxide target material with the purity of 4N (99.99%) is placed on the sputtering target source, the zinc oxide on the zinc oxide target material is bombarded and sputtered by plasma, and is scattered and deposited to be attached to the fiber surface of the non-woven fabric to form a nano-scale zinc oxide film. The power density value (electric power/area of the surface of the zinc oxide target bombarded by the plasma) of the zinc oxide target is controlled to be 1.8w/cm2～7.1w/cm2In the meantime, the thickness of the formed nano-zinc oxide is 20 to 2000nm (the zinc oxide thin film is formed by stacking the zinc oxide on the surface of the non-woven fabric one by one), as shown in fig. 2, because the nano-zinc oxide has a stronger function of inhibiting bacteria by the zinc oxide at the size. Wherein the area ratio of the non-woven fabric to the target is 0.6-1.0, and the distance between the non-woven fabric and the zinc oxide target is 5-7 cm.
The sputtering parameters and the thickness of the nano zinc oxide film in examples 1-12 are as follows:
TABLE 1 comparison of parameters of examples
In Table 1, the pressure after the argon gas was introduced was set at 0.5Pa in examples 1 to 9 and examples 11 to 12, and the pressure after the argon gas was introduced in example 10 was set at 0.3Pa in example 10 as compared with example 5, and the other parameters were kept constant.
As can be seen from table 1 and fig. 4, when the power density is variable, as can be seen from examples 1-4-5-6, the flatness of the nano zinc oxide film on the prepared fiber is significantly different as the power density increases, and as can be seen from a-b-c-d in fig. 4, the crystal grains of the zinc oxide film formed in examples 1-4-5-6 are attached to the non-woven fabric fiber, and the rugged three-dimensional structure can be clearly seen. When the area ratio of the non-woven fabric to the target is variable, as can be seen from examples 1-7-8-9, when the area ratio of the non-woven fabric to the target is increased from 0.6 to 1.0, the thickness of the deposited nano zinc oxide film does not change greatly, and when the area ratio of the non-woven fabric to the target is 0.6, a small amount of deposited zinc oxide appears on an objective table from the view of an actual scanning electron microscope and the objective table, so that a certain amount of target is wasted, but is within an acceptable range; when the area ratio is increased to 1.25, a circle of non-woven fabric has no zinc oxide film deposition at the outer edge, and bacteria can be sucked into the body from the area by people when the mask is assembled for use, so that the safety protection is invalid, and therefore when the area ratio is larger than 1, the medical mask prepared by the method has the risk of invalid safety protection. Overall, from the viewpoint of ensuring an effective antibacterial area and economy, an area ratio of 0.8 was confirmed as the optimum choice. When the distance between the non-woven fabric and the target material is increased from 5cm to 7cm, the thickness of the nano zinc oxide film is slightly reduced, which is related to the energy attenuation of sputtering atoms, when the distance is increased, the energy attenuation of the sputtering atoms is larger, the probability of depositing the nano zinc oxide film on a substrate is reduced, and the film layer is thinned. As can be seen from the comparison between examples 5 and 10, the thickness of the deposited nano zinc oxide film does not change much when the pressure of the working gas argon is changed in the range of 0.3-0.5 Pa. From examples 1-4-5-6 and examples 3-11-12, it can be seen that when the distance between the non-woven fabric and the target is large, the non-woven fabric can be properly matched with a large power density, so that the effect of depositing the nano zinc oxide film with a low power density and a small distance can be achieved.
Application example
The non-woven fabric sputtered with the nano zinc oxide in the embodiment is sequentially stacked with the water-repellent non-woven fabric, the electret polypropylene non-woven fabric and the hydrophilic super-soft non-woven fabric, an outlet cover body is prepared after sheeting, and then the mask body is subjected to ear band dotting to prepare the mask.
In addition, the non-woven fabric directly combined with the nano zinc oxide particles prepared by the method disclosed in the embodiment of the patent publication No. CN210407181 and other 3 layers of fabrics are used for manufacturing the mask as a performance test control group 1; according to the embodiment disclosed in the patent publication No. CN111172749A, an antibacterial solution prepared from nano zinc oxide antibacterial components is sprayed or impregnated on a non-woven fabric to be loaded on the non-woven fabric to be used as a mask with other 3 layers of cloth, and the mask is used as a performance test control group 2; the mask is prepared by using the nano zinc oxide non-woven fabric prepared by using conventional sputtering equipment and other 3-layer fabrics as a performance test control group 3. The mask was prepared using non-woven fabric not loaded with nano zinc oxide and other 3-layer fabrics as a control group 5 for performance test.
Performance testing
TABLE 2 Performance test standards and conditions
TABLE 3 results of performance tests of examples and control groups
The above table shows that the mask provided by the invention has excellent long-acting antibacterial and haze-preventing performances. The sterilization rate of the nano zinc oxide antibacterial non-woven fabric mask in 12 embodiments designed by the technical scheme of the invention is still more than 99.9% after the mask is used for 4 hours, and the sterilization rate is still more than 96% after the mask is used for 8 hours; the antibacterial rate of the control group 1 was already lower than 99% after 4 hours of use, probably because the antibacterial ability of the fiber surface covered with bacteria was reduced after a certain period of exposure to the bacteria because of less zinc oxide exposed on the fiber surface; compared with the control group 2, the adhesion performance and the airflow resistance of the zinc oxide film on the fiber are obviously better than those of the zinc oxide mask manufactured by direct dipping or spraying and drying, and the particle shedding of the zinc oxide film is one order of magnitude lower than that of the control group 2. Compared with the mask prepared by a control group preparation method, the mask prepared by the embodiment of the invention has higher haze protection efficiency and continuous antibacterial capability, and the mask sputtered with the nano zinc oxide has long-term antibacterial performance and better haze protection effect. It can be seen from examples 1 to 12 that, in addition to example 6, the number of particles dropped off is larger than that of the other examples, but the antibacterial property and the antibacterial durability are not affected, which indicates that when the thickness of the nano zinc oxide film exceeds 2600nm, many nano zinc oxide particles attached to the nonwoven fabric fibers are not firm and exceed the saturation state, so that the target material is wasted by increasing the film thickness (increasing the power density value). In other examples, the mask made of the non-woven fabric with the nano zinc oxide film deposited by sputtering has a good long-acting antibacterial function, and the power density and the distance between the non-woven fabric and the target have a matching and gaining effect. In addition, the most preferable antibacterial and safe nano zinc oxide film has the thickness of 400-1500 nm.
The working principle of the antibacterial mask with the 4-layer structure is as follows:
when breathing in, the mask body and the space between the mouth and the nose are in a negative pressure state, and the air flow sequentially passes through all layers of the mask from outside to inside to enter a respiratory system of a human body. The water repellent spun-bonded non-woven fabric layer 1 is used for primary filtration to filter away spray and larger particles and bacteria in the air, the nano zinc oxide antibacterial non-woven fabric layer is used for secondary filtration to intercept and kill the fine bacteria in the air by releasing zinc ions and active oxygen, the electret polypropylene spun-bonded non-woven fabric layer removes the fine particles and the bacteria through electrostatic adsorption, and finally the water repellent spun-bonded non-woven fabric layer enters a human body respiratory system through the hydrophilic super-soft spun-bonded non-woven fabric layer 4. When exhaling, the hydrophilic super gentle spunbonded nonwoven layer of the mask absorbs the exhaled water vapor. Make the mask dry and comfortable, prolong the service life
The nano zinc oxide coating has lasting antibacterial performance, so that the use safety and the durability of the mask are improved.
The present invention is not limited to the above embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention.
Claims (9)
1. The utility model provides a preparation facilities of antibiotic non-woven fabrics of nanometer zinc oxide, includes spatters the chamber of plating, its characterized in that: the front end and the rear end of the sputtering cavity are respectively connected with a pre-pumping cavity in a sealing manner, the two pre-pumping cavities are communicated with the sputtering cavity, conveying mechanisms are distributed in the pre-pumping cavity and the sputtering cavity, an objective table is arranged on the conveying mechanisms, pumping mechanisms are arranged on the pre-pumping cavity and the sputtering cavity, and the sputtering cavity is communicated with an argon source through a pipeline.
2. A preparation method of nano zinc oxide antibacterial non-woven fabric is characterized by comprising the following steps:
a sputtering target source is arranged in the sputtering cavity, a zinc oxide target with the purity of 4N is placed on the sputtering target source, when the non-woven fabric is placed in the sputtering cavity, the door of the sputtering cavity can be closed to start air exhaust, and when the pressure in the sputtering cavity reaches 6 multiplied by 10-6When the pressure is Torr, inert gas argon is filled in to ensure that the air pressure in the cavity is 0.3-0.5Pa, the area ratio of the non-woven fabric and the zinc oxide target material is not more than 1, and the power density value is controlled to be 1.8w/cm2 ~ 7.1w/cm2Argon gas is formed into Ar between the two-Plasma; when Ar is-After the zinc oxide target material is accelerated to impact, the zinc oxide target material can bombard and splash the zinc oxide and deposit and attach the zinc oxide target material on the fiber surface of the non-woven fabric to form a nano-scale zinc oxide film; after sputtering, the sputtering cavity is opened to send the non-woven fabric out of the pre-pumping cavity at the rear end.
3. The method for preparing the nano zinc oxide antibacterial non-woven fabric according to claim 2, characterized in that: the area ratio of the non-woven fabric to the zinc oxide target is 0.6-1.0, and the distance between the non-woven fabric and the zinc oxide target is 5-7 cm.
4. The method for preparing nano zinc oxide antibacterial non-woven fabric according to claim 1, which comprisesCharacterized in that the sputtering preparation step is also included, the non-woven fabric is placed on a conveying object stage before the pre-pumping cavity, the pre-pumping cavity is opened, the non-woven fabric is fed into the pre-pumping cavity, and the pressure of the pre-pumping cavity is pumped to 10 DEG-4After the Torr is carried out, the non-woven fabrics wait in the pre-pumping cavity, and once the sputtered non-woven fabrics are sent out from the sputtering cavity, the sputtering cavity can be opened to allow the non-woven fabrics to be subsequently plated to enter.
5. The method for preparing nano zinc oxide antibacterial non-woven fabric according to claim 2, 3 or 4, characterized in that: the thickness of the zinc oxide film is 20-2000 nm.
6. The utility model provides an antibiotic non-woven fabrics of nanometer zinc oxide, includes the non-woven fabrics body, its characterized in that: the non-woven fabric body is sputtered with a zinc oxide film.
7. The nano zinc oxide antibacterial non-woven fabric according to claim 6, characterized in that: the thickness of the zinc oxide film is 20-2000 nm.
8. A medical mask containing nano zinc oxide antibacterial non-woven fabric is characterized in that: include in proper order from outside to inside and refuse to glue and glue nonwoven layer, the antibiotic nonwoven layer of nanometer zinc oxide, electret polypropylene and glue nonwoven layer, hydrophilic super gentle spunbond nonwoven layer, the antibiotic nonwoven layer of nanometer zinc oxide includes the non-woven fabrics body, has sputtered the zinc oxide film on this non-woven fabrics body.
9. The medical mask containing nano zinc oxide antibacterial non-woven fabric according to claim 8, characterized in that: the thickness of the zinc oxide film is 20-2000 nm.
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