CN110983269B - Ag/TiO based on magnetron sputtering2Heat insulation fabric and preparation method thereof - Google Patents
Ag/TiO based on magnetron sputtering2Heat insulation fabric and preparation method thereof Download PDFInfo
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- CN110983269B CN110983269B CN201911214098.XA CN201911214098A CN110983269B CN 110983269 B CN110983269 B CN 110983269B CN 201911214098 A CN201911214098 A CN 201911214098A CN 110983269 B CN110983269 B CN 110983269B
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- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 75
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 72
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- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 claims description 79
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 77
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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
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/083—Oxides of refractory metals or yttrium
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
- C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
-
- 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
- C23C14/58—After-treatment
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- Chemical Or Physical Treatment Of Fibers (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公开了一种基于磁控溅射的Ag/TiO2隔热织物及其制备方法，该Ag/TiO2隔热织物包括依次制备在棉/粘胶水刺无纺布基材上的TiO2过渡层、金属银反射层以及水性聚氨酯共混ATO保护层。该Ag/TiO2隔热织物可有效反射红外线，以实现隔热的效果。Ag/TiO2隔热织物采用的多层复合结构赋予了棉/粘胶水刺无纺布基材更多的优异性能，增强了织物的隔热性，拓展了织物的应用领域。该织物设置有气孔，使得其具有良好的透气性能。
The invention discloses a magnetron sputtering-based Ag/TiO 2 heat-insulating fabric and a preparation method thereof. The Ag/TiO 2 heat-insulating fabric comprises TiO sequentially prepared on a cotton/viscose spunlace non-woven substrate. 2. Transition layer, metallic silver reflective layer and water-based polyurethane blended ATO protective layer. The Ag/TiO 2 heat insulating fabric can effectively reflect infrared rays to achieve the effect of heat insulation. The multi-layer composite structure adopted by the Ag/TiO 2 thermal insulation fabric endows the cotton/viscose spunlace non-woven fabric with more excellent properties, enhances the thermal insulation of the fabric, and expands the application field of the fabric. The fabric is provided with air holes so that it has good air permeability.
Description
Technical Field
The invention relates to the field of functional textiles, in particular to Ag/TiO based on magnetron sputtering2A heat insulating fabric and a method for preparing the same.
Background
With the continuous change of global climate environment, the sun-proof and heat-insulating requirements of outdoor activities on functional textiles are continuously improved, and the sun-proof and heat-insulating properties of common textiles generally cannot meet the special requirements of consumers, so that research and development of functional fabrics with sun-proof and heat-insulating properties and clothes thereof become a research hotspot in the field of industrial textiles. In addition, the functional textile with sun-proof and heat-insulating properties has wide application requirements in the fields of military industry, fire fighting, aerospace, building, transportation and the like.
In time and areas with high sun intensity, when people engaged in outdoor exercises wear clothes, the influence of heat generated by solar radiation on the fabric needs to be considered, on one hand, the fabric surface absorbs sunlight to cause the temperature of the fabric surface to rise, further the temperature of a human body to rise, and the comfort level of the human body during wearing clothes is reduced; on the other hand, an increase in temperature will cause the polymer material constituting the fabric to age, even photodegrade, causing damage to the fabric.
The sun-proof heat insulation fabric has a certain structure and can block three transmission modes of heat: heat conduction, heat convection, heat radiation. The visible light and the infrared ray in the sunlight are transmitted by means of heat radiation, and account for nearly 90% of the energy of the sunlight radiation, so the sun-proof heat-insulating fabric mainly isolates the visible light and the infrared ray.
The most important means for blocking visible light and infrared light is reflection, and the surface of the fabric is usually made of natural materials or chemical fibers, so that the visible light and the infrared light cannot be sufficiently reflected, and the surface of the fabric needs to be functionalized to achieve the function of light reflection.
The reflection capacity of substances to light or electromagnetic waves is different, and metals generally have better light reflection capacity due to a regular crystalline structure, so a sun-proof heat insulation design can be carried out by adopting a fabric surface metallization mode. There are several common ways of fabric surface metallization: electron beam evaporation, magnetron sputtering, gold stamping, chemical deposition and the like.
The electron beam evaporation is to bombard the coating material with heating electrons, and the kinetic energy of the electrons is converted into heat energy, so that the target material is heated and evaporated and forms a film. Suitable for evaporating high-melting point metal or compound, Chinese patent: CN103924198A discloses a method for preparing a graphene conductive film by electron beam evaporation, which is disclosed in the chinese patent: CN102169944B discloses a light emitting diode of Ag/ITO/zinc oxide based composite transparent electrode and a preparation method thereof. On the mature technical level of equipment application, people make great innovation progress, and Chinese patents: CN102492924A discloses a free ion bombardment assisted electron beam evaporation equipment and a method for coating film by using the same, which solves the problem of low binding force between films, chinese patent: CN104611682A discloses a magnetron sputtering winding film coating machine with double-sided reciprocating continuous film coating, which improves the efficiency, simplifies the machine and reduces the occupied area. However, for many compounds, electron beam evaporation is not suitable because it causes thermal decomposition.
The gold stamping fabric mainly utilizes the electrochemical aluminum printing foil, and transfers the pattern on the electrochemical aluminum printing foil to the fabric by a method of increasing temperature or applying pressure. Nowadays, gold stamping fabrics have many applications, and Chinese patents: CN206062846U discloses a preparation method of a flame-retardant gold stamping curtain, which comprises the following steps: CN205822633U discloses a preparation method of gilt wall paper. However, the gilt fabric is poor in air permeability, so that when a human body is heated and pores sweat and dissipate heat, the heat cannot be dissipated, the internal temperature of the clothes is too high, and poor dressing feeling is brought to people.
Magnetron sputtering means that electrons collide with argon atoms in the process of flying to a substrate under the action of an electric field, the argon atoms generate Ar ions and new electrons, the Ar ions accelerate to impact a target under the action of the electric field, a large number of target atoms are sputtered, and neutral target atoms are deposited on a base material. A layer of film is sputtered on the surface of the fabric by utilizing the magnetron sputtering technology, so that a functional film is easily obtained, and the method comprises the following steps: CN106637590B discloses a high light-transmitting heat-insulating fabric and its manufacturing method, chinese patent: CN102779988B discloses a method for modifying a composite negative electrode material coating film of a lithium ion battery, which is widely applied in the industries of solar batteries, semiconductors and the like, and the chinese patent: CN102779988B discloses a method for modifying a composite negative electrode material coating of a lithium ion battery, which is disclosed in the chinese patent: CN103280498B discloses a method for preparing a pointed conical zinc oxide/nickel oxide heterojunction diode. The magnetron sputtering coating has high deposition efficiency and high repeatability, can continuously and efficiently obtain a film with uniform thickness, and is easy for industrial operation.
The metal has a strong insulating effect on heat and can reflect heat of thermal radiation out. The metal silver reflecting film belongs to a high reflecting film, and the higher the glossiness of the surface of the reflecting film is, the higher the reflectivity is. Before and after heating, the reflectivity is not easy to change and soften, the highest reflectivity of visible light and infrared ray can reach more than 90%, and the Chinese patent is as follows: CN104685108B discloses a silver reflective film, a light reflective member and a method for manufacturing the light reflective member, and therefore, it has been a focus of research to isolate light radiation by using metallic silver.
Rutile type TiO2The refractive index of (a) is 2.5-2.8, and the material belongs to an inorganic oxide with a higher refractive index. A large refractive index difference is generated between the TiO2 and a film-forming substance, so that the light scattering capability of the film layer can be effectively enhanced, the visible light and near infrared light reflectivity of the film layer is improved, and the method is disclosed in the Chinese patent: CN104264112B discloses a vacuum optical coating method for a matte film. Rutile TiO2 is therefore also widely used in the field of thermal insulation.
Nanometer tin antimony oxide (ATO) is a transparent material with good conductivity, electron holes are formed in conductive particles of the ATO, absorption of current carriers can be caused, the absorption is close to one percent of absorption in an ultraviolet region (200-380nm), and a good blocking effect is achieved on visible light and infrared rays.
Disclosure of Invention
The invention aims to provide Ag/TiO based on magnetron sputtering according to the defects of the prior art2The method combines magnetron sputtering technology with metal and compounds, and provides a breathable fabric with high heat insulation and high production speed through after-treatment.
The invention provides Ag/TiO based on magnetron sputtering2Heat-insulating fabric comprising TiO sequentially prepared on cotton/viscose spunlace nonwoven fabric substrate2The coating comprises a transition layer, a metal silver reflecting layer and a waterborne polyurethane blended ATO protective layer;
wherein the mass percentage of the cotton/viscose spunlace non-woven fabric base material is 50-60%; the mass percentage of the TiO2 transition layer is 5-10%; the mass percentage of the metal silver reflecting layer is 10-25%; the mass percentage of the waterborne polyurethane blended ATO protective layer is 15-25%;
the cotton/viscose spunlace non-woven fabric base material is prepared by viscose fibers and cotton fibers in a mass ratio of 7:3 through carding and water needling processes;
the TiO is2The transition layer comprises TiO2Particles of TiO2The particles are uniformly distributed and attached to the surface of the cotton/viscose spunlace non-woven fabric substrate; the TiO is2The particles are inserted into the gaps extending to the cotton/viscose spunlace non-woven fabric base material to form a compact structure with the cotton/viscose spunlace non-woven fabric base material;
the metal silver reflecting layer is a film with a reticular structure formed by uniformly arranging a plurality of silver particles, has the thickness of 600-1500 nm, and is attached to the TiO2The surface of the transition layer; part of the silver particles being embedded in the TiO2The transition layer is filled with the TiO2A gap of the transition layer;
the Ag/TiO based on magnetron sputtering2The heat insulation fabric is provided with air holes formed by needling through a needling machine.
In a further improvement of the present invention, in the metallic silver reflective layer, the lateral direction and the longitudinal direction of the silver particles are both nano-scale.
The further improvement of the invention is that the thickness of the metallic silver reflecting layer is 900-1200 nm.
The invention is further improved in that the thickness of the cotton/viscose spunlace nonwoven fabric substrate is 1 mm.
The invention also provides Ag/TiO based on magnetron sputtering for preparing the Ag/TiO2A method of making a thermal insulating fabric, comprising the steps of:
(S1) cleaning the cotton/viscose spunlace non-woven fabric base material by using an organic solvent, and then carrying out low-pressure vacuum plasma etching; wherein, the parameters of the low-pressure vacuum plasma etching are as follows: the temperature is 30-10 DEG CAt 0 deg.C and under a pressure of 8X 10-4～1×10-3Pa, power supply power of 150-250W, time of 13-17 minutes, and working gas of argon;
(S2) with TiO2Performing magnetron sputtering to prepare TiO on the surface of the cotton/viscose spunlace non-woven fabric substrate as a target material2A transition layer; wherein the parameters of magnetron sputtering include: the distance between the cotton/viscose spunlace non-woven fabric substrate and the target is 100mm, the purity of the working gas is 98-99.9% of argon, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, the gas flow rate is 6-8 sccm, the substrate rotating speed is 9-11 r/min, the magnetron sputtering power is 145-255W, and the magnetron sputtering time is 9-16 min;
(S3) using Ag as target material in TiO2The surface of the transition layer is attached with a metal silver reflecting layer by a magnetron sputtering process; wherein the parameters of magnetron sputtering include: the distance between the substrate and the target material is 100mm, the purity of the working gas is 98-99.9% of argon, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, the gas flow rate is 6-8 sccm, the substrate rotating speed is 9-12 r/min, the magnetron sputtering power is 140-160W, and the magnetron sputtering time is 5-10 min;
(S4) preparing a nano ATO transparent heat-insulating coating by mixing the waterborne polyurethane resin (PU), the nano Antimony Tin Oxide (ATO) water-based slurry and the thickening and leveling agent; coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer by using a wire bar coater, standing at room temperature until the surface is dry, then placing in an electric heating air blast constant-temperature drying box, and curing to obtain a waterborne polyurethane blending ATO protective layer;
(S5) applying the Ag/TiO based on magnetron sputtering by using a needle machine2The heat insulating fabric is needled to form the air holes.
The invention has the further improvement that in the process of cleaning the cotton/viscose spunlace non-woven fabric base material, the cotton/viscose spunlace non-woven fabric base material is ultrasonically cleaned in ethanol for 30min, and then rinsed by distilled water and dried by an oven; wherein the rinsing mode is ultrasonic or soaking, and the rinsing time is 0.5-5 h; the drying temperature is 120 deg.C, and the drying time is 20 min.
In a further development of the invention, in step (S1), the parameters for the low-pressure vacuum plasma etching of the cotton/viscose spunlace nonwoven fabric substrate are: the temperature is 80 ℃, the background vacuum degree is 9 multiplied by 10-4Pa, the power of the power supply is 200W; the time is 15 minutes; the inert gas is argon.
The invention has the further improvement that in the process of preparing the nano ATO transparent heat-insulating coating, a certain amount of waterborne polyurethane resin (PU) is taken, the nano Antimony Tin Oxide (ATO) waterborne slurry is added into an experimental dispersing sand mill according to the weight ratio of the waterborne polyurethane resin to the nano antimony tin oxide waterborne slurry of 1:3, and the thickening and leveling agent is added for stirring, and the nano ATO transparent heat-insulating coating is prepared after even stirring; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the blending process, the rotating speed of the mill is 300 r/min-500 r/min, and the thickening and leveling agent is added and stirred for 30 min.
The invention has the further improvement that a wire bar coater adopted in the process of coating the nano ATO transparent heat-insulating coating is 20-40 μm; in the process of curing in the electric heating blowing constant-temperature drying oven, the curing temperature is 70-100 ℃, and the curing time is 3-4 h.
The invention further improves the Ag/TiO based on magnetron sputtering2In the process of needling the heat-insulating fabric, the straight true density of a needle plate is 4000 needles/m2The length of the needle is 20.2mm, the fineness of the needle is 0.5mm, the surface has no barb, the aqueous polyurethane blended ATO protective layer faces upwards, and the needle punching is carried out for three times.
The invention has the advantages that: Ag/TiO 22The heat insulation fabric can effectively reflect infrared rays to realize the heat insulation effect. Ag/TiO 22The multilayer composite structure adopted by the heat insulation fabric endows the cotton/viscose spunlace non-woven fabric substrate with more excellent performances, enhances the heat insulation property of the fabric, and expands the application field of the fabric.
Drawings
FIG. 1 shows Ag/TiO based on magnetron sputtering of the invention2A schematic cross-sectional view of an insulating fabric;
FIG. 2 is a schematic view of a magnetron sputtering apparatus used in the present invention.
Detailed Description
The features of the present invention and other related features are described in further detail below by way of example in conjunction with the following drawings to facilitate understanding by those skilled in the art:
example (b): as shown in FIG. 1, embodiments of the present invention include a magnetron sputtering based Ag/TiO2A heat-insulating fabric comprising TiO sequentially prepared on a cotton/viscose spunlace nonwoven fabric substrate 212A transition layer 22, a metallic silver reflecting layer 23 and a water-based polyurethane blended ATO protective layer 24.
Ag/TiO based on magnetron sputtering in this example2In the heat insulation fabric, the mass percentage of the cotton/viscose spunlace non-woven fabric base material 21 is 50-60%; TiO22The mass percent of the transition layer 22 is 5-10%; the mass percent of the metallic silver reflecting layer 23 is 10% -25%; the mass percentage of the water-based polyurethane blended ATO protective layer 24 is 15% -25%.
The cotton/viscose spunlace non-woven fabric base material 21 is prepared by carding and water needling of viscose fibers and cotton fibers in a mass ratio of 7:3, and has the water absorption capacity of the viscose fibers and the strength of the cotton fibers. The thickness of the cotton/viscose spunlace nonwoven fabric substrate 21 is 1 mm. TiO22The transition layer 22 comprises TiO2Particles of TiO2The particles are uniformly arranged and attached on the surface of the cotton/viscose spunlace non-woven fabric substrate 21, and part of TiO is2The particles penetrate and extend into the gaps of the cotton/viscose spunlace non-woven fabric base material 21 to form a compact structure with the cotton/viscose spunlace non-woven fabric base material 21 so as to prevent the metal silver reflecting layer 23 from being oxidized by air.
In this embodiment, the metallic silver reflective layer 23 is a film with a mesh structure formed by uniformly arranging a plurality of silver particles, and the thickness is 600-1500 nm. A metallic silver reflective layer 23 is attached to the TiO2The surface of the transition layer 22; partial silver particles being embedded in TiO2The transition layer 22 is filled with TiO2The gap of the transition layer 22. In the metallic silver reflecting layer 23, the silver particles are nano-sized in both the transverse direction and the longitudinal direction, and the size of the silver particles is closer to the wavelength of infrared rays, so that the silver particles can effectively reflect the infrared rays, and Ag/TiO based on magnetron sputtering2The heat insulating fabric may have a good heat insulating effect.
In order to enhance the permeability, the Ag/TiO based on magnetron sputtering2The heat insulation fabric is provided with air holes formed by needling through a needling machine. The air holes enable Ag/TiO based on magnetron sputtering2The heat insulation fabric can keep air permeability while insulating heat.
Ag/TiO based on magnetron sputtering in this example2The insulating fabric can be used to make garments. Ag/TiO based on magnetron sputtering2The side of the heat-insulating fabric provided with the metal silver reflecting layer 23 can be used for reflecting infrared rays, and the side faces outwards can be used for outdoor clothes in summer to reflect infrared rays in sunlight; the side faces inwards, and the clothes can be used for clothes in winter, and can reflect infrared rays radiated by a human body to avoid heat loss. Meanwhile, the air holes can discharge damp air caused by perspiration, so that the clothes have good air permeability.
Ag/TiO based on magnetron sputtering in this example2The heat-insulating fabric adopts a cotton/viscose spunlace non-woven fabric substrate 21 and TiO2The transition layer 22, the metal silver reflecting layer 23 and the water-based polyurethane blended ATO protective layer 24 are combined, so that the bonding capability among the layers is stronger, and the durability is better. The waterborne polyurethane blended ATO protective layer 24 is good in flexibility and better in wear resistance, and the waterborne polyurethane blended ATO protective layer 24 cannot be abraded and peeled off due to friction in the daily use process. The cotton/viscose spunlace non-woven fabric substrate 21 is used as a substrate, the fibers of the substrate are irregularly distributed in a net shape and have more gaps, and TiO2The bonding performance of the transition layer 22 is better. In addition, the cotton/viscose spunlace nonwoven substrate 21 is more flexible, making the final product comfortable to wear. The cotton/viscose spunlace non-woven fabric base material 21 also has certain water absorption capacity, and the phenomenon that sweat gathers on the inner side of clothes to influence the wearing experience can be avoided.
In addition, some of the prior art blends Ag particles in the fiber or in the coating to achieve the infrared reflecting effect, but this way forms a fabric in which the Ag particles are arranged dispersedly. The incidence of infrared light into the fabric causes multiple reflections, so that part of the infrared light is absorbed during the multiple reflections. In the present embodiment, the silver reflective layer 23 has a layered structure, and has a better reflective effect for infrared rays.
In some embodiments, the thickness of the metallic silver reflecting layer is 900 to 1200 nm.
The embodiment of the invention also comprises Ag/TiO based on magnetron sputtering2A method for manufacturing a heat insulation fabric. The method adopts magnetron sputtering technology to sequentially prepare TiO on a cotton/viscose spunlace non-woven fabric substrate 212 A transition layer 22, a metallic silver reflecting layer 23 and a water-based polyurethane blended ATO protective layer 24. Specifically, the method comprises the following steps:
example 1:
Ag/TiO based on magnetron sputtering of this example2The method for manufacturing the heat insulation fabric comprises the following steps:
(1) the cotton/viscose spunlace nonwoven fabric substrate 21 is cleaned. In the cleaning process, the cotton/viscose spunlace non-woven fabric base material is ultrasonically cleaned in ethanol (the purity is more than 99%) for 30min, the cotton/viscose spunlace non-woven fabric base material 21 is rinsed by distilled water after the cleaning is finished, and the drying oven is used for drying; wherein the rinsing mode is ultrasonic or soaking, and the rinsing time is 0.5-5 h; the drying temperature of the oven is 120 ℃ and the drying time is 20 min.
(2) Carrying out low-pressure vacuum plasma etching on the cotton/viscose spunlace non-woven fabric substrate 21; wherein, the parameters of the low-pressure vacuum plasma etching are as follows: background vacuum degree of 9X 10-4Pa, power supply power of 200W, time of 15 minutes, and working gas of argon. After plasma treatment, the fiber surface is rougher, so that the fibers and TiO of the cotton/viscose spunlace non-woven fabric substrate 212The bonding is easier.
(3) Preparation of TiO2 A transition layer 22. In a magnetron sputtering coating system (model MSP-300C), the cotton/viscose spunlace nonwoven fabric base material 21 to be sputtered prepared in the step (2) is placed on a sample table, and TiO is added2The target material is arranged in a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the vacuum degree in the chamber reaches 9 multiplied by 10-4Pa; then high-purity argon is introduced into the sputtering chamber until the air pressure in the sputtering chamber reaches 0.7 Pa. Opening of TiO2RF power applied to the target begins to strike the TiO2Sputtering of target material to clean TiO2And sputtering the surface of the target for 1 min. To TiO22After the surface of the target material is cleaned, the TiO is closed2The RF power applied to the target was set to 150W. Rotating the substrate to be sputtered to TiO2Target site, turn on TiO2Sputtering target position radio frequency power supply at 80 deg.C for 15min to obtain film-like TiO2 A transition layer 22.
Fig. 2 shows a magnetron sputtering apparatus used in this embodiment, which includes a motor 1, a heating coil 2, an object stage 3, a lifting cover 4, a baffle 4, a target 6, a radio frequency power supply 7, a direct current power supply 8, an Ar channel 9, an Ar switch 10, and a vacuum switch 11. The base of the stage 3 serves as a base for the cotton/viscose spunlace nonwoven fabric substrate 21, which can be considered as flush.
In the sputtering process, the cotton/viscose spunlace non-woven fabric base material 21 and TiO2The distance between the targets is 100mm, the purity of the working gas argon is 98-99.9%, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, a gas flow rate of 7sccm, and a base rotation speed of 10r/min, wherein the base is a cotton/viscose spunlace nonwoven fabric substrate 21 in this embodiment.
(4) In TiO2The surface of the transition layer 22 is provided with a metallic silver reflecting layer 23. In the process, the direct current power supply is replaced, and the flow of the high-purity argon introduced into the sputtering chamber is adjusted to be 10 sccm; background vacuum degree of 9X 10-4Pa; and rotating the hollow substrate to the Ag target position, turning on a direct-current power supply applied to the Ag target, and starting sputtering the Ag target to clean the surface of the Ag target for 1 min. And after the surface of the Ag target is cleaned, closing the direct current power supply applied to the Ag target, and setting the direct current sputtering power to be 150W. And (3) rotating the substrate to be sputtered to an Ag target position, starting an Ag target position direct current power supply, and sputtering for 5min at room temperature to obtain the film-shaped metal silver reflecting layer 23.
Other parameters in the sputtering process include: substrate (with TiO)2The distance between the cotton/viscose spunlace non-woven fabric base material 21) of the transition layer 22 and the target is 100mm, the working gas is argon, the purity is 98-99.9%, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, gas flow rateThe flow rate of the substrate was 7sccm and the substrate rotation rate was 10 r/min. In the metallic silver reflective layer 23, the size of the silver particles can be controlled by the amount of argon gas flow and the degree of vacuum in the magnetron sputtering process. In this embodiment, the silver particles in the Ag film are fine and smooth due to the argon flow and the vacuum degree, and infrared rays can be effectively reflected.
(5) And preparing a water-based polyurethane blended ATO protective layer 24 on the surface of the metal silver reflecting layer 23.
Firstly, preparing the nano ATO transparent heat-insulating coating. In the preparation process, a certain amount of waterborne polyurethane resin (PU) is taken, and nanometer tin antimony oxide (ATO) waterborne slurry is added by an experimental dispersing sand mill according to a certain proportion, wherein the weight ratio of the nanometer tin antimony oxide (ATO) waterborne slurry to the polyurethane resin is 1:3, adding a proper amount of thickening and leveling agent, stirring, and uniformly stirring to obtain the nano ATO transparent heat-insulating coating; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the preparation process, the rotating speed of the mill is 400r/min, and the thick leveling agent is added and stirred for about 30 min.
And then, coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer 23 through a wire bar coater, then, putting the coating to be surface-dried at room temperature, then, putting the coating in an electric heating blowing constant-temperature drying box, and curing for 4h at 80 ℃ to obtain the waterborne polyurethane blended ATO protective layer 24. A wire bar coater adopted in the process of coating the nano ATO transparent heat-insulating coating is 30 microns; during the curing process in the electrothermal blowing constant temperature drying oven.
(6) Forming the air holes. Magnetron sputtering based on Ag/TiO using a needle machine2The heat insulating fabric is needled to form the air holes. The air holes sequentially penetrate through the waterborne polyurethane blended ATO protective layer 24, the metal silver reflecting layer 23 and the TiO2 A transition layer 22 and a cotton/viscose spunlace nonwoven fabric substrate 21. In the needling process, the straight true density of a needle plate is 4000 needles/m 2, the needle length is 20.2mm, the needle fineness is 0.5mm, no barb exists on the surface, the aqueous polyurethane blended ATO protective layer faces upwards, and needling is carried out for three times.
Example 2:
Ag/TiO based on magnetron sputtering of this example2The method for manufacturing the heat insulation fabric comprises the following steps:
(1) the cotton/viscose spunlaced nonwoven fabric substrate 21 is cleaned in the same manner as in example 1.
(2) The cotton/viscose spunlace nonwoven fabric substrate 21 was subjected to low pressure vacuum plasma etching, which was the same as in example 1.
(3) Preparation of TiO2 A transition layer 22. In a magnetron sputtering coating system (model MSP-300C), the cotton/viscose spunlace nonwoven fabric base material 21 to be sputtered prepared in the step (2) is placed on a sample table, and TiO is added2The target material is arranged in a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the vacuum degree in the chamber reaches 9 multiplied by 10-4Pa; then high-purity argon is introduced into the sputtering chamber until the air pressure in the sputtering chamber reaches 0.7 Pa. Opening of TiO2RF power applied to the target begins to strike the TiO2Sputtering of target material to clean TiO2And sputtering the surface of the target for 1 min. To TiO22After the surface of the target material is cleaned, the TiO is closed2The RF power applied to the target was set to 200W. Rotating the substrate to be sputtered to TiO2Target site, turn on TiO2Sputtering target position radio frequency power supply at 80 deg.C for 10min to obtain film-like TiO2 A transition layer 22.
In the sputtering process, the cotton/viscose spunlace non-woven fabric base material 21 and TiO2The distance between the targets is 100mm, the purity of the working gas argon is 98-99.9%, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, a gas flow rate of 7sccm, and a base rotation speed of 10r/min, wherein the base is a cotton/viscose spunlace nonwoven fabric substrate 21 in this embodiment.
(4) In TiO2The surface of the transition layer 22 is provided with a metallic silver reflecting layer 23. In the process, the direct current power supply is replaced, and the flow of the high-purity argon introduced into the sputtering chamber is adjusted to be 10 sccm; background vacuum degree of 9X 10-4Pa; and rotating the hollow substrate to the Ag target position, turning on a direct-current power supply applied to the Ag target, and starting sputtering the Ag target to clean the surface of the Ag target for 1 min. And after the surface of the Ag target is cleaned, closing the direct current power supply applied to the Ag target, and setting the direct current sputtering power to be 150W. Rotating the substrate to be sputtered to an Ag target position, starting an Ag target position direct current power supply, and sputtering for 10min at room temperature to obtain a film-shaped metalA silver reflective layer 23.
Other parameters in the sputtering process include: substrate (with TiO)2The distance between the cotton/viscose spunlace non-woven fabric base material 21) of the transition layer 22 and the target is 100mm, the working gas is argon, the purity of the argon is 98-99.9 percent, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, gas flow rate of 7sccm, and substrate rotation speed of 10 r/min. In the metallic silver reflective layer 23, the size of the silver particles can be controlled by the amount of argon gas flow and the degree of vacuum in the magnetron sputtering process. In this embodiment, the silver particles in the Ag film are fine and smooth due to the argon flow and the vacuum degree, and infrared rays can be effectively reflected.
(5) And preparing a water-based polyurethane blended ATO protective layer 24 on the surface of the metal silver reflecting layer 23.
Firstly, preparing the nano ATO transparent heat-insulating coating. In the preparation process, a certain amount of waterborne polyurethane resin (PU) is taken, and nanometer tin antimony oxide (ATO) waterborne slurry is added by an experimental dispersing sand mill according to a certain proportion, wherein the weight ratio of the nanometer tin antimony oxide (ATO) waterborne slurry to the polyurethane resin is 1:3, adding a proper amount of thickening and leveling agent, stirring, and uniformly stirring to obtain the nano ATO transparent heat-insulating coating; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the preparation process, the rotating speed of the mill is 400r/min, and the thick leveling agent is added and stirred for about 30 min.
And then, coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer 23 through a wire bar coater, then, putting the coating to be surface-dried at room temperature, then, putting the coating in an electric heating blowing constant-temperature drying box, and curing for 4h at 80 ℃ to obtain the waterborne polyurethane blended ATO protective layer 24. A wire bar coater adopted in the process of coating the nano ATO transparent heat-insulating coating is 30 microns; during the curing process in the electrothermal blowing constant temperature drying oven.
(6) Forming the air holes. Magnetron sputtering based on Ag/TiO using a needle machine2The heat insulating fabric is needled to form the air holes. The air holes sequentially penetrate through the waterborne polyurethane blended ATO protective layer 24, the metal silver reflecting layer 23 and the TiO2 A transition layer 22 and a cotton/viscose spunlace nonwoven fabric substrate 21. In the needling process, the straight true density of the needle plate is 4000 needles/m2The needle length is 20.2mm, the needle fineness is 0.5mm, the surface has no barb, and the waterborne polyurethane is totally usedThe ATO mixture was needled three times with the protective layer facing up.
Example 3:
Ag/TiO based on magnetron sputtering of this example2The method for manufacturing the heat insulation fabric comprises the following steps:
(1) the cotton/viscose spunlace nonwoven fabric substrate 21 was cleaned in the same manner as in example 1.
(2) The cotton/viscose spunlace nonwoven fabric substrate 21 was subjected to low pressure vacuum plasma etching, which was the same as in example 1.
(3) Preparation of TiO2 A transition layer 22. In a magnetron sputtering coating system (model MSP-300C), the cotton/viscose spunlace nonwoven fabric base material 21 to be sputtered prepared in the step (2) is placed on a sample table, and TiO is added2The target material is arranged in a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the vacuum degree in the chamber reaches 9 multiplied by 10-4Pa; then high-purity argon is introduced into the sputtering chamber until the air pressure in the sputtering chamber reaches 0.7 Pa. Opening of TiO2RF power applied to the target begins to strike the TiO2Sputtering of target material to clean TiO2And sputtering the surface of the target for 1 min. To TiO22After the surface of the target material is cleaned, the TiO is closed2The RF power applied to the target was set to 250W. Rotating the substrate to be sputtered to TiO2Target site, turn on TiO2Sputtering target position radio frequency power supply at 80 deg.C for 15min to obtain film-like TiO2 A transition layer 22.
In the sputtering process, the cotton/viscose spunlace non-woven fabric base material 21 and TiO2The distance between the targets is 100mm, the purity of the working gas argon is 98-99.9%, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, gas flow rate of 7sccm, and substrate rotation speed of 10 r/min. In this embodiment, the base is a cotton/viscose spunlace nonwoven fabric substrate 21.
(4) In TiO2The surface of the transition layer 22 is provided with a metallic silver reflecting layer 23. In the process, the direct current power supply is replaced, and the flow of the high-purity argon introduced into the sputtering chamber is adjusted to be 10 sccm; background vacuum degree of 9X 10-4Pa; rotating the empty base support to the Ag target positionAnd starting a direct-current power supply applied to the Ag target, and starting sputtering the Ag target to clean the surface of the Ag target, wherein the sputtering time is 1 min. And after the surface of the Ag target is cleaned, closing the direct current power supply applied to the Ag target, and setting the direct current sputtering power to be 150W. And (3) rotating the substrate to be sputtered to an Ag target position, starting an Ag target position direct current power supply, and sputtering for 10min at room temperature to obtain the film-shaped metal silver reflecting layer 23.
Other parameters in the sputtering process include: substrate (with TiO)2The distance between the cotton/viscose spunlace non-woven fabric base material 21) of the transition layer 22 and the target is 100mm, the working gas is argon, the purity of the argon is 98-99.9 percent, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, gas flow rate of 7sccm, and substrate rotation speed of 10 r/min. In the metallic silver reflective layer 23, the size of the silver particles can be controlled by the amount of argon gas flow and the degree of vacuum in the magnetron sputtering process. In this embodiment, the silver particles in the Ag film are fine and smooth due to the argon flow and the vacuum degree, and infrared rays can be effectively reflected.
(5) And preparing a water-based polyurethane blended ATO protective layer 24 on the surface of the metal silver reflecting layer 23.
Firstly, preparing the nano ATO transparent heat-insulating coating. In the preparation process, a certain amount of waterborne polyurethane resin (PU) is taken, and nanometer tin antimony oxide (ATO) waterborne slurry is added by an experimental dispersing sand mill according to a certain proportion, wherein the weight ratio of the nanometer tin antimony oxide (ATO) waterborne slurry to the polyurethane resin is 1:3, adding a proper amount of thickening and leveling agent, stirring, and uniformly stirring to obtain the nano ATO transparent heat-insulating coating; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the preparation process, the rotating speed of the mill is 400r/min, and the thick leveling agent is added and stirred for about 30 min.
And then, coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer 23 through a wire bar coater, then, putting the coating to be surface-dried at room temperature, then, putting the coating in an electric heating blowing constant-temperature drying box, and curing for 4h at 80 ℃ to obtain the waterborne polyurethane blended ATO protective layer 24. A wire bar coater adopted in the process of coating the nano ATO transparent heat-insulating coating is 30 microns; during the curing process in the electrothermal blowing constant temperature drying oven.
(6) Air permeable holes were formed, and the process was the same as in example 1.
Comparative example 1
Ag/TiO based on magnetron sputtering of this comparative example2The method for manufacturing the heat insulation fabric comprises the following steps:
(1) the cotton/viscose spunlace nonwoven fabric substrate 21 was cleaned in the same manner as in example 1.
(2) The cotton/viscose spunlace nonwoven fabric substrate 21 was subjected to low pressure vacuum plasma etching, which was the same as in example 1.
(3) Preparation of TiO2 A transition layer 22. In a magnetron sputtering coating system (model MSP-300C), the cotton/viscose spunlace nonwoven fabric base material 21 to be sputtered prepared in the step (2) is placed on a sample table, and TiO is added2The target material is arranged in a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the vacuum degree in the chamber reaches 1 multiplied by 10-3Pa; then high-purity argon is introduced into the sputtering chamber until the air pressure in the sputtering chamber reaches 0.7 Pa. Opening of TiO2RF power applied to the target begins to strike the TiO2Sputtering of target material to clean TiO2And sputtering the surface of the target for 1 min. To TiO22After the surface of the target material is cleaned, the TiO is closed2The RF power applied to the target was set to 90W. Rotating the substrate to be sputtered to TiO2Target site, turn on TiO2Sputtering target position radio frequency power supply at 80 deg.C for 15min to obtain film-like TiO2 A transition layer 22.
(4) In TiO2The surface of the transition layer 22 is provided with a metallic silver reflecting layer 23. In the process, the direct current power supply is replaced, and the flow of the high-purity argon introduced into the sputtering chamber is adjusted to be 10 sccm; background vacuum degree of 9X 10-4Pa; and rotating the hollow substrate to the Ag target position, turning on a direct-current power supply applied to the Ag target, and starting sputtering the Ag target to clean the surface of the Ag target for 1 min. And after the surface of the Ag target material is cleaned, closing the direct current power supply applied to the Ag target material, and setting the direct current sputtering power to be 50W. And (3) rotating the substrate to be sputtered to an Ag target position, starting an Ag target position direct current power supply, and sputtering for 10min at room temperature to obtain the film-shaped metal silver reflecting layer 23.
(5) And preparing a water-based polyurethane blended ATO protective layer 24 on the surface of the metal silver reflecting layer 23.
Firstly, preparing the nano ATO transparent heat-insulating coating. In the preparation process, a certain amount of waterborne polyurethane resin (PU) is taken, and nanometer tin antimony oxide (ATO) waterborne slurry is added by an experimental dispersing sand mill according to a certain proportion, wherein the weight ratio of the nanometer tin antimony oxide (ATO) waterborne slurry to the polyurethane resin is 1: 3.5, adding a proper amount of thickening and leveling agent, stirring, and uniformly stirring to obtain the nano ATO transparent heat-insulating coating; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the preparation process, the rotating speed of the mill is 400r/min, and the thick leveling agent is added and stirred for about 40 min.
And then, coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer 23 through a wire bar coater, then, putting the coating to be surface-dried at room temperature, then, putting the coating in an electric heating blowing constant-temperature drying box, and curing for 4h at 80 ℃ to obtain the waterborne polyurethane blended ATO protective layer 24. The wire bar coater adopted in the process of coating the nano ATO transparent heat insulation coating is 30 μm.
(6) Air permeable holes were formed, and the process was the same as in example 1.
Comparative example 2
Ag/TiO based on magnetron sputtering of this comparative example2The method for manufacturing the heat insulation fabric comprises the following steps:
(1) the cotton/viscose spunlace nonwoven fabric substrate 21 was cleaned in the same manner as in example 1.
(2) The cotton/viscose spunlace nonwoven fabric substrate 21 was subjected to low pressure vacuum plasma etching, which was the same as in example 1.
(3) Preparation of TiO2 A transition layer 22. In a magnetron sputtering coating system (model MSP-300C), the cotton/viscose spunlace nonwoven fabric base material 21 to be sputtered prepared in the step (2) is placed on a sample table, and TiO is added2The target material is arranged in a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the vacuum degree in the chamber reaches 1 multiplied by 10-3Pa; then high-purity argon is introduced into the sputtering chamber until the air pressure in the sputtering chamber reaches 0.7 Pa. Opening of TiO2RF power applied to the target begins to strike the TiO2Sputtering of target material to clean TiO2And sputtering the surface of the target for 1 min. To TiO22After the surface of the target material is cleaned, the TiO is closed2The RF power applied to the target was set to 320W. Rotating the substrate to be sputtered to TiO2Target site, turn on TiO2Sputtering target position radio frequency power supply at 80 deg.C for 15min to obtain film-like TiO2 A transition layer 22.
(4) In TiO2The surface of the transition layer 22 is provided with a metallic silver reflecting layer 23. In the process, the direct current power supply is replaced, and the flow of the high-purity argon introduced into the sputtering chamber is adjusted to be 10 sccm; background vacuum degree of 9X 10-4Pa; and rotating the hollow substrate to the Ag target position, turning on a direct-current power supply applied to the Ag target, and starting sputtering the Ag target to clean the surface of the Ag target for 1 min. And after the surface of the Ag target is cleaned, closing the direct current power supply applied to the Ag target, and setting the direct current sputtering power to be 250W. And (3) rotating the substrate to be sputtered to an Ag target position, starting an Ag target position direct current power supply, and sputtering for 10min at room temperature to obtain the film-shaped metal silver reflecting layer 23. Other parameters were the same as in example 1.
(5) And preparing a water-based polyurethane blended ATO protective layer 24 on the surface of the metal silver reflecting layer 23.
Firstly, preparing the nano ATO transparent heat-insulating coating. In the preparation process, a certain amount of waterborne polyurethane resin (PU) is taken, and nanometer tin antimony oxide (ATO) waterborne slurry is added by an experimental dispersing sand mill according to a certain proportion, wherein the weight ratio of the nanometer tin antimony oxide (ATO) waterborne slurry to the polyurethane resin is 1: 3.5, adding a proper amount of thickening and leveling agent, stirring, and uniformly stirring to obtain the nano ATO transparent heat-insulating coating; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the preparation process, the rotating speed of the mill is 400r/min, and the thick leveling agent is added and stirred for about 40 min.
And then, coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer 23 through a wire bar coater, then, putting the coating to be surface-dried at room temperature, then, putting the coating in an electric heating blowing constant-temperature drying box, and curing for 4h at 80 ℃ to obtain the waterborne polyurethane blended ATO protective layer 24. The wire bar coater adopted in the process of coating the nano ATO transparent heat insulation coating is 30 μm.
(6) Air permeable holes were formed, and the process was the same as in example 1.
< experiment >
< experiment 1>
The Ag/TiO of the above examples and comparative examples2The heat insulation fabric is respectively cut into blocks with the length of 10cm and the width of 10cm, a heat radiation heat insulation tester is used for testing the heat insulation effect, the testing distance is 5cm, and the data is shown in table 1. The thermal radiation heat insulation tester adopted in the experiment comprises an infrared heat source used for providing heat to Ag/TiO2The side of the heat-insulating fabric with the metal silver reflecting layer 23 emits infrared rays, Ag/TiO2The other side of the heat insulation fabric is in a room temperature environment, Ag/TiO2Thermocouples for measuring temperature are arranged on the front side and the back side of the heat insulation fabric.
TABLE 1 Ag/TiO of the above examples and comparative examples2Thermal insulation testing of thermal insulation fabrics
| Front temperature (. degree. C.) | Reverse temperature (. degree. C.) | Temperature difference (. degree. C.) | |
| Example 1 | 102 | 64 | 38 |
| Example 2 | 102 | 67 | 35 |
| Example 3 | 101 | 70 | 34 |
| Comparative example 1 | 102 | 75 | 27 |
| Comparative example 2 | 100 | 66 | 34 |
As can be seen from the above table, the temperature differences in examples 1, 2, and 3 and comparative example were all 34 ℃ or more, and had good high-temperature insulation effects, and the insulation effect of comparative example 1 was poor. Analysis showed that in examples 1, 2 and 3, Ag thin film and TiO were formed2The film and the ATO film had a good synergistic effect, the synergistic effect in comparative example 1 was poor, and the sample of comparative example 2 also had a good heat insulating effect because of its large thickness. In comparative example 2, the Ag film was thick, the cost was higher, the production efficiency was lower, but the heat insulating effect was not significantly improved.
< experiment 2>
The Ag/TiO of the above examples and comparative examples2The insulation fabric was subjected to abrasion resistance test and the data are shown in table 2.
TABLE 2 Ag/TiO of the above examples and comparative examples2Abrasion resistance test of Heat insulating Fabric
| Examples | Ag/TiO2Heat insulation fabricNumber of times of rubbing |
| Example 1 | 430 |
| Example 2 | 415 |
| Example 3 | 427 |
| Comparative example 1 | 354 |
| Comparative example 2 | 300 |
From the above table, examples 1, 2, and 3 all had good abrasion resistance and uniform distribution, comparative example 1 was no good abrasion resistance due to too low film thickness, and comparative example 2 was poor abrasion resistance due to too large thickness and poor binding force of TiO 2.
< experiment 3>
The Ag/TiO of the above examples and comparative examples2The insulation fabric was subjected to air permeability test and the data are shown in table 3.
TABLE 3 Ag/TiO of the above examples and comparative examples2Air permeability test of insulating fabrics
| Air permeability (mm/s) | |
| Example 1 | 159.2 |
| Example 2 | 162.3 |
| Example 3 | 150.5 |
| Comparative example 1 | 144.6 |
| Comparative example 2 | 153.4 |
The air permeability of the five schemes is uniform and is equivalent to that of common cotton fabrics, so that the heat-insulating fabric with better air permeability can be obtained by the needle punching method, and the heat-insulating effect of the fabric is not influenced.
Although specific embodiments of the present invention have been described above, it will be appreciated by those skilled in the art that these are merely examples and that many variations or modifications may be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is therefore defined by the appended claims.
Claims (10)
1. Ag/TiO based on magnetron sputtering2The heat insulation fabric is characterized by comprising TiO sequentially prepared on a cotton/viscose spunlace non-woven fabric substrate2The coating comprises a transition layer, a metal silver reflecting layer and a waterborne polyurethane blended ATO protective layer;
wherein the mass percentage of the cotton/viscose spunlace non-woven fabric base material is 50-60%; the mass percentage of the TiO2 transition layer is 5-10%; the mass percentage of the metal silver reflecting layer is 10-25%; the mass percentage of the waterborne polyurethane blended ATO protective layer is 15-25%;
the cotton/viscose spunlace non-woven fabric base material is prepared by viscose fibers and cotton fibers in a mass ratio of 7:3 through carding and water needling processes;
the TiO is2The transition layer comprises TiO2Particles of TiO2The particles are uniformly distributed and attached to the surface of the cotton/viscose spunlace non-woven fabric substrate; the TiO is2The particles are inserted into the gaps extending to the cotton/viscose spunlace non-woven fabric base material to form a compact structure with the cotton/viscose spunlace non-woven fabric base material;
the metal silver reflecting layer is a film with a reticular structure formed by uniformly arranging a plurality of silver particles, has the thickness of 600-1500 nm, and is attached to the TiO2The surface of the transition layer; part of the silver particles being embedded in the TiO2The transition layer is filled with the TiO2A gap of the transition layer;
the Ag/TiO based on magnetron sputtering2The heat insulation fabric is provided with air holes formed by needling through a needling machine.
2. The Ag/TiO based on magnetron sputtering of claim 12The heat insulation fabric is characterized in that in the metal silver reflecting layer, the transverse direction and the longitudinal direction of the silver particles are nano-scale.
3. The Ag/TiO based on magnetron sputtering of claim 12The heat insulation fabric is characterized in that the thickness of the metal silver reflecting layer is 900-1200 nm.
4. The Ag/TiO based on magnetron sputtering of claim 12The heat insulation fabric is characterized in that the thickness of the cotton/viscose spunlace non-woven fabric substrate is 1 mm.
5. A method for preparing Ag/TiO based on magnetron sputtering according to any one of claims 1 to 42A method of making a thermal insulating fabric, comprising the steps of:
(S1) CottonCleaning the viscose spunlace non-woven fabric base material by using an organic solvent, and then carrying out low-pressure vacuum plasma etching; wherein, the parameters of the low-pressure vacuum plasma etching are as follows: the temperature is 30-100 ℃, and the pressure is 8 multiplied by 10-4～1×10-3Pa, power supply power of 150-250W, time of 13-17 minutes, and working gas of argon;
(S2) with TiO2Performing magnetron sputtering to prepare TiO on the surface of the cotton/viscose spunlace non-woven fabric substrate as a target material2A transition layer; wherein the parameters of magnetron sputtering include: the distance between the cotton/viscose spunlace non-woven fabric substrate and the target is 100mm, the purity of the working gas is 98-99.9% of argon, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, the gas flow rate is 6-8 sccm, the substrate rotating speed is 9-11 r/min, the magnetron sputtering power is 145-255W, and the magnetron sputtering time is 9-16 min;
(S3) using Ag as target material in TiO2The surface of the transition layer is attached with a metal silver reflecting layer by a magnetron sputtering process; wherein the parameters of magnetron sputtering include: the distance between the substrate and the target material is 100mm, the purity of the working gas is 98-99.9% of argon, and the vacuum degree is 2.0 multiplied by 10-4～1.5×10-3Pa, the gas flow rate is 6-8 sccm, the substrate rotating speed is 9-12 r/min, the magnetron sputtering power is 140-160W, and the magnetron sputtering time is 5-10 min;
(S4) preparing a nano ATO transparent heat-insulating coating by mixing the waterborne polyurethane resin (PU), the nano Antimony Tin Oxide (ATO) water-based slurry and the thickening and leveling agent; coating the nano ATO transparent heat-insulating coating on the surface of the metal silver reflecting layer by using a wire bar coater, standing at room temperature until the surface is dry, then placing in an electric heating air blast constant-temperature drying box, and curing to obtain a waterborne polyurethane blending ATO protective layer;
(S5) applying the Ag/TiO based on magnetron sputtering by using a needle machine2The heat insulating fabric is needled to form the air holes.
6. Ag/TiO based on magnetron sputtering according to claim 52The preparation method of the heat insulation fabric is characterized in that the fabric is not spun-laced by cotton/viscose glueDuring the process of cleaning the spun fabric base material, ultrasonically cleaning the cotton/viscose spunlace non-woven fabric base material in ethanol for 30min, rinsing the cotton/viscose spunlace non-woven fabric base material by using distilled water after cleaning, and drying by using an oven; wherein the rinsing mode is ultrasonic or soaking, and the rinsing time is 0.5-5 h; the drying temperature is 120 deg.C, and the drying time is 20 min.
7. Ag/TiO based on magnetron sputtering according to claim 52The method for preparing the heat-insulating fabric is characterized in that in the step (S1), parameters of the low-pressure vacuum plasma etching on the cotton/viscose spunlace non-woven fabric substrate are as follows: the temperature is 80 ℃, the background vacuum degree is 9 multiplied by 10-4Pa, the power of the power supply is 200W; the time is 15 minutes; the inert gas is argon.
8. Ag/TiO based on magnetron sputtering according to claim 52The preparation method of the heat-insulating fabric is characterized in that in the process of preparing the nano ATO transparent heat-insulating coating, a certain amount of water-based polyurethane resin (PU) is taken, the water-based slurry of nano tin antimony oxide (ATO) is added into an experimental dispersing sand mill according to the weight ratio of the water-based polyurethane resin to the water-based slurry of nano tin antimony oxide (1: 3), a thickening and leveling agent is added, the mixture is stirred, and the nano ATO transparent heat-insulating coating is prepared after the mixture is uniformly stirred; when bubbles appear, adding an organic silicon defoaming agent for defoaming; in the blending process, the rotating speed of the mill is 300 r/min-500 r/min, and the thickening and leveling agent is added and stirred for 30 min.
9. Ag/TiO based on magnetron sputtering according to claim 52The preparation method of the heat insulation fabric is characterized in that a wire bar coater adopted in the process of coating the nanometer ATO transparent heat insulation coating is 20-40 mu m; in the process of curing in the electric heating blowing constant-temperature drying oven, the curing temperature is 70-100 ℃, and the curing time is 3-4 h.
10. Ag/TiO based on magnetron sputtering according to claim 52The preparation method of the heat insulation fabric is characterized in that the fabric is based on magnetic controlSputtered Ag/TiO2In the process of needling the heat-insulating fabric, the straight true density of a needle plate is 4000 needles/m2The length of the needle is 20.2mm, the fineness of the needle is 0.5mm, the surface has no barb, the aqueous polyurethane blended ATO protective layer faces upwards, and the needle punching is carried out for three times.
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