CN109208322B - Electromagnetic shielding non-woven fabric, preparation method thereof and electromagnetic shielding wall - Google Patents
Electromagnetic shielding non-woven fabric, preparation method thereof and electromagnetic shielding wall Download PDFInfo
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- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/92—Protection against other undesired influences or dangers
- E04B2001/925—Protection against harmful electro-magnetic or radio-active radiations, e.g. X-rays
Abstract
The invention provides an electromagnetic shielding non-woven fabric and a preparation method thereof, wherein the electromagnetic shielding non-woven fabric is prepared from raw materials comprising a carbon nano tube, a hydroxyapatite ultra-long nano wire and a magnetic medium, the carbon nano tube and the hydroxyapatite ultra-long nano wire form a cloth-shaped object with a network structure, and the magnetic medium is filled in the network structure of the cloth-shaped object. Compared with the traditional electromagnetic wave shielding material, the electromagnetic shielding non-woven fabric provided by the invention has biocompatibility and can realize no pollution or even zero pollution; in addition, the electromagnetic non-woven fabric has good strength and toughness. The results of the embodiment show that the strength of the electromagnetic shielding non-woven fabric prepared by the invention is 30-50 Mpa, and the electromagnetic shielding effectiveness reaches 40-50 dB at a frequency band of 30-1500 MHz. The invention also provides another electromagnetic shielding wall body which takes the electromagnetic shielding non-woven fabric as a middle shielding layer.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to an electromagnetic shielding non-woven fabric, a preparation method thereof and an electromagnetic shielding wall.
Background
With the development of modern war informatization, electromagnetic wave interference on enemies becomes more and more common. The electromagnetic wave interference technology can cause the fighting communication equipment to be interfered and even not to work normally. This will also have a great effect on the accurate transmission and reception of the own combat command, and can even determine the success or failure of a battle. In order to reduce the interference of the host side from electromagnetic waves, the electromagnetic shielding protection by adopting the electromagnetic shielding material is the most effective means in field operations.
The electromagnetic shielding protection mainly adopts certain materials or structures to reflect and absorb electromagnetic waves, and the traditional electromagnetic shielding materials mainly comprise high-conductivity metals, alloys and the like. And the simple adoption of high-conductivity metals and alloys as shielding materials greatly increases the cost of the shielding body, and the surface of the shielding body is easy to cause secondary electromagnetic pollution to the reflection of electromagnetic waves. In addition, the existing electromagnetic shielding material still has difficulty in achieving the maximum electromagnetic wave shielding requirement of field electromagnetic shielding and the requirement of good toughness for the electromagnetic shielding performance.
Disclosure of Invention
In view of the above, the present invention provides an electromagnetic shielding nonwoven fabric, a method for preparing the same, and an electromagnetic shielding wall, wherein the electromagnetic shielding nonwoven fabric provided by the present invention has biocompatibility, and reduces secondary electromagnetic pollution; meanwhile, the electromagnetic shielding material has good toughness and excellent electromagnetic shielding performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an electromagnetic shielding non-woven fabric, which comprises the following steps:
(1) mixing the carbon nano tube dispersion liquid with a magnetic medium to obtain a magnetic medium-carbon nano tube composite dispersion liquid;
(2) mixing the magnetic medium-carbon nano tube composite dispersion liquid and the hydroxyapatite ultra-long nanowire to obtain a composite suspension;
(3) carrying out vacuum filtration on the composite suspension to deposit solid components in the composite suspension on a filtration substrate, and stripping the deposit on the surface of the filtration substrate to obtain an electromagnetic non-woven fabric precursor;
(4) and sequentially drying and rolling the electromagnetic non-woven fabric precursor to obtain the electromagnetic shielding non-woven fabric.
Preferably, the method for preparing the carbon nanotube dispersion in step (1) includes: wetting a carbon nano tube by using an organic solvent, and mixing the obtained wetted carbon nano tube, a dispersing agent and water to obtain a carbon nano tube dispersion liquid; the mass ratio of the carbon nano tube to the organic solvent is 1: (5-15); the mass ratio of the carbon nanotubes to the water in the carbon nanotube dispersion liquid is 1: (150 to 250); the mass ratio of the carbon nanotubes to the dispersing agent in the carbon nanotube dispersing liquid is 1: (0.05-0.1).
Preferably, the magnetic medium in step (1) includes one or more of ferrite, carboxyl iron and elementary metal, and the mass ratio of the magnetic medium to the carbon nanotubes in the carbon nanotube dispersion liquid is 1: (10-20); the elemental metal comprises one or more of silver, copper and iron.
Preferably, the elementary metal is elementary metal powder with the particle size of 50-400 nm.
Preferably, in the step (2), the mass ratio of the carbon nanotubes to the hydroxyapatite ultralong nanowires in the magnetic medium-carbon nanotube composite dispersion liquid is (3-7): (7-3); the diameter of the hydroxyapatite ultralong nanowire is 5-100 nm, and the length of the hydroxyapatite ultralong nanowire is 30-1200 mu m.
Preferably, the mixing mode in the step (2) is shear mixing; the time of shearing and mixing is 30-60 min, and the rotating speed of shearing and mixing is 1800-2500 r/min.
Preferably, the drying temperature in the step (4) is 60-85 ℃, and the time is 12-24 hours.
The invention provides the electromagnetic shielding non-woven fabric prepared by the preparation method in the scheme, which is prepared from raw materials comprising a carbon nano tube, a hydroxyapatite ultra-long nano wire and a magnetic medium, wherein the carbon nano tube and the hydroxyapatite ultra-long nano wire form a cloth-shaped object with a network structure, and the magnetic medium is filled in the network structure of the cloth-shaped object.
The invention provides an electromagnetic shielding wall which comprises an outer rain-proof layer, a middle shielding layer and an inner decoration layer, wherein the middle shielding layer is composed of the electromagnetic shielding non-woven fabric in the technical scheme.
Preferably, the thickness ratio of the outer rain-proof layer to the middle shielding layer to the inner decoration layer is (1-3): (1-3): (1-3).
The invention provides a preparation method of an electromagnetic shielding non-woven fabric, which comprises the following steps of firstly, mixing a carbon nano tube dispersion liquid with a magnetic medium to obtain a magnetic medium-carbon nano tube composite dispersion liquid; mixing the magnetic medium-carbon nano tube composite dispersion liquid and the hydroxyapatite ultra-long nanowire to obtain a composite suspension; then, carrying out vacuum filtration on the composite suspension to deposit solid components in the composite suspension on filter paper, and stripping the deposit on the surface of the filtration substrate to obtain an electromagnetic non-woven fabric precursor; and then, drying and rolling the precursor in sequence to obtain the electromagnetic shielding non-woven fabric.
Compared with the traditional electromagnetic wave shielding material, the electromagnetic shielding non-woven fabric provided by the invention has biocompatibility, the carbon nano tubes in the electromagnetic wave shielding non-woven fabric can form a conductive network framework, when electromagnetic waves are incident, the polarization effect is generated in the material to generate eddy currents, and along with the increase of frequency, current distribution is converged to the surface of the material to cause a skin effect. When the skin effect is increased, the eddy current loss is increased, so that the electromagnetic energy is converted into heat energy to be lost, secondary electromagnetic pollution caused by the reflection of electromagnetic waves by the surface of a high-conductivity metal or alloy shielding material is avoided, and no pollution or even zero pollution can be realized; moreover, the hydroxyapatite ultralong nanowires and the carbon nanotubes are both in fibrous structures, so that when the hydroxyapatite ultralong nanowires and the carbon nanotubes are made into non-woven fabrics, the hydroxyapatite ultralong nanowires and the carbon nanotubes can be well lapped into a three-dimensional skeleton structure, and a shielding network is formed in the non-woven fabrics, so that a good shielding effect is achieved; meanwhile, the nano fibers are mutually overlapped to form a three-dimensional network structure, so that the electromagnetic non-woven fabric has good strength and toughness. The results of the embodiment show that the strength of the electromagnetic shielding non-woven fabric prepared by the invention is 30-50 Mpa, and the electromagnetic shielding effectiveness reaches 40-50 dB at a frequency band of 30-1500 MHz; and the electromagnetic wave emitted to the surface of the non-woven fabric can be completely absorbed, and no secondary electromagnetic pollution exists.
Drawings
FIG. 1 is a schematic cross-sectional view of the carbon nanotube-hydroxyapatite electromagnetic shielding wall according to the present invention;
wherein, 1-inner layer decoration layer, 2-middle shielding layer, and 3-outer layer rain-proof layer.
Detailed Description
The invention provides a preparation method of an electromagnetic shielding non-woven fabric, which comprises the following steps:
(1) mixing the carbon nano tube dispersion liquid with a magnetic medium to obtain a magnetic medium-carbon nano tube composite dispersion liquid;
(2) mixing the magnetic medium-carbon nano tube composite dispersion liquid and the hydroxyapatite ultra-long nanowire to obtain a composite suspension;
(3) coating the composite suspension on a substrate, carrying out vacuum filtration to deposit solid components in the composite suspension on the filtration substrate, and stripping the deposit on the surface of the filtration substrate to obtain an electromagnetic non-woven fabric precursor;
(4) and sequentially drying and rolling the electromagnetic non-woven fabric precursor to obtain the electromagnetic shielding non-woven fabric.
The invention mixes the carbon nano tube dispersion liquid and the magnetic medium to obtain the magnetic medium-carbon nano tube composite dispersion liquid. In the present invention, the method for preparing the carbon nanotube dispersion preferably includes: after wetting the carbon nano tube by using an organic solvent, mixing the obtained wetted carbon nano tube, a dispersing agent and water to obtain a carbon nano tube dispersion liquid.
The invention wets the carbon nano tube by adopting an organic solvent to obtain a wetted carbon nano tube; the organic solvent is preferably dripped on the carbon nano tube to realize the wetting of the carbon nano tube. In the present invention, the organic solvent is preferably acetone and/or ethanol; in the present invention, the carbon nanotubes in the carbon nanotube dispersion are preferably whisker-shaped multi-walled carbon nanotubes; the diameter of the carbon nano tube is preferably 30-150 nm, more preferably 35-100 nm, and even more preferably 40-80 nm; the length of the carbon nano tube is preferably 5-10 mu m, and more preferably 6-9.5 mu m; the purity of the carbon nanotubes is preferably 95% or more. The invention controls the specification and the size of the carbon nano tube, is convenient to form a three-dimensional network structure with the hydroxyapatite ultra-long nano wire, and is further beneficial to improving the obdurability and the electromagnetic shielding performance of the non-woven fabric. In the present invention, the mass ratio of the organic solvent to the carbon nanotubes is preferably 1: (5-15), more preferably 1: (8-12).
After the wet carbon nano tube is obtained, the wet carbon nano tube and a dispersing agent are dispersed in water to obtain a carbon nano tube dispersion liquid.
In the present invention, the mass ratio of the carbon nanotubes (based on the mass of the carbon nanotubes that are not wetted with the organic solvent) to water in the carbon nanotube dispersion is preferably 1: (150 to 250), more preferably 1: (180-245), more preferably 1: (200-220). In the invention, the dispersant is preferably one or more of Sodium Dodecyl Sulfate (SDS), polyvinyl pyrrolidone (PVP) and sodium dodecyl sulfate (SDBS); the mass ratio of the carbon nanotubes to the dispersing agent in the carbon nanotube dispersing liquid is 1: (0.05 to 0.1), more preferably 1: (0.06-0.1). In the invention, the dispersing mode comprises ultrasonic dispersing and shearing mixing which are carried out in sequence; the ultrasonic time is preferably 1-3 h; the power of the ultrasonic wave is preferably 50-150 KHz, and further preferably 80-120 KHz; the present invention does not require special embodiments of the ultrasound, as will be appreciated by those skilled in the art. In the invention, the rotation speed of the shearing and mixing is preferably 1800-2500 r/min, and more preferably 2000-2300 r/min; the time for shearing and mixing is preferably 30-60 min, and more preferably 45-50 min. The present invention does not require special embodiments of the shear mixing, as will be appreciated by those skilled in the art; in the examples of the present invention, it is carried out in particular in a high-shear emulsifier. The invention wets the carbon nano tube by the organic solvent, and then disperses in the water under the action of the dispersant, which can prevent the carbon nano tube from directly adding and floating on the water surface.
In the present invention, the magnetic medium preferably includes one or more of ferrite, carboxyl iron, and elemental metal; the elemental metal comprises silver, copper or iron; the simple substance metal is preferably simple substance metal powder, the particle size is preferably 50-400 nm, more preferably 80-320 nm, and even more preferably 100-300 nm. In the present invention, the ferrite and the carboxyiron are preferably provided in the form of powder, and the particle diameters of the ferrite powder and the carboxyiron powder are independently preferably 100 to 200 nm. In the invention, the magnetic medium attenuates electromagnetic waves by causing natural resonance, hysteresis loss, eddy current loss and domain wall resonance, and the composite carbon nanotube can attenuate the electromagnetic waves in both electric and magnetic aspects, thereby obtaining better performance.
In the present invention, the mass ratio of the magnetic medium to the carbon nanotubes (in terms of the mass of unwetted carbon nanotubes) in the carbon nanotube dispersion is preferably 1: (10-20), more preferably 1: (12-18), more preferably 1: 15.
The invention preferably disperses the magnetic medium into the carbon nano tube dispersion liquid under the ultrasonic condition to obtain the magnetic medium-carbon nano tube composite dispersion liquid. In the invention, the ultrasonic time is preferably 1-3 h, and the ultrasonic power is preferably 50-150 KHz, and more preferably 100-120 KHz. The invention adopts an ultrasonic dispersion mode, which is convenient for promoting the uniform mixing of the magnetic medium and the carbon nano tube dispersion liquid.
After the magnetic medium-carbon nano tube composite dispersion liquid is obtained, the magnetic medium-carbon nano tube composite dispersion liquid and the hydroxyapatite ultra-long nanowire are mixed to obtain a composite suspension liquid. In the invention, the diameter of the hydroxyapatite ultralong nanowire is preferably 5-100 nm, more preferably 10-80 nm, and even more preferably 25-50 nm; the length of the hydroxyapatite ultralong nanowire is preferably 30-1200 mu m, more preferably 300-1000 mu m, and even more preferably 600-1000 mu m. The source of the hydroxyapatite ultralong nanowire is not specially required, the hydroxyapatite ultralong nanowire which is well known by technical personnel in the field, such as a commercially available hydroxyapatite ultralong nanowire, is purchased from Shanghai silicate research institute of Chinese academy of sciences; can also be prepared by itself.
When the hydroxyapatite ultra-long nanowire is provided in a self-preparation manner, the preparation method of the hydroxyapatite ultra-long nanowire preferably includes:
(I) mixing calcium chloride solution, NaOH solution and NaH2PO4·2H2Dropwise adding the O aqueous solution into the oleic acid alcoholic solution in sequence to obtain a mixed solution;
(II) carrying out hydrothermal reaction on the mixed solution to obtain a hydrothermal reaction product;
(IIII) cooling the hydrothermal reaction product to room temperature, and then sequentially carrying out alcohol washing and water washing to obtain the hydroxyapatite ultra-long nanowire.
The invention preferably mixes calcium chloride solution, NaOH solution and NaH2PO4·2H2And dropwise adding the O aqueous solution into the oleic acid alcohol solution to obtain a mixed solution. In the invention, the concentration of the calcium chloride solution is preferably 5-15 mol/L; the calcium chloride solution is preferably prepared by mixing anhydrous calcium chloride with water to obtain a calcium chloride solution. In the invention, the concentration of the NaOH solution is preferably 10-20 mol/L, and more preferably 15-18 mol/L. In the present invention, the NaH is2PO4·2H2The concentration of the O aqueous solution is preferably 10 to 20mol/L, and more preferably 12 to 15 mol/L. According to the invention, preferably, oleic acid is dissolved in absolute ethyl alcohol to obtain an oleic acid solution; the mass ratio of the oleic acid to the absolute ethyl alcohol is preferably 1: (1-3).
In the present invention, the volume ratio of the calcium chloride solution to the oleic acid alcohol solution is preferably 1: (1-1.5); the preferable dropping speed of the calcium chloride solution is 0.2-0.5 mL/s.
In the present invention, the volume ratio of the NaOH solution to the oleic acid alcohol solution is preferably 1: (2.5-5), and more preferably 1: (3-4.5); the dropping rate of the NaOH solution is preferably 0.2-0.5 mL/s.
In the present invention, the NaH is2PO4·2H2The volume ratio of the O aqueous solution to the oleic acid alcoholic solution is preferably 1: (5-10), more preferably 1: (6.5-7.5); the NaH2PO4·2H2The dropping rate of the O aqueous solution is preferably 0.2-0.5 mL/s.
The invention adopts calcium chloride solution, NaOH solution and NaH2PO4·2H2The O aqueous solution is sequentially dripped into the oleic acid alcoholic solution, and the dosage and the dripping speed of the solution are strictly controlled, so that the uniform mixing of the components is guaranteed.
After the mixed solution is obtained, the invention preferably carries out hydrothermal reaction on the mixed solution to obtain a hydrothermal reaction product. In the invention, the temperature of the hydrothermal reaction is preferably 150-250 ℃, and more preferably 200-220 ℃; the time of the hydrothermal reaction is preferably 8-15 hours, and more preferably 10-12 hours. The invention can form an intermediate product CaHPO in the hydrothermal reaction process4、Ca2P2O4Finally, Ca is generated10(PO4)6(OH)2。
After the hydrothermal reaction product is obtained, the invention preferably cools the hydrothermal reaction product to room temperature, and then sequentially carries out alcohol washing and water washing to obtain the hydroxyapatite ultra-long nanowire. The cooling method of the invention has no special requirement, and the feed liquid cooling method known to the skilled person can be adopted. In the present invention, the number of times of the alcohol washing and the water washing is preferably 3 times, respectively; the invention has no special requirement on the modes of alcohol washing and water washing, and the washing mode known by the technical personnel in the field can be adopted.
In the invention, the mass ratio of the carbon nanotubes to the hydroxyapatite ultralong nanowires in the magnetic medium-carbon nanotube composite dispersion liquid is preferably (3-7): (7-3), more preferably (5-6): (6-5); in embodiments of the invention, specifically 3:7, 4:6, 5:5, 6:4 or 7: 3. In the present invention, the mixing is preferably shear mixing; the rotation speed of the shearing and mixing is preferably 1800-2500 r/min, and more preferably 2000-2300 r/min; the time for shearing and mixing is preferably 30-60 min, and more preferably 45-50 min. The present invention does not require special embodiments of the shear mixing, as will be appreciated by those skilled in the art; in the examples of the present invention, it is carried out in particular in a high-shear emulsifier. According to the invention, the composite dispersion liquid and the carboxyl apatite ultra-long nanowire are uniformly mixed through shearing and mixing, so that the composite suspension liquid is obtained.
After the composite suspension is obtained, the composite suspension is subjected to vacuum filtration, so that solid components in the composite suspension are deposited on a filtration substrate, and the filtration substrate is peeled off to obtain the carbon nanotube-hydroxyapatite ultra-long nanowire-magnetic medium electromagnetic non-woven fabric precursor. In the invention, the time of vacuum filtration is preferably 2-5 min, and the vacuum degree of vacuum filtration is preferably 0.05-0.08 MPa; the suction filtration substrate is preferably filter paper or filter cloth; the invention has no special requirements on the specific implementation mode of vacuum filtration, and the vacuum filtration mode which is well known by the technical personnel in the field is adopted; in the embodiment of the invention, the composite suspension is firstly poured into a funnel with a suction filtration substrate, and then suction filtration is carried out on the composite suspension, so that solid components are deposited on the suction filtration substrate. According to the invention, liquid components are evaporated through vacuum filtration, solid components in the composite suspension are deposited on the filter paper, the carbon nano tubes and the hydroxyapatite ultra-long nanowires are used as nano fibers to be mutually interwoven to obtain a cloth-shaped substance matrix with a three-dimensional network structure, and the magnetic medium is filled in the network structure of the cloth-shaped substance matrix. The carbon nanotube-hydroxyapatite ultralong nanowire-magnetic medium electromagnetic non-woven fabric precursor is obtained after stripping the suction filtration substrate.
The stripping method of the suction filtration substrate is not particularly required in the present invention, and a stripping method known to those skilled in the art may be used.
After stripping is finished, the electromagnetic non-woven fabric precursor is sequentially dried and rolled to obtain the electromagnetic shielding non-woven fabric. In the invention, the drying temperature is preferably 65-80 ℃, and more preferably 70-75 ℃; the drying time is preferably 12-24 hours, and more preferably 15-18 hours. The invention has no special requirements on the specific implementation mode of the drying, and the drying mode which is well known by the technicians in the field can be adopted; in an embodiment of the invention, the drying is carried out in a vacuum oven. The invention removes the residual moisture in the electromagnetic non-woven fabric precursor by drying.
After drying, the invention rolls the dried precursor to obtain the electromagnetic non-woven fabric. In the invention, the rolling pressure is preferably 120-150 KN/m, and the rolling times are preferably 3-5. According to the invention, the three-dimensional network structure in the non-woven fabric substrate is more compact and the magnetic medium is more tightly combined with the substrate through the rolling.
The invention has no special requirement on the rolling shape, can be directly rolled into a specific shape and size according to the target requirement, and also can be firstly rolled into a sheet shape and then cut into the required shape and size. The present invention does not require special embodiments of the rolling process, as is well known to those skilled in the art; the present invention preferably performs rolling using a twin-roll machine.
In the invention, the hydroxyapatite ultralong nanowire has good flexibility, high temperature resistance, corrosion resistance and good biological safety, and the carbon nanotube has a good porous structure; because the carbon nano tube has no ferromagnetism, the carbon nano tube composite material can strongly attenuate electromagnetic waves on a wide waveband from the aspects of electricity and magnetism by adding a magnetic medium, and obtains better shielding performance.
The invention also provides the electromagnetic shielding non-woven fabric prepared by the preparation method in the technical scheme, which is prepared from raw materials comprising the carbon nano tube, the hydroxyapatite ultra-long nano wire and the magnetic medium, wherein the carbon nano tube and the hydroxyapatite ultra-long nano wire form a cloth-shaped object with a network structure, and the magnetic medium is filled in the network structure of the cloth-shaped object. In the invention, the thickness of the electromagnetic shielding non-woven fabric is preferably 0.1-1 mm, and more preferably 0.2-0.5 mm; the density of the electromagnetic shielding non-woven fabric is preferably 0.4-0.8 g/cm3More preferably 0.5 to 0.75g/cm3。
The invention provides an electromagnetic shielding wall which comprises an outer rain-proof layer, a middle shielding layer and an inner decoration layer. In the present invention, the middle shielding layer is the electromagnetic shielding nonwoven fabric according to the above technical scheme, and details are not repeated herein.
As shown in fig. 1, the electromagnetic shielding wall provided by the invention comprises an inner decoration layer 1, an intermediate shielding layer 2 and an outer rain-proof layer 3.
In the invention, the outer rain-proof layer is preferably made of PVC plastic; the source of the outer rain repellent layer is not particularly required in the present invention and may be any source known to those skilled in the art.
In the invention, the inner decorative layer is preferably a wallpaper material; the source of the inner layer modification layer is not particularly required in the present invention, and commercially available products known to those skilled in the art may be used.
In the invention, the thickness ratio of the outer rain-proof layer, the middle shielding layer and the inner decoration layer is preferably (1-3): (1-3): (1-3); in embodiments of the present invention, 2:1:2, 2:1:3, 3:1:2, 1:1:1, 2:1:1 may be specific. In the invention, the outer rain-proof layer, the middle shielding layer and the inner decoration layer are preferably connected in an adhesive manner; the glue may be any commercially available glue known to those skilled in the art.
The invention has no special requirements on the preparation method of the electromagnetic shielding wall body, and the preparation method of the layered wall body known by the technical personnel in the field is adopted. The electromagnetic shielding room constructed by the electromagnetic shielding wall has excellent electromagnetic interference resistance, and the electromagnetic shielding efficiency in a frequency band of 30-1500 MHz reaches 40-50 dB.
In the invention, the electromagnetic shielding wall body is used for a rapid field electromagnetic shielding room, can provide a protection place for fighters, weaponry and the like, and can prevent electromagnetic weapons from attacking, and keep the viability and the fighting capacity.
The electromagnetic shielding nonwoven fabric, the method for preparing the same, and the electromagnetic shielding wall according to the present invention will be described in detail with reference to the following embodiments, which should not be construed as limiting the scope of the present invention.
Example 1
Dissolving 12g of oleic acid in 12g of absolute ethyl alcohol, uniformly stirring and standing for 10min, then dropwise adding a 5mol/L calcium chloride solution into an oleic acid alcohol solution at a speed of 0.2mL/s under the condition of magnetic stirring, and standing for 30 min; then continuously stirring 10mol/L NaOH solution under the condition of magnetic stirringDropwise adding the mixture into the oleic acid alcohol solution at the same speed, and continuously stirring for 1h after dropwise adding is finished; then 10mol/L of NaH2PO4·2H2And continuously dropwise adding the O aqueous solution into the oleic acid alcohol solution under the magnetic stirring condition, and magnetically stirring for 3 hours.
And placing the obtained mixed solution in a reaction kettle, preserving heat for 8 hours at the temperature of 150 ℃ in a vacuum drying oven, then cooling to room temperature along with the furnace, washing with alcohol for 3 times, and washing with water for 3 times to obtain the hydroxyapatite ultra-long nanowire for later use, wherein the diameter of the hydroxyapatite ultra-long nanowire is about 80nm, and the length of the hydroxyapatite ultra-long nanowire is about 600 mu m.
Preparing non-woven fabric:
(1) dropping absolute ethyl alcohol onto 2g of carbon nano tubes according to the mass ratio of the absolute ethyl alcohol to the carbon nano tubes of 1:5, then dispersing the wetted carbon nano tubes into 500mL of distilled water by using 0.2g of SDS dispersing agent, performing ultrasonic dispersion treatment for 1 hour by 150KHz, and shearing in a high-speed emulsification shearing machine for 30min to obtain carbon nano tube dispersion liquid for later use.
(2) And (2) adding 0.15g of ferrite particles (with the average particle size of 120nm) into the carbon nano tube dispersion liquid obtained in the step (1), and performing ultrasonic dispersion for 1 hour at 150KHz to uniformly disperse the carbon nano tubes and the ferrite particles in the liquid to obtain the composite dispersion liquid.
(3) And (3) stirring and mixing the composite dispersion liquid and 2g of hydroxyapatite nanowires, and fully mixing and dispersing the composite dispersion liquid and the hydroxyapatite nanowires by a high-speed shearing emulsifying machine (the shearing time is 60min, and the rotating speed is 2500r/min) to obtain a composite suspension.
(4) And depositing the composite suspension on filter paper by adopting a vacuum filtration method, peeling the filter paper to obtain a carbon nanotube-hydroxyapatite electromagnetic shielding non-woven fabric precursor, placing the precursor in a vacuum drying box, and drying for 15 hours at 65 ℃.
(5) Rolling the dried non-woven fabric precursor by a double-roller mill to obtain the non-woven fabric precursor with the density of about 0.42g/cm3And the thickness is 0.1 mm.
Example 2
Hydroxyapatite ultra-long nanowires were prepared in the manner of example 1, with the difference that: the temperature of the vacuum drying oven is 200 ℃, and the obtained hydroxyapatite ultra-long nanowire is ready for use, the diameter of the hydroxyapatite ultra-long nanowire is 50nm, and the length of the hydroxyapatite ultra-long nanowire is 300 microns.
Preparing non-woven fabric:
(1) dropping absolute ethyl alcohol onto 2.5g of carbon nano tubes according to the mass ratio of the absolute ethyl alcohol to the carbon nano tubes of 1:15, then dispersing the wetted carbon nano tubes into 600mL of distilled water by using 0.25g of SDS dispersing agent, performing ultrasonic dispersion treatment for 1 hour by using 120KHz, and shearing in a high-speed emulsification shearing machine for 40min to obtain carbon nano tube dispersion liquid for later use.
(2) And (2) adding 0.2g of hydroxyl iron powder (with the particle size of 80nm) into the carbon nanotube dispersion liquid obtained in the step (1), and performing 150KHz ultrasonic dispersion for 1 hour to uniformly disperse the carbon nanotubes and the hydroxyl iron powder in the liquid to obtain a composite dispersion liquid.
(3) And (3) stirring and mixing the composite dispersion liquid and 2g of hydroxyapatite nanowires, and fully mixing and dispersing the composite dispersion liquid and the hydroxyapatite nanowires by a high-speed shearing emulsifying machine (the shearing time is 30min, and the rotating speed is 1800r/min) to obtain a composite suspension.
(4) And depositing the composite suspension on filter paper by adopting a vacuum filtration method, peeling the filter paper to obtain a carbon nanotube-hydroxyapatite electromagnetic shielding non-woven fabric precursor, placing the precursor in a vacuum drying box, and drying for 16 hours at 65 ℃.
(5) Rolling the dried non-woven fabric precursor by a double-roller mill to obtain the non-woven fabric precursor with the density of about 0.69g/cm3And the thickness is 0.05 mm.
Example 3
Hydroxyapatite ultra-long nanowires were prepared in the manner of example 1, with the difference that: the temperature of the vacuum drying oven is 200 ℃, the heat preservation time is 15h, and the obtained hydroxyapatite ultra-long nanowire is ready for use, the diameter of the hydroxyapatite ultra-long nanowire is 100nm, and the length of the hydroxyapatite ultra-long nanowire is 1200 mu m.
Preparing non-woven fabric:
(1) dropping absolute ethyl alcohol onto 2g of carbon nano tubes according to the mass ratio of the absolute ethyl alcohol to the carbon nano tubes of 1:5, then dispersing the wetted carbon nano tubes into 500mL of distilled water by using 0.2g of SDS dispersing agent, carrying out ultrasonic dispersion treatment for 1 hour by using 140KHz, and shearing in a high-speed emulsification shearing machine for 30min to obtain a carbon nano tube dispersion liquid for later use.
(2) And (2) adding 0.2g of hydroxyl iron powder (with the particle size of 150nm) into the carbon nanotube dispersion liquid obtained in the step (1), and performing 150KHz ultrasonic dispersion for 1 hour to uniformly disperse the carbon nanotubes and the simple substance iron powder (with the particle size of 400nm) in the liquid to obtain the composite dispersion liquid.
(3) And (3) stirring and mixing the composite dispersion liquid and 2g of hydroxyapatite nanowires, and fully mixing and dispersing the composite dispersion liquid and the hydroxyapatite nanowires by a high-speed shearing emulsifying machine (the shearing time is 60min, and the rotating speed is 2500r/min) to obtain a composite suspension.
(4) And depositing the composite suspension on filter paper by adopting a vacuum filtration method, peeling the filter paper to obtain a carbon nanotube-hydroxyapatite electromagnetic shielding non-woven fabric precursor, placing the precursor in a vacuum drying box, and drying at 65 ℃ for 18 h.
(5) Rolling the dried non-woven fabric precursor by a double-roller mill to obtain the non-woven fabric precursor with the density of about 0.68g/cm3And the thickness is 0.053 mm.
Example 4
An electromagnetically shielding nonwoven fabric was produced in the same manner as in example 3, except that the magnetic medium used was copper powder having a particle size of about 200nm, and a density of about 0.71g/cm was obtained3And the thickness is 0.043 mm.
Example 5
An electromagnetic shielding nonwoven fabric was prepared in the manner as in example 3, except that the magnetic medium used was silver powder having a particle diameter of about 50nm, and a density of about 0.75g/cm was obtained3And the thickness is 0.040 mm.
Example 6
A non-woven fabric was prepared in the manner of example 2, wherein the hydroxyapatite ultra-long nanowires were prepared in a manner different from that of the following: the temperature of the vacuum drying oven is 200 ℃, the heat preservation time is 15h, and the obtained hydroxyapatite ultra-long nanowire is ready for use, the diameter of the hydroxyapatite ultra-long nanowire is 100nm, and the length of the hydroxyapatite ultra-long nanowire is 1200 mu m.
The final density obtained was about 0.69g/cm3Of thickness 0.051mmElectromagnetic shielding non-woven fabric.
Examples 7 to 9
Using the hydroxyapatite ultra-long nanowires (denoted as nanowires) prepared in example 1, electromagnetic shielding nonwoven fabrics were prepared in the manner of example 1, and the amounts of the materials are shown in table 1; the performance parameters of each material are shown in table 2.
TABLE 1 amounts (unit: g) of raw materials used in preparation of non-woven fabrics of examples 7 to 9
| Carbon nanotube | Anhydrous ethanol | Water (W) | Dispersing agent | Magnetic medium | Nanowire and method of manufacturing the same | |
| Example 7 | 5 | 25 | 150 | 0.5 | 0.5 | 5 |
| Example 8 | 3 | 30 | 500 | 0.4 | 0.3 | 7 |
| Example 9 | 7 | 100 | 1050 | 0.07 | 0.5 | 3 |
TABLE 2 Performance parameters of raw materials in preparation of non-woven fabrics of examples 7 to 9
TABLE 3 preparation Process parameters and non-woven Fabric construction parameters of the raw materials in the preparation of non-woven fabrics of examples 7 to 9
The strength test (tensile strength test using a weight attached under the electromagnetic shielding nonwoven fabric of unit cross-sectional area) was performed on the electromagnetic shielding nonwoven fabrics obtained in examples 1 to 9, and the test results are shown in table 4.
TABLE 4 toughness of electromagnetic shielding nonwoven fabrics of examples 1 to 9
| Case(s) | Strength (MPa) |
| Example 1 | 32 |
| Example 2 | 48 |
| Example 3 | 50 |
| Example 4 | 30 |
| Example 5 | 47 |
| Example 6 | 46.5 |
| Example 7 | 49.2 |
| Example 8 | 49.5 |
| Example 9 | 45 |
An AV3620 type vector network analyzer is used to prepare an electromagnetic shielding wall from the electromagnetic shielding nonwoven fabric obtained in examples 1 to 9 according to the structure shown in fig. 1, the inner layer modification layer is made of commercially available wallpaper, the outer layer rain-proof layer is made of PCV plastic with a thickness ratio of 2:1:2 (inner layer 2mm, middle layer 1mm, outer layer 2mm), and then the wall is subjected to an electromagnetic shielding effectiveness test in a frequency band of 30 to 1500MHz, with test results shown in table 5.
TABLE 5 electromagnetic shielding performance of electromagnetic shielding nonwoven fabric of examples 1 to 9
| Case(s) | Shielding effectiveness (dB) |
| Example 1 | 49 |
| Example 2 | 41 |
| Example 3 | 40 |
| Example 4 | 44 |
| Example 5 | 47 |
| Example 6 | 44 |
| Example 7 | 45.2 |
| Example 8 | 42.5 |
| Example 9 | 46 |
As can be seen from Table 5, the strength of the electromagnetic shielding non-woven fabric obtained by the invention is 30-50 MPa, the electromagnetic shielding effectiveness reaches 40-50 dB at the frequency band of 30-1500 MHz, and the electromagnetic shielding non-woven fabric has excellent electromagnetic shielding performance.
Example 10
The electromagnetic shielding non-woven fabric obtained in the embodiment 1 is used for preparing electromagnetic shielding walls according to the structures shown in fig. 1, the electromagnetic shielding walls correspond to the wall 1, the wall 2, the wall 3, the wall 4 and the wall 5 respectively, the inner layer modification layer adopts commercially available wallpaper, the outer layer rain-proof layer adopts PCV plastic, the wall thickness parameters are shown in a table 6, and an electromagnetic shielding room is built according to the method.
TABLE 6 thickness parameters of different walls
| Inner layer decorative layer (mm) | Middle shielding layer (mm) | Outer layer rain-proof layer (mm) | |
| |
2 | 1 | 2 |
| |
2 | 1 | 3 |
| |
3 | 1 | 2 |
| Wall 4 | 1.3 | 1 | 1 |
| Wall 5 | 2 | 1 | 1 |
The AV3620 type vector network analyzer is adopted to carry out electromagnetic shielding effectiveness tests on the wall bodies with different thicknesses in the table 6, and therefore, in the frequency range of 30-1500 MHz, the electromagnetic shielding effectiveness of the wall bodies 1-5 are respectively 44dB, 43dB, 41dB and 42 dB.
According to the results, the method has the advantages of simple process, no addition of any organic solvent, low cost and suitability for large-scale industrial production.
According to the invention, the carbon nano tube and the hydroxyapatite nanowire are compounded to prepare the carbon nano tube/hydroxyapatite nanowire non-woven fabric, so that the non-woven fabric has good fireproof and shielding effects. Meanwhile, a magnetic medium type shielding material is added to further optimize the shielding effectiveness; compared with the traditional electromagnetic wave shielding material, the electromagnetic shielding non-woven fabric provided by the invention has biocompatibility, does not have secondary electromagnetic pollution caused by the reflection of electromagnetic waves by the surface of a high-conductivity metal or alloy shielding material, can achieve no pollution or even zero pollution, and has good strength and toughness and better shielding effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of electromagnetic shielding non-woven fabric comprises the following steps:
(1) mixing the carbon nano tube dispersion liquid with a magnetic medium to obtain a magnetic medium-carbon nano tube composite dispersion liquid;
(2) mixing the magnetic medium-carbon nano tube composite dispersion liquid and the hydroxyapatite ultra-long nanowire to obtain a composite suspension;
(3) carrying out vacuum filtration on the composite suspension to deposit solid components in the composite suspension on a filtration substrate, and stripping the deposit on the surface of the filtration substrate to obtain an electromagnetic non-woven fabric precursor;
(4) drying and rolling the electromagnetic non-woven fabric precursor in sequence to obtain the electromagnetic shielding non-woven fabric;
the mass ratio of the carbon nano tubes to the hydroxyapatite ultralong nanowires in the magnetic medium-carbon nano tube composite dispersion liquid in the step (2) is (3-7): (7-3); the diameter of the hydroxyapatite ultralong nanowire is 5-100 nm, and the length of the hydroxyapatite ultralong nanowire is 30-1200 mu m.
2. The production method according to claim 1, wherein the production method of the carbon nanotube dispersion liquid in the step (1) comprises: wetting a carbon nano tube by using an organic solvent, and mixing the obtained wetted carbon nano tube, a dispersing agent and water to obtain a carbon nano tube dispersion liquid; the mass ratio of the carbon nano tube to the organic solvent is 1: (5-15); the mass ratio of the carbon nanotubes to the water in the carbon nanotube dispersion liquid is 1: (150 to 250); the mass ratio of the carbon nanotubes to the dispersing agent in the carbon nanotube dispersing liquid is 1: (0.05-0.1).
3. The preparation method according to claim 1, wherein the magnetic medium in step (1) comprises one or more of ferrite, carboxyl iron and elementary metal, and the mass ratio of the magnetic medium to the carbon nanotubes in the carbon nanotube dispersion is 1: (10-20); the elemental metal comprises one or more of silver, copper and iron.
4. The preparation method according to claim 3, wherein the elemental metal is elemental metal powder with a particle size of 50-400 nm.
5. The production method according to claim 1, wherein the mixing in the step (2) is performed by shear mixing; the time of shearing and mixing is 30-60 min, and the rotating speed of shearing and mixing is 1800-2500 r/min.
6. The preparation method according to claim 1, wherein the drying temperature in the step (4) is 60-85 ℃ and the drying time is 12-24 h.
7. The electromagnetic shielding non-woven fabric prepared by the preparation method of any one of claims 1 to 6 is prepared from raw materials including carbon nanotubes, hydroxyapatite ultra-long nanowires and a magnetic medium, wherein the carbon nanotubes and the hydroxyapatite ultra-long nanowires form a cloth-like object with a network structure, and the magnetic medium is filled in the network structure of the cloth-like object.
8. An electromagnetic shielding wall comprising an outer rain-proof layer, an intermediate shielding layer and an inner decorative layer, wherein the intermediate shielding layer is formed of the electromagnetic shielding nonwoven fabric as claimed in claim 7.
9. The electromagnetic shielding wall according to claim 8, wherein the thickness ratio of the outer layer rain-proof layer, the middle shielding layer and the inner layer decoration layer is (1-3): (1-3): (1-3).
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