CN113436824A - Magnetic wave-absorbing material, preparation method, application and health-care product thereof - Google Patents
Magnetic wave-absorbing material, preparation method, application and health-care product thereof Download PDFInfo
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
- A61N2/00—Magnetotherapy
- A61N2/004—Magnetotherapy specially adapted for a specific therapy
- A61N2/008—Magnetotherapy specially adapted for a specific therapy for pain treatment or analgesia
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Radiology & Medical Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pain & Pain Management (AREA)
- Hospice & Palliative Care (AREA)
- Biomedical Technology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Power Engineering (AREA)
- Magnetic Treatment Devices (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
Abstract
The invention relates to a magnetic wave-absorbing material, a preparation method, application and a health-care product thereof. The magnetic wave-absorbing material is a ternary composite material formed by expanded graphene, iron and cobalt, the ternary composite material is provided with a pore channel with a hollow interior, and the iron and the cobalt are bonded or deposited in the pore channel. The magnetic wave-absorbing material has excellent microwave absorption characteristics and electromagnetic impedance characteristics, a wrist ring and a neck ring are formed by preparing the magnetic wave-absorbing material, clinical tests prove that the neck ring has a warming effect, and can relieve symptoms of patients and pain symptoms of neck and shoulder vertebrae, the magnetic wave-absorbing material is benefited from absorbing and storing environmental microwaves, and the magnetic wave-absorbing material acts on cells of an organism by utilizing the excellent microwave absorption characteristics and the electromagnetic impedance characteristics to cause resonance of atoms and molecules of body fluid of the organism, so that the activity of the cells of the whole body is activated, blood circulation of a user can be promoted, and health-care effects such as pain relieving are achieved.
Description
Technical Field
The invention relates to the technical field of medical care products, in particular to a magnetic wave-absorbing material, a preparation method and application thereof and a health care product.
Background
Nowadays, the requirements for wave absorbing materials are higher and higher, and the wave absorbing materials have better strength, hardness and toughness, also have aging resistance, corrosion resistance and temperature resistance, and also meet the indexes of thinness, lightness, width and strength. The electric loss type wave-absorbing material has good electromagnetic wave penetrability and light weight, but has poor loss capacity to electromagnetic waves, namely the magnetic loss type wave-absorbing material has outstanding loss capacity but large specific gravity, and cannot meet the indexes of thinness, lightness, width and strength due to the limitation of Snvek limit. Therefore, the single-component wave-absorbing material cannot meet the current requirements, and the wave-absorbing materials with different losses are usually compounded to prepare materials with both electromagnetic properties, for example, in the field of medical health-care products, the purpose of preparing health-care products or treatment products is realized by utilizing the special microwave absorption characteristics and electromagnetic impedance characteristics of the magnetic wave-absorbing materials.
Disclosure of Invention
In view of the above, the present invention provides a magnetic wave-absorbing material, which satisfies the unique microwave absorption characteristics and electromagnetic impedance characteristics to achieve the purpose of preparing health products or therapeutic products.
In a first aspect, the embodiment of the invention discloses a magnetic wave-absorbing material, which is a ternary composite material formed by expanded graphene, iron and cobalt, wherein the ternary composite material is provided with a pore channel with a hollow interior, and the iron and the cobalt are bonded or deposited in the pore channel.
In an embodiment of the invention, the iron and cobalt bonds are connected between expanded graphene layers.
In embodiments of the invention, the iron and the cobalt are deposited in the pore channels in a crystalline formation.
In a second aspect, an embodiment of the present invention provides a method for preparing a magnetic wave-absorbing material in the first aspect, including the following steps:
dispersing the activated expanded graphene in ultrapure water, and uniformly stirring to obtain a first solution;
preparing a second solution comprising iron inorganic salt, cobalt inorganic salt and ethanol;
mixing iron powder, cobalt powder, the first solution and the second solution, stirring, treating at 150-180 ℃, separating solids in the solution, and washing to obtain a primary material;
and then, placing the preliminary material in a mixed gas of hydrogen and argon for treatment, and controlling the temperature to rise to 700-900 ℃ for treatment to obtain the magnetic wave-absorbing material.
In the embodiment of the invention, the second solution contains 15-20 mol/L of iron element, 15-20 mol/L of cobalt element and 25-40 v/v% of ethanol.
In the embodiment of the invention, the mixing mass ratio of the iron powder, the cobalt powder, the expanded graphene, the iron inorganic salt and the cobalt inorganic salt in the reactant is (3-6): 100-150): 5-10.
In the embodiment of the invention, the volume ratio of the hydrogen to the argon in the mixed gas is (50-60): 40-50.
In a third aspect, the embodiment of the invention discloses a health-care product prepared on the basis of the magnetic wave-absorbing material in the first aspect or the magnetic wave-absorbing material prepared by the preparation method in the second aspect.
In an embodiment of the invention, the health care product comprises at least one of a collar, a wrist band, a waist band and an ankle band.
In a fourth aspect, the embodiment of the invention discloses an application of the magnetic wave-absorbing material in the first aspect or the magnetic wave-absorbing material prepared by the preparation method in the second aspect in preparing a health-care product for improving cervical vertebra pain.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the embodiment of the invention, the expanded graphene, the iron and the cobalt form the ternary composite material, the ternary composite material has a pore channel with a hollow interior, and the iron and the cobalt are bonded or deposited in the pore channel. The ternary composite material is based on expanded graphene to form an inclusion, and the nano particles formed by iron and cobalt are wrapped in the inclusion, so that the formed microscopic nano structure has a synergistic electromagnetic improvement effect, and a plurality of dielectric medium and magnetic loss peak values are generated in a frequency dependence graph of the complex dielectric constant and the complex magnetic permeability, which shows that the magnetic wave-absorbing material has excellent microwave absorption characteristics and electromagnetic impedance characteristics, and a health-care product with a magnetic therapy effect is expected to be prepared by utilizing the characteristics, so that the ternary composite material has a very wide application prospect.
The magnetic wave-absorbing material is prepared to form a collar, and clinical tests prove that the collar has the health-care effects of relieving the symptoms of patients and the pain of the cervical and shoulder vertebrae, so that the collar is beneficial to absorbing and storing environmental microwaves with the magnetic wave-absorbing material, acts on body cells by utilizing excellent microwave absorption characteristics and electromagnetic impedance characteristics, causes the resonance of atoms and molecules of body fluid of the body, activates the activity of cells of the whole body, can further activate blood for users, promotes blood circulation, and achieves the health-care effects of relieving pain and the like.
Drawings
Fig. 1 is an SEM image of a magnetic wave-absorbing material provided in embodiment 1 of the present invention.
Figure 2 is an XRD pattern provided by example 1 of the present invention.
Fig. 3 is an XPS chart provided in example 1 of the present invention.
FIG. 4 shows dielectric constants ε of example 1, comparative example 5 and comparative example 11 of the present inventionr' frequency distribution diagram.
FIG. 5 shows dielectric constants ε of example 1, comparative example 5 and comparative example 11 of the present inventionr"is used as a frequency distribution map.
FIG. 6 shows dielectric losses tan. delta. of examples 1, 5 and 11 of the present inventionεA frequency distribution map of (a).
FIG. 7 shows permeability constants μ of example 1, comparative example 5 and comparative example 11 of the present inventionr' frequency distribution diagram.
FIG. 8 is a graph showing magnetic permeability constants μ of example 1, comparative example 5 and comparative example 11 of the present inventionr"is used as a frequency distribution map.
FIG. 9 shows magnetic losses tan. delta. of examples 1, 5 and 11 of the present inventionμA frequency distribution map of (a).
FIG. 10 is a graph of the reflection loss of the absorber of example 1 of the present invention between 0.5 and 5.0mm thick.
FIG. 11 is a graph showing reflection loss of comparative example 1 of the present invention in which the thickness of the absorber is 0.5 to 5.0 mm.
FIG. 12 is a graph showing reflection loss of comparative example 5 of the present invention in which the thickness of the absorber is 0.5 to 5.0 mm.
FIG. 13 is a graph showing reflection loss of comparative example 11 of the present invention in which the thickness of the absorber is 0.5 to 5.0 mm.
FIG. 14 is an infrared thermal view of a user's arm according to an embodiment of the present invention.
Fig. 15 is an infrared thermal view of a wrist of a user wearing a wrist band made of the magnetic wave-absorbing material according to example 1.
FIG. 16 is an infrared thermal view of a user's shoulder and neck provided by an embodiment of the present invention.
Fig. 17 is an infrared thermal view of a user wearing a collar prepared based on the magnetic wave-absorbing material of example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The magnetic metal powder has the advantages of good wave absorbing performance and low cost, so that the magnetic metal powder becomes an absorbent with the greatest application prospect, but the application is limited due to the overlarge density of the magnetic metal powder. The expanded graphene has the advantages of low density, thin matching thickness, high complex dielectric constant, high specific surface area and the like. However, the single expanded graphene has poor impedance matching characteristics, and the magnetic loss composite material can be prepared by permeating magnetic metal powder. The magnetic loss composite material can be prepared by using expanded graphite with the density far lower than that of natural graphite, the density of the expanded graphite is about 200 times of that of the natural graphite, and the magnetic loss composite material has larger dielectric loss and has a great application prospect. Meanwhile, the material with single component and single loss mechanism is difficult to meet the requirements of thinness, lightness, width and strength. Therefore, the embodiment of the invention discloses a ternary composite material which is formed by expanded graphene, iron and cobalt, wherein the ternary composite material is provided with a pore channel with a hollow interior, and the iron and the cobalt are bonded or deposited in the pore channel. The ternary composite material is based on expanded graphene to form an inclusion, and the nano particles formed by iron and cobalt are wrapped in the inclusion, so that the formed microscopic nano structure has a synergistic electromagnetic improvement effect, and a plurality of dielectric medium and magnetic loss peak values are generated in a frequency dependence graph of the complex dielectric constant and the complex magnetic permeability, which shows that the magnetic wave-absorbing material has excellent microwave absorption characteristics and electromagnetic impedance characteristics, and a health-care product with a magnetic therapy effect is expected to be prepared by utilizing the characteristics, so that the ternary composite material has a very wide application prospect.
Specifically, iron and cobalt bonds are attached to the expanded graphene layer. Through the pore channels of the expanded graphite, iron and cobalt form nano particles and are wrapped in the pore channels to form an inclusion body, so that the whole structure is promoted to generate excellent microwave absorption characteristics and electromagnetic impedance characteristics. Alternatively, iron and cobalt are deposited in the channels in crystalline form.
In addition, the embodiment of the invention also discloses a preparation method of the magnetic wave-absorbing material, which comprises the following steps:
s1, dispersing the activated expanded graphene in ultrapure water, and uniformly stirring to obtain a first solution;
s2, preparing a second solution containing iron inorganic salt, cobalt inorganic salt and ethanol;
s3, mixing iron powder, cobalt powder, the first solution and the second solution, stirring, treating at 150-180 ℃, separating solids in the solution, and washing to obtain a primary material;
s4, placing the preliminary material in a mixed gas of hydrogen and argon for treatment, and controlling the temperature to rise to 700-900 ℃ for treatment to obtain the magnetic wave-absorbing material.
The ternary composite material disclosed by the embodiment of the invention can be prepared by the method, and particularly has a microstructure. In order to form the microstructure, the ratio of the iron element and the cobalt element in the second solution and the mixing mass ratio of the final iron powder, the cobalt powder, the expanded graphene, the iron inorganic salt and the cobalt inorganic salt are controlled to be (3-6): 100-150: (5-10): 5-10).
Further, in step S3, the pH is adjusted, for example, to not less than 8, by using a lye. For example, the alkaline solution is sodium hydroxide solution and the inorganic salt of iron is FeCl3，Fe2(SO4)3Or Fe (NO)3)3The inorganic cobalt salt is CoCl3，Co2(SO4)3Or Co (NO)3)3. The iron powder and the cobalt powder can be common solid powder, and can also be nano iron powder and nano cobalt powder.
In addition, in the final high-temperature treatment step, the volume ratio of the hydrogen to the argon in the mixed gas is (50-60): 40-50. By controlling the proportion of hydrogen in the mixed gas, the deposition or bonding mode of iron and cobalt in the expanded graphite can be controlled. Meanwhile, the temperature rise rate and the high-temperature treatment time in the process (step S4) can also play a role in controlling the manner in which iron and cobalt are deposited or bonded in the expanded graphite. In the step S4, the time required for raising the temperature from 150-180 ℃ to 700-900 ℃ in the step S3 is the temperature raising time, the controlled temperature raising rate is the temperature raising rate generated in the interval, and the high temperature processing time is the time for post-processing after raising the temperature to 700-900 ℃.
Preparation and characterization of magnetic wave-absorbing material
In order to further explain the preparation process and performance of the magnetic wave-absorbing material provided by the embodiment of the invention in detail, the following description is given with reference to more specific embodiments, and the description is shown in table 1.
TABLE 1
In table 1, the column S2 shows the concentrations of iron and cobalt in the second solution prepared in the step S2, and the volume concentration of ethanol; the S4 column shows the ratio of hydrogen in the mixed gas used in the S4 step, the rate of temperature increase, and the treatment time, and the reactant column shows the molar mass ratios of the iron powder, cobalt powder, expanded graphene, and the iron inorganic salt and cobalt inorganic salt added during the final reaction.
For example, the specific procedure for example 1 is as follows:
accurately weighing 30g of expanded graphene (analytically pure, Qingdao Oko graphite products factory), soaking in a strong alkali solution for 2h, taking out, washing with ultrapure water to be neutral, uniformly dispersing in 10L of ultrapure water, and uniformly stirring at 2-8 ℃ to obtain a first solution.
Accurately weighing 8.125g FeCl3、6.55g CoCl2The second solution was prepared by dissolving in 2.5L of ultrapure water containing 25 v/v%.
Mixing 10L of the first solution and 2.5L of the second solution, adding 4.875g of iron powder and 3.930g of nickel powder into the mixed solution, stirring, treating at 175 ℃ for 2 hours, separating solids in the solution, and washing to obtain a primary material;
and then placing the primary material in mixed gas of hydrogen and argon (55 v/v% of hydrogen) for treatment, and controlling the temperature to rise to 850 ℃ for treatment 2, wherein the temperature rise rate is 2 ℃/min, so as to obtain the magnetic wave-absorbing material.
Other examples and comparative examples can be made with reference to the specific procedure of example 1.
Properties of magnetic wave-absorbing materials
1. Characterization of microscopic features
(1) Scanning Electron microscope analysis (SEM)
A small amount of samples (prepared in examples 1-11 and comparative examples 1-13 respectively) are ultrasonically dispersed in absolute ethyl alcohol in a 10mL centrifuge tube, the solution is dripped on clean aluminum foil paper, after the ethyl alcohol is completely volatilized, small pieces of aluminum foil paper with better sample dispersion are cut off and pasted on carbon conductive gel of a sample table, and the prepared samples are observed for the surface appearance of the samples through a cold field emission scanning electron microscope (FE-SEM, Hitachi 5-4800, Hitachi, Japan, 5kV acceleration voltage). The content of the elements in the sample can be analyzed by an energy spectrum analyzer (EDX) matched with a Hitachi S-4800 type scanning electron microscope.
(2) X-ray diffraction analysis (XRD)
And filling the dried powder sample in a sample groove, compacting the sample groove by using a glass slide, and measuring the X-ray diffraction pattern of the sample by using a DIMAX-RB type target-rotating X-ray diffractometer in a scanning range of 10-80 degrees by using CuKalpha rays, wherein the wavelength lambda is 0.1452nm, and the step number is 10 DEG/min.
(3) X-ray photoelectron spectroscopy (XPS)
Pressing the dried powder sample into a sheet by a tablet press, clamping a small sample with smooth surface by forceps, pasting the small sample on the carbon conductive adhesive of a sample table, and carrying out X-ray photoelectron spectroscopy analysis on the surface of the sample by an X-ray photoelectron spectrometer (ESCALB 250Xi type).
2. Performance testing
(1) Magnetostatic Performance test (VSM)
About 20mg of sample is weighed by an analytical balance to the raw material adhesive tape, the three layers are wrapped into a sphere, and then the sphere is filled into a sample cup. The hysteresis loop of the sample was measured with a vibrating sample magnetometer (model LakeShore 7404) at room temperature and the static magnetic properties were analyzed.
(2) Electromagnetic parameter testing (EM)
Stirring and mixing the powder sample and the base material paraffin according to a certain proportion under the condition of heating, then pressing the mixture into a cylindrical sample by using a grinding tool, and measuring four electromagnetic parameters (epsilon) of the sample by using a network vector analyzer (Agilent N5234A, USA)r'，εr"，μr' and mur") the dynamic magnetic properties were analyzed. And use the reflection loss RLTo evaluate the microwave absorption characteristics. The reflection loss (RL in dB) was calculated from the following normalization equation. The normalization formula is as follows:
in the formula: zinThe input impedance, Ω, at the boundary of free space and the wave-absorbing coating.
εr＝εr'-jεr"and μr＝μr'-jμr"complex dielectric constant and complex permeability of the wave-absorbing material, respectively; d is the thickness of the wave-absorbing coating, and is mm; f is the frequency of the incident electromagnetic wave, Hz; c is the speed of light, m/s. Using tan delta epsilon ═ epsilonr"/εr' denotes dielectric loss by tan deltaμ＝μr"/μr' denotes magnetic loss.
3. Results
(1) Phase analysis
The phase and grain size of the samples were analyzed by XRD characterization (figure 2). A peak at 25.3 ° at 10 ° to 2 θ to 90 ° is a characteristic peak position of the expanded graphite; peaks at 32.4 °,40.3 °,52.3 ° and 64.3 ° respectively correspond to the Fe crystal plane, peaks at 46.49 °,51.84 ° and 76.37 ° respectively correspond to the cobalt crystal plane, and no other impurity peak appears. The resulting sample consisted of expanded graphene, Fe and cobalt. The diffraction peak of expanded graphite (expanded graphene) is sharp and narrow, indicating that the crystallinity of expanded graphene is good.
(2) Micro-morphology
The surface morphology of the composite material can be adjusted by changing the volume of the iron and the cobalt. The SEM further revealed the surface morphology and microstructure of the product. As shown in fig. 1, a bulk microstructure is smooth on the surface, has wrinkles on the edges, and has opaque diffraction spots in the middle of the bulk, which may be nanocrystalline particles of iron or cobalt.
Further XPS results enabled the determination of the composition of the sample surface and its chemical state (figure 3). As shown in FIG. 3, the product consists of three elements, namely Fe, Co and C, and the peaks with binding energies of 51.9,286.0,685.8,708.1 and 725.4eV are respectively attributed to Fe 3p, C1s, Co 2p1/2, Fe 2p3/2 and Fe 2p 1/2.
(3) Static magnetic property
The magnetostatic properties of the sample composites were measured using a vibrating sample magnetometer and it was found by plotting the M-H curves that almost all of the composites prepared in examples and comparative examples exhibited typical sigmoidal M-H curves indicating the presence of ferromagnetism, and the magnetostatic properties of the ternary composites prepared in each of examples and comparative examples are shown in table 2.
TABLE 2
Since pure expanded graphite is a diamagnetic material, the saturation magnetization is small. When it is compounded with Fe and cobalt, the specific saturation magnetization (M) of the compound is increased with the increase of the amount of the iron inorganic salt and the cobalt inorganic salt within the range defined in the practice of the present inventionS) Gradually increasing to 85.41-98.45 emu/g, almost mixing with M of pure block ferroferric oxide (92emu/g)SThe value is in the same level and is higher than that of the common ferroferric oxide nano (30.90-77.71 emu/g).
In general, the composition, surface spin disorder and grain size determine MSKey factor of value size. The heterostructure ternary composite material disclosed in the embodiment is composed of diamagnetic expanded graphite, ferromagnetic iron and ferromagnetic cobalt. Thus, MSThe value of (a) depends mainly on the iron and cobalt contents and the microstructure they form. MSThe relationship between the respective iron and cobalt contents can be expressed by the lorentz equation. In addition, larger values of D result in reduced surface spin disorder or increased magnetic moment, which ensures higher MSThe value of D is also determined by the structure formed by the expanded graphene coated iron crystal particles and cobalt crystal particles formed by the invention.
According to the embodiment of the invention, after the iron crystal particles and the cobalt crystal particles are compounded in the expanded graphene, the coercive force (Hc) of the compound is gradually reduced to 204.76Oe from 3213.8Oe of iron and cobalt alloy, and the value of Hc is obviously higher than that of octahedron Fe3O4161.67Oe, Fe of particles3O455.65Oe, Fe nanospheres3O420.69Oe of nanoring. Affecting the magnitude of Hc may be related to several factors: (1) specific heterostructure materials produce coupling and spatial confinement effects. The heterostructure consists of expanded graphite, Fe and cobalt. The interaction between the expanded graphite and the magnetic particles (iron and cobalt) hinders the magnetic response of the magnetic particles to the applied magnetic field and the adjoining magnetic particles. The coupling between the magnetic particles decreases with spacing or the magnetic particlesGrain formation increases. (2) The shape anisotropy of Fe/Co nanocrystals will prevent them from magnetizing in directions other than their easy axis, resulting in a decrease in Hc. (3) Crystal size is a critical factor in determining the size of Hc. The crystal size (15.6-32.5 nm) is very close to that of single magnetic domain Fe3O4Critical dimension (Dc) (about 25 nm). When the crystal size is lower than Dc, Hc decreases with decreasing crystal size because thermal energy affects the magnetic moment orientation in the domain, exhibiting superparamagnetic behavior. In contrast, if the crystal size is larger than Dc, Hc decreases with an increase in the crystal size because the magnetization changes into domain wall motion.
From table 2, it is found that the specific saturation magnetizations of examples 1 to 11 are all higher than those of comparative examples 1 to 13, and the coercive force of the composites prepared in the examples is significantly lower than that of the comparative examples. This shows that the compound prepared by the embodiment has larger ferromagnetism, lower coercive force and easier magnetization, and the microstructure formed by wrapping iron grains and cobalt grains by the expanded graphite is more favorable for realizing magnetization.
(4) Microwave absorption performance
The composition of the sample and the microwave absorption characteristics dependent on the surface topography were studied in the range of 2-18 GHz, as shown in FIGS. 10-13 and Table 3.
In table 3, the examples are in a lower microwave range in the frequency range of RL ≦ 10dB compared to the comparative examples, which shows that the magnetic wave-absorbing material prepared in the examples has a lower microwave absorption effect, and the examples have a lower reflection loss value and correspond to a larger theoretical sample matching thickness. Wherein the theoretical matching thickness (t)m) Can pass through
Wherein f ismFor matching the frequency, c is the speed of light, μrIs complex permeability, epsilonrIs the complex dielectric constant.
In table 3, in the comparative examples 1 to 4, compared to example 1, in the second solution preparation process in step S2, the mixing ratio of the iron salt, the cobalt salt or the ethanol is not controlled reasonably, so that the frequency of the reflection loss RL ≦ 10dB is increased, and the frequency is shifted away from the microwave range. Comparative examples 5 to 13 are those in which the ratio of reactants used is out of the range defined in the above example or the treatment conditions at step S4 are not reasonable as in example 1, resulting in a further increase in the frequency at which the reflection loss RL ≦ 10dB is further increased, a further shift away from the microwave range, and a further increase in the maximum reflection loss value, and deterioration in the wave-absorbing property. In addition, comparative examples 1 to 13 have matching thicknesses with smaller maximum reflection loss values than example 1, which is disadvantageous for practical use.
TABLE 3
Electromagnetic parameters can reveal the microwave absorption mechanism of the composite material. The expanded graphene is a resistive loss type wave-absorbing material, and has high conductivity ((0.07m Ω · cm) and dielectric loss (tan δ ∈ ═ 1.6 to 91.8 and E ″: 0.47165.37)r' and εr"sharp drop (fig. 4, 5). Fe3O4Is an absorber with low conductivity and low dielectric constant, while Fe is a double loss absorber with high conductivity and dielectric constant. The sample expanded graphene/Fe/Co composite material can eliminate the eddy current loss, so that the complex dielectric constant epsilon of the composite materialrOnly slight changes will occur. The composite material shows a lower value at low frequencies and a higher value at high frequencies compared to pure expanded graphene. The complex permittivity value first increases and then decreases from sample S3 to S4.
In general, εr' and εrThe increase in the "value is associated with an increase in space charge, orientation or interfacial polarization caused by an increase in defects (represented by internal stress), aspect ratio and specific surface area (SBET), respectively. Based on the above results, the enhanced dielectric constant of the expanded graphene/Fe/Co composite material reported herein is due to the composition and surface morphology of the expanded graphene/Fe/Co composite material.
The interface and dipole are two key factors that determine the polarization of the interface. In the heterostructure expanded graphene/Fe/Co composite, additional interfaces exist between the expanded graphene and Fe and between the expanded graphene and Co. As can be seen from the SEM image in fig. 1, an additional interface is formed due to grain formation of Fe and Co.
This additional interface results in the work function of the expanded graphene (2.0-5.0eV), Fe (4.5eV), Fe (3.7eV) being lower than Fe3O4A work function (about 5.52eV) promotes the electron transition from the expanded graphene to Fe or Co for the composite. The charge accumulated at the heterogeneous interface forms many dipoles, contributing to an increase in the dielectric constant. The polarization and relaxation of the expanded graphene with high conductivity result from the migration of electrons in the graphite plane direction and the hopping of electrons between disordered graphite layers. When the expanded graphene is compounded with Fe and Co, the charges accumulated on the surfaces of Fe, Co and the expanded graphene generate debye relaxation processes at the interface between two different dielectrics under external alternating voltage. In addition, the plasmon resonance effect should also be the cause of the enhancement of the electromagnetic field, i.e., the increase in the composite dielectric constant of the composite material.
The expanded graphene/Fe/Co composite has an additional interface that causes a localized surface plasmon resonance effect. Under an alternating electromagnetic field, the excitation state of free electron collective oscillation of the iron nano-crystal and the cobalt nano-crystal is coupled and combined with incident photons to form a mixed excitation state. Free electrons in the nanocrystals and expanded graphene collectively oscillate as waves, resulting in significant enhancement of polarization and local electric fields. The growth of the nanocrystalline on the surface of the expanded graphene/Fe/Co composite material is gradually increased, the number of excited electrons is increased, and the plasma resonance effect is enhanced. In addition, the Fe/Co nano particles form a local power grid on the surface of the expanded graphene, and micro-current is generated in an alternating electric field along the direction of a graphite surface. When a micro-current passes through the interface between Fe/Co and expanded graphene, many dipoles are formed on their interface, thereby enhancing the dielectric constant. These results indicate that the expanded graphene Fe/Co composite has a stronger storage capacity and has a stronger electrical and magnetic loss capacity than expanded graphene.
As shown in FIGS. 7-9, the pure expanded graphene has diamagnetic properties and shows low mur' and mur"value". In contrast, expanded graphene/Fe/Co compositesMu of materialr' and murThe "value shows different degrees of increase with the introduction of iron and cobalt grains. As is well known, the magnetic permeability is inversely proportional to the coercivity Hc and proportional to the saturation magnetization Ms.
As such, the plasmon resonance effect plays a key role in magnetic permeability enhancement. In the above examples, examples 1 to 11 and comparative examples 1 to 13 were prepared with different proportions of reactants to produce different degrees of enhancement of plasmon resonance. Whereas the decrease in the values of μ r' and μ r "is due to the decrease in the plasmon resonance effect.
Eddy current loss is further researched, and a magnetic loss mechanism of the expanded graphene/Fe/Co composite material is disclosed. Under a weak electromagnetic field of 2-18 GHz, the magnetic loss of the multi-domain material is mainly determined by eddy current loss, natural resonance and exchange resonance. According to the skin effect, if the magnetic loss is generated only by the eddy current loss effect, its value remains unchanged as the frequency changes.
As can be seen from fig. 7, two broad resonance peaks were observed for the expanded graphene/Fe/Co composite. Therefore, the magnetic loss of the expanded graphene/Fe/Co composite material is mainly due to natural resonance at low frequency and exchange resonance at high frequency. Therefore, the excellent microwave absorption properties are attributed to the heterostructure of magnetic Fe, Co and layered expanded graphene, which results in enhanced permittivity, permeability, multiple scattering, multi-polarization and multiple resonance.
Health care product
The embodiment of the invention also discloses health-care products prepared by the magnetic wave-absorbing material of the embodiment, and the health-care products comprise at least one of a collar, a wrist ring, a waist ring and an ankle ring.
In order to solve the chronic diseases caused by metabolism, a plurality of solutions are provided in modern medicine and traditional Chinese medicine health preservation, but the effect is limited. To date, there is no more scientific, safe, effective, and economical technique to address the health problems caused by metabolism. Because 65% -70% of human body is made up of water, the function of water in human body is to transmit nutrients, promote blood circulation, help digestion, excrete wastes, keep respiratory function, lubricate joints and regulate body temperature. The water not only plays the role of conveying and mediating substances in the body, but also directly participates in the structure of the biomacromolecules, and the water and the biomacromolecules complete the substance metabolism, the energy metabolism and the information metabolism of the human body together. Water is directly related to aging, life, immunity and metabolism, and is the source of life and the healthy root. When the amount of bound water becomes large, it means that the metabolic capability of the human body is deteriorated. When the free water content in the body is increased, the metabolic capability of cells is accelerated, and meanwhile, more electrons and ions are obtained.
Based on the provided health-care product, the unique microwave absorption performance and electromagnetic property of the magnetic wave-absorbing material can be utilized, the free water content in tissue fluid of an organism can be greatly increased, the number of electrons in the organism is increased, negative charges are increased, and the oxidation resistance of cells and tissue environments is enhanced; meanwhile, the blood flow and the hemoglobin quantity passing through the unit time can be increased, the immunity of the organism can be enhanced, various diseases can be resisted or relieved, and the removing effect is particularly realized on the blood circulation and the cold syndrome of the neck. The following description will be made in connection with specific clinical trials.
First, warm heat test
In order to confirm the warming effect of the silica gel bracelet or necklace prepared by wearing the magnetic wave-absorbing material provided by the embodiment of the invention on the skin surface of a user, the temperature change of the neck part after wearing is measured by thermotherapy.
1. Materials and methods
The following tests were performed: the test products are silica gel wrist rings and collars; measuring environment: room temperature 22 ℃ and humidity 41%; measurement machine: NEC III
(l) charging サ - モトレ - サ -TH 3100MR type;
the wrist ring and the collar are manufactured by using the magnetic wave-absorbing materials obtained in the embodiment 1, the comparative example 5 and the comparative example 11 respectively, for example, the manufactured annular body and a coating such as silica gel coated outside the annular body are manufactured into a shape which is beneficial to wearing.
And (3) determination: adult women (age 54) of healthy persons as subjects were allowed to measure the skin surface temperature after 20 minutes of ambient temperature adaptation in an environment of room temperature 22 ℃ and humidity 41%; then, a silica gel bracelet and a necklace were worn, and the surface temperature of the skin at the neck was measured by heat therapy 30 minutes later, and these results were subjected to thermal image display.
2. Results and analysis
TABLE 4 average temperature before and after wear
As shown in Table 4, the temperature of the arm increased by 1 ℃ and the temperature of the neck increased by 1.4 ℃ in the group of example 1 after using the wrist band; no obvious body surface temperature increase effect is observed in other groups. Fig. 14-17 show the infrared thermal views of the wrist band and the collar of the group of example 1 before and after the use, respectively, and it can be seen that the infrared thermal views are obvious when the user wears the wrist band or the collar. Therefore, the wearing of the silica gel wrist ring and the collar has good warm-heat characteristics, and further indirectly proves that the magnetic wave-absorbing material prepared in the embodiment of the invention has the warm-heat characteristics, while the magnetic wave-absorbing materials prepared in the comparative examples 1, 5 and 11 do not have the functions, which may be related to the preparation process and the microstructure thereof.
Second, neck and shoulder pain test
1. Clinical bed data
1.1 general data
Patient symptom criteria were selected: the patient has limited neck movement, stiff muscles, soreness, distension, numbness and pain in the neck, shoulders and arms, and may be accompanied by hand numbness. Symptoms correspond to the corresponding nerve root innervation regions. The body is positive in an intervertebral foramen squeezing experiment or a nerve root traction experiment. The X-ray film prompts the cervical vertebra to degenerate, the CT or MRI prompts the cervical disc to protrude, the nerve root is pressed, and the upper arm symptom can be clearly found by combining with electromyogram examination.
1.2, treatment
The observed cases are total255 patients with cervical spondylosis of single segment nerve root type or mixed type, who have neck and shoulder pain as the main symptom, are counted. They were divided into example 1 group, comparative example 5 group, comparative example 11 group and reference group, respectively, with 51 persons each. The cases of the example 1 group, the comparative example 5 group, and the comparative example 11 group worn collars manufactured respectively based on the example 1, the comparative example 5, and the comparative example 11 materials for 1 month. The reference group did not wear the collar. The neck ring comprises an annular body made of the magnetic wave-absorbing material and a coating such as silica gel coated outside the annular body, and the shape of the neck ring is convenient to wear. The gender, age, course and lesion segment composition of the two groups are compared in table 4. Wherein the age and disease course are compared by t test and the diseased segment is compared by X test2Test, "' indicates relative to the reference group P>0.05 means that the difference is not statistically significant.
TABLE 4
| Group of | Average age (year of age) | Mean course of disease (moon) | Neck 34 | Neck 45 | Neck 56 | Neck 67 |
| EXAMPLE 1 group | 42±2.3* | 62±1.4* | 11* | 13* | 15* | 12* |
| Comparative example 1 group | 43±1.5* | 55±2.3* | 11* | 12* | 16* | 12* |
| Comparative example 5 group | 42±2.2* | 61±0.8* | 11* | 12* | 15* | 13* |
| Comparative example 11 group | 43±1.6* | 59±1.7* | 11* | 13* | 15* | 12* |
| Reference group | 42±0.7 | 58±2.3 | 11 | 12 | 15 | 12 |
1.3, clinical criteria for case selection:
firstly, there is a cervical pain accompanied by a radicular pain.
② the patients are between 30-60 years old.
And the disease course is 1-3 years after more than three months of various conservative treatments.
And fourthly, checking whether the intervertebral foramen extrusion experiment or the nerve root traction experiment is positive or not, and the upper limb numbness phenomenon exists or not.
1.4, imaging standard: the projections were shown to occupy less than 40% of the cross-sectional area of the spinal canal based on imaging examination.
1.5, exclusion criteria
The prominences are calcified more seriously, and the like.
② the accompanied centrum slippage degree reaches II degree and above.
And protrusion or prolapse type cervical disc herniation.
Fourthly, some contraindications exist in the traditional Chinese medicine, such as bleeding tendency, spinal canal tumor, psychologic disease patients and the like.
1.6, statistical treatment
And (3) carrying out outpatient service or telephone follow-up visit on the patient three months after the test is finished, carrying out curative effect evaluation by adopting an improved Macnab curative effect evaluation standard, grading the pain degree of the patient before and after the operation by adopting VAS (virtual approach space) grading, and recording and collating data. The SPSS 19.0 Chinese version statistical software package is adopted, the measurement data are expressed by X +/-s, and the comparison between the two averages adopts t test; using X as calculation data2Test, "+" indicates P compared to the reference group<0.05 had statistically significant differences.
2. Comparison of efficacy evaluation by Macnab
The Macnab therapeutic evaluation criteria are: and (3) excellent: the symptom signs completely disappear, the motor function is not limited, and the original work and life are recovered; good: slight symptoms exist, the activity is slightly limited, and the work and life are not affected; can be as follows: symptoms are relieved, activities are limited, and normal work and life are influenced; difference: before and after treatment, the disease is not different or even aggravated. The yield is (excellent + excellent)/total number of cases × 100%.
The comparison result is shown in table 6, and it can be seen from the data in the table that the curative effect of the group in example 1 is more obvious in comparison and is significantly higher than that of other groups, which indicates that the neck ring made of the magnetic wave-absorbing material provided by the embodiment of the invention can greatly modify the cervical spondylosis of patients.
TABLE 5
| Group of | Number of cases | Superior food | Good wine | Can be used for | Difference (D) | Good yield (%) |
| EXAMPLE 1 group | 51 | 47 | 2 | 1 | 1 | 96.08** |
| Comparative example 1 group | 51 | 32 | 2 | 0 | 17 | 66.67* |
| Comparative example 5 group | 51 | 5 | 3 | 5 | 35 | 15.69* |
| Comparative example 11 group | 51 | 4 | 6 | 7 | 34 | 19.61* |
| Reference group | 51 | - | - | 5 | 46 | - |
3. VAS score comparison of neck and shoulder pain before and after treatment
The VAS scoring system is a visual simulation scoring system, the pain degree grading is carried out by taking 0-10 as the pain degree, the neck and shoulder pain degree is quantified, the score of each group after the neck ring is worn is counted, all cases of each group are counted, the neck and shoulder pain degree is scored, and the scoring result is listed in a table 6. As shown in table 6, both the example 1 group and the comparative example 1 group significantly reduced the score relative to the reference group, while the other two groups did not change, and the score of the example 1 group was also significantly lower than that of the comparative example 1 group. The neck ring made of the magnetic wave-absorbing material provided by the embodiment of the invention can relieve neck and shoulder pain of a patient, and has a unique health-care physiotherapy effect.
TABLE 6
| Group of | Statistics of the number of cases | Before wearing | After wearing |
| EXAMPLE 1 group | 51 | 5.62±0.27 | 1.08±0.08** |
| Comparative example 1 group | 51 | 5.46±0.51 | 3.38±0.82* |
| Comparative example 5 group | 51 | 5.37±0.25 | 5.18±0.14 |
| Comparative example 11 group | 51 | 5.43±0.25 | 5.09±0.33 |
| Reference group | 51 | 5.32±0.36 | 5.12±0.13 |
In summary, in the embodiments of the present invention, the expanded graphene, the iron and the cobalt form a ternary composite material, the ternary composite material has a hollow pore channel, and the iron and the cobalt are bonded or deposited in the pore channel. The ternary composite material is based on expanded graphene to form an inclusion, and the nano particles formed by iron and cobalt are wrapped in the inclusion, so that the formed microscopic nano structure has a synergistic electromagnetic improvement effect, and a plurality of dielectric medium and magnetic loss peak values are generated in a frequency dependence graph of the complex dielectric constant and the complex magnetic permeability, which shows that the magnetic wave-absorbing material has excellent microwave absorption characteristics and electromagnetic impedance characteristics, and a health-care product with a magnetic therapy effect is expected to be prepared by utilizing the characteristics, so that the ternary composite material has a very wide application prospect.
The wrist ring and the neck ring are formed by preparing the magnetic wave-absorbing material, and clinical tests prove that the neck ring has a warming effect, so that immune cells of a user can be greatly activated, and the immune function of the user is improved. In addition, clinical tests of the shoulder and cervical vertebra prove that the wrist ring and the neck ring prepared from the magnetic wave-absorbing material have the effects of relieving the symptoms of patients and the pain symptoms of the neck and the shoulder vertebra, which are possibly absorbed and stored with the magnetic wave-absorbing material to the environment microwave, and act on cells of an organism by utilizing excellent microwave absorption characteristics and electromagnetic impedance characteristics to cause resonance of atoms and molecules of body fluid of the organism, activate the activity of cells of the whole body, and simultaneously promote the blood circulation of a user due to the warming effect of the body fluid so as to achieve the effects of relieving pain and relieving health care.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. The magnetic wave-absorbing material is a ternary composite material formed by expanded graphene, iron and cobalt, the ternary composite material is provided with a pore channel with a hollow interior, and the iron and the cobalt are bonded or deposited in the pore channel.
2. A magnetic wave absorbing material according to claim 1 wherein the iron and cobalt bonds are connected between expanded graphene layers.
3. The magnetic wave absorbing material of claim 1 wherein the iron and cobalt are deposited in the channels in a crystalline formation.
4. A method for preparing a magnetic wave-absorbing material according to any one of claims 1 to 3, comprising the following steps:
dispersing the activated expanded graphene in ultrapure water, and uniformly stirring to obtain a first solution;
preparing a second solution comprising iron inorganic salt, cobalt inorganic salt and ethanol;
mixing iron powder, cobalt powder, the first solution and the second solution, stirring, treating at 150-180 ℃, separating solids in the solution, and washing to obtain a primary material;
and then, placing the preliminary material in a mixed gas of hydrogen and argon for treatment, and controlling the temperature to rise to 700-900 ℃ for treatment to obtain the magnetic wave-absorbing material.
5. The method according to claim 4, wherein the second solution contains 15 to 20mol/L of iron element, 15 to 20mol/L of cobalt element, and 25 to 40 v/v% of ethanol.
6. The preparation method according to claim 4, wherein the mixing mass ratio of the iron powder, the cobalt powder, the expanded graphene, the iron inorganic salt and the cobalt inorganic salt in the reactants is (3-6): 100-150): 5-10: (5-10).
7. The method according to claim 4, wherein the volume ratio of the hydrogen gas to the argon gas in the mixed gas is (50-60) to (40-50).
8. A health product prepared on the basis of the magnetic wave-absorbing material of any one of claims 1 to 3 or the magnetic wave-absorbing material prepared by the preparation method of any one of claims 4 to 7.
9. The health product of claim 8, wherein the health product comprises at least one of a collar, a wrist band, a waist band, and an ankle band.
10. The magnetic wave-absorbing material according to any one of claims 1 to 3 or the magnetic wave-absorbing material prepared by the preparation method according to any one of claims 4 to 7 is applied to the preparation of health-care products for improving cervical vertebra pain.
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