CN108570211B - Composite material with low-frequency-dispersion negative dielectric property and preparation method thereof - Google Patents
Composite material with low-frequency-dispersion negative dielectric property and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/0856—Iron
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Abstract
The invention discloses a composite material with low-frequency dispersion negative dielectric property and a preparation method thereof, belonging to the field of metamaterial with negative dielectric constant. The composite material with the low-frequency-dispersion negative dielectric property comprises the following components in parts by weight: 18-23 parts of carbon fiber, 5-12 parts of insulating coated iron powder and the balance of epoxy resin. The invention provides a composite material with low-frequency-dispersion negative dielectric property and a preparation method thereof, wherein a carbon fiber material is uniformly dispersed in an epoxy resin matrix, and iron particles coated by insulation are added to obtain a carbon fiber-iron particles-epoxy resin ternary composite material with low-frequency-dispersion negative dielectric property; the invention has the advantages of low preparation cost, stable process, simple operation and treatment and large performance regulation interval.
Description
Technical Field
The invention belongs to the field of metamaterials with negative dielectric constants, and particularly relates to a composite material with low-frequency-dispersion negative dielectric properties and a preparation method thereof.
Background
The dielectric constant is a fundamental electrical parameter of a material, characterizing its ability to generate polarization charges under an external electric field. In general, the dielectric constant is positive and a function of frequency. The requirements for dielectric constant are different in different frequency ranges and different application fields. When used in kHz capacitors, the materials are required to have a high dielectric constant and low dielectric loss; when the material is used as a GHz wave-transmitting material, the low dielectric constant and the low dielectric loss are beneficial to the transmission of electromagnetic waves; when used as a wave-absorbing material, the material needs to have a low dielectric constant to satisfy impedance matching, and a high dielectric loss realizes strong absorption. Therefore, the method has important application significance in the field of electronics and electricians for regulating and controlling the dielectric constant of the material.
When the dielectric constant is negative, such materials are called negative dielectric materials, and the novel electromagnetic properties caused by the negative dielectric materials attract great attention of researchers at home and abroad. The negative dielectric generated by metal plasma oscillation can be used as electromagnetic shielding, the negative capacitance effect of the ferroelectric material can promote the loss reduction and miniaturization design of the transistor, and the negative dielectric metal particle array greatly improves the propagation distance of surface plasmons. When the negative dielectric structure and the negative magnetic conductivity structure are compounded in a certain arrangement mode, perfect stealth of a microwave band can be realized; the high-resolution imaging technology based on the negative dielectric material and the negative magnetic conductivity material can break the diffraction limit of the traditional lens imaging, and greatly improves the resolution. Therefore, to drive the development of new electronic devices, the construction and performance control of negative dielectric materials becomes especially important.
Negative dielectric materials are classified into two types, an array type and an intrinsic type. The array type is researched more, and the realization mode is that functional units are arranged according to a certain rule mainly by a micro-processing method, and the propagation path of electromagnetic waves is accurately controlled in a resonance mode. The array type is also called as metamaterial or a metamaterial medium because the composition and the microstructure of the material in the array type are not concerned, but the macroscopic geometry, the size and the arrangement mode of the functional units are changed to realize the controllability of the performance. The research on the intrinsic type is late, and the intrinsic property of the materials such as the chemical components and the microstructure of the materials is controlled to regulate and control the negative dielectric constant, so that the intrinsic negative dielectric material is called. Compared with the array type, the intrinsic type has the greatest advantage of low cost and is suitable for industrialization.
Intrinsic type negative dielectric materials (hereinafter all negative dielectric materials are intrinsic type) are typical conductor-insulator heterocomposites. Research shows that by adding conductive phases such as metal, carbon nano tubes and graphene into an insulating ceramic or polymer matrix, negative dielectric performance can be realized when the conductive phases are connected into a conductive network in the matrix. And the size and the frequency dispersion of the negative dielectric constant can be regulated and controlled by controlling the composition, the particle size and the shape of the filler. Theoretical studies indicate that the negative dielectric constant is due to plasma oscillation, and the dispersion relation of the negative dielectric satisfies Drude model. However, the Drude type negative dielectric has high dielectric loss and serious dispersion in the MHz band and the kHz band. Although the dielectric loss can be compensated by introducing gain in practical application, the high frequency dispersion is the specific property of the negative dielectric material and is difficult to improve through auxiliary accessories, which seriously limits the use of the negative dielectric material in a wider frequency band, in particular to the impedance matching problem in the fields of wave absorption and the like. Therefore, the preparation of the negative dielectric material with low frequency dispersion characteristic has important significance for expanding the frequency band and the field of negative dielectric application.
Experimental studies show that the conductive phase can contribute to negative dielectric property when being communicated, and the conductive phase can improve positive dielectric property when existing in an isolated state; when an isolated conductive phase is added to the negative dielectric material, the dispersion characteristics of the negative dielectric can be adjusted. The conductive phases themselves have distributed capacitance, whether they are connected or isolated.
Disclosure of Invention
In order to solve the problems that the negative dielectric material in the prior art has serious frequency dispersion and cannot meet the broadband impedance matching, the invention provides a composite material with broadband low-frequency-dispersion negative dielectric property in a 100MHz frequency band and a preparation method thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a composite material with low-frequency dispersion negative dielectric property, which comprises the following components in parts by volume:
18-23 parts of carbon fiber
5-12 parts of insulating coated iron powder
The balance of epoxy resin.
Further, the insulating coated iron powder is an iron-phosphorus compound with insulating property, and the iron powder is carbonyl iron powder and is spherical particles with the particle size of 1-5 mu m; the length of the carbon fiber is 30-50 mu m, and the diameter of the carbon fiber is 1-5 mu m; the epoxy resin is bisphenol AB type solid powder, and the epoxy resin is thermosetting resin. Only when the volume fraction of the carbon fiber is between 18% and 23%, a network structure can be formed in the composite material, and the negative dielectric constant of the composite material can be regulated and controlled by adding the insulating coated metal powder.
In another aspect, the present invention further provides a preparation method of the composite material with low frequency dispersion negative dielectric property, including:
step 1: synthesizing insulating coated iron powder;
step 2: the insulating coated iron powder regulates and controls the negative dielectric property of the carbon fiber/epoxy resin composite material.
Further, the step 1 specifically comprises the following steps:
11) taking a phosphoric acid solution, putting iron powder into the phosphoric acid solution, and reacting for a period of time under certain conditions;
12) and filtering and cleaning to obtain the insulating coated iron powder.
Further, in the step 11), the reaction is carried out for 1-2 hours at normal temperature or for 30-40 min at 60 ℃ in water bath under certain conditions.
Forming a layer of compact iron and phosphorus compounds with insulating property on the surface of the iron powder, thus forming the insulating coated iron powder; wherein, the concentration, the reaction temperature and the reaction time of the phosphoric acid solution all have influence on the subsequent negative dielectric constant regulation.
Further, the step 2 specifically comprises the following steps:
21) weighing carbon fibers, epoxy resin and insulation coated iron powder, and putting into a vibration ball milling tank for ball milling;
22) and putting the mixed powder into a mold, and carrying out hot press molding to obtain the composite material with the low-frequency-dispersion negative dielectric property.
Further, in the step 21), the volume ratio of the carbon fibers to the epoxy resin is 1: 3-4; the mass of the insulated coated iron powder is 5-12% of the total volume of the mixed powder.
Further, the ball milling is performed by firstly vibrating at a low frequency for 30-40 seconds, then vibrating at a high frequency for 30-50 seconds, and circulating for 2-3 times to uniformly mix;
the hot pressing temperature is 75-85 ℃, and the pressure is 30 MPa.
The invention provides a composite material with low-frequency dispersion negative dielectric property in a MHz frequency band and a preparation method thereof, and the composite material has the following beneficial effects:
1) uniformly dispersing a carbon fiber material in an epoxy resin matrix, keeping the volume fraction of the carbon fiber unchanged, and adding insulated and coated iron particles to obtain a carbon fiber-iron particle-epoxy resin ternary composite material;
2) obtaining a material with low-frequency-dispersion negative dielectric property by regulating the content of the iron particles coated in an insulating way;
3) the invention adopts the conductive fiber material as the functional body to realize the negative dielectric property, reduces the influence of the distributed capacitance effect on the negative dielectric, and further adjusts the frequency dispersion characteristic of the negative dielectric by adding the isolated phase (namely the iron particles coated by insulation) in the negative dielectric material so as to improve the defect of serious frequency dispersion;
4) the invention has the advantages of low preparation cost, stable process, simple operation and treatment and large performance regulation interval.
Drawings
FIG. 1 is a dielectric spectrum of a 23% carbon fiber/epoxy composite prepared in comparative example 1 of the present invention;
FIG. 2 is an SEM image of carbonyl iron powder;
fig. 3 shows the dielectric spectrum of the carbon fiber/insulation coated metal powder/epoxy resin composite material prepared in examples 3, 4 and 5 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is made with reference to specific embodiments and accompanying drawings.
The above-described scheme is further illustrated below with reference to specific examples. It should be understood that these examples are for illustrative purposes and are not intended to limit the scope of the present invention. The conditions used in the examples may be further adjusted according to the conditions of the particular manufacturer, and the conditions not specified are generally the conditions in routine experiments.
Materials, reagents and the like used in the following examples are commercially available. The iron powder is carbonyl iron powder with the particle size of 1-5 mu m and is spherical particles, as shown in figure 2; the length of the carbon fiber is 30-50 mu m, and the diameter of the carbon fiber is 1-5 mu m; the epoxy resin is bisphenol AB type solid powder.
The invention provides a composite material with low-frequency dispersion negative dielectric property and a preparation method thereof, and the specific material dosage and experimental process are shown in the following examples.
Example 1:
a composite material with low-frequency dispersion negative dielectric property is composed of the following components in parts by volume:
18 parts of carbon fiber
Insulating coated iron powder 5 parts
The balance of epoxy resin.
The preparation method of the composite material with the low-frequency dispersion negative dielectric property comprises the following steps:
step 1: synthesis of insulating coated iron powder
11)400mL of phosphoric acid solution with the mass fraction of 0.016g/mL, and 20 g of iron powder is put into the phosphoric acid solution to react for 2h at normal temperature;
12) and filtering and cleaning to obtain the insulating coated iron powder.
Step 2: regulating and controlling negative dielectric property of carbon fiber/epoxy resin composite material by insulating coated iron powder
21) Taking the carbon fibers, the epoxy resin and the insulation coated iron powder in parts by volume, putting the carbon fibers, the epoxy resin and the insulation coated iron powder into a vibration ball milling tank for ball milling, firstly vibrating at low frequency for 30 seconds, then vibrating at high frequency for 30 seconds, circulating for 2 times to uniformly mix, and uniformly mixing; wherein the volume ratio of the carbon fiber to the epoxy resin is 1: 3; the mass of the insulating coated iron powder is 5% of the total volume of the mixed powder;
22) and putting the mixed powder into a die, and carrying out hot press molding at the hot press temperature of 75 ℃ and the pressure of 30MPa to obtain the composite material with the low-frequency-dispersion negative dielectric property.
Example 2:
a composite material with low-frequency dispersion negative dielectric property is composed of the following components in parts by volume:
20 parts of carbon fiber
8 portions of insulating coated iron powder
The balance of epoxy resin.
The preparation method of the composite material with the low-frequency dispersion negative dielectric property comprises the following steps:
step 1: synthesis of insulating coated iron powder
11)400mL of phosphoric acid solution with the mass fraction of 0.016g/mL, 20 g of iron powder is put into the phosphoric acid solution and reacts for 30min in a water bath at the temperature of 60 ℃;
12) and filtering and cleaning to obtain the insulating coated iron powder.
Step 2: regulating and controlling negative dielectric property of carbon fiber/epoxy resin composite material by insulating coated iron powder
21) Taking the carbon fibers, the epoxy resin and the insulation coated iron powder in parts by volume, putting the carbon fibers, the epoxy resin and the insulation coated iron powder into a vibration ball milling tank for ball milling, firstly vibrating at low frequency for 40 seconds, then vibrating at high frequency for 50 seconds, circulating for 3 times to uniformly mix, and uniformly mixing;
22) and putting the mixed powder into a die, and carrying out hot press molding at the hot press temperature of 80 ℃ and the pressure of 30MPa to obtain the composite material with the low-frequency-dispersion negative dielectric property.
Example 3:
a composite material with low-frequency dispersion negative dielectric property is composed of the following components in parts by volume:
carbon fiber 23 parts
10 portions of insulating coated iron powder
The balance of epoxy resin.
The preparation method of the composite material with the low-frequency dispersion negative dielectric property comprises the following steps:
step 1: synthesis of insulating coated iron powder
11)400mL of phosphoric acid solution with the mass fraction of 0.016g/mL, 20 g of iron powder is put into the phosphoric acid solution and reacts for 40min in a water bath at the temperature of 60 ℃;
12) and filtering and cleaning to obtain the insulating coated iron powder.
Step 2: regulating and controlling negative dielectric property of carbon fiber/epoxy resin composite material by insulating coated iron powder
21) Taking the carbon fibers, the epoxy resin and the insulation coated iron powder in parts by volume, putting the carbon fibers, the epoxy resin and the insulation coated iron powder into a vibration ball milling tank for ball milling, firstly vibrating at low frequency for 35 seconds, then vibrating at high frequency for 40 seconds, circulating for 3 times to uniformly mix, and uniformly mixing;
22) and putting the mixed powder into a die, and carrying out hot press molding at the hot press temperature of 85 ℃ and the pressure of 30MPa to obtain the composite material with the low-frequency-dispersion negative dielectric property.
Example 4:
a composite material with low-frequency dispersion negative dielectric property is composed of the following components in parts by volume:
carbon fiber 23 parts
12 portions of insulating coated iron powder
The balance of epoxy resin.
The preparation method of the composite material with the low-frequency dispersion negative dielectric property comprises the following steps:
step 1: synthesis of insulating coated iron powder
11)400mL of phosphoric acid solution with the mass fraction of 0.016g/mL, and 20 g of iron powder is put into the phosphoric acid solution to react for 1h at normal temperature;
12) and filtering and cleaning to obtain the insulating coated iron powder.
Step 2: regulating and controlling negative dielectric property of carbon fiber/epoxy resin composite material by insulating coated iron powder
21) Taking the carbon fibers, the epoxy resin and the insulation coated iron powder in parts by volume, putting the carbon fibers, the epoxy resin and the insulation coated iron powder into a vibration ball milling tank for ball milling, firstly vibrating at low frequency for 30 seconds, then vibrating at high frequency for 30 seconds, circulating for 2 times to uniformly mix, and uniformly mixing;
22) and putting the mixed powder into a die, and carrying out hot press molding at the hot press temperature of 80 ℃ and the pressure of 30MPa to obtain the composite material with the low-frequency-dispersion negative dielectric property.
Example 5:
a composite material with low-frequency dispersion negative dielectric property is composed of the following components in parts by volume:
carbon fiber 23 parts
Insulating coated iron powder 5 parts
The balance of epoxy resin.
The preparation method of the composite material with the low-frequency dispersion negative dielectric property comprises the following steps:
step 1: synthesis of insulating coated iron powder
11)400mL of phosphoric acid solution with the mass fraction of 0.016g/mL, and 20 g of iron powder is put into the phosphoric acid solution to react for 1h at normal temperature;
12) and filtering and cleaning to obtain the insulating coated iron powder.
Step 2: regulating and controlling negative dielectric property of carbon fiber/epoxy resin composite material by insulating coated iron powder
21) Taking the carbon fibers, the epoxy resin and the insulation coated iron powder in parts by volume, putting the carbon fibers, the epoxy resin and the insulation coated iron powder into a vibration ball milling tank for ball milling, firstly vibrating at low frequency for 30 seconds, then vibrating at high frequency for 30 seconds, circulating for 2 times to uniformly mix, and uniformly mixing;
22) and putting the mixed powder into a die, and carrying out hot press molding at the hot press temperature of 80 ℃ and the pressure of 30MPa to obtain the composite material with the low-frequency-dispersion negative dielectric property.
To further illustrate the electrical properties of the composite material with low frequency dispersion negative dielectric properties prepared in accordance with the present invention, a comparative example was constructed as follows, taking example 4 as an example.
Comparative example 1:
a composite material is composed of the following components in parts by volume:
carbon fiber 23 parts
The balance of epoxy resin.
The preparation method of the composite material comprises the following steps:
1) taking the carbon fibers and the epoxy resin in parts by volume, putting the carbon fibers and the epoxy resin into a vibration ball milling tank for ball milling, firstly vibrating at low frequency for 30 seconds, then vibrating at high frequency for 30 seconds, circulating for 2 times to uniformly mix, and uniformly mixing;
2) and putting the mixed powder into a die, and carrying out hot press molding at the hot press temperature of 80 ℃ and the pressure of 30MPa to obtain the composite material with the low-frequency-dispersion negative dielectric property.
The dielectric spectra of the above examples and comparative examples are shown in fig. 1 and 3, and the dielectric spectrum of comparative example 1 is shown in fig. 1, and it can be seen that the dispersion phenomenon of the dielectric constant of 23% carbon fiber/epoxy resin composite material is serious; after the addition of the insulating coated iron powder, examples 3 to 5 showed dielectric spectra as shown in fig. 3, in which the dispersion phenomenon of the dielectric constant was controlled and the dispersion property was low.
The invention provides a composite material with low-frequency-dispersion negative dielectric property and a preparation method thereof, wherein a carbon fiber material is uniformly dispersed in an epoxy resin matrix, and iron particles coated by insulation are added to obtain a carbon fiber-iron particles-epoxy resin ternary composite material with low-frequency-dispersion negative dielectric property; the invention has the advantages of low preparation cost, stable process, simple operation and treatment and large performance regulation interval.
The experiments are only preferred examples of the present invention and are not intended to limit the scope of the present invention. It should be noted that modifications and adaptations may occur to those skilled in the art without departing from the principles of the present invention and should be considered within the scope of the present invention.
Claims (9)
1. The composite material with the low-frequency-dispersion negative dielectric property is characterized by comprising the following components in parts by volume:
18-23 parts of carbon fiber
5-12 parts of insulating coated iron powder
The balance of epoxy resin;
the insulating coated iron powder is prepared by coating a layer of iron-phosphorus compound with insulating property on the surface of iron powder,
the iron-phosphorus compound is formed by the reaction of iron powder and a phosphoric acid solution.
2. The composite material with low-frequency-dispersion negative dielectric properties of claim 1, wherein the iron powder is carbonyl iron powder, and the particle size is 1-5 μm spherical particles.
3. The composite material with low frequency dispersion negative dielectric properties of claim 1, wherein said carbon fibers are 30-50 μ ι η long and 1-5 μ ι η in diameter; the epoxy resin is bisphenol AB type solid powder.
4. A method of preparing a composite material having negative dielectric properties with low frequency dispersion according to any of claims 1 to 3, comprising:
step 1: synthesizing insulating coated iron powder;
step 2: the insulating coated iron powder regulates and controls the negative dielectric property of the carbon fiber/epoxy resin composite material.
5. The method for preparing the composite material with low-frequency-dispersion negative dielectric property according to claim 4, wherein the step 1 comprises the following specific steps:
11) taking a phosphoric acid solution, putting iron powder into the phosphoric acid solution, and reacting for a period of time under a certain condition to form an insulating layer on the surface of the iron powder;
12) and filtering and cleaning to obtain the insulating coated iron powder.
6. The preparation method of the composite material with low frequency dispersion negative dielectric property as claimed in claim 5, wherein in the step 11), the reaction is carried out for 1-2 h at normal temperature or 30-40 min at 60 ℃ in water bath.
7. The method for preparing the composite material with low-frequency-dispersion negative dielectric property according to claim 4, wherein the step 2 comprises the following specific steps:
21) weighing carbon fibers, epoxy resin and insulation coated iron powder, and putting into a vibration ball milling tank for ball milling;
22) and putting the mixed powder into a mold, and carrying out hot press molding to obtain the composite material with the low-frequency-dispersion negative dielectric property.
8. The method for preparing the composite material with low-frequency-dispersion negative dielectric property as claimed in claim 7, wherein in the step 21), the mass of the insulation coated iron powder is 5-12% of the total volume of the mixed powder.
9. The preparation method of the composite material with the low-frequency-dispersion negative dielectric property as claimed in claim 7, wherein the ball milling is performed by performing low-frequency vibration for 30-40 seconds, then performing high-frequency vibration for 30-50 seconds, and performing circulation for 2-3 times to uniformly mix;
the hot pressing temperature is 75-85 ℃, and the pressure is 30 MPa.
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| "Epoxy-silicone filled with multi-walled carbon nanotubes and carbonyl iron particles as a microwave absorber";Qing Yuchang et al.;《Carbon》;20100716;第48卷(第14期);第4074-4080页 * |
| "导电填料树脂基复合材料的负介电性能";候晴;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20160115(第01期);第B020-64页 * |
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