CN108393487A - A kind of negative dielectric material and preparation method thereof based on metal powder insulating wrapped - Google Patents
A kind of negative dielectric material and preparation method thereof based on metal powder insulating wrapped Download PDFInfo
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- CN108393487A CN108393487A CN201810575436.1A CN201810575436A CN108393487A CN 108393487 A CN108393487 A CN 108393487A CN 201810575436 A CN201810575436 A CN 201810575436A CN 108393487 A CN108393487 A CN 108393487A
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- metal powder
- insulating wrapped
- dielectric material
- negative dielectric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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Abstract
The invention discloses a kind of negative dielectric material and preparation method thereof based on metal powder insulating wrapped, this approach includes the following steps：Step 1：Prepare the metal powder of silicon dioxide insulator cladding；Step 2：The metal powder of insulating wrapped and untreated metal powder are pressed 0 1.5：1 mass ratio is mixed, and mixed metal powder is obtained；Step 3：Mixed metal powder and epoxy resin powder are pressed 14：1 mass ratio is mixed, and composite powder is obtained；Step 4：By composite powder machine-shaping, the negative dielectric material based on metal powder insulating wrapped is obtained.The negative permittivity of the negative dielectric material based on metal powder insulating wrapped prepared by the present invention is adjustable in 10MHz 1GHz frequency ranges, and negative permittivity size can accuracy controlling in 2000 to 0 range.Regulation and control method is mainly, by regulate and control the metal powder of insulating wrapped and the ratio of uncoated metal powder and with the ratio of epoxy resin, it is easy to operate, it is at low cost.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of negative dielectric material based on metal powder insulating wrapped and its
Preparation method.
Background technology
Dielectric constant is dielectric basic electricity parameter.Under normal conditions, dielectric constant is positive value, is the letter of frequency
Number, there is different Polarization Mechanisms, such as ionic polarization, electronic polarization, interfacial polarization etc. in different frequency ranges.Namely
It says, positive dielectric constant derives from the short range motion of charge, this charge is also referred to as electric dipole.However, some materials or states of matter tool
There are negative dielectric constant, such as semiconductor and metal in infrared band.Although radio communication has benefited from atmosphere ionosphere
Negative dielectric properties, but negative dielectric properties do not cause extensive concern until Meta Materials appearance.Negative dielectric Meta Materials have
Biological monitoring can be achieved for example, it is combined with drug in extensive market application prospect, and the part as waveguide cavity can be achieved
The tunnelling of electromagnetic wave can also be used as electromagnetic shielding material with the compound achievable high dielectric property of positive dielectric material.Meta Materials
Negative dielectric properties are also referred to as artificial performance, this is because it derives from artificial structure's unit of Meta Materials rather than its material sheet
Body.From this, negative dielectric properties also cause research boom in the Meta Materials not containing artificial structure's unit.These traditional materials
Also referred to as intrinsic Meta Materials or super structure composite material, such material, which is usually associated with to exceed, oozes phenomenon.In ceramic-metal composite
In polymer matrix composite, negative dielectric properties are widely studied, however how effectively to be regulated and controled negative dielectric properties and be still
One problem, especially its numerical value and frequency range accurately control.
By literature survey, we are it is found that negative permittivity derives from the oscillation of free electron.It is, being adjusted when conductive
When simple harmonic motion occurs for the free electron in material, the polarized electric field in material can be made identical with the direction of extra electric field, to
Effective dielectric constant is set to become negative value.Because negative permittivity is generated from the motion analysis of electronics, rather than from energy
What the angle of storage generated, so the presence of negative permittivity does not violate law of conservation of energy.It, can when considering the movement of electronics
To draw a conclusion, the movable distance length of electronics is very big on negative permittivity influence, although this length is difficult to define.Work as movement
Distance in short-term, dipole can be regarded as, generate positive dielectric, when the distance of movement is long, occur simple harmonic motion, generate bear dielectric.
Therefore, this phenomenon is to we provide a kind of Effective Regulation mode of negative permittivity.
Invention content
The object of the present invention is to provide a kind of negative dielectric material and preparation method thereof based on metal powder insulating wrapped, with solution
Certainly above-mentioned problem of the prior art.
In order to achieve the above objectives, the present invention provides a kind of preparation sides of the negative dielectric material based on metal powder insulating wrapped
Method comprising following steps：
Step 1：Prepare the metal powder of silicon dioxide insulator cladding；
Step 2：The metal powder of insulating wrapped and untreated metal powder are pressed into 0-1.5：1 mass ratio is mixed, and is obtained
To mixed metal powder；
Step 3：Mixed metal powder and epoxy resin powder are pressed into 1-4：1 mass ratio is mixed, and composite powder is obtained；
Step 4：By composite powder machine-shaping, the negative dielectric material based on metal powder insulating wrapped is obtained.
The preparation method of the above-mentioned negative dielectric material based on metal powder insulating wrapped, wherein in step 1, utilize silicic acid
The hydrolysis of sodium completes the silicon dioxide insulator cladding of metal powder.
The preparation method of the above-mentioned negative dielectric material based on metal powder insulating wrapped, wherein the grain size of the metal powder
It is 1 μm -200 μm.
The preparation method of the above-mentioned negative dielectric material based on metal powder insulating wrapped, wherein the epoxy resin is double
Phenol A types.
The preparation method of the above-mentioned negative dielectric material based on metal powder insulating wrapped, wherein the grain of the epoxy resin
Diameter is 1 μm -5 μm.
The preparation method of the above-mentioned negative dielectric material based on metal powder insulating wrapped, wherein in step 2 and step 3
It is mixed using ball milling method.
The preparation method of the above-mentioned negative dielectric material based on metal powder insulating wrapped, wherein in step 4, the processing
Molding mode is hot-forming.
The present invention also provides a kind of preparations of the preparation method of above-mentioned negative dielectric material based on metal powder insulating wrapped
The negative dielectric material based on metal powder insulating wrapped.
Compared with the existing technology, the invention has the advantages that：
The negative permittivity of the negative dielectric material based on metal powder insulating wrapped prepared by the present invention is in 10MHz-1GHz
Adjustable in frequency range, negative permittivity size can accuracy controlling in -2000 to 0 range.Regulation and control method is mainly, exhausted by regulating and controlling
The metal powder of edge cladding and the ratio of uncoated metal powder and the ratio with epoxy resin, it is easy to operate, it is at low cost.
Description of the drawings
Fig. 1 is the SEM figures of FeSiB amorphous metal powder used in the embodiment of the present invention 1；
Fig. 2 is the SEM figures of the negative dielectric material based on metal powder insulating wrapped prepared by the embodiment of the present invention 1；
Fig. 3 is the dielectric and magnetic of the negative dielectric material based on metal powder insulating wrapped prepared by embodiment 1；
Fig. 4 is the close-up schematic view of Fig. 3.
Specific implementation mode
Below in conjunction with attached drawing, by specific embodiment, the invention will be further described, these embodiments are merely to illustrate
The present invention is not limiting the scope of the invention.
The present invention provides a kind of preparation methods of the negative dielectric material based on metal powder insulating wrapped comprising following step
Suddenly：
Step 1：Prepare the metal powder of silicon dioxide insulator cladding；
Specifically：Between the particle size range for the metal powder that the present invention uses is 1 μm -200 μm.By metal powder stock dispersion in
In ethylene glycol, mass ratio 1:50 (this ratio is optimum efficiency), and ultrasonic disperse 60min.This mixed solution is transferred to
In thermostat water bath, mechanical force stirring, 90 DEG C.By the sulfuric acid solution of 1mol/L sodium silicate solutions and 1mol/L with 200mL/h
Speed simultaneously be added drop-wise in mixed solution.It is kept stirring 2 hours.It can be obtained the metal powder of silicon dioxide insulator cladding.
Step 2：The metal powder of insulating wrapped and untreated metal powder are pressed into 0-1.5：1 mass ratio is mixed, and is obtained
To mixed metal powder；
Specifically：The metal powder of insulating wrapped and untreated metal powder press 0-1.5：1 mass ratio weighs.Mixed media
For ball mill, dry grinding.When being mixed using planetary ball mill, total ratio of grinding media to material is 1~2, rotational speed of ball-mill 100r/min-
260/min, Ball-milling Time 10-20min；When using vibrator batch mixing, ratio of grinding media to material 1-2, first low-frequency vibration 15 seconds,
Then it high-frequency vibration 20-40 seconds, recycles 1-3 times.
Step 3：Mixed metal powder and epoxy resin powder are pressed into 1-4：1 mass ratio is mixed, and composite powder is obtained；
Specifically：Epoxy resin is bisphenol A-type, and grain size is 1 μm -5 μm.The quality of mixed metal powder and epoxy resin powder
Than for 1-4：1.Mixed media is ball mill, dry grinding.When being mixed using planetary ball mill, total ratio of grinding media to material (is most preferably matched for 2
Than), rotational speed of ball-mill 260r/min, Ball-milling Time is 1-2 hours；When using vibrator batch mixing, ratio of grinding media to material is 1~3,
It first low-frequency vibration 12-25 seconds, then high-frequency vibration 90-120 seconds, recycles 3-6 times.
Step 4：By composite powder machine-shaping, the negative dielectric material based on metal powder insulating wrapped is obtained；
Specifically：The size of mold is designed according to the scantling of required preparation.Molding mode is hot-forming.First by powder
Material pours into mold, and 20-40min is preheated at 60 DEG C -140 DEG C.Then it pressurizes.When pressurization, prior to pressurize 3- under 20MPa
10min；Then the pressurize under 30MPa, is no longer heat up at this time, and when being cooled to room temperature, pressure release, pressure release rate is 5MPa/
Natural cooling or circulating water may be selected in min-30MPa/min, the type of cooling.
The present invention also provides a kind of preparations of the preparation method of above-mentioned negative dielectric material based on metal powder insulating wrapped
The negative dielectric material based on metal powder insulating wrapped.
The materials, reagents and the like used in the following examples is commercially available.Wherein, FeSiB metal powders is straight
Diameter is about 100 μm；Epoxy powder is bisphenol A-type, and grain size is 1 μm -5 μm.
Embodiment 1：
A kind of preparation method of the negative dielectric material based on metal powder insulating wrapped, including：
Step 1：Silicon dioxide insulator coats Fe78Si9B13(FeSiB) non-crystalline flour.The metal powder used in the present embodiment is
FeSiB amorphous metal powder, grain size are 100 μm or so, see Fig. 1.FeSiB powder is scattered in ethylene glycol, mass ratio 1:50,
And ultrasonic disperse 60min.This mixed solution is transferred in thermostat water bath, mechanical force stirring, 90 DEG C.By 1mol/L sodium metasilicate
The sulfuric acid solution of solution and 1mol/L are added drop-wise in mixed solution with the speed of 200mL/h simultaneously.It is kept stirring 2 hours.It obtains
Obtain the FeSiB powder of silicon dioxide insulator cladding.
Step 2：Untreated FeSiB powder and insulating bag whiting mix in varing proportions.Weigh two kinds of metal powders, ratio
It is followed successively by 7:3、8:2、8.5:1.5、9:1、9.5:0.5、10:0.Using vibrator batch mixing, ratio of grinding media to material 2, first low frequency shakes
15 seconds dynamic, then high-frequency vibration 20 seconds, recycle 2 times.
Step 3：Mixed metal powder is mixed with epoxy resin powder with certain proportion.Mixed metal powder and epoxy resin powder
Mass ratio be 6:4.Using vibrator batch mixing, ratio of grinding media to material 2, first low-frequency vibration 20 seconds, then high-frequency vibration 90 seconds, are followed
Ring 4 times.
Step 4：Above-mentioned mixed powder is shaped to have effigurate composite material.Die size is diameter 20mm,
Thickness is the disk of 2mm.Molding mode is hot-forming.First powder is poured into mold, 30min is preheated at 80 DEG C.Then
Pressurization.When pressurization, prior to pressurize 5min under 20MPa；Then the pressurize under 30MPa, is no longer heat up at this time, naturally cools to room
Temperature, pressure release, pressure release rate are 5MPa/min.Negative dielectric material manufactured in the present embodiment based on metal powder insulating wrapped it is micro-
Structure is as shown in Figure 2.Its negative dielectric properties is as shown in Figure 3 and Figure 4, (FeSiB in figurexcoated-FeSiB1-x)0.6Epoxy0.4
Indicate the expression formula of the prepared negative dielectric material based on metal powder insulating wrapped, in formula, FeSiBxCoated is titanium dioxide
The FeSiB powder of silicon insulating wrapped, FeSiB1-xFor untreated FeSiB powder, Epoxy is epoxy resin powder, and in the embodiment
In, x=0.7,0.8,0.85,0.9,0.95,1, as can be seen from figs. 3 and 4, the present invention prepared by based on metal powder insulating wrapped
Negative dielectric material negative permittivity it is adjustable in 10MHz-1GHz frequency ranges, negative permittivity size is in -2000 to 0 range
It can accuracy controlling.
Embodiment 2：
A kind of preparation method of the negative dielectric material based on metal powder insulating wrapped, including：
Step 1：Silicon dioxide insulator coats Fe powder.The metal powder used in the present embodiment is Fe powder, and grain size is 120 μm of left sides
It is right.Fe powder is scattered in ethylene glycol, mass ratio 1:60, and ultrasonic disperse 60min.This mixed solution is transferred to constant temperature
In water-bath, mechanical force stirring, 90 DEG C.By the sulfuric acid solution of 1mol/L sodium silicate solutions and 1mol/L with the speed of 200mL/h
It spends while being added drop-wise in mixed solution.It is kept stirring 2 hours.Obtain the Fe powder of silicon dioxide insulator cladding.
Step 2：Untreated Fe powder and insulating bag whiting mix in varing proportions.Weigh two kinds of metal powders, ratio according to
Secondary is 7:3、8:2、8.5:1.5、9:1、9.5:0.5、10:0.Use vibrator batch mixing, ratio of grinding media to material 2, first low-frequency vibration
15 seconds, then high-frequency vibration 20 seconds, recycled 2 times.
Step 3：Mixed metal powder is mixed with epoxy resin powder with certain proportion.Mixed metal powder and epoxy resin powder
Mass ratio be 7:3.Using vibrator batch mixing, ratio of grinding media to material 2, first low-frequency vibration 20 seconds, then high-frequency vibration 90 seconds, are followed
Ring 4 times.
Step 4：Above-mentioned mixed powder is shaped to have effigurate composite material.Die size is diameter 20mm,
Thickness is the disk of 2mm.Molding mode is hot-forming.First powder is poured into mold, 30min is preheated at 100 DEG C.Then
Pressurization.When pressurization, prior to pressurize 5min under 20MPa；Then the pressurize under 40MPa, is no longer heat up at this time, naturally cools to room
Temperature, pressure release, pressure release rate are 5MPa/min.
Embodiment 3：
A kind of preparation method of the negative dielectric material based on metal powder insulating wrapped, including：
Step 1：Silicon dioxide insulator coats Cu powder.The metal powder used in the present embodiment is Cu powder, and grain size is 20 μm of left sides
It is right.Cu powder is scattered in ethylene glycol, mass ratio 1:40, and ultrasonic disperse 60min.This mixed solution is transferred to constant temperature
In water-bath, mechanical force stirring, 90 DEG C.By the sulfuric acid solution of 1mol/L sodium silicate solutions and 1mol/L with the speed of 200mL/h
It spends while being added drop-wise in mixed solution.It is kept stirring 2 hours.Obtain the Cu powder of silicon dioxide insulator cladding.
Step 2：Untreated Cu powder and insulating bag whiting mix in varing proportions.Weigh two kinds of metal powders, ratio according to
Secondary is 7:3、8:2、8.5:1.5、9:1、9.5:0.5、10:0.Use vibrator batch mixing, ratio of grinding media to material 2, first low-frequency vibration
15 seconds, then high-frequency vibration 20 seconds, recycled 2 times.
Step 3：Mixed metal powder is mixed with epoxy resin powder with certain proportion.Mixed metal powder and epoxy resin powder
Mass ratio be 8:2.Using vibrator batch mixing, ratio of grinding media to material 2, first low-frequency vibration 20 seconds, then high-frequency vibration 90 seconds, are followed
Ring 4 times.
Step 4：Above-mentioned mixed powder is shaped to have effigurate composite material.Die size is diameter 20mm,
Thickness is the disk of 2mm.Molding mode is hot-forming.First powder is poured into mold, 30min is preheated at 90 DEG C.Then
Pressurization.When pressurization, prior to pressurize 5min under 20MPa；Then the pressurize under 40MPa, is no longer heat up at this time, naturally cools to room
Temperature, pressure release, pressure release rate are 10MPa/min.
In conclusion the negative permittivity of the negative dielectric material based on metal powder insulating wrapped prepared by the present invention exists
Adjustable in 10MHz-1GHz frequency ranges, negative permittivity size can accuracy controlling in -2000 to 0 range.Regulation and control method is mainly,
By regulate and control insulating wrapped metal powder and uncoated metal powder ratio and with the ratio of epoxy resin, it is easy to operate,
It is at low cost.
Although present disclosure is discussed in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read the above, for the present invention's
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (8)
1. a kind of preparation method of the negative dielectric material based on metal powder insulating wrapped, which is characterized in that include the following steps：
Step 1：Prepare the metal powder of silicon dioxide insulator cladding；
Step 2：The metal powder of insulating wrapped and untreated metal powder are pressed into 0-1.5：1 mass ratio is mixed, and is mixed
Close metal powder；
Step 3：Mixed metal powder and epoxy resin powder are pressed into 1-4：1 mass ratio is mixed, and composite powder is obtained；
Step 4：By composite powder machine-shaping, the negative dielectric material based on metal powder insulating wrapped is obtained.
2. the preparation method of the negative dielectric material based on metal powder insulating wrapped as described in claim 1, which is characterized in that step
In rapid 1, the silicon dioxide insulator that metal powder is completed using the hydrolysis of sodium metasilicate is coated.
3. the preparation method of the negative dielectric material based on metal powder insulating wrapped as described in claim 1, which is characterized in that institute
The grain size for stating metal powder is 1 μm -200 μm.
4. the preparation method of the negative dielectric material based on metal powder insulating wrapped as described in claim 1, which is characterized in that institute
It is bisphenol A-type to state epoxy resin.
5. the preparation method of the negative dielectric material based on metal powder insulating wrapped as described in claim 1, which is characterized in that institute
The grain size for stating epoxy resin is 1 μm -5 μm.
6. the preparation method of the negative dielectric material based on metal powder insulating wrapped as described in claim 1, which is characterized in that step
Rapid 2 and step 3 in be all made of ball milling method and mixed.
7. the preparation method of the negative dielectric material based on metal powder insulating wrapped as described in claim 1, which is characterized in that step
In rapid 4, the mode of the machine-shaping is hot-forming.
8. a kind of preparation side of negative dielectric material based on metal powder insulating wrapped as described in any one of claim 1-7
Negative dielectric material based on metal powder insulating wrapped prepared by method.
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| CN201810575436.1A CN108393487B (en) | 2018-06-06 | 2018-06-06 | Negative dielectric material based on metal powder insulation coating and preparation method thereof |
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