CN1099444C - Microwave medium material and preparing process thereof - Google Patents

Microwave medium material and preparing process thereof Download PDF

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CN1099444C
CN1099444C CN98117868A CN98117868A CN1099444C CN 1099444 C CN1099444 C CN 1099444C CN 98117868 A CN98117868 A CN 98117868A CN 98117868 A CN98117868 A CN 98117868A CN 1099444 C CN1099444 C CN 1099444C
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polymer
fluorine
soft magnetic
microwave medium
dielectric material
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CN1246500A (en
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孙克
赵见高
李德新
凌启芬
嵇天浩
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Institute of Physics of CAS
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Abstract

The present invention relates to a high molecular/magnetic nanometer composite microwave medium material prepared by mixing a high molecular material of a fluorine containing high polymer and a fluorine-free high polymer or a high molecular material of a copolymer of the fluorine containing high polymer and the fluorine-free high polymer and a cross blend of the fluorine containing high polymer and the fluorine-free high polymer and metal, an alloy or a ferrite soft magnetic material according to the weight portion ratio of 1:1 to 1:10. The present invention provides a method comprises: high molecular magnetic materials in the form of powder or suspensions are uniformly compounded with the methods of stirring, ball milling or ultrasonic, etc., made into a certain shape at the pressure of 0.4 to 4 ton/cm<2> and thermally treated in air, argon, nitrogen or hydrogen at the temperature of 120 to 400DEG C for 30 minutes to obtain the high molecular/magnetic nanometer composite microwave medium material which can be used within the high frequency range of 0.1GHz to 2GHz. The high molecular/magnetic nanometer composite microwave medium material has the advantages of high dielectric constant, high magnetoconductivity, low electric loss and low magnetic loss.

Description

A kind of microwave dielectric material and preparation method thereof
The present invention relates to a kind of microwave dielectric material, particularly the composite microwave medium material.
At high frequency, microwave regime need be used dielectric material, as the medium loaded antenna, and dielectric circuit plate etc.When hertzian wave by having relative permittivity ε rWith relative permeability μ rMaterial the time, wavelength decreases
Figure C9811786800041
Times, thereby plant bulk is reduced.Therefore, ε rAnd μ rAt high frequency, keep the basic demand that higher value is exactly this class dielectric material under the microwave, and require loss low, in light weight, the physical strength height.This class dielectric material has following a few class at present: pottery or macromolecule medium, because its ε rHigher, be the material of using always, but the loss of pottery is big, the μ of polymer device rBe 1 only, be capacitive character, defectiveness all in the use.Referring to document 1:A.A.Kishk, M.R.Zunobi, O.Kajfez, IEEETrans., AP-41 (1993) 813; Document 2:R.K.Mongia, et al., ElectronicsLetters, 25 (1989) 462.
Another kind of available material is high μ rSoft magnetic materials, its ε rAnd μ rAll very high, but resistivity is not high, is difficult to use high frequency, as crystalline state, the metal alloy of non-crystalline state and crystalline state nanometer, resistivity is 10 -3Below the Ω .cm, eddy-current loss is big, low frequency applications (reference 3:M.Fujinami, etal., Jpn.J.Appl.Phys., 29 (1990) .L447.) that can only be below 0.1MHz; Even the resistivity of soft magnetic ferrite also not too high (10 2-10 9Ω .cm scope), be difficult to use the above scope of 100MHz, be used in below the 10MHz mostly, and very big in the resonance loss at limiting frequency place, even be used in higher frequency, also very low (the reference 4:S.K.Ghosh of the efficient of device, M.N.Roy, IEEE Trans.AP-25 (1987) 1036 and A.Petosa et al., Electronics Letters, 30 (1994) 1021.).
The object of the present invention is to provide a kind of polymer/magnetic Nano composite microwave medium material and preparation method thereof, this material has higher ε in the microwave range of 0.1-2.0GHz rμ rValue and low total loss value.The object of the present invention is achieved like this:
Polymer provided by the invention/magnetic Nano composite microwave medium material is mixed by 10: 1 to 1: 1 weight ratios by the little macromolecular material of the soft magnetic materials of 10-1000 nanoparticle and electrical loss and forms.
The soft magnetic materials of wherein said 10-1000 nanoparticle can be prepared by one of following ordinary method: 1. adopt chemical coprecipitation method or sol-gel method to obtain ferritic nanoparticle, the nanoparticle scope is in the 10-1000 nanometer, and ferrite can be Fe 3O 4, (MnZn) Fe 2O 4, (NiZn) Fe 2O 42. adopt the reduction of iron carbonyl (nickel) thermolysis or ferric oxide (nickel) to obtain the nanoparticle of iron and nickel, its scope is in the 10-1000 nanometer.3. the nanoparticle that adopts ammonia to handle iron obtains the nanoparticle of iron-nitride.4. adopt the melt quick-quenching method to obtain amorphous alloy and nanometer crystal alloy, become nanoparticle with Prepared by Ball Milling again.
The character of polymer of the present invention/magnetic Nano composite microwave medium material is as follows: DIELECTRIC CONSTANT r' 〉=3-10, magnetic permeability mu r' 〉=3-5, loss angle tg δ＜10 -1-10 -3(range of frequency 0.1-2GHz)
The main application of this material: this material can be used for making the high frequency microwave electron device of 0.1-2GHz range of frequency, as microwave antenna, and power divider, microwave printed substrate etc.
The method of the above-mentioned polymer of preparation provided by the invention/magnetic Nano composite microwave medium material comprises: get particle at the soft magnetic materials 1-10 of 10-1000 nanoparticle weight part 1.; 2. the little macromolecular material weight part of power taking loss is 1 part, with the above-mentioned particle soft magnetic materials uniform mixing in the 10-1000 nanometer; 3. the material that mixes is 80-100 ℃ of oven dry; With the oven dry polymer/magnetic Nano composite microwave medium material with 0.4-4 ton/cm 2Pressure compression moulding; The polymer of compression moulding/magnetic Nano composite microwave medium material at air, argon gas carries out temperature and is 120-400 ℃ thermal treatment in nitrogen or the hydrogen, heat treatment time is 0.5 hour.
The invention provides a kind of can in the 0.1-2GHz high-frequency range, the use, and ε rμ rBe worth greatlyyer, loss is little, and density is little, and is in light weight, and technology is simple, and easy-formation can be processed, comprehensive good polymer such as good toughness/magnetic Nano composite microwave medium material.
The present invention is described in further detail below in conjunction with implementing: Embodiment 1:
Prepared Fe 3O 4Ferrite and macromolecular material copolymerization perfluoroethylene-propylene (copolymer) are by the polymer/magnetic Nano composite microwave medium material of 10: 1 weight ratio compositions, and concrete technology is: use Fe 2+And Fe 3+Learn the Fe that precipitates preparation and obtain wrapping up with alkalization with the processing of KH550 silane surface active agent 3O 4The 10nm suspension liquid, by weight sneaking into copolymerization perfluoroethylene-propylene (copolymer) suspension liquid at 10: 1, with 500 watts of supersound process 0.5 hour compound after, in baking oven with 90 ℃ of temperature oven dry, with 4 tons/cm 2Pressure be prepared into the annulus of (φ 16-10) * 5mm, with thermal treatment under 400 ℃ of nitrogen protections 20 minutes.The specific inductivity that the gained material records (real part) ε ', specific inductivity (imaginary part) ε ", permeability (real part) μ ', permeability (imaginary part) μ " be respectively:
ε’ ε” μ’ μ”
100MHz 10.5 1.9×10 -4 5.48 2.2×10 -2
1500MHz 10.6 2.5 * 10 -33.40 4.2 * 10 -1 Embodiment 2:
Prepared α-Fe metal and polyphosphazene polymer R 1216 are by the polymer/magnetic Nano composite microwave medium material of 1: 1 weight ratio composition, concrete technology is: make the Fe powder that iron particle and surface passivation Processing of Preparation get 150nm from the iron carbonyl thermal degradation, by weight 1: 1 and polyhexafluoropropylene powder mixes, add an amount of polyethylene glycol type nonionogenic tenside, and after stirring, with 0.4 ton/cm 2Pressure be prepared into the garden sheet of φ 80 * 3mm, again with 350 ℃ of thermal treatments 30 minutes under argon shield.The specific inductivity that the gained material records (real part) ε ', specific inductivity (imaginary part) ε ", permeability (real part) μ ', permeability (imaginary part) μ " be respectively:
ε’ ε” μ’ μ”
500MHz 3.7 1.4×10 -3 4.8 3.3×10 -3
1000MHz 3.0 4.4 * 10 -24.7 4.5 * 10 -2 Embodiment 3:
Prepared (MnZn) Fe 2O 4Ferrite and macromolecular material tetrafluoroethylene are by the polymer/magnetic Nano composite microwave medium material of 10: 1 weight ratio compositions, and concrete technology is: with (MnZn) Fe 2O 4Ferrite process ball milling porphyrize is the particle about 1000 nanometers, add an amount of polyethylene glycol type nonionogenic tenside and carry out after the surface treatment after ULTRASONIC COMPLEX, making sample with the identical method of embodiment 1 with the tetrafluoroethylene suspension liquid, and with 400 ℃ of thermal treatments 20 minutes in air.The specific inductivity that the gained material records (real part) ε ', specific inductivity (imaginary part) ε ", permeability (real part) μ ', permeability (imaginary part) μ " be respectively:
ε’ ε” μ’ μ”
100MHz 8.9 3.5×10 -3 3.8 2.5×10 -1
700MHz 8.0 1.2 * 10 -23.7 3.8 * 10 -1 Embodiment 4:
Prepared non-crystalline state FeCoSiB alloy and macromolecular material polystyrene are by the polymer/magnetic Nano composite microwave medium material of 5: 1 weight ratio compositions, concrete technology is: make FeCoSiB non-crystalline state band with the melt quick quenching technique, be ground into the powder about 1000nm, compound by weight 5: 1 with the polystyrene powder, method with embodiment 2 after stirring prepares sample, but thermal treatment temp is 120 ℃.The specific inductivity that the gained material records (real part) ε ', specific inductivity (imaginary part) ε ", permeability (real part) μ ', permeability (imaginary part) μ " be respectively:
ε’ ε” μ’ μ”
500MHz 3.0 3.7×10 -2 5.1 4.2×10 -2
1000MHz 3.0 7.2 * 10 -24.8 6.1 * 10 -1 Embodiment 5:
Prepared FeN compound and macromolecular material polyhexafluoropropylene are by the polymer/magnetic Nano composite microwave medium material of 1: 1 weight ratio composition, concrete technology is: make from carbonyl Fe thermal degradation behind the iron powder of 150nm with ammonia handle obtain iron nitride after, by weight 1: 1 and polyhexafluoropropylene powder mixes, add an amount of poly-second two pure type nonionogenic tensides, and ball milling evenly after, press embodiment 2 the same terms and handle the specific inductivity of gained sample (real part) ε ' specific inductivity (imaginary part) ε " permeability (real part) μ ' permeability (imaginary part) μ " be respectively:
ε’ ε” μ’ μ”
500MHz 3.5 8.1×10 -3 4.5 7.2×10 -3
2000MHz 3.2 2.1 * 10 -23.4 1.1 * 10 -1 Embodiment 6:
Prepared nano soft magnetic alloy FeCuNbSiB and macromolecular material tetrafluoroethylene are by the polymer/magnetic Nano composite microwave medium material of 10: 1 weight ratio compositions, concrete technology is: make FeCuNbSiB nano-crystal soft magnetic alloy band with the melt quick quenching technique, be ground into the powder about 1000nm, and carry out surface treatment with the KH550 silane surface active agent, by weight 10: 1 with the tetrafluoroethylene suspension liquid through 500 watts ultrasonic 0.5 hour compound after, prepare sample with embodiment 1 identical method, and with 400 ℃ of thermal treatments 0.5 hour under hydrogen.The specific inductivity of gained material (real part) ε ' specific inductivity (imaginary part) ε " permeability (real part) μ ' permeability (imaginary part) μ " be respectively:
ε’ ε” μ’ μ”
100MHz 3.5 2.1×10 -2 5.2 3.3×10 -2
1000MHz 3.0 8.4×10 -2 4.8 8.0×10 -2

Claims (6)

1. microwave dielectric material, it is characterized in that: with particle at the soft magnetic materials of 10-1000 nanometer with commercially available KH550 silane, oleic acid or nonionic surface active agent wrap up, and make polymer/magnetic Nano composite microwave medium material with the macromolecular material that electrical loss is little by weight 10: 1 to 1: 1 uniform mixing.
2. by the described microwave dielectric material of claim 1, it is characterized in that: described particle can be a metal at the soft magnetic materials of 10-1000 nanometer, alloy or ferrite.
3. by the described microwave dielectric material of claim 1, it is characterized in that: the macromolecular material that described electrical loss is little is fluorine-containing, not fluorine-containing superpolymer or their copolymerization, blend.
4. method for preparing the described microwave dielectric material of claim 1 is characterized in that this method is that in the following order several steps carries out:
(1) gets particle in the soft magnetic materials 1-10 of 10-1000 nanometer weight
Part; With commercially available KH550 silane, oleic acid or non-ionic type surface
Promoting agent wraps up;
(2) the little macromolecular material weight part of power taking loss is 1 part, with above-mentioned
The soft magnetic materials uniform mixing of 10-1000 nano particle;
(3) material that mixes is 80-100 ℃ of oven dry;
(4) with the oven dry polymer/magnetic Nano composite microwave medium material with
0.4-4 ton/cm 2Pressure compression moulding;
(5) the polymer of compression moulding/magnetic Nano composite microwave medium material
At air, argon gas, carrying out temperature in nitrogen or the hydrogen is 120-400 ℃
Thermal treatment, heat treatment time is 0.5 hour.
5. by the described method for preparing the described microwave dielectric material of claim 1 of claim 4, it is characterized in that: the macromolecular material that described electrical loss is little can be powder or outstanding turbid night.
6. by the described method for preparing the described microwave dielectric material of claim 1 of claim 4, it is characterized in that: the uniform mixing of soft magnetic materials and macromolecular material can be a ball milling, stirs or ultrasonic mixing.
CN98117868A 1998-09-01 1998-09-01 Microwave medium material and preparing process thereof Expired - Fee Related CN1099444C (en)

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CN102627821A (en) * 2011-12-02 2012-08-08 兰州理工大学 Filled modified teflon seal material and its preparation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0053748A2 (en) * 1980-12-04 1982-06-16 Bayer Ag Micro-wave reflexion of metallised textile articles
US4518737A (en) * 1978-12-26 1985-05-21 Rogers Corporation Dielectric material and method of making the dielectric material
EP0496112A2 (en) * 1991-01-23 1992-07-29 BASF Aktiengesellschaft Polymer blend containing ferromagnetic or ferroelectric fillers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4518737A (en) * 1978-12-26 1985-05-21 Rogers Corporation Dielectric material and method of making the dielectric material
EP0053748A2 (en) * 1980-12-04 1982-06-16 Bayer Ag Micro-wave reflexion of metallised textile articles
EP0496112A2 (en) * 1991-01-23 1992-07-29 BASF Aktiengesellschaft Polymer blend containing ferromagnetic or ferroelectric fillers

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