CN1346135A - Ultratvide frequency band metal organic compound magnetic material and ultrawide frequency band organic magnetic base material using same as base material - Google Patents
Ultratvide frequency band metal organic compound magnetic material and ultrawide frequency band organic magnetic base material using same as base material Download PDFInfo
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- CN1346135A CN1346135A CN00116118A CN00116118A CN1346135A CN 1346135 A CN1346135 A CN 1346135A CN 00116118 A CN00116118 A CN 00116118A CN 00116118 A CN00116118 A CN 00116118A CN 1346135 A CN1346135 A CN 1346135A
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Abstract
The present invention relates to a kind of superwide frequency band metal organic compound magnetic material and its superwide frequency band organic magnetic base material using the above-mentioned material as basic material. Said superwide frequency band organic magnetic material is formed from at least one of component A or component B and component C and component D by mixing them, in which the component A is one of organic compounds of metallocenes of ferrocene, cobaltocene or nickelocene containing carbonyl group carboxyl group, amino-group and amido-group, and the component B is benzene compound with two N-containing group, and the described N-containing group may be one of amide-group amino-group, hydrazine or oxime, the component C is one of chloride, acetate, sulfate or oxalate, and component D is one of inorganic soft magnetic ferrites.
Description
What the present invention relates to is a kind ofly to can be used for making the ultratvide frequency band metal organic complex magnetic material of microstrip antenna and microstrip circuit and be the ultratvide frequency band organic magnetic base-material of stock with it.
In modern science and technology, microwave communication and microstrip circuit just develop towards the direction of lightweight, miniaturization and complanation.Ferrite, metal, and traditional inorganic soft magnetic material such as alloy material producing and though each side such as life has early had and uses widely, but it can increasing and sharply increase with frequency of utilization than great and magnetic loss, therefore these traditional inorganic soft magnetic materials and dielectric material have been difficult to adapt to the requirement of microwave communication, particularly are difficult to satisfy the needs of the following low-frequency range material of the 500MHz of present increasingly extensive application.It is light, little, thin for microwave device is realized, at present can realize that the dielectric material substrate of suitability for industrialized production has ceramic substrate, titanium dioxide-barium titanate (strontium titanates), polytetrafluoroethylene and glass fibre composite dielectric substrate, and polytetrafluoroethylene or polystyrene substrate etc. are several.Wherein, ceramic substrate is after being 99.99% ceramic spiritual high temperature sintering with purity, in surface evaporation crome metal to be arranged, and copper facing becomes substrate again.Though it has the dielectric constant height, loss is low, and technology vice president is crisp firmly, and processing difficulties costs an arm and a leg.Titanium dioxide-barium titanate (strontium titanates), polytetrafluoroethylene composite dielectric substrate are after the three is fully mixed, to form through hot-forming and compound copper sheet.It has certain dielectric constant, and processing is relatively easy, but property is crisp firmly, high price.Directly with polytetrafluoroethylene or polystyrene as dielectric substrate, though easy to process, dielectric constant only is 2～3, the physical dimension of electronic device is too big, thereby only can be applicable to some bottom surface communications service.The inventor once provided a kind of macromolecule magnetic polymer base material material at application number in for 99114711.1 Chinese patent application, to adapt to the needs of making light, little, thin microstrip antenna, microstrip circuit and microwave device, but its technology is still complicated, price is also higher relatively, and its application band also still is difficult to adapt to the needs of rapid broadening.
Given this, the objective of the invention is to provide a kind of at above-mentioned situation is particularly suitable for making the ultratvide frequency band metal organic complex magnetic material of microstrip antenna and microstrip circuit and is the ultratvide frequency band organic magnetic base-material of stock with it, its application band can reach the super wide range of 100MHz～17.0GHz as required, and be easy to realize commercialization production, technology is simple, low price.
At least a by in component A or the B component of ultratvide frequency band metal organic complex magnetic material of the present invention mixes composition with component C and component D, and the weight of each component is:
At least a total amount 10-70% in component A or the B component,
Component C 15-60%,
Component D 5-50%, wherein: component A is a kind of in the two metallocene organic compounds of medium ferrocene, cobaltocene or the dicyclopentadienyl nickel that contains carbonyl, carboxyl, amino or amido of two formyl ferrocene, diacetyl ferrocene, ferrocene dicarboxylic acid, ferrocene diformamide, ferrocene diacetayl amide, ferrocene phenylenediamine, ferrocene benzidine, ferrocene two hydrazines, ferrocene amido phenylate, ferrocene dioxime, cobaltocene dioctyl phthalate, two formyl cobaltocenes, diacetyl cobaltocene, dicyclopentadienyl nickel dioctyl phthalate, diacetyl dicyclopentadienyl nickel;
B component is o-phenylenediamine, m-phenylene diamine (MPD), p-phenylenediamine (PPD), diaminourea phenylate, MDA, terephthalamide, benzidine, to benzene two hydrazines, benzene dioxime etc. is contained a kind of in the benzene compound that two amidos, amino, hydrazine or oximes etc. contain the N group;
Component C is a kind of in chloride, acetate, sulfate or the oxalates of iron, cobalt, nickel, copper.
Component D is a kind of in the inorganic soft magnetic ferrites such as the dilval, amorphous alloy, silica, carborundum of carbonyl iron, carbonyl nickel, nickel-zinc ferrite, tri-iron tetroxide, crystalline state.
In above-mentioned ultratvide frequency band metal organic complex magnetic material, except that independent use A component or B component, when using the blending ingredients form of forming by A, B two components, can mix mutually by the component A and the B component of equivalent.
The preparation of above-mentioned metal organic complex magnetic material can be carried out in multiple organic solvent, for example can be at alcohols, particularly at C
3-C
6Monohydric alcohol or dihydroxylic alcohols, amine is selected in the organic solvents such as oxolane or dioxane.With Powdered, particularly become micron order or nano level each dusty raw materials component to place suitable organic solvent, refluxing and reacting under the stirring fast, then through filtration, washing and the oven dry of routine, promptly obtain said metal organic complex magnetic material powder, can be for the further organic magnetic base-material use of the appropriate format of the suitable different needs of processing.
In above-mentioned preparation process, change the component in all kinds of raw materials, and when reaction used solvent species, all can be to the character of resulting metal organic complex magnetic material, particularly pairing suitable frequency range and magnetic loss thereof are exerted an influence and change.In following embodiment, also will make specific description to this.
With above-mentioned ultratvide frequency band metal organic complex magnetic material is the ultratvide frequency band organic magnetic base-material of basis, fully mixed with additive and thermoplastic resin by above-mentioned said ultratvide frequency band metal organic complex magnetic material and to form, the weight of its each component is:
Above-mentioned metal organic complex magnetic material 10-70%
Additive 5-40%,
Thermoplastic resin 10-70%, wherein, what said additive can be in titanium dioxide, barium titanate, strontium titanates, alchlor, silica flour, carbon black, the charcoal fiber is a kind of; Said thermoplastic resin can be in polyethylene, polypropylene, polystyrene, poly-p-methylstyrene, Merlon, polysulfones, polyphenylene sulfide, unsaturated-resin, the polytetrafluoroethylene a kind of.Said abundant mixing can be in blending equipments such as the twin-roll machine of routine, kneader, and each composition is mixed fully or mediates, and reach to make thermoplastic resin modified purpose.For making it can realize modification better, on the basis that above-mentioned base-material is formed, can also in said thermoplastic resin, be incorporated as the titanate ester of base-material total weight 2-10% or in the silane coupling agent any.
Below by specific embodiment foregoing of the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following example.The consumption of each component is weight portion in the example.
Embodiment 1
After 5 parts of MDAs and 3 parts of Schweinfurt greens were refluxed 1 hour, add 2 parts of carbonyl iron dusts in 100 parts of amylalcohols, refluxed 3 hours down in vigorous stirring (agitator speed 〉=2500 rev/min, as follows).Cooling back conventional filtration with 95% hot ethanol and the oven dry of distilled water washing (as follows) back, obtains the metal organic complex magnetic respectively.
With 4 parts of resulting metal organic complex magnetics, with 2 parts of titanium dioxide, after 0.5 part barium titanate and 3.5 parts of polystyrene mix, on twin-roll machine, descended mixing 40 minutes in 120 ℃-180 ℃, promptly obtain a kind of metal organic complex magnetic base-material, its permeability (μ ') ≈ 2.5, loss angle tangent (tg δ) ≈ 1 * 10
-3, be microstrip antenna and the microstrip circuit of 100MHz-17.0GHz applicable to making frequency range.
Embodiment 2
Change the MDA among the embodiment 1 into the diaminourea phenylate, other component, consumption and condition are all constant, the loss angle tangent of resulting organic magnetic base-material (tg δ) ≈ 1 * 10
-2, suitable frequency range is 300MHz-2.0GHz.
Embodiment 3
Change the reaction dissolvent among the embodiment 1 into butanols by amylalcohol, other component, consumption and condition are all constant, the loss angle tangent of resulting organic magnetic base-material (tg δ) ≈ 3.5 * 10
-2, suitable frequency range is 100MHz-1.0GHz.
Embodiment 4
Raw material components carbonyl iron among the embodiment 1 changed into use nano level tri-iron tetroxide, other component, consumption and condition are all constant, the loss angle tangent of resulting organic magnetic base-material (tg δ) ≈ 5 * 10
-2, suitable frequency range is 200MHz-5.0GHz.
More than each example show that the used concrete composition and the change of reaction dissolvent in the kinds of ingredients all can influence the character of resulting metal organic complex and organic magnetic base-material thereof, particularly its pairing suitable frequency range and magnetic loss thereof are exerted an influence.Therefore, according to application aims, field and parameters needed, character, flexible and bigger range of choice can be arranged.
Embodiment 5
With 5 parts of ferrocene diaminourea phenylates and 3 parts of nickel chlorides reflux after 1 hour in 10 parts of butanols, under vigorous stirring, add 1 part of commercially available chemical pure tri-iron tetroxide and refluxed 2 hours.Conventional filtration, washing, oven dry obtains ferrocene metal organic complex magnetic.Get 4 parts of these metal organic complex magnetics, with 2 parts of barium titanates, 0.2 part of carbon black, 0.8 part alchlor and 3 parts of polyethylene powders, in blender, fully mixed 40 minutes under the normal temperature, cross 120 orders (aperture～0.12 millimeter) sieve, obtain ferrocene metal organic complex magnetic base-material.Its μ ' ≈ 2.5, tg δ ≈ 5 * 10
-3, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～10.0GHz.
Embodiment 6
Reflux in 10 parts of ethanol added 2 parts of carbonyl iron dusts after 2 hours under vigorous stirring with 5 parts of p-phenylenediamine (PPD) and 2 parts of cobalt acetates, refluxed 3 hours again.Conventional filtration, washing, oven dry obtains the metal organic complex magnetic.Get 5 parts of this metal organic complex magnetics, with 1 part of titanium dioxide, 0.5 part of strontium titanates and 3.5 parts of polyethylene powders fully mixed 40 minutes in blender, after 120 mesh sieves, made metal organic complex magnetic base-material.Its μ ' ≈ 3.0, tg δ ≈ 5 * 10
-3, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 200MHz～10.0GHz.
Embodiment 7
With 1 part of diacetyl ferrocene and 5 parts of cobalt chlorides reflux 1 hour in 10 parts of oxolanes, adding 3 parts of nickel-zinc ferrite (NiZnFe
2O
4), vigorous reflux is 2 hours again.Conventional filtration, washing, oven dry obtains ferrocene metal organic complex magnetic.Get 4 parts of this metal organic complex magnetics, with 1.5 parts of barium titanates, 0.5 the titanate coupling agent of part charcoal fiber and 4 parts of Merlon and material total weight 1%, in kneader commonly used in 250 ℃～300 ℃ fully mediate down after, pulverize again, obtain ferrocene metal organic complex magnetic base-material, its μ ' ≈ 1.8, tg δ ≈ 7 * 10
-3, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～12.0GHz.
Embodiment 8
2.5 parts of diacetyl ferrocene, 2.5 parts of p-phenylenediamine (PPD) and 2 parts of Schweinfurt greens reflux in 10 parts of butanols were added 1 part of carborundum after 2 hours under vigorous stirring, 0.5 part of carbonyl iron refluxed 2 hours again.Conventional filtration, washing, oven dry obtains ferrocene metal organic complex magnetic.Get 2 parts of these metal organic complex magnetics, with 2 parts of barium titanates, 0.5 part of titanium dioxide, 0.5 part strontium titanates and 6 parts of polyphenylene sulfides fully pulverizing after the mixing in 250 ℃～300 ℃ on the twin-roll machine, make ferrocene metal organic complex magnetic base-material again, its μ ' ≈ 2.3, tg δ ≈ 1 * 10
-3, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～17.0GHz.
Embodiment 9
5 parts are added 1 part of chemical pure tri-iron tetroxide and refluxed 2 hours again after 4 hours benzene two hydrazines, 2 parts of Schweinfurt greens reflux in 10 parts of amylalcohols under vigorous stirring.Conventional filtration, washing, oven dry obtains the metal organic complex magnetic.Get 4 parts of this metal organic complex magnetics, with 1 part of barium titanate, 2 parts of titanium dioxide and 3 parts of powdered polypropylenes fully mixed 8 hours in mixer, crossed 120 mesh sieves, made metal organic complex magnetic base-material, its μ ' ≈ 2.0, tg δ ≈ 1 * 10
-2, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 250MHz～10.0GHz.
Embodiment 10
With 3 part of two formyl ferrocene, 0.5 part to benzene dioxime and 2 parts of Schweinfurt greens reflux in 10 parts of dimethyl formamides (DMF) added 2.5 parts of carbonyl irons and refluxed 2 hours again after 2 hours under vigorous stirring.Conventional filtration, washing, oven dry makes ferrocene metal organic complex magnetic.Get 5 parts of this complex metal organic complex magnetics, 1 part of strontium titanates and 4 parts of polyethylene powders, fully mixing on twin-roll machine, make ferrocene metal organic complex magnetic base-material, its μ ' ≈ 2.8, tg δ ≈ 6 * 10
-3, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～10.0GHz.
Embodiment 11
With 5 parts of diacetyl cobaltocenes, 2 parts of nickel acetates reflux in 10 parts of dioxane added 1 part of nickel-zinc ferrite (NiZnFe after 1 hour under vigorous stirring
2O
4) refluxed again 2 hours.Conventional filtration, washing, oven dry makes cobaltocene metal organic complex magnetic.Get 5 parts of this magnetics, with 1 part of titanium dioxide, 1 part of alchlor, 3 parts of poly-methyl-monosilane coupling agents to benzyl styrene and material total amount 2%, fully mixing on twin-roll machine, make cobaltocene metal organic complex magnetic base-material, its μ ' ≈ 2.0, tg δ ≈ 1 * 10
-2, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～17.0GHz.
Embodiment 12
With 2 parts of diacetyl ferrocene, 3 parts of cobalt chlorides reflux in 10 parts of butanols added 2 parts of carbonyl nickels after 2 hours under vigorous stirring, and 2 parts of tri-iron tetroxides refluxed 1 hour again.Conventional filtration, washing, oven dry makes ferrocene metal organic complex magnetic.Get 2 parts of this magnetics, with 2 parts of silica flours, 2 parts of barium titanates, the titanate coupling agent of 6 parts of poly-p-methylstyrenes and material total amount 2% is fully mediated on kneader, makes metal organic complex magnetic base-material, its μ ' ≈ 2.8, tg δ ≈ 6 * 10
-3, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～12.0GHz.
Embodiment 13
With 3 parts of diacetyl ferrocene, 4 parts of cobalt chlorides refluxed in 10 parts of amylalcohols after 2 hours, added 1 part of carbonyl nickel under vigorous stirring, refluxed 1 hour again.Conventional filtration, washing, oven dry makes ferrocene metal organic complex magnetic.Get 6 parts of this magnetics, with 1 part of titanium dioxide, 0.5 part of carbon black, 0.5 the titanate coupling agent of part barium titanate and 2 parts of polyethylene powders and material total amount 1.5% after fully mixing, is crossed 120 mesh sieves in mixer, make ferrocene metal organic complex magnetic base-material, its μ ' ≈ 2.0, tg δ ≈ 1 * 1
-2, be applicable to that making frequency range is microstrip antenna and the microstrip circuit of 100MHz～10.0GHz.
The characteristic of property contrast of tape base material can be as shown in the table slightly for the present invention's above-mentioned metal organic complex magnetic base-material and present:
| Commercially available ceramic substrate | Polytetrafluoroethylene (PTFE) composite dielectric base material | 99114711.1 number patent application contracting ripple base material | Metal organic complex magnetic base-material of the present invention | |
| Machinability | Hard crisp difficult processing, uniformity is relatively poor | Hard crisp difficult processing, uniformity is relatively poor | Processability is good, and isotropism, technology are complicated | Processability is good, isotropism, and technology is simpler |
| Dielectric constant (ε ') | 10～15 | 5～10 | 5～10 | 5～20 |
| Loss angle tangent (tg δ) | 1×10 -4 | 1×10 -3 | 3×10 -3 | 3×10 -3 |
| Permeability (μ ') | 1 | 1 | ≈3.0 | ≈3.0 |
| Physical dimension | Heavy, thin, little | Heavy, thin, little | Gently, thin, little | Gently, thin, little |
| Be suitable for frequency range (Hz) | 100M～3.0G | 300M～2.0G | 200M～3.0G | 100M～17.0G |
Claims (7)
1. ultratvide frequency band metal organic complex magnetic material, at least a by in component A or the B component mixes composition with component C and component D, and the weight of each component is:
At least a total amount 10-70% in component A or the B component,
Component C 15-60%,
Component D 5-50%, wherein: component A is a kind of in the two metallocene organic compounds of the ferrocene, cobaltocene or the dicyclopentadienyl nickel that contain carbonyl, carboxyl, amino or amido;
B component is to have two benzene compounds that contain the N group, saidly contains a kind of that the N group can be in amido, amino, hydrazine or the oxime;
Component C is a kind of in chloride, acetate, sulfate or the oxalates of iron, cobalt, nickel, copper;
Component D is a kind of in the inorganic soft magnetic ferrite.
2. ultratvide frequency band metal organic complex magnetic material as claimed in claim 1, what it is characterized in that said component A can be in diformazan acyl ferrocene, diacetyl ferrocene, ferrocene dicarboxylic acid, ferrocene diformamide, ferrocene diacetayl amide, ferrocene phenylenediamine, ferrocene benzidine, ferrocene two hydrazines, ferrocene amido phenylate, ferrocene dioxime, cobaltocene dioctyl phthalate, two formyl cobaltocenes, diacetyl cobaltocene, dicyclopentadienyl nickel dioctyl phthalate, the diacetyl dicyclopentadienyl nickel is a kind of.
3. ultratvide frequency band metal organic complex magnetic material as claimed in claim 1 is characterized in that said B component can be for o-phenylenediamine, m-phenylene diamine (MPD), p-phenylenediamine (PPD), diaminourea phenylate, MDA, terephthalamide, benzidine, to benzene two hydrazines, a kind of in the benzene dioxime.
4. ultratvide frequency band metal organic complex magnetic material as claimed in claim 1, what it is characterized in that said component D can be in the dilval of carbonyl iron, carbonyl nickel, nickel-zinc ferrite, tri-iron tetroxide, crystalline state, amorphous alloy, silica, the carborundum is a kind of.
5. as the described ultratvide frequency band metal organic complex of one of claim 1 to 4 magnetic material, it is characterized in that total amount at least a in said component A or the B component is made of jointly the component A and the B component of equivalent.
6. one kind is the ultratvide frequency band organic magnetic base-material of basis with the said ultratvide frequency band metal organic complex of claim 1 magnetic material, it is characterized in that fully being mixed with additive and thermoplastic resin by the said ultratvide frequency band metal organic complex of claim 1 magnetic material and form, the weight of each component is:
Above-mentioned metal organic complex magnetic material 10-70%
Additive 5-40%,
Thermoplastic resin 10-70%, wherein, said additive is a kind of in titanium dioxide, barium titanate, strontium titanates, alchlor, silica flour, carbon black, the charcoal fiber, and what said thermoplastic resin can be in polyethylene, polypropylene, polystyrene, poly-p-methylstyrene, Merlon, polysulfones, polyphenylene sulfide, unsaturated-resin, the polytetrafluoroethylene is a kind of.
7. ultratvide frequency band organic magnetic base-material as claimed in claim 6 is characterized in that also adding a kind of in the titanate ester of promising base-material total weight 2-10% or the silane coupling agent in said thermoplastic resin.
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