CN110283373A - A kind of thermoplastic magnetic composite and preparation method - Google Patents
A kind of thermoplastic magnetic composite and preparation method Download PDFInfo
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- CN110283373A CN110283373A CN201910653837.9A CN201910653837A CN110283373A CN 110283373 A CN110283373 A CN 110283373A CN 201910653837 A CN201910653837 A CN 201910653837A CN 110283373 A CN110283373 A CN 110283373A
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- carbonyl iron
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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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
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
Abstract
The present invention relates to a kind of thermoplastic magnetic composites and preparation method thereof.The preparation method is reacted with carbonyl iron dust, first surface modifying agent, alcohols solvent, water, ammonium hydroxide and silicon source precursor is made coated silica carbonyl iron dust, then using coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant as raw material, the carbonyl iron/resin composite materials are made through mixing granulator, injection molding after each raw material component is mixed.The composite material shows higher electromagnetic property in 1.0-3.9GHz frequency range, can be widely applied to the electronic fields such as antenna, feeding network, microwave device.
Description
Technical field
The present invention relates to Electromagnetic Function Composite technical field more particularly to a kind of thermoplastic magnetic composite and preparations
Method.
Background technique
With the fast development in smart phone market, in mobile phone, electronic component quantity is more and more, size is smaller and smaller,
And the electromagnetic interference between component is just inevitable in a limited space, has to the communication function of antenna for mobile phone serious dry
It disturbs, weakens the intensity transmission of signal, or even antenna is made thoroughly to fail.Must be added between device thus with high magnetic permeability,
The electromagnetic shielding material of high magnetic loss carrys out effective solution this problem.
Carbonyl iron dust has a wide range of applications and occupies an important position in electromagnetic transmission technology, is electronic component
Core material can be absorbed in microwave range magnetic conductivity with higher and the clutter between device is lost.Carbonyl at present
The production method of iron powder mainly rests in a small number of developed countries such as the U.S., Canada, Germany, and domestic enterprise's output is unable to satisfy
Demand of the domestic market to carbonyl iron dust, therefore domestic carbonyl iron dust still relies on import, so that using carbonyl iron dust as raw material
Material production cost it is higher.The disadvantages of that there are inoxidizability is poor for carbonyl iron dust, easy-to-rust causes using carbonyl iron dust
Inevitably there is certain loss in the process and production cost is further increased.
On the one hand the electromagnetic performances of magnetoelectric composites depends on the attenuation characteristic of composite material, i.e., entering composite material
Internal electromagnetic wave is as much as possible to decay and sponges, and on the other hand additionally depends on the impedance matching property of composite material, i.e.,
Incident electromagnetic wave can enter composite material to the maximum extent, and cannot encounter composite material and reflect.Carbonyl iron dust category
In magnetic material, while there is magnetic loss and dielectric loss, but the difference between dielectric properties and magnetic property is larger, so that with carbonyl
Base iron powder is poor as the impedance matching of the magnetoelectric composites of preparation component, largely leads to magnetoelectric composites
Electromagnetic performance is performed poor.
The prior art is usually compound using liquid-state epoxy resin and carbonyl iron dust progress, then using compression molding electromagnetism
Composite material.But this preparation method is there is complex process, compact dimensions are single, low efficiency, is difficult to mass production etc. and lacks
Point.
Summary of the invention
The invention aims to by carbonyl iron dust cladding processing with thermoplastic resin bonding it is compound, provide one kind have it is excellent
The preparation method of the functional composite material of electromagnetic property meets answering in terms of high-performance electronic component with novel Electromagnetic Material
With.
To achieve the goals above, the present invention provides the following technical scheme that
A kind of preparation method of thermoplastic magnetic composite, the preparation method with carbonyl iron dust, first surface modifying agent,
Alcohols solvent, water, ammonium hydroxide and silicon source precursor, which react, is made coated silica carbonyl iron dust, then with coated silica carbonyl
Base iron powder, thermoplastic resin, second surface modifying agent and lubricant be raw material, after each raw material component is mixed through mixing granulator,
The thermoplastic magnetic composite is made in injection molding.
Preferably, the first surface modifying agent and second surface modifying agent are silane coupling agent, the silane coupling agent
For 3- (the third oxygen of 2,3- epoxy) propyl trimethoxy silicane；
The alcohols solvent is ethyl alcohol；And/or
The silicon source presoma is ethyl orthosilicate.
Preferably, the quality of the first surface modifying agent is the 3-4wt% of the carbonyl iron dust quality；
The quality of the alcohols solvent is the 10-15wt% of the carbonyl iron dust quality；
The quality of the silicon source presoma is the 1-5wt% of the carbonyl iron dust quality；And/or
The quality of the ammonium hydroxide is the 40-50wt% of the silicon source forerunner weight.
Preferably, the thermoplastic resin is polyethylene, polypropylene, polyvinyl chloride, polystyrene, poly-methyl methacrylate
Ester, polyester, polyformaldehyde, polyamide, polycarbonate, polyphenylene oxide, acrylonitrile-butadiene-styrene copolymer, thermoplastic elastic are poly-
Urethane, vulcanized rubber, synthetic rubber, ethylene-vinyl acetate copolymer, styrene-isoprene-styrene block copolymer,
One of Styrene-Butadiene-Styrene Block Copolymer, styrene ethylene butadiene-styrene block copolymer etc.
Or it is a variety of；Preferably polypropylene；And/or
The lubricant is olein.
Preferably, the quality of the thermoplastic resin is coated silica carbonyl iron dust, thermoplastic resin, second surface
The 5-10wt% of modifying agent and lubricant gross mass.
Preferably, the quality of the lubricant is coated silica carbonyl iron dust, thermoplastic resin, second surface are modified
The 1-5wt% of agent and lubricant gross mass, preferably 1-3wt%.
Preferably, the preparation method includes the following steps:
(1) it prepares coated silica carbonyl iron dust: carbonyl iron dust, first surface modifying agent, alcohols solvent and water is mixed
It closes, adds ammonium hydroxide and silicon source precursor is reacted, obtain coated silica carbonyl iron dust；
(2) mixing granulator: by coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant
Mixing granulator is carried out, composite granule is obtained；
(3) by composite granule injection molding, the carbonyl iron/resin composite materials injection molding: are obtained.
Preferably, in step (2), by coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and
Lubricant adds twin-screw extrude the mixing extrusion at 130-230 DEG C, and then cutting is granulated, and obtains the composite granule.
Preferably, in step (3), the injection molding carries out at 180-230 DEG C, injection pressure 100-
130MPa, mold temperature are 70-130 DEG C.
The present invention also provides a kind of thermoplastic magnetic composites, are made using the preparation method provided by the invention.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
Preparation method provided by the invention carries out coated with silica to carbonyl iron dust, and silica is chemical inertness material
Material, good in oxidation resistance, cost is relatively low, and in the surface covering silicon dioxide film of carbonyl iron dust, the anti-of carbonyl iron dust can be improved
Oxidation susceptibility.In addition, the dielectric constant and dielectric loss of the magnetoelectric composites using the preparation of coated silica carbonyl iron dust
It decreases, so that the impedance matching of composite material is preferable, to improve electromagnetic performance.
The present invention passes through to first surface modifying agent, alcohols solvent, silicon source presoma, ammonium hydroxide, thermoplastic resin, lubricant
Optional material and/or component be optimized, have developed that a kind of efficiency is higher, cost is relatively low, can in high volume generate
Preparation process.
The present invention uses chemical method coating carbonyl iron powder first, by thermoplastic resin and powder mixing granulator, with injection molding
Technological forming carbonyl iron/resin magnetoelectric composites, the magnetic conductivity with higher in 1.0-3.9GHz band limits, can be wide
It is general to be applied in each field electronic equipments such as mobile communication, radio and television.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of carbonyl iron/trees in 1.0-3.9GHz frequency range with low-k and low-dielectric loss
The preparation method of resin composite material, the preparation method with carbonyl iron dust, first surface modifying agent, alcohols solvent, water, ammonium hydroxide and
Silicon source precursor react be made coated silica carbonyl iron dust, then with coated silica carbonyl iron dust, thermoplastic resin,
Second surface modifying agent and lubricant are raw material, and the carbonyl is made through mixing granulator, injection molding after each raw material component is mixed
Base iron/resin composite materials.
Preparation method provided by the invention carries out coated with silica to carbonyl iron dust, and silica is chemical inertness material
Material, good in oxidation resistance, cost is relatively low, and in the surface covering silicon dioxide film of carbonyl iron dust, the anti-of carbonyl iron dust can be improved
Oxidation susceptibility.In addition, the dielectric constant and dielectric loss of the magnetoelectric composites using the preparation of coated silica carbonyl iron dust
It decreases, so that the impedance matching of composite material is preferable, to improve electromagnetic performance.
In some preferred embodiments, institute first states surface modifier and second surface modifying agent is silane coupled
Agent, the silane coupling agent are 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane also known as KH560 or KH-560.Described
The quality of one surface modifier is preferably the 3-4wt% of the carbonyl iron dust quality, can be any number within the scope of this, example
Such as, can for 3wt%, 3.1wt%, 3.2wt%, 3.3wt%, 3.4wt%, 3.5wt%, 3.6wt%, 3.7wt%,
3.8wt%, 3.9wt%, 4wt%.Surface modification is carried out to carbonyl iron dust using KH560 to be conducive to answer with silica membrane
It closes, improves interface binding power.Inventor has found the dosage of surface modifier (for example, it is preferable to KH560) only in the course of the research
The 3-4wt% for reaching carbonyl iron dust quality can be obtained significant effect, be based on cost consideration, preparation side provided by the invention
Method can be by the dosage of the first face of table modifying agent (for example, it is preferable to KH560) when carrying out surface modification treatment to carbonyl iron dust
It is limited to the 3-4wt% of carbonyl iron dust quality used.
In addition to the optional material to first surface modifying agent and second surface modifying agent and its other than dosage is optimized, this
Invention also to preparation component in alcohols solvent, silicon source presoma, ammonium hydroxide, thermoplastic resin, lubricant optional material and/or
Component is optimized, to have developed the preparation process that a kind of efficiency is higher, cost is relatively low, can in high volume generate.With
Under be technical solution after every content optimization:
In some preferred embodiments, the alcohols solvent is ethyl alcohol, and quality is the carbonyl iron dust quality
10-15wt% can be any number within the scope of this, for example, can for 10wt%, 11wt%, 12wt%, 13wt%,
14wt%, 15wt%.
In some preferred embodiments, the silicon source presoma is ethyl orthosilicate (TEOS), and quality is described
The 1-5wt% of carbonyl iron dust quality can be any number within the scope of this, for example, can for 1wt%, 2wt%, 3wt%,
4wt%, 5wt%.
In some preferred embodiments, the quality of the ammonium hydroxide is the 40-50wt% of the silicon source forerunner weight,
Can be any number within the scope of this, for example, can for 40wt%, 41wt%, 42wt%, 43wt%, 44wt%,
45wt%, 46wt%, 47wt%, 48wt%, 49wt%, 50wt%.
In some preferred embodiments, the thermoplastic resin be polyethylene (can be high density polyethylene (HDPE), can also
Think low density polyethylene (LDPE)), polypropylene, polyvinyl chloride, polystyrene, polymethyl methacrylate, polyester, polyformaldehyde, polyamides
Amine, polycarbonate, polyphenylene oxide, acrylonitrile-butadiene-styrene copolymer, thermoplastic elastic polyurethane, vulcanized rubber, synthesis
Rubber, ethylene-vinyl acetate copolymer, styrene-isoprene-styrene block copolymer, styrene-butadiene-benzene second
One of alkene block copolymer, styrene ethylene butadiene-styrene block copolymer etc. are a variety of, and more preferably poly- third
Alkene.The quality of the thermoplastic resin is coated silica carbonyl iron dust, thermoplastic resin and lubricant gross mass
7-10wt% can be any number within the scope of this, for example, can be 7wt%, 8wt%, 9wt%, 10wt%.
In some preferred embodiments, the lubricant is olein.The quality of the lubricant is packet
The 1-5wt% of silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant gross mass is covered, it can be with
For any number within the scope of this, for example, can be 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, preferably 1-3wt%.
More specifically, this preparation method provided by the invention includes the following steps:
(1) coated silica carbonyl iron dust is prepared
Carbonyl iron dust, first surface modifying agent, alcohols solvent and water are mixed, ammonium hydroxide is added and silicon source precursor carries out
Reaction, obtains coated silica carbonyl iron dust.More specifically, can be by carbonyl iron dust, first surface modifying agent, alcohols solvent
It is mixed with water, the mixing of above-mentioned each component can be realized by way of stirring.Then, ammonium hydroxide is added in a manner of dropwise addition respectively
It is reacted with silicon source precursor (such as ethyl orthosilicate) into mixed liquor, in this step, the time of reaction can control
1-3 hours.It washes and dries finally, carrying out alcohol to the product of acquisition after reaction, obtain coated silica carbonyl iron dust.Institute
Stating first surface modifying agent is preferably silane coupling agent, and the silane coupling agent is 3- (2,3- the third oxygen of epoxy) propyl trimethoxy
Silane, quality are preferably the 3-4wt% of the carbonyl iron dust quality.In addition to first surface modifying agent optional material and its
Outside dosage is optimized, the present invention is also to alcohols solvent, the silicon source presoma, ammonium hydroxide, thermoplastic resin, profit in preparation component
The optional material and/or component of lubrication prescription are optimized, to have developed, a kind of efficiency is higher, cost is relatively low, can be large quantities of
Measure the preparation process generated.Be the technical solution after every content optimization below: the alcohols solvent can be ethyl alcohol, quality
For the 10-15wt% of the carbonyl iron dust quality.The silicon source presoma can be ethyl orthosilicate, and quality is the carbonyl
The 1-5wt% of iron powder quality.The quality of the ammonium hydroxide is preferably the 40-50wt% of the silicon source forerunner weight.
It should be noted that ammonium hydroxide used in the present invention is commercially available 25% ammonium hydroxide, NH3Content is in 25-28wt%, density
In 0.90-0.91g/cm3。
(2) mixing granulator
Coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant are subjected to mixing granulator,
Obtain composite granule.More specifically operation can be with are as follows: by coated silica carbonyl iron dust, thermoplastic resin, second surface
It (can be any number within the scope of this, for example, can that modifying agent and lubricant, which are added twin-screw extrude at 130-230 DEG C,
Think 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 230 DEG C) under be kneaded
It squeezes out, then cutting is granulated, and obtains the composite granule.
In this step, it (can be high density polyethylene (HDPE), or low close that the thermoplastic resin, which can be polyethylene,
Spend polyethylene), polypropylene, polyvinyl chloride, polystyrene, polymethyl methacrylate, polyester, polyformaldehyde, polyamide, poly- carbonic acid
Ester, polyphenylene oxide, acrylonitrile-butadiene-styrene copolymer, thermoplastic elastic polyurethane, vulcanized rubber, synthetic rubber, ethylene-
Vinyl acetate co-polymer, styrene-isoprene-styrene block copolymer, s-B-S block copolymerization
One of object, styrene ethylene butadiene-styrene block copolymer etc. are a variety of, more preferably polypropylene.The heat
The quality of plastic resin is preferably coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant four
The 5-10wt% of person's gross mass.The excessively high influence composite material electromagnetic performance of the accounting of thermoplastic resin；Accounting is excessively few then to lead to difficulty
With even adhesion, lead to not form, technique is poor.
The lubricant is preferably olein, and quality is preferably coated silica carbonyl iron dust, thermoplasticity
The 1-5wt% of resin, second surface modifying agent and lubricant gross mass.
The second surface modifying agent is preferably silane coupling agent, and the silane coupling agent is 3- (2,3- the third oxygen of epoxy) third
Base trimethoxy silane, quality are preferably coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and profit
The 2-3wt% of lubrication prescription gross mass.
(3) injection molding
By composite granule injection molding, the carbonyl iron/resin composite materials are obtained.In some preferred embodiments
In, the injection molding 180-230 DEG C (can be any number within the scope of this, for example, can for 180 DEG C, 190 DEG C,
200 DEG C, 210 DEG C, 220 DEG C, 230 DEG C) under carry out, injection pressure 100-130MPa can be any number within the scope of this,
For example, can be 100MPa, 105MPa, 110MPa, 115MPa, 120MPa, 125MPa, 130MPa, mold temperature 70-130
DEG C, can be any number within the scope of this, for example, can for 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C, 100 DEG C,
105℃、110℃、115℃、120℃、125℃、130℃。
The present invention, which provides one kind in second aspect, has low-k and low-dielectric loss in 1.0-3.9GHz frequency range
Carbonyl iron/resin composite materials, this composite material using preparation method provided by the invention be made, have lower dielectric
Constant and dielectric loss, impedance matching are preferable.
It is the embodiment that the present invention enumerates below.
Embodiment 1
Directly adopt carbonyl iron dust and thermoplastic resin be compound prepares carbonyl iron/resin composite materials, not to carbonyl iron into
Row coated with silica.
Specific preparation method includes the following steps:
S1,6.8kg carbonyl iron dust, 1.2kg LDPE (Low Density Polyethylene low density polyethylene are weighed
Alkene), 0.21kg KH560,0.12kg olein add twin-screw extrude, setting Heating Zone Temperature is respectively 105
DEG C, 110 DEG C, 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 130 DEG C, 130 DEG C, 125 DEG C, screw speed 300rpm, be kneaded
It is granulated three times, obtains carbonyl iron/masterbatch resin.
S2, obtained carbonyl iron/masterbatch resin is added in injection molding machine, the setting of screw rod warm area is respectively 130 DEG C, 135 DEG C,
140 DEG C, 150 DEG C, 155 DEG C, 145 DEG C, injection pressure 113MPa, mold temperature be 75 DEG C, final injection molding obtain carbonyl iron/
LDPE composite material.
Embodiment 2
The present embodiment first carries out silica surface cladding to carbonyl iron dust, then with thermoplastic resin is compound prepares carbonyl
Iron/resin composite materials.
Specific preparation method includes the following steps:
S1,10kg carbonyl iron dust is weighed and 300mL KH560,1500mL ethyl alcohol, 400mL deionized water are stirred, with
Ammonium hydroxide (commercially available 25% ammonium hydroxide, NH is added dropwise respectively afterwards3Content is in 25-28wt%, and density is in 0.90-0.91g/cm3)60mL、TEOS
(ethyl orthosilicate) 120mL reacts 6h into mixed liquor, and last alcohol obtains coated Si O after washing, drying2Carbonyl iron dust.
S2,9.1kg coated Si O is weighed2Carbonyl iron dust, 1.0kg HDPE (High Density Polyethylene, height
Density polyethylene), 0.27kg KH560,0.15kg olein add twin-screw extrude, Heating Zone Temperature is set
Respectively 160 DEG C, 160 DEG C, 165 DEG C, 175 DEG C, 185 DEG C, 200 DEG C, 205 DEG C, 195 DEG C, 195 DEG C, 195 DEG C, screw speed
350rpm, mixing granulator three times, obtain carbonyl iron/masterbatch resin.
S3, carbonyl iron/masterbatch resin is added in injection molding machine, the setting of screw rod warm area is respectively 180 DEG C, 185 DEG C, 200 DEG C,
205 DEG C, 210 DEG C, 210 DEG C, injection pressure 113MPa, mold temperature are 105 DEG C, and it is multiple that final injection molding obtains carbonyl iron/HDPE
Condensation material.
Embodiment 3
The present embodiment first carries out silica surface cladding to carbonyl iron dust, then with thermoplastic resin is compound prepares carbonyl
Iron/resin composite materials.
Specific preparation method includes the following steps:
S1,10kg carbonyl iron dust is weighed and 300mL KH560,1500mL ethyl alcohol, 400mL deionized water are stirred, with
Ammonium hydroxide (commercially available 25% ammonium hydroxide, NH is added dropwise respectively afterwards3Content is in 25-28wt%, and density is in 0.90-0.91g/cm3)60mL、TEOS
(ethyl orthosilicate) 120mL reacts 6h into mixed liquor, and last alcohol obtains coated Si O after washing, drying2Carbonyl iron dust.
S2,8.7kg coated Si O is weighed2Carbonyl iron dust, 0.5kg HDPE (High Density Polyethylene, height
Density polyethylene), 0.26kg KH560,0.13kg olein add twin-screw extrude, Heating Zone Temperature is set
Respectively 160 DEG C, 160 DEG C, 165 DEG C, 175 DEG C, 185 DEG C, 200 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, screw speed
400rpm, mixing granulator three times, obtain carbonyl iron/masterbatch resin.
S3, carbonyl iron/masterbatch resin is added in injection molding machine, the setting of screw rod warm area is respectively 180 DEG C, 190 DEG C, 200 DEG C,
210 DEG C, 220 DEG C, 230 DEG C, injection pressure 113MPa, mold temperature are 130 DEG C, and it is multiple that final injection molding obtains carbonyl iron/HDPE
Condensation material.
Embodiment 4
The present embodiment first carries out silica surface cladding to carbonyl iron dust, then with thermoplastic resin is compound prepares carbonyl
Iron/resin composite materials.
Specific preparation method includes the following steps:
S1,10kg carbonyl iron dust is weighed and 300mL KH560,1500mL ethyl alcohol, 400mL deionized water are stirred, with
Ammonium hydroxide (commercially available 25% ammonium hydroxide, NH is added dropwise respectively afterwards3Content is in 25-28wt%, and density is in 0.90-0.91g/cm3)60mL、TEOS
(ethyl orthosilicate) 120mL reacts 6h into mixed liquor, and last alcohol obtains coated Si O after washing, drying2Carbonyl iron dust.
S2,8.2kg coated Si O is weighed2Carbonyl iron dust, 0.5kg PP (Polypropylene, polypropylene), 0.24kg
KH560,0.13kg olein add twin-screw extrude, setting Heating Zone Temperature is respectively 180 DEG C, 180 DEG C,
185 DEG C, 195 DEG C, 195 DEG C, 210 DEG C, 215 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, screw speed 400rpm, mixing granulator three times,
Obtain carbonyl iron/masterbatch resin.
S3, carbonyl iron/masterbatch resin is added in injection molding machine, the setting of screw rod warm area is respectively 180 DEG C, 195 DEG C, 205 DEG C,
215 DEG C, 225 DEG C, 230 DEG C, injection pressure 113MPa, mold temperature are 130 DEG C, and it is compound that final injection molding obtains carbonyl iron/PP
Material.
Table 1 describes the preparation process condition of embodiment 1 to 4.
Table 1
Note: the quality of the carbonyl iron dust of coated with silica is not carried out referred to.According to SJ20512-1995 to embodiment 1
It is tested to carbonyl iron/resin composite materials electromagnetic parameter made from embodiment 4, test result is listed in Table 2 below.
Table 2
Note: ε ' is the real part of opposite complex dielectric permittivity；ε " is the imaginary part of opposite complex dielectric permittivity；μ ' is complex permeability
Real part；μ " is the imaginary part of complex permeability；tanσdFor electrical loss tangent angle；tanσmFor magnetic loss tangent angle.
It can be seen that from embodiment 1 and the test result comparison of embodiment 2 to 4, pass through SiO2Gained carbonyl after cladding processing
Iron/thermoplastic resin composite material has lower dielectric constant and dielectric loss in 1.0-3.9GHz, makes the dielectric of composite material
Difference between performance and magnetic property reduces, and the impedance matching of composite material is preferable.
It can be seen that from embodiment 2 and the test result comparison of embodiment 3, with the raising of carbonyl iron dust additive amount, can mention
High composite material dielectric constant, magnetic conductivity, magnetic loss.
It can be seen that from embodiment 3 and the test result comparison of embodiment 4, bonded using PP (polypropylene) as thermoplastic resin
Agent can reduce composite material dielectric loss to a greater degree.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of thermoplastic magnetic composite, which is characterized in that the preparation method is with carbonyl iron dust, the first table
Face modifying agent, alcohols solvent, water, ammonium hydroxide and silicon source precursor, which react, is made coated silica carbonyl iron dust, then with cladding
Silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant are raw material, are passed through after each raw material component is mixed
The thermoplastic magnetic composite is made in mixing granulator, injection molding.
2. preparation method according to claim 1, which is characterized in that the first surface modifying agent and second surface are modified
Agent is silane coupling agent, and the silane coupling agent is 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane；
The alcohols solvent is ethyl alcohol；And/or
The silicon source presoma is ethyl orthosilicate.
3. preparation method according to claim 2, which is characterized in that the quality of the first surface modifying agent is the carbonyl
The 3-4wt% of base iron powder quality；
The quality of the alcohols solvent is the 10-15wt% of the carbonyl iron dust quality；
The quality of the silicon source presoma is the 1-5wt% of the carbonyl iron dust quality；And/or
The quality of the ammonium hydroxide is the 40-50wt% of the silicon source forerunner weight.
4. preparation method according to any one of claims 1 to 3, which is characterized in that the thermoplastic resin be polyethylene,
Polypropylene, polyvinyl chloride, polystyrene, polymethyl methacrylate, polyester, polyformaldehyde, polyamide, polycarbonate, polyphenylene oxide,
Acrylonitrile-butadiene-styrene copolymer, thermoplastic elastic polyurethane, vulcanized rubber, synthetic rubber, ethylene-vinyl acetate
Copolymer, styrene-isoprene-styrene block copolymer, Styrene-Butadiene-Styrene Block Copolymer, styrene-
One of ethylene-butadiene-styrene block copolymer etc. is a variety of；Preferably polypropylene；And/or
The lubricant is olein.
5. the preparation method according to claim 4, which is characterized in that the quality of the thermoplastic resin is cladding titanium dioxide
Silicon carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant gross mass 5-10wt%.
6. the preparation method according to claim 4, which is characterized in that the quality of the lubricant is coated silica carbonyl
Base iron powder, thermoplastic resin, second surface modifying agent and lubricant gross mass 1-5wt%, preferably 1-3wt%.
7. preparation method according to any one of claims 1 to 6, which is characterized in that the preparation method includes following step
It is rapid:
(1) it prepares coated silica carbonyl iron dust: carbonyl iron dust, first surface modifying agent, alcohols solvent and water is mixed, then
Ammonium hydroxide is added and silicon source precursor is reacted, obtains coated silica carbonyl iron dust；
(2) mixing granulator: coated silica carbonyl iron dust, thermoplastic resin, second surface modifying agent and lubricant are carried out
Mixing granulator obtains composite granule；
(3) by composite granule injection molding, the carbonyl iron/resin composite materials injection molding: are obtained.
8. preparation method according to claim 7, which is characterized in that in step (2), by coated silica carbonyl iron
Powder, thermoplastic resin, second surface modifying agent and lubricant add twin-screw extrude the mixing extrusion at 130-230 DEG C,
Then cutting is granulated, and obtains the composite granule.
9. preparation method according to claim 7, which is characterized in that in step (3), the injection molding is in 180-
It is carried out at 230 DEG C, injection pressure 100-130MPa, mold temperature is 70-130 DEG C.
10. a kind of thermoplastic magnetic composite, which is characterized in that using any one of claim 1 to the 9 preparation method system
?.
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