CN105017604B - The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material - Google Patents
The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material Download PDFInfo
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- CN105017604B CN105017604B CN201510350026.3A CN201510350026A CN105017604B CN 105017604 B CN105017604 B CN 105017604B CN 201510350026 A CN201510350026 A CN 201510350026A CN 105017604 B CN105017604 B CN 105017604B
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- polyethylene
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- conductive composite
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
- B29C71/02—Thermal after-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- 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
- C08K2201/011—Nanostructured additives
Abstract
The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material, it are related to a kind of heat-conductive composite material containing inorganic conductive particle.The invention aims to solving the technical problem of polyethylene low thermal conductivity.This method is as follows:Take ferroso-ferric oxide and polyethylene is placed in alcohol and is stirred mixing and pours heating in hydrothermal synthesis reaction kettle into, filter, drying is hot-forming, plus magnetic, obtains final product.The present invention prepares nano-particle in gained nano ferriferrous oxide/composite polyethylene material and is uniformly dispersed, and ferroso-ferric oxide significantly improves the capacity of heat transmission of polyethylene, the composite particularly plus after magnetic treatment.The invention belongs to the preparation field of heat-conductive composite material.
Description
Technical field
The present invention relates to a kind of heat-conductive composite material containing inorganic conductive particle.
Background technology
Polyethylene (PE) is a kind of nontoxic insulating polymeric material of light weight, and which has the electrical insulating property of brilliance and dielectricity
Can, lower temperature resistance, enough mechanical properties are so as to widely be applied.But the shortcoming of polyethylene is it is also obvious that its thermal conductivity
The little only 0.28～0.44W/m K of rate is narrow using temperature range.The thermal conductivity of metal and its oxide is larger, usually high score
100 times of sub- material and more than, so be filled in macromolecular material as heat filling to improve its thermal conductivity.System
Standby heat-conduction electric insulation polyethylene can give full play to the higher thermal conductivity of the intrinsic excellent electrical properties of polyethylene and composite, this kind of
Material may be used also in addition to for the insulating radiation of electronic device, encapsulation and other specific uses under the relatively low occasion of some heat resistances
Radiating requirements for nonisulated occasion.
Content of the invention
The invention aims to solving the technical problem of polyethylene low thermal conductivity, there is provided the oxidation of a kind of nanometer four three
The preparation method of iron/polyethylene heat-conductive composite material.
The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material is as follows：
First, take ferroso-ferric oxide and polyethylene is placed in alcohol and mixing is stirred, suspension is obtained, four oxygen in suspension
The mass ratio for changing three-iron with polyethylene is 1%～30%；
2nd, step one gained suspension is poured in hydrothermal synthesis reaction kettle, packing ratio is 70～85%, in temperature is
1～24h is incubated under conditions of 100～130 DEG C；
3rd, suspension is poured out from hydrothermal synthesis reaction kettle, is filtered, dry 1～12h at 50 DEG C, obtain mixed-powder；
4th, the mixed-powder in step 3 is placed in mould and is placed on vulcanizing press, be 0～10MPa, mould in pressure
Under conditions of pressure temperature is 110～130 DEG C, 5min～35min is hot-forming for pressurization, is cooled to room temperature, obtains heat conduction composite wood
Material；
5th, by step 4 gained heat-conductive composite material heating-up temperature be 110～130 DEG C, plus magnetoelectricity stream be 10～16A's
Under the conditions of plus magnetic treatment 30min, be then cooled to 15～60 DEG C, obtain final product nano ferriferrous oxide/polyethylene heat-conductive composite material.
As the density of polyethylene is less than 1, the density of ferroso-ferric oxide is more than 1, and during application immersion method, polyethylene can be floated over
Face waterborne, ferroso-ferric oxide can sink to the bottom, and therefore ferroso-ferric oxide cannot be uniform in polyethylene surface growth.The present invention is selected
Solvent-thermal method is selected, alcohol selected by solvent, because alcohol density can so make ferroso-ferric oxide less than polyethylene and ferroso-ferric oxide
Homoepitaxial is in polyethylene surface.When carrying out plus magnetic treatment to ferroso-ferric oxide/polyethylene heat-conductive composite material, its heat conduction can be made
Passage is more likely formed, and the capacity of heat transmission is improved further.
In the present invention, nano ferriferrous oxide/polyethylene heat-conductive composite material preparation method, is metal oxide/polyethylene
Composite provides a kind of new complex method, causes the ferroso-ferric oxide for producing to be coated in poly- second by solution synthetic method
Alkene surface, and its composite is carried out plus magnetic treatment, preparation technology and equipment needed thereby are simple, with low cost, easily implement.System
In standby gained nano ferriferrous oxide/composite polyethylene material, nano-particle is uniformly dispersed, and ferroso-ferric oxide significantly improves poly-
The capacity of heat transmission of ethene, the composite particularly plus after magnetic treatment.
Description of the drawings
Fig. 1 is the XRD spectrum for testing the nano ferriferrous oxide/polyethylene heat-conductive composite material prepared in, in figure ◆
Represent polyethylene, ● represent ferroso-ferric oxide；
Fig. 2 is to test the heat-conductive composite material that in prepared by step 4 to be combined with nano ferriferrous oxide/polyethylene heat conduction
The thermal conductivity curve comparison figure of material, in figure 1 represent that the thermal conductivity of nano ferriferrous oxide/polyethylene heat-conductive composite material is bent
Line, 2 represent heat-conductive composite material thermal conductivity curve prepared by step 4；
Fig. 3 is to test the schematic flow sheet that step 3 in prepares mixed-powder.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also includes between each specific embodiment
Any combination.
Specific embodiment one：The preparation method of present embodiment nano ferriferrous oxide/polyethylene heat-conductive composite material
As follows：
First, take ferroso-ferric oxide and polyethylene is placed in alcohol and mixing is stirred, suspension is obtained, four oxygen in suspension
The mass ratio for changing three-iron with polyethylene is 1%～30%；
2nd, step one gained suspension is poured in hydrothermal synthesis reaction kettle, packing ratio is 70～85%, in temperature is
1～24h is incubated under conditions of 100～130 DEG C；
3rd, suspension is poured out from hydrothermal synthesis reaction kettle, is filtered, dry 1～12h at 50 DEG C, obtain mixed-powder；
4th, the mixed-powder in step 3 is placed in mould and is placed on vulcanizing press, be 0～10MPa, mould in pressure
Under conditions of pressure temperature is 110～130 DEG C, 5min～35min is hot-forming for pressurization, is cooled to room temperature, obtains heat conduction composite wood
Material；
5th, by step 4 gained heat-conductive composite material heating-up temperature be 110～130 DEG C, plus magnetoelectricity stream be 10～16A's
Under the conditions of plus magnetic treatment 30min, be then cooled to 15～60 DEG C, obtain final product nano ferriferrous oxide/polyethylene heat-conductive composite material.
Specific embodiment two：Present embodiment and four oxidations three described in step one unlike specific embodiment one
Iron is 1% with the mass ratio of polyethylene.Other are identical with specific embodiment one.
Specific embodiment three：Described in step one unlike one of present embodiment and specific embodiment one or two
Ferroso-ferric oxide is 5% with the mass ratio of polyethylene.Other are identical one of with specific embodiment one or two.
Specific embodiment four：Described in step one unlike one of present embodiment and specific embodiment one to three
Ferroso-ferric oxide is 10% with the mass ratio of polyethylene.Other are identical one of with specific embodiment one to three.
Specific embodiment five：Hydro-thermal in step 2 unlike one of present embodiment and specific embodiment one to four
In synthesis reaction vessel, temperature is 110 DEG C, is incubated 4h.Other are identical one of with specific embodiment one to four.
Specific embodiment six：Hydro-thermal in step 2 unlike one of present embodiment and specific embodiment one to five
In synthesis reaction vessel, temperature is 120 DEG C, is incubated 6h.Other are identical one of with specific embodiment one to five.
Specific embodiment seven：Hydro-thermal in step 2 unlike one of present embodiment and specific embodiment one to six
In synthesis reaction vessel, temperature is 130 DEG C, is incubated 8h.Other are identical one of with specific embodiment one to six.
Specific embodiment eight：Will step in step 5 unlike one of present embodiment and specific embodiment one to seven
In rapid four, gained heat-conductive composite material is placed in the double yoke single tuning adjustable air gap electromagnet of SBV, is heated to 130 DEG C, is opened
Electric current starts plus magnetic, plus magnetoelectricity stream is adjusted to 16A, stops heating, after temperature is down to 60 DEG C, close electric current after insulation 30min.Other
Identical with one of specific embodiment one to seven.
Using following experimental verifications effect of the present invention：
Experiment one：
The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material, is realized according to the following steps：
First, take ferroso-ferric oxide and polyethylene be placed in alcohol and be stirred mixing, in suspension ferroso-ferric oxide with
The mass ratio of polyethylene is 15%.
2nd, step one gained suspension liquid is poured in hydrothermal synthesis reaction kettle, packing ratio is 80%, temperature is 110 DEG C,
Insulation 4h.
3rd, suspension is poured out from water heating kettle, through filtering, and at 50 DEG C, is dried 12h, is obtained mixed-powder.
4th, mixed powder is put in vulcanizing press, on vulcanizing press, molding temperature is 120 DEG C, is pressurizeed with 0MPa
5min, with 5MPa pressurization 5min, with 10MPa pressurization 5min, hot-forming with 15MPa pressurization 5min, it is finally cooled to room temperature and obtains
To heat-conductive composite material.
5th, the heat-conductive composite material of step 4 is placed in the double yoke single tuning adjustable air gap electromagnet of SBV, is heated to
130 DEG C, open electric current and start plus magnetic, plus magnetoelectricity stream is adjusted to 16A, stops heating, after temperature is down to 60 DEG C, close after insulation 30min
Electric current is closed, obtains final product nano ferriferrous oxide/polyethylene heat-conductive composite material.
The mass fraction of the ferroso-ferric oxide in this experiment in gained nano ferriferrous oxide/polyethylene heat-conductive composite material
For 15%.
During preparing nano ferriferrous oxide/polyethylene heat conduction composite granule, ferroso-ferric oxide is with polyethylene powders in machine
Under tool stirring, ferroso-ferric oxide can be bonded at polyethylene surface, under conditions of water heating kettle high temperature high pressure, ferroso-ferric oxide crystal
Can grow and be coated in polyethylene surface.Fig. 1 is 15% XRD spectrum for adding the composite after magnetic for ferroso-ferric oxide amount fraction.
Tested by LFA447 laser heat conducting instrument and characterize composite and measure thermal conductivity, solvent heat add magnetic after the receiving of 15% mass fraction
Rice ferroso-ferric oxide/polyethylene heat-conductive composite material thermal conductivity increases 30.16% than the thermal conductivity of pure polyethylene.By more than
Data obtain nano ferriferrous oxide coating polyethylene and carry out plus magnetic treatment after composite there is good heat conductivility.
Claims (8)
1. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material, it is characterised in that nano ferriferrous oxide/poly-
The preparation method of ethene heat-conductive composite material is as follows：
First, take ferroso-ferric oxide and polyethylene is placed in alcohol and mixing is stirred, suspension is obtained, four oxidation three in suspension
Iron is 1%～30% with the mass ratio of polyethylene；
2nd, step one gained suspension is poured in hydrothermal synthesis reaction kettle, packing ratio be 70～85%, temperature be 100～
1～24h is incubated under conditions of 130 DEG C；
3rd, suspension is poured out from hydrothermal synthesis reaction kettle, is filtered, dry 1～12h at 50 DEG C, obtain mixed-powder；
4th, the mixed-powder in step 3 is placed in mould and is placed on vulcanizing press, be 0～10MPa, be molded temperature in pressure
Spend for, under conditions of 110～130 DEG C, 5min～35min is hot-forming for pressurization, is cooled to room temperature, obtains heat-conductive composite material；
5th, step 4 gained heat-conductive composite material is 110～130 DEG C, adds the condition that magnetoelectricity stream is 10～16A in heating-up temperature
Down plus magnetic treatment 30min, then it is cooled to 15～60 DEG C, obtains final product nano ferriferrous oxide/polyethylene heat-conductive composite material.
2. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
Ferroso-ferric oxide described in step one is 1% with the mass ratio of polyethylene.
3. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
Ferroso-ferric oxide described in step one is 5% with the mass ratio of polyethylene.
4. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
Ferroso-ferric oxide described in step one is 10% with the mass ratio of polyethylene.
5. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
In step 2, in hydrothermal synthesis reaction kettle, temperature is 110 DEG C, is incubated 4h.
6. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
In step 2, in hydrothermal synthesis reaction kettle, temperature is 120 DEG C, is incubated 6h.
7. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
In step 2, in hydrothermal synthesis reaction kettle, temperature is 130 DEG C, is incubated 8h.
8. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material according to claim 1, it is characterised in that
Gained heat-conductive composite material in step 4 is placed in the double yoke single tuning adjustable air gap electromagnet of SBV in step 5, heat temperature raising
To 130 DEG C, open electric current and start plus magnetic, plus magnetoelectricity stream is adjusted to 16A, stops heating after insulation 30min, after temperature is down to 60 DEG C,
Close electric current.
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