CN105017604A - Preparation method of nanometer ferriferous oxide/polyethylene heat conduction composite material - Google Patents
Preparation method of nanometer ferriferous oxide/polyethylene heat conduction composite material Download PDFInfo
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- CN105017604A CN105017604A CN201510350026.3A CN201510350026A CN105017604A CN 105017604 A CN105017604 A CN 105017604A CN 201510350026 A CN201510350026 A CN 201510350026A CN 105017604 A CN105017604 A CN 105017604A
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- composite material
- preparation
- conductive composite
- polyethylene
- ferriferrous oxide
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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 invention discloses a preparation method of a nanometer ferriferous oxide/polyethylene heat conduction composite material and relates to an inorganic heat conduction particle-containing heat conduction composite material. The preparation method solves the problem that polyethylene heat conductivity is low. The preparation method comprises putting ferriferous oxide and polyethylene into alcohol, carrying out stirring mixing, pouring the mixture into a hydro-thermal synthesis reaction vessel, carrying out heating, carrying out filtration, carrying out drying hot pressing molding, and carrying out magnetization. The nanometer ferriferous oxide/polyethylene heat conduction composite material has uniform nanoparticle dispersity. Ferriferous oxide substantially improves a polyethylene heat conduction capability and especially, heat conduction capability of the magnetized composite material is improved. The preparation method belongs to the field of heat conduction composite material preparation.
Description
Technical field
The present invention relates to a kind of heat-conductive composite material containing inorganic conductive particle.
Background technology
Polyethylene (PE) is the insulating polymeric material that a kind of light weight is nontoxic, and it has remarkable electrical insulating property and dielectric properties, lower temperature resistance, enough mechanical properties thus applied widely.But poly shortcoming also clearly, its thermal conductivity is little only has 0.28 ~ 0.44W/mK, use temperature narrow range.The thermal conductivity of metal and oxide compound thereof is comparatively large, be generally 100 times of macromolecular material and more than, so it can be used as heat conductive filler to be filled in macromolecular material can improve its thermal conductivity.Prepare heat-conduction electric insulation polyethylene and can give full play to the intrinsic excellent electrical properties of polyethylene and the higher thermal conductivity of matrix material, this kind of material, except for except the insulating radiation of electron device under the lower occasion of some thermotolerances, encapsulation and other special purposes, also can be used for the radiating requirements of nonisulated occasion.
Summary of the invention
The present invention seeks to, in order to solve the low technical problem of polyethylene thermal conductivity, to provide the preparation method of a kind of nano ferriferrous oxide/polyethylene heat-conductive composite material.
The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material is as follows:
One, get Z 250 and polyethylene is placed in alcohol and is uniformly mixed, obtain suspension liquid, in suspension liquid, Z 250 and poly mass ratio are 1% ~ 30%;
Two, pour in hydrothermal synthesis reaction still by step one gained suspension liquid, packing ratio is 70 ~ 85%, is to be incubated 1 ~ 24h under the condition of 100 ~ 130 DEG C in temperature;
Three, from hydrothermal synthesis reaction still, pour out suspension liquid, filter, dry 1 ~ 12h at 50 DEG C, obtain mixed powder;
Four, the mixed powder in step 3 being placed in mould is placed on vulcanizing press, pressure be 0 ~ 10MPa, under molding temperature is the condition of 110 ~ 130 DEG C, 5min ~ 35min is hot-forming in pressurization, is cooled to room temperature, obtains heat-conductive composite material;
Five, step 4 gained heat-conductive composite material is 110 ~ 130 DEG C in Heating temperature, adds under magnetoelectricity stream is the condition of 10 ~ 16A and add magnetic treatment 30min, be then cooled to 15 ~ 60 DEG C, obtain nano ferriferrous oxide/polyethylene heat-conductive composite material.
Because poly density is less than 1, the density of Z 250 is greater than 1, and during application immersion method, polyethylene can float on the water face, and Z 250 can sink to the bottom, and therefore Z 250 just can not be even in polyethylene surface growth.The hot method of selective solvent of the present invention, alcohol selected by solvent, because alcohol density is less than polyethylene and Z 250, Z 250 homoepitaxial can be made like this at polyethylene surface.When adding magnetic treatment to Z 250/polyethylene heat-conductive composite material, its passage of heat can be made more easily to be formed, and the capacity of heat transmission improves further.
Nano ferriferrous oxide in the present invention/polyethylene heat-conductive composite material preparation method, for metal oxide/composite polyethylene material provides a kind of new complex method, the Z 250 produced is made to be coated in polyethylene surface by solution synthesis method, and magnetic treatment is added to its matrix material, preparation technology and required equipment simple, with low cost, easily implement.Prepare nanoparticle dispersion in gained nano ferriferrous oxide/composite polyethylene material even, Z 250 significantly improves the poly capacity of heat transmission, particularly adds the matrix material after magnetic treatment.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the nano ferriferrous oxide/polyethylene heat-conductive composite material of preparation in experiment one, in figure ◆ represent polyethylene, ● represent Z 250;
Fig. 2 is the thermal conductivity curve comparison figure of heat-conductive composite material that in experiment one prepared by step 4 and nano ferriferrous oxide/polyethylene heat-conductive composite material, the thermal conductivity curve of 1 expression nano ferriferrous oxide/polyethylene heat-conductive composite material in figure, 2 represent heat-conductive composite material thermal conductivity curve prepared by step 4;
Fig. 3 is the schematic flow sheet that in experiment one, step 3 prepares mixed powder.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment nano ferriferrous oxide/polyethylene heat-conductive composite material is as follows:
One, get Z 250 and polyethylene is placed in alcohol and is uniformly mixed, obtain suspension liquid, in suspension liquid, Z 250 and poly mass ratio are 1% ~ 30%;
Two, pour in hydrothermal synthesis reaction still by step one gained suspension liquid, packing ratio is 70 ~ 85%, is to be incubated 1 ~ 24h under the condition of 100 ~ 130 DEG C in temperature;
Three, from hydrothermal synthesis reaction still, pour out suspension liquid, filter, dry 1 ~ 12h at 50 DEG C, obtain mixed powder;
Four, the mixed powder in step 3 being placed in mould is placed on vulcanizing press, pressure be 0 ~ 10MPa, under molding temperature is the condition of 110 ~ 130 DEG C, 5min ~ 35min is hot-forming in pressurization, is cooled to room temperature, obtains heat-conductive composite material;
Five, step 4 gained heat-conductive composite material is 110 ~ 130 DEG C in Heating temperature, adds under magnetoelectricity stream is the condition of 10 ~ 16A and add magnetic treatment 30min, be then cooled to 15 ~ 60 DEG C, obtain nano ferriferrous oxide/polyethylene heat-conductive composite material.
Embodiment two: present embodiment and embodiment one are 1% unlike the Z 250 described in step one and poly mass ratio.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two are 5% unlike the Z 250 described in step one and poly mass ratio.Other is identical with one of embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are 10% unlike the Z 250 described in step one and poly mass ratio.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four are 110 DEG C unlike temperature in hydrothermal synthesis reaction still in step 2, insulation 4h.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are 120 DEG C unlike temperature in hydrothermal synthesis reaction still in step 2, insulation 6h.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are 130 DEG C unlike temperature in hydrothermal synthesis reaction still in step 2, insulation 8h.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven pour out suspension liquid unlike in step 3 from water heating kettle, filters, and under the condition of 60 DEG C, dries 12h.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight are 120 DEG C unlike molding temperature in step 4, be 0MPa hot pressing 5min at vulcanizing press pressure, be 5MPa hot pressing 5min at vulcanizing press pressure, being 10MPa hot pressing 5min at vulcanizing press pressure, is 15MPa hot pressing 5min at vulcanizing press pressure.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine are unlike in step 5, gained heat-conductive composite material in step 4 being placed in the two yoke single tuning adjustable air gap electro-magnet of SBV, be heated to 130 DEG C, open electric current to start to add magnetic, add magnetoelectricity stream and be adjusted to 16A, heating is stopped after insulation 30min, after temperature is down to 60 DEG C, close current.Other is identical with one of embodiment one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material, realizes according to the following steps:
One, get Z 250 and polyethylene is placed in alcohol and is uniformly mixed, in suspension liquid, Z 250 and poly mass ratio are 15%.
Two, pour in hydrothermal synthesis reaction still by step one gained suspension liquid liquid, packing ratio is 80%, and temperature is 110 DEG C, insulation 4h.
Three, from water heating kettle, pour out suspension liquid, after filtration, and at 50 DEG C, dry 12h, obtain mixed powder.
Four, be put in vulcanizing press by mixed powder, on vulcanizing press, molding temperature is 120 DEG C, with 0MPa pressurization 5min, with 5MPa pressurization 5min, with 10MPa pressurization 5min, hot-forming with 15MPa pressurization 5min, be finally cooled to room temperature and obtain heat-conductive composite material.
Five, the heat-conductive composite material of step 4 is placed in the two yoke single tuning adjustable air gap electro-magnet of SBV, be heated to 130 DEG C, open electric current to start to add magnetic, add magnetoelectricity stream and be adjusted to 16A, heating is stopped after insulation 30min, after temperature is down to 60 DEG C, close current, obtains nano ferriferrous oxide/polyethylene heat-conductive composite material.
The massfraction of the Z 250 in this experiment in gained nano ferriferrous oxide/polyethylene heat-conductive composite material is 15%.
To prepare in nano ferriferrous oxide/polyethylene heat conduction composite granule process Z 250 and polyethylene powders under mechanical stirring, Z 250 can be bonded at polyethylene surface, in water heating kettle High Temperature High Pressure condition under, Z 250 crystal can grow and be coated in polyethylene surface.Fig. 1 to be Z 250 amount mark be 15% XRD figure spectrum adding the matrix material after magnetic.Characterize matrix material by the test of LFA447 laser heat conducting instrument and record thermal conductivity, the nano ferriferrous oxide/polyethylene heat-conductive composite material thermal conductivity of 15% massfraction after solvent thermal adds magnetic increases 30.16% than pure poly thermal conductivity.Nano ferriferrous oxide coating polyethylene is obtained and carries out adding the matrix material after magnetic treatment that there is good heat conductivility by above data.
Claims (10)
1. the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material, is characterized in that the preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material is as follows:
One, get Z 250 and polyethylene is placed in alcohol and is uniformly mixed, obtain suspension liquid, in suspension liquid, Z 250 and poly mass ratio are 1% ~ 30%;
Two, pour in hydrothermal synthesis reaction still by step one gained suspension liquid, packing ratio is 70 ~ 85%, is to be incubated 1 ~ 24h under the condition of 100 ~ 130 DEG C in temperature;
Three, from hydrothermal synthesis reaction still, pour out suspension liquid, filter, dry 1 ~ 12h at 50 DEG C, obtain mixed powder;
Four, the mixed powder in step 3 being placed in mould is placed on vulcanizing press, pressure be 0 ~ 10MPa, under molding temperature is the condition of 110 ~ 130 DEG C, 5min ~ 35min is hot-forming in pressurization, is cooled to room temperature, obtains heat-conductive composite material;
Five, step 4 gained heat-conductive composite material is 110 ~ 130 DEG C in Heating temperature, adds under magnetoelectricity stream is the condition of 10 ~ 16A and add magnetic treatment 30min, be then cooled to 15 ~ 60 DEG C, obtain 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, is characterized in that Z 250 described in step one and poly mass ratio are 1%.
3. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, is characterized in that Z 250 described in step one and poly mass ratio are 5%.
4. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, is characterized in that Z 250 described in step one and poly mass ratio are 10%.
5. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, is characterized in that in step 2, in hydrothermal synthesis reaction still, temperature is 110 DEG C, insulation 4h.
6. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, is characterized in that in step 2, in hydrothermal synthesis reaction still, temperature is 120 DEG C, insulation 6h.
7. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, is characterized in that in step 2, in hydrothermal synthesis reaction still, temperature is 130 DEG C, insulation 8h.
8. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, is characterized in that from water heating kettle, pouring out suspension liquid in step 3, filters, and under the condition of 60 DEG C, dries 12h.
9. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, it is characterized in that in step 4, molding temperature is 120 DEG C, be 0MPa hot pressing 5min at vulcanizing press pressure, be 5MPa hot pressing 5min at vulcanizing press pressure, being 10MPa hot pressing 5min at vulcanizing press pressure, is 15MPa hot pressing 5min at vulcanizing press pressure.
10. the preparation method of nano ferriferrous oxide described in 1/polyethylene heat-conductive composite material as requested, it is characterized in that in step 5, gained heat-conductive composite material in step 4 being placed in the two yoke single tuning adjustable air gap electro-magnet of SBV, be heated to 130 DEG C, open electric current to start to add magnetic, add magnetoelectricity stream and be adjusted to 16A, heating is stopped after insulation 30min, after temperature is down to 60 DEG C, close current.
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| CN201510350026.3A CN105017604B (en) | 2015-06-23 | 2015-06-23 | The preparation method of nano ferriferrous oxide/polyethylene heat-conductive composite material |
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Cited By (1)
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| CN106085318A (en) * | 2016-06-03 | 2016-11-09 | 安徽福源光电科技有限公司 | A kind of composite epoxy casting glue of LED display magnetic heat radiation |
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