KR20170091411A - Method for manufacturing the circular-type ceramic insulation composite filler added h-BN nano-plate and the thermally conductive composition including the circular-type ceramic insulation composite filler - Google Patents
Method for manufacturing the circular-type ceramic insulation composite filler added h-BN nano-plate and the thermally conductive composition including the circular-type ceramic insulation composite filler Download PDFInfo
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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Abstract
The present invention relates to a method for producing a spherical ceramic insulated composite filler to which an h-BN nanoplate is added, a ceramic insulated composite filler and a thermally conductive composition comprising the insulated composite filler. More particularly, A step of preparing a slurry of a plate-like h-BN insulating filler into an h-BN nano-plate having a thickness of several hundred nano by peeling off a mixture of insulating fillers using mechanical milling; (2) feeding the slurry and the solvent of the step (1) to a ball mill and forming a slurry by ball milling at 100 to 200 rpm; (3) spraying the slurry of step (2) into a hot air drier and spray-drying it at a rotating speed of 5,000 ~ 18,000 rpm in a drying furnace under the condition of temperature of 230 ± 20 ° C, 4) Sieving the granules obtained in step 3) to obtain spherical ceramic insulated composite filler with h-BN nanoplate having an average particle size of 45 to 250 탆 and preparing h-BN nanoplate-added spherical ceramic insulated composite filler A ceramic-insulated composite filler produced thereby, and a thermally conductive composition comprising the ceramic-insulated composite filler.
Description
TECHNICAL FIELD The present invention relates to a method for manufacturing a spherical ceramic insulated composite filler with h-BN nanoplate, a ceramic insulated composite filler and a thermally conductive composition including the insulated composite filler, and more particularly, A plate-shaped h-BN insulating filler having a thickness of 5 mu m was peel off from a h-BN nanoplate having a thickness of several hundred nanometers, and the prepared h-BN nanoplate was sprayed with a ceramic filler or a single composition The present invention relates to a method for producing a high thermal conductive spherical ceramic insulating composite filler by granulating it into a spherical insulating composite filler using a spray drying method and a heat conductive composition comprising the insulating composite filler and the insulating composite filler.
In recent years, electronic devices used in automobiles, electric / electronic fields, etc. have been pursued to be lightweight, thin, miniaturized and multifunctional. As these electronic devices are highly integrated, more heat is generated. Malfunction of the device, deterioration of the substrate, and the like.
From the viewpoint of the material of the thermally conductive filler in the thermally conductive epoxy composite material, the metal particles and the like are effective for improving the thermal conductivity but are not used as the thermally conductive filler since they have no electric insulation property. A material having electric insulation is mainly used. A thermal pathway must be made in which the thermally conductive fillers are in direct contact within the polymer matrix, and more specifically, the thermally conductive filler should be arranged at a desired location. In order to obtain optimal thermal conductivity, it is necessary to develop a thermally conductive polymer composite material having excellent heat radiation performance by constructing a thermal pathway of a thermally conductive filler in a polymer matrix of an epoxy composite material.
The inventors of the present invention used the excellent heat transfer characteristics of the BN nanoplate as a bridge between the plate-like h-BN fillers in constructing the thermal pathway of the thermally conductive filler in the polymer matrix of the epoxy composite material, And a method for manufacturing a spherical ceramic insulated composite filler to which an h-BN nanoplate is added with improved thermal conductivity.
Another object of the present invention is to provide a high thermal conductive ceramic insulating composite filler having improved thermal conductivity compared to a conventional plate-like filler, and on the other hand, a manufacturing method capable of reducing production cost while ensuring high thermal conductivity .
The inventors of the present invention focused on the fact that a spherical powder having certain particles can be processed by using the spray drying method, and thus it is possible to produce a spherical high thermal conductive ceramic insulating composite filler by applying the spray drying method The present invention has been accomplished in view of the fact that when the high thermal conductive ceramic insulated composite filler is manufactured into a spherical shape, it is advantageous to catch the phenomenon that powder is blown in the process of extrusion or injection.
A method for manufacturing a spherical ceramic insulated composite filler with h-BN nanoplate according to the present invention, which solves the above problems,
(1) a slurry preparation step in which a mixture of a solvent and a plate-like h-BN insulating filler is peel off by mechanical milling to obtain a plate-like h-BN insulating filler into an h-BN nanoplate having hundreds of nano thickness;
(2) feeding the slurry and the solvent of the step (1) to a ball mill and forming a slurry by ball milling at 100 to 200 rpm;
(3) spraying the slurry of step (2) into a hot air drier and spray-drying it at a rotating speed of 5,000 ~ 18,000 rpm in a drying furnace under the condition of temperature of 230 ± 20 ° C,
(4) Sieving the granules obtained in the step (3) to obtain a spherical ceramic insulating composite filler having an average particle size of 45 to 250 μm with the h-BN nanoplate added thereto.
Here, the step (1) is mechanically milled using a basket mill, and a plate-like h-BN insulating filler having a bead size of 0.1 to 0.5 mm is introduced into a basket, and the h- At a speed of 1 to 3 hours.
In the step (2), any one of the fillers selected from the group consisting of aluminum nitride (AlN), aluminum oxide (Al2O3), magnesium oxide (MgO) 20 to 80: 80 to 20, and a solvent is supplied to the mixture to form a mixed slurry by ball milling at 100 to 200 rpm.
Further, in the present invention is produced by the method disclosed above, the average particle size of 45 ~ 250㎛, thermal conductivity 4 ~ 15W / mK, an apparent density of 0.9 ~ 1.7g / cm 3, the breakdown voltage strength of 8 ~ 10kV / mm The present invention provides a spherical ceramic insulated composite filler to which an h-BN nanoplate is added.
The h-BN nanoplate-added spherical ceramic insulated composite filler according to the present invention is simple and economical and has an average particle size of 45 to 250 μm, a horizontal thermal conductivity of 17 to 28 W / mK, an apparent density of 0.9 to 1.7 g / cm < 3 >, an insulation breakdown voltage strength of 4 to 12 kVDC / mm and an improved thermal conductivity, h-BN nanoplate-added spherical ceramic insulating composite filler.
In addition, the present invention can provide a thermally conductive composition containing a spherical filler having improved thermal conductivity compared to a conventional flake-shaped filler.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a block diagram showing an example of a method for manufacturing a spherical ceramic insulated composite filler with h-BN nanoplate according to the present invention.
2 shows a process of a basket mill used in the production method of the present invention.
FIG. 3 is a SEM photograph showing a microstructure of the plate-shaped BN filler according to an embodiment of the present invention with respect to the peel-off process time.
FIG. 4 is a graph showing the results of a horizontal thermal conductivity test using a spherical ceramic insulated composite filler manufactured according to the peel off process time of the plate BN filler according to an embodiment of the present invention, It is a SEM photograph.
BRIEF DESCRIPTION OF THE DRAWINGS The present invention will be described in more detail with reference to the accompanying drawings.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a block diagram showing an example of a method for producing a spherical ceramic insulated composite filler with h-BN nanoplate according to the present invention.
The present invention relates to a method for manufacturing a spherical ceramic insulated composite filler with an h-BN nanoplate and a ceramic insulated composite filler using the same. More particularly, the present invention relates to a ceramic insulated composite filler comprising h- Was peel-off with h-BN nanoplates having hundreds of nano-thickness, and granulated with a ceramic filler or a single composition into an insulating composite filler using a spray drying method to form a high thermal conductive spherical ceramic A method of manufacturing an insulating composite filler, which will be described in more detail with reference to FIG. 1,
(1) a slurry preparation step in which a mixture of a solvent and a plate-like h-BN insulating filler is peel off by mechanical milling to obtain a plate-like h-BN insulating filler into an h-BN nanoplate having hundreds of nano thickness;
(2) feeding the slurry and the solvent of the step (1) to a ball mill and forming a slurry by ball milling at 100 to 200 rpm;
(3) spraying the slurry of step (2) into a hot air drier and spray-drying it at a rotating speed of 5,000 ~ 18,000 rpm in a drying furnace under the condition of temperature of 230 ± 20 ° C,
(4) Sieving the granules obtained in the step (3) to obtain a spherical ceramic insulated composite filler having an average particle size of 45 to 250 탆 and containing h-BN nanoplate.
According to the present invention, the first step is a mechanical milling using a basket mill. As shown in FIG. 2, a plate-like h-BN insulating filler having a thickness of 1 to 5 m is placed in a basket container, And is then subjected to a basket milling operation for 1 to 3 hours at a speed of 1,000 to 3,000 rpm in a container filled with a solvent.
In detail, the
At this time, any solvent selected from among MEK, ethanol and acetone is used as the solvent. Preferably, the amount of the h-BN insulating filler to be loaded on the plate is 50 to 80% by weight based on the total weight of the solvent, and the basket milling operation is performed. If the amount is out of the critical range, sufficient milling effect can not be obtained. If the required amount is less than 50 wt%, the milling effect will be excessive during 1 to 3 hours of basket milling, so that the h- There is a problem that a phenomenon of damage is exhibited and a phenomenon in which the milling effect is weak when the content is more than 80% by weight does not cause a feel off.
After the basket mill is finished, the resulting h-BN nanoplate has a thickness of 50 to 800 nm. Preferably, the h-BN nanoplate is manufactured to have a thickness of 200 to 500 nm.
The basket mill is a gaiter mill in which beads are held in a container called a basket and a bead by a pin is strongly impacted to obtain a shearing force necessary for dispersion, , And it has an advantage of obtaining a BN nanoplate having a size of 100 to 500 nm because it has a good product recovery rate and has a uniform dispersion distribution and a fast time to reach a required particle size when using a dispersant and can be used in a relatively high viscosity. It is a mechanical milling device.
According to the present invention, any one of the fillers selected from the group consisting of aluminum nitride (AlN), aluminum oxide (Al 2 O 3), magnesium oxide (MgO) filler, : The filler is added in a weight ratio of 20 to 80:80 to 20, and a solvent is supplied, and the mixture is ball milled at 100 to 200 rpm to form a mixed slurry.
According to the present invention, it is preferable that the ball mill is performed for 2 to 5 hours in the second step. This is because there is a disadvantage in that uniform mixing can not be attained when the time is less than 2 hours, and aluminum nitride (AlN), aluminum oxide (Al2O3) and magnesium oxide (MgO) fillers are broken when the time exceeds 5 hours .
The spray drying method according to one embodiment of the present invention can be carried out according to the method disclosed in Korean Patent Publication No. 10-1538379 invented by the inventors of the present invention.
The h-BN nanoplate-added spherical ceramic insulated composite filler according to the present invention produced by the method as described above has an average particle size of 45 to 250 탆, a thermal conductivity of 4 to 15 W / mK, an apparent density of 0.9 to 1.7 g / cm 3 and an insulation breakdown voltage of 8 to 10 kV / mm.
Hereinafter, the present invention will be described in more detail with reference to preferred embodiments. It should be understood, however, that there is no intention to limit the invention to the specific embodiments disclosed, but it is to be understood that the invention is not limited to the disclosed embodiments, but is capable of modifications within the scope of the invention.
[Examples 1 to 4]
The h-BN insulating filler powder (BYK-182 manufactured by BYK Co., Ltd.) was prepared, and the powder was placed in a basket container, immersed in a basket filled with ethanol as a solvent, and then the basket container was rotated at 1,000 to 3,000 rpm And then subjected to a basket mill peel-off process for 0, 1, 3 and 5 hours to prepare an h-BN nano-plate slurry having a thickness of 50 to 800 nm. The slurry was supplied to a ball mill with ethanol as a solvent and ball milled at 100 to 200 rpm for 2 to 5 hours to form a slurry. The slurry was sprayed into a hot air drier and spray- Spray-dried at a rotation speed of 18,000 rpm to granulate the spheres, and sieved to prepare spherical ceramic insulated composite filler with h-BN nanoplate having an average particle size of 45 to 250 μm.
The aspect ratio of the formed nano-plate was measured by analyzing the microstructure of the insulated composite filler manufactured as described above according to the peel off process time (0, 1, 2, 3, 5 hr). The results are shown in FIG. 3 and Table 1 Respectively. As a result, it was found that the thickness of the nano plate became thinner as the peel off process time increased.
(t, m)
As a result of the above Table 1, it can be seen that h-BN nanoplate having a thickness of 320 to 680 nm can be obtained by performing mechanical milling.
On the other hand, a horizontal thermally conductive test piece was produced by a usual method using a spherical ceramic insulated composite filler produced by the peel off process time of the plate-like BN filler obtained from the above embodiments, The structure was analyzed, and the results are shown in the SEM photograph shown in Fig. As a result of the microstructural analysis, the plate-like BN filler without peel-off process was found to have a horizontal thermal conductivity. On the fracture surface of the specimen, no nanoplate with a thickness of several hundred nanometers was found. As a result of peel off process with basket mill, The thickness of the plate was thinned and the amount of the nanoplate was increased.
It is another object of the present invention to provide an insulating filler having excellent thermal conductivity and breakdown voltage strength by making an h-BN insulating filler into an h-BN nanoplate to produce an insulating filler. The horizontal thermal conductivity of the h-BN nanoplate insulating filler obtained from 4 to 4 was compared with that of the horizontal thermal conductivity test specimen using commercial plate h-BN filler. . The comparative sample was prepared and compared with a horizontal thermal conductivity test piece using a conventional flake type filler. The results are shown in Table 2 below.
Process time (hr)
(W / mK)
(kV / mm)
As a result of the above Table 3, it was found that the thermal conductivity of about 30% or more was improved in the peel off process time of 1 hour and 3 hours, and that the 5 hours result was improved than that of the conventionally used flake type But it was lower than 1 hour and 3 hours treatment. The reason for this is that as the time after 3 hours is increased, the thickness of the BN nanoplate becomes thinner and the amount thereof increases, but the plate-like h-BN filler and BN nanoplate particles are judged to be damaged. Accordingly, as shown in Table 2, it can be seen that the optimum process time of the peel-off process is within 1 to 3 hours, and that the improvement in the horizontal thermal conductivity is excellent, and the process time can be shortened considerably.
[Examples 5 to 13]
A basket mill peel-off process was performed in Example 2 to prepare an h-BN nano-plate slurry A0 having a thickness of 400 to 650 nm. Then, the slurry and the AlN filler A1, the Al2O3 filler A2, MgO filler (A3), followed by ball milling. Thereafter, a mixed slurry was prepared, and the subsequent steps were carried out under the same conditions to obtain a spherical ceramic insulation with an h-BN nanoplate having an average particle size of 45 to 250 mu m Composite fillers were prepared and horizontal thermal conductivity test specimens were prepared using the insulated composite filler. The horizontal thermal conductivity and dielectric breakdown voltage were measured. The mixing conditions and the measurement results are shown in Table 3 below .
(W / mK)
(kV / mm)
As a result of the above Table 3, it can be seen that the horizontal thermal conductivity and the breakdown voltage strength are lowered compared with the case where the h-BN nanoplate is used alone to produce a filler. Nevertheless, it was confirmed that the material has a very good physical property value compared to the conventional flake type insulating filler. In this case, the h-BN nanoplate alone can provide a more excellent insulating filler, but it has a disadvantage in that the unit price is very high. Therefore, relatively low-cost Aln, MgO, Al2O3 fillers are used It is possible to provide a filler having a very high thermal conductivity while dramatically reducing the production cost thereof.
Meanwhile, in the embodiments described above, the horizontal thermal conductivity and the dielectric breakdown voltage strength are measured as follows.
1. Horizontal Thermal Conductivity Measurement Method
- Test items: Horizontal thermal conductivity measurement at room temperature
- Test specification: Thermal diffusivity / ASTM E-1461
Specific heat / ASTM E-1269
- Test conditions: Measuring temperature: 25 ℃ (- + 1 ℃)
Measuring atmosphere: N2 (high purity) 60 ml / min
Sample holder: Ф 25.4mm inplane holder
Measuring method: Vertical direction thermal conductivity measurement
- Test equipment: Thermal conductivity measurement: LFA 467, DSC 200 F3
- Horizontal thermal conductivity The density (the apparent density using the Archimedes method) and the thermal diffusivity measured by LFA 467 multiplied by the specific heat measured by DSC 200 F3 are the horizontal thermal conductivity values.
2. Measurement of dielectric breakdown voltage strength
- Measured using withstand voltage meter.
- Bond the specimen (Ф25.2mm X t 1mm) with the withstanding voltage measuring jig.
- Measure the kV value at which insulation breaks up by rising from 0kV to 12kV at regular intervals.
- Determine the breakdown voltage strength value (kV / mm) by dividing the breakdown kV value by the specimen thickness.
10: outer container
20: plate h-BN insulation filler
30: Basket container
40: Solvent
Claims (5)
(2) feeding the slurry and the solvent of the step (1) to a ball mill and forming a slurry by ball milling at 100 to 200 rpm;
(3) spraying the slurry of step (2) into a hot air drier and spray-drying it at a rotating speed of 5,000 ~ 18,000 rpm in a drying furnace under the condition of temperature of 230 ± 20 ° C,
(4) sieving the granules obtained in the step (3) to obtain a spherical ceramic insulated composite filler with an h-BN nanoplate having an average particle size of 45 to 250 탆, wherein the h-BN nanoplate- Method of making composite filler.
The step (1) is mechanically milled using a basket mill, and a plate-like h-BN insulating filler having a bead size of 0.1 to 0.5 mm is introduced into a basket container. The h-BN insulating filler is poured into a container filled with a solvent at a speed of 1,000 to 3,000 rpm Wherein the filler is peeled off by a basket milling operation for 1 to 3 hours to form the h-BN nanoplate.
In the step (2), any one of the fillers selected from the group consisting of aluminum nitride (AlN), aluminum oxide (Al2O3), magnesium oxide (MgO) Wherein the mixed slurry is added at a weight ratio of 80: 80 to 20, and the mixed slurry is formed by supplying a solvent and ball milling at 100 to 200 rpm to produce the spherical ceramic insulating composite filler.
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