CN115974011A - Spherical hexagonal boron nitride and preparation method thereof - Google Patents
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- CN115974011A CN115974011A CN202211661325.5A CN202211661325A CN115974011A CN 115974011 A CN115974011 A CN 115974011A CN 202211661325 A CN202211661325 A CN 202211661325A CN 115974011 A CN115974011 A CN 115974011A
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 132
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 239000012798 spherical particle Substances 0.000 claims abstract description 46
- 239000002002 slurry Substances 0.000 claims abstract description 37
- 239000011164 primary particle Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000005469 granulation Methods 0.000 claims abstract description 18
- 230000003179 granulation Effects 0.000 claims abstract description 18
- 239000007921 spray Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 241000446313 Lamella Species 0.000 claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000002776 aggregation Effects 0.000 claims description 8
- 238000004220 aggregation Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- -1 polyoxyethylenes Polymers 0.000 claims description 3
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 6
- 239000003292 glue Substances 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004931 aggregating effect Effects 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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Abstract
The application discloses spherical hexagonal boron nitride and a preparation method thereof, which belong to the technical field of boron nitride materials, the preparation method comprises the steps of preparing slurry with the viscosity of 55 to 85ku from hexagonal boron nitride, auxiliary materials and pure water, then carrying out spray granulation on the slurry to obtain spherical particles, wherein the spherical particles are formed by gathering primary hexagonal boron nitride particles in a continuous bridging and overlapping mode, the primary hexagonal boron nitride particles are in a contact state of a prism surface and a plane, and finally fixing the bridging, overlapping and gathering mode of boron nitride lamella crystals through glue discharge and sintering to obtain the spherical hexagonal boron nitride. The primary particles of the spherical hexagonal boron nitride are in a state of mutual contact between a plane and a ridge surface, a continuous heat conduction channel is easy to form, and 40% of the spherical hexagonal boron nitride is mixed with 60% of silicone oil, the viscosity is 30 to 75 ten thousand mPa.s, the heat conductivity is 2 to 4W/m.K, and the spherical hexagonal boron nitride can be widely applied to the field of heat conduction.
Description
Technical Field
The invention relates to the technical field of boron nitride materials, in particular to spherical hexagonal boron nitride and a preparation method thereof.
Background
Hexagonal boron nitride has thermal conductivity anisotropy, and its thermal conductivity in plane is several tens times that perpendicular to the in-plane direction. When hexagonal boron nitride is applied to a heat conducting system, the hexagonal boron nitride easily generates orientation due to its layered structure when dispersed in the system, thereby causing anisotropy in heat conduction of the heat conducting system.
When the hexagonal boron nitride is filled in a heat-conducting system in a large amount, the viscosity of the system is greatly increased, and the application of the hexagonal boron nitride is severely limited. Research shows that the inorganic filler with large length-diameter ratio increases the viscosity of an application system because the inorganic filler is easy to be intertwined with each other. The length-diameter ratio of the hexagonal flaky boron nitride is far larger than that of the spherical hexagonal boron nitride, so that the problem that the flaky hexagonal boron nitride is anisotropic in heat conduction in a heat-conducting matrix material and difficult to fill in a large amount can be remarkably solved by preparing the hexagonal flaky boron nitride into a spherical shape. In the prior art, a patent of 'a method for preparing spherical hexagonal boron nitride agglomerates' produces spherical hexagonal boron nitride agglomerates, which show isotropic heat conduction, but the boron nitride primary particles are directly accumulated between planes, and when the agglomerates are used as a heat-conducting filler, the heat conductivity is low.
Disclosure of Invention
Based on the above, the application provides spherical hexagonal boron nitride and a preparation method thereof, the preparation method comprises the steps of preparing hexagonal boron nitride, auxiliary materials and water into slurry with the viscosity of 55 to 85ku, carrying out spray granulation on the slurry to obtain spherical particles, wherein the spherical particles are formed by aggregating hexagonal boron nitride primary particles in a continuous bridging lap joint mode, the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane, and fixing the bridging lap joint aggregation mode of boron nitride lamella crystals by glue discharge and sintering to obtain the spherical hexagonal boron nitride. The primary particles of the spherical hexagonal boron nitride are in a state of mutual contact of planes and edge surfaces, a continuous heat conduction channel is easy to form, and 40% of the spherical hexagonal boron nitride is mixed with 60% of silicone oil, the viscosity is 30-75 ten thousand mPa.s, and the heat conductivity is 2-4W/m.K.
The technical scheme adopted by the invention is as follows:
the spherical hexagonal boron nitride is formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane; wherein 40% of spherical hexagonal boron nitride is mixed with 60% of silicone oil, the viscosity is 30-75 ten thousand mPa.s, and the thermal conductivity is 2-4W/m.K.
Further, the D50 of the spherical hexagonal boron nitride is 60-200 μm.
Based on the same inventive concept, the application also discloses a preparation method of the spherical hexagonal boron nitride, and particularly,
the preparation method of the spherical hexagonal boron nitride comprises the following steps:
s1, preparing slurry with the viscosity of 55 to 85ku by using hexagonal boron nitride, auxiliary materials and pure water;
s2, conveying the slurry into a spray granulation tower, and performing centrifugal spraying and drying to obtain spherical particles; the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane;
s3, conveying the spherical particles into a muffle furnace, introducing air, and heating to 600 to 750 ℃ to fully decompose organic matters in the spherical particles;
and S4, sending the spherical particles into a sintering furnace, introducing inert gas for protection, heating to 1700-2000 ℃ for sintering, and fixing the bridging lap joint aggregation mode of the boron nitride lamella crystals to obtain the spherical hexagonal boron nitride.
The application finds that when the viscosity of the slurry is controlled to be 55 to 85ku, spherical particles with hexagonal boron nitride primary particles in a contact state of a prism surface and a plane can be obtained through spray granulation, and the spherical particles have better heat conductivity than spherical boron nitride aggregates stacked in a contact state of a plane and a plane.
In the preparation method of the present application, in the step S1, the auxiliary materials include a binder, a dispersant and a sintering aid.
In the preparation method of the present application, the binder is PVA or acrylic resin;
the dispersing agent is a polymer containing quaternary ammonium groups, polyoxyethylenes or polyamides;
the sintering aid is one or more of calcium oxide, yttrium oxide, calcium fluoride, magnesium oxide, silicon dioxide and aluminum oxide.
In the preparation method, in the step S1, the mass ratio of the hexagonal boron nitride to the auxiliary material is 3 to 10.
In the preparation method of the present application, in the step S1, a specific preparation method of the slurry is: stirring pure water, hexagonal boron nitride and an auxiliary material for 1 to 3 hours at the rotating speed of 300 to 1000rpm to uniformly disperse the material; sampling and testing the viscosity of the slurry in the stirring kettle, and controlling the viscosity of the slurry to be 55 to 85ku.
In the preparation method, in the step S2, the temperature difference of the drying gas at the inlet and the outlet of the spray granulation tower is 120 to 150 ℃.
In the preparation method of the present application, in the step S4, the sintering manner is: firstly, vacuumizing to be below 100Pa under the greenhouse condition, and then continuously introducing inert gas to reach the standard atmospheric pressure of +15kPa; the temperature is programmed to 1700 to 2000 ℃ from the room temperature at the speed of 10 to 15 ℃/min, and the temperature is kept for 2 to 6 hours.
In the production method of the present application, the inert gas is nitrogen.
The invention has the beneficial effects that:
the invention provides spherical hexagonal boron nitride and a preparation method thereof, the preparation method comprises the steps of preparing slurry with the viscosity of 55-85ku from hexagonal boron nitride, auxiliary materials and pure water, carrying out spray granulation on the slurry to obtain spherical particles, wherein the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging and overlapping mode, the hexagonal boron nitride primary particles are in a state that prism surfaces are in contact with planes to form a continuous heat conduction channel, and fixing the bridging, overlapping and gathering mode of boron nitride platelets through binder removal and sintering to obtain the spherical hexagonal boron nitride. The D50 of the spherical hexagonal boron nitride is 60 to 200 mu m; mixing 40% of spherical hexagonal boron nitride with 60% of silicone oil, and performing viscosity and thermal conductivity tests to find that the viscosity is 30-75 ten thousand mPa.s, the thermal conductivity is 2-4W/m.K, and the composite material can be widely used in the field of heat conduction.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a first SEM image of spherical hexagonal boron nitride according to example 1 of the present application;
FIG. 2 is a scanning electron micrograph of spherical hexagonal boron nitride according to example 1 of the present application;
fig. 3 is a scanning electron microscope photograph iii of spherical hexagonal boron nitride according to example 1 of the present application.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present application more comprehensible, embodiments accompanying the present application are described in detail below with reference to the accompanying drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the application and are not limiting of the application. It should be further noted that, for the convenience of description, only some of the structures related to the present application are shown in the drawings, not all of the structures. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The terms "including" and "having," as well as any variations thereof, in this application are intended to cover a non-exclusive inclusion. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Reference in the specification to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the specification. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
The application discloses spherical hexagonal boron nitride and a preparation method thereof, wherein the preparation method of the spherical hexagonal boron nitride comprises the following steps:
s1, preparing slurry with the viscosity of 55 to 85ku by using hexagonal boron nitride, auxiliary materials and pure water;
s2, conveying the slurry into a spray granulation tower, and performing centrifugal spraying and drying to obtain spherical particles; the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane;
s3, conveying the spherical particles into a muffle furnace, introducing air, heating to 600-750 ℃, and fully decomposing organic matters in the spherical particles;
and S4, sending the spherical particles into a sintering furnace, introducing inert gas for protection, heating to 1700-2000 ℃ for sintering, and fixing the bridging lap joint aggregation mode of the boron nitride lamella crystals to obtain the spherical hexagonal boron nitride.
According to the method, hexagonal boron nitride, auxiliary materials and pure water are prepared into slurry with the viscosity of 55 to 85ku, the slurry is subjected to spray granulation to obtain spherical particles, the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, the hexagonal boron nitride primary particles are in a state that edges and planes are in contact, and then the bridging lap joint gathering mode of boron nitride platelets is fixed through glue discharge and sintering to obtain the spherical hexagonal boron nitride.
The D50 of the spherical hexagonal boron nitride is 60-200 mu m; mixing 40% of spherical hexagonal boron nitride with 60% of silicone oil, and testing viscosity and thermal conductivity, wherein the viscosity is 30 to 75 ten thousand mPa.s, the thermal conductivity is 2 to 4W/m.K, and the spherical hexagonal boron nitride can be widely applied to the field of heat conduction.
The present application found that when the viscosity of the slurry was controlled to 55 to 85ku, spherical particles in which hexagonal boron nitride primary particles were in a state of contact between a prism surface and a plane were obtained by granulating the slurry, and the spherical particles exhibited isotropy in heat conduction, and since the thermal conductivity in the hexagonal boron nitride plane was several tens of times that in a direction perpendicular to the plane, the hexagonal boron nitride primary particles were in contact between a prism surface and a plane, and the spherical boron nitride aggregate stacked in contact between a plane and a plane had better thermal conductivity.
Specifically, in step S1, the auxiliary materials include a binder, a dispersant and a sintering aid.
The binder is PVA, acrylic resin or other water-based binders.
The dispersant is polymer containing quaternary ammonium group, polyoxyethylene, polyamide or other water dispersant.
The sintering aid is one or more of calcium oxide, yttrium oxide, calcium fluoride, magnesium oxide, silicon dioxide and aluminum oxide.
Specifically, in step S1, the specific preparation method of the slurry is: stirring pure water, hexagonal boron nitride and an auxiliary material for 1 to 3 hours at the rotating speed of 300 to 1000rpm to uniformly disperse the material; sampling and testing the viscosity of the slurry in the stirring kettle, and controlling the viscosity of the slurry to be 55 to 85ku.
Specifically, the temperature difference of the drying gas at the inlet and the outlet of the spray granulation tower is 120 to 150 ℃.
Specifically, in step S4, the sintering method is: firstly, vacuumizing to be below 100Pa under the greenhouse condition, and then continuously introducing nitrogen to reach the standard atmospheric pressure of +15kPa; the temperature is programmed to 1700 to 2000 ℃ from the room temperature at the speed of 10 to 15 ℃/min, and the temperature is kept for 2 to 6 hours.
Example 1
Firstly, stirring pure water, hexagonal boron nitride, PVA, polyoxyethylene ether and magnesium oxide for 3 hours at the rotating speed of 300rpm, and uniformly dispersing the materials; the viscosity of the slurry in the stirred tank was sampled and tested to maintain the viscosity of the slurry at 55ku. Feeding the slurry into a spray granulation tower, wherein the temperature difference of drying gas at an inlet and an outlet of the spray granulation tower is 120 ℃, and obtaining spherical particles through centrifugal spraying and drying; the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane; then sending the spherical particles into a muffle furnace, introducing air, heating to 600 ℃, and fully decomposing organic matters in the spherical particles; finally, the spherical particles are sent to a sintering furnace, firstly, the spherical particles are vacuumized to be below 100Pa under the greenhouse condition, and then, nitrogen is continuously introduced to the sintering furnace until the standard atmospheric pressure is plus 15kPa; and (3) carrying out temperature programming from room temperature to 1700 ℃ at the speed of 10 ℃/min, carrying out heat preservation for 6h, enabling the sintering aid to generate a liquid phase, and fixing the bridging lapping aggregation mode of the boron nitride lamella to obtain the spherical hexagonal boron nitride. The morphology of the spherical hexagonal boron nitride is shown in the accompanying drawings 1-3, the spherical hexagonal boron nitride is formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a state that prism surfaces and planes are in contact.
Example 2
Firstly, stirring pure water, hexagonal boron nitride, acrylic resin, polyamide and yttrium oxide for 2 hours at the rotating speed of 600rpm, and uniformly dispersing the materials; the slurry in the stirred tank was sampled and tested for viscosity so that the viscosity of the slurry was maintained at 70ku. Feeding the slurry into a spray granulation tower, wherein the temperature difference of drying gas at an inlet and an outlet of the spray granulation tower is 130 ℃, and obtaining spherical particles through centrifugal spraying and drying; the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane; then sending the spherical particles into a muffle furnace, introducing air, heating to 650 ℃, and fully decomposing organic matters in the spherical particles; finally, the spherical particles are sent to a sintering furnace, firstly, the spherical particles are vacuumized to be below 100Pa under the greenhouse condition, and then, nitrogen is continuously introduced to the sintering furnace until the standard atmospheric pressure is plus 15kPa; and (3) carrying out temperature programming from room temperature to 1900 ℃ at the speed of 10 ℃/min, carrying out heat preservation for 3h, enabling the sintering aid to generate a liquid phase, and fixing the bridging lapping aggregation mode of the boron nitride lamella to obtain the spherical hexagonal boron nitride.
Example 3
Firstly, stirring pure water, hexagonal boron nitride, PVA, polyoxyethylene ether, calcium oxide and silicon dioxide for 1h at the rotating speed of 1000rpm, and uniformly dispersing the materials; the slurry in the stirred tank was sampled and tested for viscosity so that the viscosity of the slurry was maintained at 85ku. Feeding the slurry into a spray granulation tower, wherein the temperature difference of drying gas at the inlet and the outlet of the spray granulation tower is 150 ℃, and obtaining spherical particles through centrifugal spraying and drying; the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane; then sending the spherical particles into a muffle furnace, introducing air, heating to 750 ℃, and fully decomposing organic matters in the spherical particles; finally, the spherical particles are sent to a sintering furnace, firstly, the spherical particles are vacuumized to be below 100Pa under the greenhouse condition, and then, nitrogen is continuously introduced to the sintering furnace until the standard atmospheric pressure is plus 15kPa; and (3) raising the temperature from room temperature to 2000 ℃ at a speed of 15 ℃/min by programming, keeping the temperature for 2h, generating a liquid phase by using the sintering aid, and fixing the bridged lapping aggregation mode of the boron nitride lamella to obtain the spherical hexagonal boron nitride.
Comparative example 1
The results of comparing hexagonal platelet boron nitride of different particle sizes with spherical hexagonal boron nitride of different particle sizes prepared herein are shown in table 1.
The preparation method comprises the steps of preparing slurry with the viscosity of 55 to 85ku from hexagonal boron nitride, auxiliary materials and pure water, carrying out spray granulation on the slurry to obtain spherical particles, aggregating primary hexagonal boron nitride particles in a continuous bridging lapping mode, forming a continuous heat conduction channel in a state that the primary hexagonal boron nitride particles are in a contact state of a prism surface and a plane, and fixing the bridging lapping aggregation mode of a boron nitride lamella crystal by degumming and sintering to obtain the spherical hexagonal boron nitride. The D50 of the spherical hexagonal boron nitride is 60 to 200 mu m; mixing 40% of spherical hexagonal boron nitride with 60% of silicone oil, and testing viscosity and thermal conductivity, wherein the viscosity is 30 to 75 ten thousand mPa.s, the thermal conductivity is 2 to 4W/m.K, and the spherical hexagonal boron nitride can be widely applied to the field of heat conduction.
The present invention has been described in terms of the preferred embodiment, and it is not intended to be limited to the embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The spherical hexagonal boron nitride is characterized in that the spherical hexagonal boron nitride is formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane; wherein, 40 percent of the spherical hexagonal boron nitride is mixed with 60 percent of silicone oil, the viscosity is 30 to 75 ten thousand mPa.s, and the thermal conductivity is 2 to 4W/m.K.
2. The spherical hexagonal boron nitride according to claim 1, wherein the spherical hexagonal boron nitride has a D50 of 60 to 200 μ ι η.
3. The method for preparing spherical hexagonal boron nitride according to claim 1, comprising the steps of:
s1, preparing slurry with the viscosity of 55 to 85ku by using hexagonal boron nitride, auxiliary materials and pure water;
s2, conveying the slurry into a spray granulation tower, and performing centrifugal spraying and drying to obtain spherical particles; the spherical particles are formed by gathering hexagonal boron nitride primary particles in a continuous bridging lap joint mode, and the hexagonal boron nitride primary particles are in a contact state of a prism surface and a plane;
s3, conveying the spherical particles into a muffle furnace, introducing air, heating to 600-750 ℃, and fully decomposing organic matters in the spherical particles;
and S4, sending the spherical particles into a sintering furnace, introducing inert gas for protection, heating to 1700-2000 ℃ for sintering, and fixing the bridging lap joint aggregation mode of the boron nitride lamella crystals to obtain the spherical hexagonal boron nitride.
4. The method for preparing spherical hexagonal boron nitride according to claim 3, wherein in step S1, the auxiliary materials comprise a binder, a dispersant and a sintering aid.
5. The method for preparing spherical hexagonal boron nitride according to claim 4, wherein the binder is PVA or acrylic resin;
the dispersing agent is a polymer containing quaternary ammonium groups, polyoxyethylenes or polyamides;
the sintering aid is one or more of calcium oxide, yttrium oxide, calcium fluoride, magnesium oxide, silicon dioxide and aluminum oxide.
6. The method for preparing spherical hexagonal boron nitride according to claim 3, wherein in the step S1, the mass ratio of hexagonal boron nitride to auxiliary materials is 3 to 10.
7. The method for preparing spherical hexagonal boron nitride according to claim 3, wherein in step S1, the slurry is prepared by the following specific method: stirring pure water, hexagonal boron nitride and an auxiliary material for 1 to 3 hours at the rotating speed of 300 to 1000rpm to uniformly disperse the material; and sampling and testing the viscosity of the slurry in the stirring kettle to control the viscosity of the slurry to be 55 to 85ku.
8. The method for preparing hexagonal spherical boron nitride according to claim 3, wherein in the step S2, the temperature difference of the drying gas at the inlet and outlet of the spray granulation tower is 120 to 150 ℃.
9. The method for preparing spherical hexagonal boron nitride according to claim 3, wherein in step S4, the sintering method is as follows: firstly, vacuumizing to be below 100Pa under the greenhouse condition, and then continuously introducing inert gas to reach the standard atmospheric pressure of +15kPa; the temperature is programmed to 1700 to 2000 ℃ from the room temperature at the speed of 10 to 15 ℃/min, and the temperature is kept for 2 to 6 hours.
10. The method of preparing hexagonal spherical boron nitride according to claim 9, wherein the inert gas is nitrogen.
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