KR20140110439A - Method for producing the spherical agglomerate type Boron Nitride and the spherical agglomerate type Boron Nitride made thereby - Google Patents

Method for producing the spherical agglomerate type Boron Nitride and the spherical agglomerate type Boron Nitride made thereby Download PDF

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KR20140110439A
KR20140110439A KR1020130024746A KR20130024746A KR20140110439A KR 20140110439 A KR20140110439 A KR 20140110439A KR 1020130024746 A KR1020130024746 A KR 1020130024746A KR 20130024746 A KR20130024746 A KR 20130024746A KR 20140110439 A KR20140110439 A KR 20140110439A
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boron nitride
spherical
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weight
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강성호
김인섭
이진욱
양진오
김주성
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주식회사 신한세라믹
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Abstract

More particularly, the present invention relates to a process for producing spherical boron nitride by applying a spray drying method and a boron nitride produced by the method, wherein the boron nitride precursor and the inorganic A step of processing the mixture obtained by mixing and adding the additive and the dispersant into a spherical powder having a certain particle size by a spray drying method and heat-treating the spherical powder at a high temperature of 1200 to 2100 캜 under a nitrogen atmosphere A method for producing spherical boron nitride is disclosed.

Description

FIELD OF THE INVENTION The present invention relates to a method for producing spherical boron nitride and a method for producing the spherical boron nitride using boron nitride,

The present invention relates to a process for producing boron nitride, and more particularly to a process for producing spherical boron nitride by applying a spray drying method and boron nitride produced thereby.

Boron nitride is a highly refractory material that is of increasing commercial importance. Typically, boron nitride is prepared by a process using boric acid as the source of boron having a reactive composition. The proposed process for preparing boron nitride from boric acid is described in U.S. Patent No. 2,922,699; 3,241,918; And 3,261,667, as well as British patents 874,166; 874,165; And 1,241,206. Japanese Patent Publication No. 06-040713 discloses a method for producing boron nitride from colemanite.

In this conventional process for producing boron nitride, the borate starting material containing an alkali metal / alkaline earth metal compound, particularly sodium and calcium compounds, is purged with ammonia at a temperature of 1200 ° C or higher, To form a boron nitride + by-product that requires an additional wash / treatment step to recover. Some of the byproducts are various forms of calcium borate that are removed from the boron nitride by leaching with hydrochloric acid. In other processes, boron nitride is purified using deionized water washing. U.S. Pat. No. 3,415,625 discloses a continuous or batch process for high purity boron nitride product after a wash / treatment step.

U.S. Patent No. 4,045,186 discloses a method of reacting boron nitride having a small particle size using Li 3 N and recrystallizing crystalline hexacyclopentyl boron nitride having a large particle size from a mixture at an elevation temperature of 1100 ° C or higher. German Patent Publication No. DE4108367 C1 discloses a suspension of lithium nitrate (in anhydrous di (2-6C) alkyl ether) in excess of trioleuoroborane di (1-6C) while stirring at 20-230 ° C for 2-24 hours. A process for producing boron nitride mainly having a hexagonal system structure including reacting with an alkyl etherate (preferably, dibutyl etherate) is disclosed.

In addition to the process for preparing boron nitride as described above, a process for preparing boron nitride of the prior art documents described below is disclosed. These are in particular related to a process for the preparation of cubic boron nitride or a process for the production of hexavalent boron nitride.

The prior art disclosed in the above is a technique for producing hexagonal or cubic boron nitride, and a technique for grinding boron nitride, which has been conventionally produced by a technique related to a method for producing spherical boron nitride, , There is no known technique for producing spherical boron nitride without using the previously prepared boron nitride.

1. Korean Patent Publication No. 10-2006-0092997 "Process for producing boron nitride" 2. Korean Patent Laid-Open Publication No. 10-2007-0001878 "High purity hexagonal boron nitride single crystal which emits high-brightness atomic light and its production method, and high-luminance non-atomic light emitting element made of said single crystal and solid laser and solid light emitting element using this element " 3. Korean Patent Registration No. 10-0748909 entitled "Cubic Boron Boron Sintered Body" 4. Korean Patent Registration No. 10-0341723 entitled " Method for producing hexagonal boron nitride powder using spinning high-temperature reaction synthesis method " 5. Korean Patent Registration No. 10-0625733 entitled " Method of producing cubic boron nitride " 6. Korean Patent Registration No. 10-0525962 entitled " Method for producing cubic boron nitride and product obtained by this method " 7. Korean Registered Patent No. 10-0333459 entitled "Cubic Boron Nitride Sintered Body" 8. Korean Registered Patent No. 10-0323941 entitled "Boron Nitride and Method for Producing the Same & 9. US Patent 6,645,612 entitled " HIGH SOLIDS HBN SLURRY, HBN PASTE, SPHERICAL HBN POWDER, AND METHODS OF MAKING AND USING THEM " 10. US Patent No. 7,976,941 entitled "BORON NITRIDE PARTICLES OF SPHERICAL GEOMETRY AND PROCESS FOR MAKING THEREOF"

In the present invention, a mixture of a boron source, an inorganic filler and a dispersing agent is spray-dried to produce a spherical powder having a certain particle size, and the powder is subjected to high-temperature heat treatment to form a spherical nitride It is an object of the present invention to provide a method for producing boron.

Another object of the present invention is to provide spherical boron nitride which is produced according to the above-described production method and has an improved thermal conductivity of 30% or more compared to conventional plate-shaped boron nitride

The inventors of the present invention focused on the fact that spherical powder having a predetermined particle size can be processed by using the spray drying method, and thus it is possible to produce spherical boron nitride by applying the spray drying method Thus completing the present invention.

The method for producing spherical boron nitride according to the present invention which solves the above problems is characterized in that boron nitride precursors, inorganic additives and dispersants are added to a mixer and the mixture is processed into a spherical powder having a certain particle size by a spray drying method, And a step of subjecting the processed spherical powder to a heat treatment at a high temperature of 1200 to 2100 캜 under a nitrogen atmosphere.

Wherein the mixture is mixed so as to include 60 to 95 parts by weight of the boron nitride precursor, 2 to 40 parts by weight of the inorganic additive and 0.1 to 3 parts by weight of the dispersing agent.

Herein, 0.1 to 7 parts by weight of the binder is added to the total amount of the mixture, and the mixture is mixed.

The present invention provides spherical boron nitride which is produced by the above-described production method and has a spherical shape and has an average particle size of 20 to 150 μm and a thermal conductivity of 2 to 40 W / m · K.

The method of producing spherical boron nitride provided according to the present invention can provide a simple and economical method of producing spherical boron nitride.

In addition, the production method according to the present invention can provide spherical boron nitride having a thermal conductivity higher than that of conventional plate-shaped boron nitride by 30% or more.

1 shows an example of a spray dryer used to implement the present invention.
2 is a SEM photograph of a spherical powder produced by the spray drying method according to the present invention.
3 is a SEM photograph of boron nitride powder after heat treatment of spherical boron nitride powder produced according to an embodiment of the present invention.
4 is an XRD analysis graph of a spherical boron nitride powder prepared according to an embodiment of the present invention.
FIG. 5 is a graph showing comparative measurement of thermal conductivity between spherical boron nitride produced according to the present invention and conventional plate-shaped boron nitride.

BRIEF DESCRIPTION OF THE DRAWINGS The invention will now be described more fully hereinafter with reference to the accompanying drawings, in which: FIG.

The boron nitride obtained according to the aimed method of the present invention is a compound of B and N having a crystal structure similar to that of graphite and has electrical insulation and is a white graphite identical to graphite except for the white color.

Boron nitride has almost the same crystal structure as graphite in that B and N are combined at a ratio of 1: 1. It is similar to graphite in physical properties, and its bonding mode is mainly covalent, but it has a higher ratio of ionic bond than graphite and has no free electrons because it has no metal bonding property, and is electrically insulating and white.

Boron nitride is most advantageous in that it is easy to process. This is because the interlaminar bond strength of the layered structure similar to graphite is weaker than the other directions, and it can be easily processed by knife, saw, lathe and the like.

Boron nitride is oxidized to B 2 O 3 at about 600 ° C in air, but has a heat resistance of 2,000 ° C or more in N 2 . The strength at high temperature and the decrease in electrical insulating properties are small, and the thermal conductivity is high and the Young's modulus is small. It is known that boron nitride also has a high hardness such as diamond due to the presence of a high-pressure phase such as CBN, as well as the presence of diamond as an isotope of graphite.

Boron nitride having such physical properties is indispensable as an insulating material for vacuum equipment and experimental equipment to be used in a heated state, since it can be precisely processed in addition to excellent heat resistance and electrical insulation. Also, because of its electrical insulation and high thermal conductivity, it is used as an insulating material for transistors, substrates for ICs, and sealing heaters. In addition, PBN is rapidly growing in applications of gallium, arsenic and CBN as steel cutting tools due to its high purity and corrosion resistance. And is also used as a B diffusion source for IC fabrication. However, because it is a relatively expensive material, its intended use is limited.

The present invention provides a method for producing boron nitride having the above-mentioned physical properties, and in particular, the present invention has been completed in order to provide a method for producing boron nitride for application as an insulating filler.

BACKGROUND ART [0002] Many known methods for producing boron nitride are known for producing cubic boron nitride, hexagonal boron nitride, or boron nitride in a fiber form. Most of the boron nitride used as an insulating filler is a spherical type boron nitride ≪ / RTI >

The inventors of the present invention focused on the fact that a spherical filler as an insulating filler used as a filler of an insulator is superior in terms of interfacial thermal resistance and through-plane thermal conductivity, thereby improving thermal conductivity as a whole. Thus, using a conventional plate-shaped boron nitride powder The present inventors have completed a method of producing spherical boron nitride having improved thermal conductivity by producing spherical boron nitride.

The method for producing spherical boron nitride according to the present invention is characterized in that a boron nitride precursor, an inorganic additive and a dispersant are added to a mixer and the mixture is processed into a spherical powder having a certain particle size by a spray drying method, Treating the powder at a high temperature of 1200 to 2100 캜 under a nitrogen atmosphere.

According to the present invention, it is preferable that the mixture is mixed so as to include 60 to 95 parts by weight of the boron nitride precursor, 2 to 40 parts by weight of the inorganic additive and 0.1 to 3 parts by weight of the dispersant, based on the total amount of the mixture. If the amount of the boron nitride precursor is less than 60 parts by weight, there may be a problem that the amount of spherical BN to be synthesized is small and the desired thermal conductivity is not exhibited. If the boron nitride precursor is more than 95 parts by weight There is a problem that the synthesized spherical particles are weak in strength and are easily broken and practicality is limited.

The inorganic additive may be any one selected from the group consisting of oxide ceramics, non-oxide ceramics, and mixtures thereof, which serves as a coupling catalyst for boron and nitrogen in a boron nitride precursor under a nitrogen atmosphere. , There may be a problem that it is difficult to produce practical spherical BN particles because of the role of the boron and nitrogen bonding catalyst of the precursor and the role of enhancing the strength of the spherical BN particles, and when it exceeds 40 parts by weight There may be a problem that the content of synthesized BN is low and thermal conductivity characteristics are lowered. Preferably, the inorganic additive is pulverized and mixed in powder form having an average particle size of 1 to 20 mu m.

As the oxide ceramics used as the inorganic additive, Al 2 O 3 , MgO, CaO and the like can be used, and as the non-oxide ceramics, SiC, B 4 C, Si 3 N 4 , AlN and the like can be used.

The dispersant is used to improve the dispersibility of the boron nitride precursor and the inorganic additive. When the amount of the boron nitride precursor is less than 0.1 parts by weight, the dispersibility of the boron nitride precursor and the inorganic additive deteriorates, If the amount is more than 3 parts by weight, the dispersibility is deteriorated.

According to the present invention, the boron nitride precursor may be a compound in a liquid state as a boron compound, or may be a powdery compound. It is preferable to use a powdery boron compound, and the boron compound may be any compound that contains boron. Preferably, the powdery boron compound has an average particle size of 1 to 20 Lt; 2 > / m < 2 >.

According to the present invention, 0.1 to 7 parts by weight of the binder may be further added to the mixture, based on the total weight of the mixture. The binder is used to enhance the bonding strength between the boron nitride precursor and the inorganic additive to be mixed, and it is preferable to use at least one of general organic binders such as PVA and PEG.

FIG. 1 illustrates an embodiment of a spray dryer 100 according to an embodiment of the present invention. The spray dryer 100 includes a boron nitride precursor and a boron nitride precursor The inorganic additive and the dispersant are mixed and mixed in a mixer and then the mixture of the mixer is introduced into the raw material tank 10 so that the mixture introduced into the raw material tank 10 is supplied to the drying furnace 40 by the raw material feed pump 20 And the mixture is supplied to the spray nozzle 30 so that the mixture is supplied to the drying furnace by the spray nozzle 30.

At this time, the spray nozzle 30 used was a disk type atomizer in which the raw material was regulated at a constant rpm so as to form a vortex in the drying furnace to be dried.

When the mixture is supplied to the drying furnace 40 by the spray nozzle 30 as described above, the air is sucked into the drying furnace 40 through the suction device 52 for sucking the outside air and the blower for supplying the outside air sucked by the suction device 52 A hot air generating device 54 for generating hot air by heating the outside air supplied from the fan 58 and the blowing fan 58 and a hot air generator 54 for filtering the impurities before supplying the hot air heated by the hot air generator 54 to the drying furnace The hot air supply device 50 composed of the hot air filter 56 for supplying hot air to the drying furnace 40 simultaneously supplies hot air at a high temperature.

At this time, the mixture is dried in the drying furnace 40 by the supplied hot air.

2, the spherical shaped boron nitride powder 200 is discharged from the discharge port 40 of the drying furnace 40. The boron nitride powder 200 is dried in the drying furnace 40, (42) and is collected by the collector (80).

On the other hand, the hot air supplied to the drying furnace 40 is discharged to the outside through the discharge pipe 72 coupled to the ventilation fan 70 by the ventilation fan 70, And the discharge pipe 66 is connected to the cyclone 60 which is a collecting means provided between the drying furnace 40 and the ventilation fan 70.

The fine powder in the spherical powder produced in the drying furnace 40 is sucked into the discharge pipe 72. The sucked fine powder flows into the cyclone 60 and the inflow fine powder is powder having a relatively large particle size And recovered from the powder recovery port 62 formed at the lower portion of the cyclone 60. The remaining powder having a relatively small particle diameter is collected in the filter 64 constituting the inside of the cyclone 60.

At this time, the spherical boron nitride powder 200 collected has an average particle size of 20 to 150 mu m.

The spherical boron nitride powder (200) produced by the spray drying as described above was placed in a high-temperature synthesis furnace and subjected to a high-temperature heat treatment in a nitrogen atmosphere to produce final spherical boron nitride as shown in FIG. At this time, the heat treatment is preferably performed within a temperature range of 1200 to 2000 ° C.

The spray drying method exemplified above is an example for explaining the present invention, and is not limited to the above-mentioned method, and may be variously changed according to the design of the manufacturing process. That is, depending on the design of the average particle size of the desired powder, such as the feed rate for feeding the mixture containing the boron compound to be supplied to the drying furnace, the spraying rate to be supplied to the drying furnace, It is possible.

As described above, the present invention is a method for producing spherical boron nitride using a spray drying method, wherein the final spherical boron nitride obtained by the above method has an average particle size of 20 to 150 탆, a thermal conductivity of 2 to 40 W / mK of boron nitride can be obtained. As shown in FIG. 5, the thermal conductivity shows an improved thermal conductivity of 30% or more as compared with the conventional plate-shaped boron nitride.

Accordingly, the present invention provides spherical boron nitride, which is produced by the above-described production method and has a spherical shape and has an average particle size of 20 to 150 μm and a thermal conductivity of 2 to 40 W / m · K You can.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention. And can be modified in any way within the scope of the present invention.

[Example 1]

Boron nitride precursor to boron compound also mean particle size 6㎛ the h-BN powder 90 parts by weight, an average particle size of the inorganic additive 2㎛ powder Al 2 O 3 5 parts by weight of a cationic 7347C to 5 parts by weight of CaO and dispersing agents Were thoroughly mixed in a mixer to prepare a mixture.

The mixture was poured into a raw material tank of the spray dryer of FIG. 1 and then supplied to a drying furnace at a feed rate of 20 g / sec. The mixture was dried under the spray drying conditions shown in Table 1 to obtain spherical particles having an average particle size of 20 to 150 μm Powder was obtained.

Next, the spherical powder was subjected to a high-temperature heat treatment in a high-temperature synthesis furnace at a temperature of 2000 占 폚 under a nitrogen atmosphere for 5 hours to obtain spherical boron nitride as shown in Fig.

The results of the XRD analysis of the spherical boron nitride obtained as described above can be confirmed to be a single crystal of h-BN as shown in Fig.

Spray drying conditions Inlet temperature (° C) Outlet temperature (℃) rpm 230 110 10,000

[Example 2]

Boron nitride was prepared in the same manner as in Example 1, except that the heat treatment was performed at a high temperature of 1800 캜.

As a result, it was confirmed that spherical boron nitride as shown in Fig. 3 was obtained.

[Example 3]

Spherical boron nitride was prepared in the same manner as in Example 1, except that PVA was further added as a binder to 2 parts by weight based on the total amount of the mixture.

As a result, it was confirmed that spherical boron nitride as shown in Fig. 3 was obtained.

As a result of XRD analysis, the results shown in Fig. 4 were obtained.

<Thermal conductivity analysis>

Each of the insulators using the spherical boron nitride prepared in Examples 1 to 3 as the insulating filler and the comparative example using the conventional plate-shaped boron nitride as the insulating filler were prepared, and the thermal conductivity of each insulator was measured with a laser flash Flash) method. As a result, the results shown in Table 2 and FIG. 5 were obtained. In this case, the conventional plate-shaped boron nitride used had an average particle size of 15 mu m, the spherical boron nitride prepared in Example was 70 mu m, and the insulating filler filled in the insulator contained 50 parts by weight Respectively. At this time, the resin used is phenol resin.

division Thermal conductivity
(Through Plane) Example 1 3.84 W / m · K Example 2 3.75 W / m · K Example 3 3.80 W / m · K Comparative Example 2.98 W / m · K

As a result of the above Table 2 and FIG. 5, when the spherical boron nitride provided in the example of the present invention was used as the insulating filler, the thermal conductivity was 30% or more Respectively.

10: raw material tank 20: raw material supply pump
30: Spray nozzle 40: Drying furnace
42: outlet 50: heat supply device
52: intake device 54: hot air generating device
56: hot air filter 58: blowing fan
60: Cyclone 62: Powder recovery port
64: filter 66, 68: discharge pipe
80, 82: Collector 100: Spray dryer
200: boron nitride powder

Claims (4)

The mixture obtained by mixing the boron nitride precursor, the inorganic additive and the dispersant into the mixer was mixed and processed into a spherical powder having a predetermined particle size by a spray drying method. The spherical powder thus processed was calcined at a high temperature of 1200 to 2100 캜 And then heat-treating the spherical boron nitride. The method according to claim 1,
Wherein the mixture is mixed so as to include 60 to 95 parts by weight of the boron nitride precursor and 2 to 40 parts by weight of the inorganic additive. The method according to claim 1,
Wherein 0.1 to 7 parts by weight of the binder and 0.1 to 3 parts by weight of the dispersing agent are further added to the mixture and mixed. And is characterized in that it has a spherical shape and has an average particle size of 20 to 150 μm and a thermal conductivity of 2 to 40 W / m · K, which is produced by the production method of any one of claims 1 to 3 Spherical boron nitride.
KR1020130024746A 2013-03-08 2013-03-08 Method for producing the spherical agglomerate type Boron Nitride and the spherical agglomerate type Boron Nitride made thereby KR20140110439A (en)

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US10238583B2 (en) 2015-06-30 2019-03-26 Amorepacific Corporation Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same
CN109988409A (en) * 2017-12-29 2019-07-09 广东生益科技股份有限公司 A kind of boron nitride aggregate includes its compositions of thermosetting resin and application thereof
KR20200113846A (en) * 2019-03-26 2020-10-07 주식회사 엘지화학 Boron-Substituted Aluminum Nitride Powder and Method of Preparing the Same

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10238583B2 (en) 2015-06-30 2019-03-26 Amorepacific Corporation Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same
US10624822B2 (en) 2015-06-30 2020-04-21 Amorepacific Corporation Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same
CN109988409A (en) * 2017-12-29 2019-07-09 广东生益科技股份有限公司 A kind of boron nitride aggregate includes its compositions of thermosetting resin and application thereof
US11661378B2 (en) 2017-12-29 2023-05-30 Shengyi Technology Co., Ltd. Boron nitride agglomerate, thermosetting resin composition containing same, and use thereof
KR20200113846A (en) * 2019-03-26 2020-10-07 주식회사 엘지화학 Boron-Substituted Aluminum Nitride Powder and Method of Preparing the Same

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