KR20160086648A - Manufacturing method for aluminum nitride whisker - Google Patents

Manufacturing method for aluminum nitride whisker Download PDF

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KR20160086648A
KR20160086648A KR1020150004269A KR20150004269A KR20160086648A KR 20160086648 A KR20160086648 A KR 20160086648A KR 1020150004269 A KR1020150004269 A KR 1020150004269A KR 20150004269 A KR20150004269 A KR 20150004269A KR 20160086648 A KR20160086648 A KR 20160086648A
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aluminum nitride
aluminum
carbon
source
alumina
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KR1020150004269A
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정우식
최호성
유광현
김원식
김성국
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엘티씨 (주)
영남대학교 산학협력단
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Priority to KR1020150004269A priority Critical patent/KR20160086648A/en
Priority to PCT/KR2015/000306 priority patent/WO2016114413A1/en
Publication of KR20160086648A publication Critical patent/KR20160086648A/en

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    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C01B21/0726—Preparation by carboreductive nitridation
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62286—Fibres based on nitrides
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    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/424—Carbon black
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02538—Group 13/15 materials
    • H01L21/0254—Nitrides
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02587—Structure
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    • H01L21/02603—Nanowires
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types

Abstract

The present invention relates to a manufacturing method of an aluminum nitride whisker. More particularly, the manufacturing method of an aluminum nitride whisker comprises the following steps of: forming a mixture by mixing an aluminum source and a carbon source; and nitriding and reducing the aluminum source to an aluminum nitride whisker by conducting a reaction of the mixture under the nitriding atmosphere. The carbon source includes a fixed amount of an activator. The manufacturing method can manufacture an aluminum nitride whisker at low costs using a carbothermal reduction and nitridation method.

Description

[0001] The present invention relates to a method for manufacturing an aluminum nitride whisker,

The present invention relates to the production of aluminum nitride (AlN), and more particularly to a method of manufacturing aluminum nitride whiskers.

BACKGROUND ART [0002] In recent years, electronic devices used in automobiles, electric and electronic fields have been pursued to be lightweight, thin, miniaturized, and multifunctional. As these electronic devices become more highly integrated, more heat is generated. This heat not only deteriorates the function of the device but also causes malfunction of peripheral devices and deterioration of the substrate. ought. Particularly, the material of the high heat dissipation circuit board can utilize the thermal conductivity of the base metal substrate, which is advantageous for manufacturing power devices, LED modules, and other components consuming high power and generating a lot of heat.

As the heat radiating material, a composite material in which a high thermal conductive filler material such as a carbon material or a ceramic material and a polymer material are mixed is used. Composite materials can impart the characteristics of metals and ceramics while retaining the advantages of conventional polymer materials, such as easy processability, low cost, light weight, and variety of product form. The reason why the composite material is used is that the high thermal conductive filler material has excellent thermal conductivity but has no adhesive force, and the polymer material has good adhesion but low thermal conductivity. Therefore, in order to achieve a high thermal conductivity of the polymer composite material, a large amount of filler capable of shortening the heat transfer path is contained. In such a case, the processing conditions are complicated and the physical properties of the product are deteriorated. In order to shorten the heat transfer path of the heat dissipation material, there are a method of increasing the filler filling rate, a study of developing a filler having a higher thermal conductivity, a study of increasing the particle diameter of the filler, have.

Aluminum nitride has a theoretical thermal conductivity of 10 times or more that of alumina and is excellent in electrical insulation. The thermal expansion coefficient of aluminum nitride is smaller than that of alumina and is similar to that of silicon. Furthermore, aluminum nitride is excellent in mechanical strength and suitable for securing the durability of semiconductor devices, and is expected to be used as a heat radiation material.

 Recently, aluminum nitride having anisotropy in shape in order to use aluminum nitride as a heat-radiating filler has been proposed in which aluminum nitride whiskers having a high aspect ratio (that is, a value obtained by dividing the major axis by the minor axis) Has been attempted. Examples of the synthesis method of aluminum nitride whisker include a direct nitriding method, a chemical vapor phase reaction method, a sublimation-condensation method using a temperature gradient, and a thermal carbon reduction nitriding method. The double direct nitridation method, sublimation-condensation method, and chemical vapor phase method can obtain high-quality whiskers, but the starting materials are expensive and the equipment is complicated in configuration, which is not compatible with mass production. The thermal carbon reduction nitriding method is an economical method of producing aluminum nitride, but generally, the shape of aluminum nitride is similar to that of aluminum oxide, which is a starting material. Therefore, when a conventional aluminum oxide powder having a substantially spherical shape is used as a starting material, There is a problem that wire-shaped aluminum nitride whiskers having an aspect ratio can not be manufactured.

An object of the present invention is to provide a method for economically producing aluminum nitride whiskers using a thermal carbon reduction nitriding method. However, these problems are exemplary and do not limit the scope of the present invention.

According to one aspect of the present invention, there is provided a method of forming a mixture, comprising: mixing an aluminum source and a carbon source to form a mixture; And reacting the mixture in a nitriding atmosphere to reduce nitriding the aluminum source to an aluminum nitride whisker. Wherein the carbon source may be one containing an activator.

The activator may have a content in the carbon source ranging from 500 ppm to 25000 ppm.

The activator includes at least one selected from the group consisting of Fe, Ni, Mg, Co, Mn, Mo, Nb and Cu. can do.

The aluminum source may comprise aluminum oxide or hydrate which can be aluminum oxide by heating. Specifically, the aluminum source is selected from the group consisting of alpha-alumina, delta-alumina, gamma -alumina, boehmite, diaspore, 3 ). ≪ / RTI >

The aluminum source may comprise a powder having an aspect ratio of 3 or more.

The nitridation atmosphere may include a reactive gas atmosphere comprising nitrogen, ammonia or a cyanide compound. In addition to the reaction gas, hydrogen (H 2 ) gas may be further included. The cyan compound may include at least one selected from, for example, acetonitrile, propanenitrile, benzonitrile, and hydrogen cyanide.

The carbon source may be at least one selected from graphite, activated carbon, carbon nanotubes (CNT), carbon nanofibers (CNF), carbon black, graphene and fullerene. One can be included.

On the other hand, after the step of reducing nitriding the aluminum source with aluminum nitride whiskers, calcining and removing the remaining carbon may be further included.

The reducing nitridation may be performed at a temperature of 1300 ° C to 1700 ° C.

According to the embodiment of the present invention as described above, a method of manufacturing an aluminum nitride whisker can be implemented. The aluminum nitride whiskers have a low electron affinity and a high thermal conductivity, so that the use of such aluminum nitride whiskers in products such as semiconductors greatly improves start-up time, robustness and sustainability. In addition, when used as a heat radiating material, the heat transfer path is shortened, so that the heat radiation characteristic is improved. Of course, the scope of the present invention is not limited by these effects.

1 is a flowchart schematically showing a method of manufacturing an aluminum nitride whisker according to an embodiment of the present invention.
FIG. 2 is a schematic view illustrating an apparatus for manufacturing an aluminum nitride whisker according to an embodiment of the present invention.
Figures 3 and 4 are the results of Raman spectroscopy and X-ray diffraction analysis of aluminum nitride whiskers prepared according to the embodiments of the present invention, respectively.
Fig. 5 shows the results of electron microscopic observation of aluminum nitride whiskers prepared according to Examples and Comparative Examples of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. It should be understood, however, that the invention is not limited to the disclosed embodiments, but may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, Is provided to fully inform the user. Also, for convenience of explanation, the components may be exaggerated or reduced in size.

1 is a flowchart schematically showing a method of manufacturing an aluminum nitride whisker according to an embodiment of the present invention.

Referring to FIG. 1, a method for manufacturing an aluminum nitride whisker according to an embodiment of the present invention includes the steps of mixing an aluminum source and a carbon source (100), reacting the mixture in a nitriding atmosphere to produce an aluminum nitride whisker (S200) . After the step S200 of manufacturing the aluminum nitride whiskers is finished, the remaining carbon may be further calcined and removed (S300).

The aluminum source may comprise aluminum oxide (Al 2 O 3 , alumina) as a starting material for aluminum nitride whiskers. For example, aluminum oxide may include alumina having a crystal structure such as?,?,?,?,?,?,? Or the like. Other examples include alumina hydrates that dehydrate and transfer by heating, such as Boehmite, Diaspore, aluminum hydroxide (Al (OH) 3 ), and eventually transition to alumina.

The aluminum source may include, for example, a powder form, and the shape is not particularly limited, and may have a shape such as a spherical shape, a fibrous shape, a plate shape, and a cylindrical shape. According to the embodiment of the present invention, it is possible to manufacture aluminum nitride whiskers regardless of the shape of the aluminum supply source. For example, it is possible to produce wire-shaped nitrated alumina whiskers with an aspect ratio well over 3, even if alpha-alumina having an aspect ratio of less than 3 is used as the aluminum source. The aluminum source may be, for example, a material having a particle diameter of 5 탆 or less, although the particle diameter is not particularly limited.

The carbon source is a material for supplying carbon used in a reductive nitrification reaction, for example, graphite, activated carbon, carbon nanotube (CNT), carbon nanofiber (CNF), carbon black Carbon Black, Graphene, and Fullerene. In addition, the carbon source may include, for example, a powder form, and the particle diameter is not particularly limited, but a particle having a particle size of 300 mu m or less can be used.

In particular, the carbon source is characterized by containing an activator as a constituent element. The activator is an element that promotes the growth of aluminum nitride in a whisker form during the process of reducing aluminum oxide to aluminum by carbon, for example, and then reacting with nitrogen to form aluminum nitride. These activators include metal components and include, for example, Fe, Ni, Mg, Co, Mn, Mo and Nb and copper Cu). ≪ / RTI > It is believed that such an activator is present in the interior of the carbon source and contributes to the growth of aluminum nitride in the form of whiskers after being vaporized during the high temperature reaction to escape from the carbon source.

The step of mixing the aluminum supply source and the carbon supply source may be, for example, a wet mixing method and a dry mixing method. The wet mixing method can be carried out using a solvent such as water, methanol, ethanol, isopropyl alcohol, acetone, toluene, xylene and the like. The slurry, which is uniformly mixed, is dried to remove the solvent. The dry mixing method is a simple mixing method using a mixer and an impeller, and a method using a ball mill is also possible.

The mixture of the aluminum source and the carbon source is introduced into the reaction chamber through a predetermined reaction, and is then allowed to react in a nitriding atmosphere. The nitridation atmosphere can be formed by, for example, introducing a gas containing nitrogen (N 2 ), ammonia (NH 3 ), or a cyanide compound into the inside of the reactor. The cyan compound may include at least one selected from, for example, acetonitrile, propanenitrile, benzonitrile, and hydrogen cyanide. The nitrogen source is preferably in the gaseous state, but there is no particular limitation.

The temperature of the nitriding atmosphere may be in the range of 1300 ° C to 1700 ° C, strictly 1500 ° C to 1700 ° C, more strictly 1500 ° C to 1650 ° C. If the temperature of the nitriding atmosphere is too low, the reductive nitrification reaction may be delayed and abnormal aluminum nitride may be formed. In addition, if the temperature of the nitriding atmosphere is too high, the reductive nitrification reaction occurs too rapidly to decrease the purity and form aluminum nitride in a fine powder form, and it is difficult to realize the whisker shape.

The time of the nitriding atmosphere may range from 3 hours to 10 hours. If the time of the nitriding atmosphere is too short, the reduction nitrification reaction does not sufficiently take place, and if the time is too long, abnormal aluminum nitride tends to form. The flow rate of the nitriding atmosphere is preferably 150 mL / min to 250 mL / min, for example.

When this mixture is reacted in a nitriding atmosphere, a wire-shaped aluminum nitride whisker having a remarkable difference in aspect ratio from the spherical shape is produced by the activator contained in the carbon source even though the aluminum source has spherical powder. At this time, the amount of the produced aluminum nitride whiskers tends to increase as the content of the activator contained in the carbon source increases.

If the carbon source remains after the reaction is complete, it may undergo a decarburization process to remove it by calcination. The step of calcining the residual carbon can be carried out, for example, by oxidizing the carbon by heat treatment in air. The time for calcining the residual carbon is usually limited by the amount of residual carbon, and the amount of residual carbon is limited by the amount of carbon source added and the addition rate. For example, when the amount of the carbon source added is large or the addition rate is high, the time for calcining the residual carbon becomes long.

The aluminum nitride whiskers of the present invention have a low electron affinity and a high thermal conductivity, so that they are greatly improved in start-up time, robustness, and sustainability when used in devices such as semiconductors. In addition, when used as a filler for a heat radiating material, the heat transfer path can be shortened without increasing the filling rate of the filler.

FIG. 2 is a structural view illustrating an example of a manufacturing apparatus 100 capable of manufacturing an aluminum nitride whisker according to an embodiment of the present invention. Referring to FIG. 2, the apparatus 100 for manufacturing an aluminum nitride whisker has a shape of a furnace shell (110). The box-type nitriding furnace 110 includes a gas supply line 120 for supplying nitrogen, ammonia or cyanide to form a nitriding atmosphere, and a gas exhaust line 130 for discharging carbon dioxide or carbon monoxide generated in the reductive nitrification reaction . The reaction vessel 150 may be disposed inside the box-shaped nitrification furnace 110. Such a reaction vessel may include an alumina boat, a graphite boat, and the like. As the reaction vessel 150, a mixture 160 in which an aluminum source and a carbon source are mixed may be provided. A heater 140 may be disposed on the outer circumferential surface of the box-shaped nitrite furnace 100 to supply heat to the inside of the box-shaped nitrite furnace 100. When the heater 140 forms a high-temperature atmosphere in the box-shaped nitriding furnace 100, the mixture 160 undergoes a reduction nitrification reaction to realize an aluminum nitride whisker according to an embodiment of the present invention.

Hereinafter, experimental examples are provided to facilitate understanding of the present invention. It should be understood, however, that the following examples are for the purpose of promoting understanding of the present invention and are not intended to limit the scope of the present invention.

Experimental Example 1)

5.00 g of the alpha -alumina powder as the aluminum supply source was mixed with 2.00 g of the carbon black powder as the carbon supply source and charged into an alumina boat as a reaction vessel and charged into the box type nitride shown in Fig. At this time, carbon black contained 500 ppm of iron (Fe) as an activator. The reaction was carried out at 1600 ° C. for 5 hours in a nitrogen atmosphere (flow rate: 200 mL / min). After completion of the reaction, the residual carbon was calcined in air for 1 hour.

Experimental Example 2)

An experiment was conducted in the same manner as in Experimental Example 1, except that the content of iron (Fe) contained in the carbon black was 25000 ppm.

Comparative Example 1)

Except that iron-free carbon black powder was used in place of the carbon black powder. At this time, the carbon black powder not containing iron was obtained by immersing the commercially available carbon black powder in a concentrated hydrochloric acid solution for 1 week to dissolve the iron component.

 Comparative Example 2)

Except that carbon black powder not containing iron was used, and 1 mg of nano iron powder was further added to a mixture of? -Alumina powder and black carbon powder, in the same manner as in Experimental Example 1 described above.

The aluminum nitride was analyzed by Raman spectroscopy and X-ray diffractometer to confirm the formation of aluminum nitride. Representative results of the analysis of Example 1 are shown in FIG. 3 and FIG.

As a result of the analysis of the Raman spectrometer in FIG. 3, the peaks detected as shown are all those corresponding to the aluminum nitride peak. On the other hand, all the X-ray diffraction peaks in Fig. 4 were peaks of aluminum nitride.

5 is a result of observing aluminum nitride produced according to embodiments of the present invention with a scanning electron microscope (SEM). 5 (a) and 5 (b) show the results of observation of aluminum nitride produced by Comparative Examples 1 and 2, and FIGS. 5 (c) and 5 This is the result of observing aluminum.

5 (c) and 5 (d), it can be seen that wire-shaped aluminum nitride whiskers are formed together with the substantially spherical aluminum nitride powder. It can also be seen that a larger amount of aluminum nitride whisker is produced in Example 2 where the content of iron as an activator is higher.

On the other hand, referring to FIG. 5 (a), it can be seen that no whiskers are formed when carbon black does not contain iron. 5 (b), unlike Examples 1 and 2, when iron as an activator was separately added, some whiskers were produced, but the amount thereof was remarkably smaller than those of Examples 1 and 2.

From these results, it can be seen that, in the production of aluminum nitride whiskers by the thermal carbon reduction nitriding method, an activator must be supplied, and it is more effective that such an activator should be contained in a carbon source rather than being supplied separately. This is inferred to be related to the distribution of the activator before the production of the aluminum nitride whisker. That is, given the reaction temperature at which aluminum nitride is formed, the added activator is expected to be vaporized during the reaction to produce aluminum nitride, where the activator is contained in the carbon source and is supplied separately from the carbon source It is expected that the vaporized activator will come into contact with the aluminum source, such as aluminum oxide, in a more uniform and broad area. For this reason, it is interpreted that the probability of forming aluminum nitride whiskers is high.

While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the invention. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.

Claims (12)

Mixing an aluminum source and a carbon source to form a mixture; And
Reacting the mixture in a nitriding atmosphere to reduce nitridation of the aluminum source to an aluminum nitride whisker,
Wherein the carbon source comprises an activator.
Method for manufacturing aluminum nitride whiskers. The method according to claim 1,
Wherein the activator has a content in the range of 500 ppm to 25000 ppm in the carbon source. The method according to claim 1,
The activator includes at least one selected from the group consisting of Fe, Ni, Mg, Co, Mn, Mo, Nb and Cu. Gt; aluminum nitride whisker. ≪ / RTI > 2. The method of claim 1, wherein the aluminum source comprises aluminum oxide or a hydrate capable of becoming aluminum oxide by heating. 5. The method of claim 4,
The aluminum source is alpha-alumina (α-alumina), delta alumina (δ-alumina), gamma-alumina (γ-alumina), boehmite (boehmite), diamond spokes O (diaspore), aluminum hydroxide (Al (OH) 3) ≪ / RTI > wherein the aluminum nitride whisker is selected from the group consisting of aluminum nitride and aluminum nitride. The method according to claim 1,
Wherein the aluminum source comprises a powder having an aspect ratio of 3 or greater. The method according to claim 1,
Wherein the nitridation atmosphere includes a reactive gas atmosphere containing nitrogen, ammonia or a cyanide compound. 8. The method of claim 7,
Further it includes method for producing aluminum nitride whiskers to the hydrogen (H 2) in addition to the reaction gas. 8. The method of claim 7,
Wherein the cyan compound comprises at least one selected from acetonitrile, propanenitrile, benzonitrile and hydrogen cyanide. The method according to claim 1,
The carbon source may be at least one selected from graphite, activated carbon, carbon nanotubes (CNT), carbon nanofibers (CNF), carbon black, graphene and fullerene. RTI ID = 0.0 > 1, < / RTI > The method according to claim 1,
And calcining the remaining carbon after performing the step of reducing nitriding the aluminum source to an aluminum nitride whisker. The method according to claim 1,
Wherein the reducing nitriding is performed at a temperature of 1300 캜 to 1700 캜.

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KR20210079870A (en) * 2019-12-20 2021-06-30 한국알루미나 주식회사 Manufacturing method of aluminum nitride using porous carbon crucible
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