JPH0686286B2 - Manufacturing method of aluminum nitride - Google Patents
Manufacturing method of aluminum nitrideInfo
- Publication number
- JPH0686286B2 JPH0686286B2 JP12876588A JP12876588A JPH0686286B2 JP H0686286 B2 JPH0686286 B2 JP H0686286B2 JP 12876588 A JP12876588 A JP 12876588A JP 12876588 A JP12876588 A JP 12876588A JP H0686286 B2 JPH0686286 B2 JP H0686286B2
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- compound
- aluminum nitride
- aluminum
- nitrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 15
- -1 nitrogen-containing compound Chemical class 0.000 claims description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 description 13
- 239000000758 substrate Substances 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000010304 firing Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005121 nitriding Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000004131 Bayer process Methods 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ この発明は、たとえば高熱伝導率のセラミックス基板を
製造するために使用されるような窒化アルミニウム粉末
の製造技術の分野に属する。TECHNICAL FIELD The present invention belongs to the field of manufacturing technology of aluminum nitride powder such as used for manufacturing a ceramic substrate having high thermal conductivity.
［従来の技術］ IC等に代表されるような半導体素子の高集積化や大電力
化が進み、これに伴って放熱性のよい電気絶縁材料が要
求されるようになった。これに応えて各種の高熱伝導性
セラミックス基板が提案されている。その中でも特に窒
化アルミニウムセラミックス基板が、熱伝導性、熱膨張
性、電気絶縁性等の点で優れていると言うことから、実
用化が進んでいる。[Prior Art] With higher integration and higher power consumption of semiconductor elements represented by ICs and the like, along with this, there has been a demand for electrically insulating materials with good heat dissipation. In response to this, various high thermal conductivity ceramic substrates have been proposed. Among them, the aluminum nitride ceramics substrate is particularly put to practical use because it is excellent in terms of thermal conductivity, thermal expansion property, electrical insulation property, and the like.
ところで、窒化アルミニウムセラミックス基板は価格が
高ことが欠点であると指摘されている。この高価格の原
因としては、基板を製造する際に原料とされる、窒化ア
ルミニウム粉末が高価格であること、基板を得るための
焼結に高温を必要とすること等が挙げられている。By the way, it has been pointed out that the high cost of the aluminum nitride ceramics substrate is a drawback. The reason for this high price is that aluminum nitride powder, which is a raw material when manufacturing the substrate, is expensive, and that high temperature is required for sintering to obtain the substrate.
従来から窒化アルミニウム粉末は、アルミニウムの直接
窒化やアルミナの炭素還元等の方法によって製造されて
いる。Conventionally, aluminum nitride powder has been produced by methods such as direct nitriding of aluminum and carbon reduction of alumina.
アルミニウムの直接窒化法は、金属アルミニウムを窒素
ガス気流中で、1100〜1200℃の高温で熱処理することに
よって実施される。The direct nitriding method of aluminum is carried out by heat treating metallic aluminum in a nitrogen gas stream at a high temperature of 1100 to 1200 ° C.
アルミナの炭素還元法においては、一般にはアルミナと
炭素粉末を混合した後、窒素ガス中で、1600〜1700℃で
焼成する方法が採られている。In the carbon reduction method of alumina, generally, a method of mixing alumina and carbon powder and then calcining at 1600 to 1700 ° C. in a nitrogen gas is adopted.
［発明が解決しようとする課題］ アルミニウムの直接窒化法は、高純度で粒径の小さい窒
化アルミニウム粉末を得ることが困難である。粒径が大
きいと基板を製造する際に焼結性が悪く、または焼結に
高温を要する。また粒径を小さくするために粉砕を施す
と、その工程中で純度が低下し、結局基板の熱伝導性が
悪くなる欠点がある。[Problems to be Solved by the Invention] It is difficult to obtain an aluminum nitride powder having a high purity and a small particle size by the direct nitriding method of aluminum. If the particle size is large, the sinterability is poor when the substrate is manufactured, or the sintering requires a high temperature. Further, if pulverization is performed in order to reduce the particle size, there is a drawback that the purity decreases during the process and the thermal conductivity of the substrate eventually deteriorates.
一方、アルミナの炭素還元法においては、高純度の窒化
アルミニウム粉末を得るためには、原料のアルミナとし
て高純度のアルミナの使用が要求されるので（これは高
価格である）、結局窒化アルミニウムの価格が高くな
る。On the other hand, in the carbon reduction method of alumina, in order to obtain high-purity aluminum nitride powder, it is required to use high-purity alumina as the raw material alumina (this is high price), so that aluminum nitride The price will be high.
バイヤー法により製造されるアルミナは低価格である。
しかし、このアルミナは不純物として含有されるソーダ
成分が多く、したがって電気絶縁性が悪く、通常は電気
用基板の製造のためには使用されない。前記ソーダ成分
を低レベルに押さえたアルミナが提供されているが、な
お、珪素（Si）、遷移金属（Fe等）の不純物の含有量が
多いために熱伝動性が悪く、窒化アルミニウム基板用と
しては使用できない。Alumina produced by the Bayer process is inexpensive.
However, this alumina has many soda components contained as impurities, and therefore has a poor electric insulating property, and is usually not used for manufacturing an electric substrate. Alumina has been provided in which the soda component is suppressed to a low level. However, since the content of impurities such as silicon (Si) and transition metal (Fe, etc.) is high, the heat conductivity is poor and it is used for aluminum nitride substrates. Cannot be used.
このような理由から、アルミナの炭素還元法は高純度の
アルミナを使用せざるを得ず、結局製造価格を高くして
いたのである。For this reason, the carbon reduction method of alumina was forced to use high-purity alumina, which eventually increased the manufacturing cost.
本発明は、以上のような事情に鑑みてなされたものであ
り、炭素還元法において、安価に高純度で、微粒子の窒
化アルミニウムを合成する方法を提供することを目的と
する。The present invention has been made in view of the above circumstances, and an object thereof is to provide a method for synthesizing aluminum nitride in the form of fine particles at a low cost with high purity in the carbon reduction method.
［課題を解決するための手段］ 本発明は、アルミニウム源としてアルミナまたは／およ
び水酸化アルミニウム使用し、これと塩基性塩化アルミ
ニウムおよび高温で炭素となる化合物および／または窒
素含有化合物を水と共に混合して均一に分散させた後、
乾燥して得られた混合物を窒素を含む非酸化性雰囲気中
で焼成することを特徴とする。Means for Solving the Problems The present invention uses alumina or / and aluminum hydroxide as a source of aluminum, which is mixed with basic aluminum chloride and a compound which becomes carbon at high temperature and / or a nitrogen-containing compound together with water. And evenly disperse
It is characterized in that the mixture obtained by drying is fired in a non-oxidizing atmosphere containing nitrogen.
本発明は、アルミニウム源としてアルミナ、水酸化アル
ミニウムが使用できる。これらは単独でも使用でき、あ
るいは両方を併用することもできる。本発明において
は、アルミニウム源として、たとえばバイヤー法により
得られるような安価なアルミナ、あるいはその原料とし
て使用される水酸化アルミニウムも使用することができ
る。In the present invention, alumina and aluminum hydroxide can be used as the aluminum source. These can be used alone or in combination of both. In the present invention, as the aluminum source, inexpensive alumina obtained by, for example, the Bayer method, or aluminum hydroxide used as the raw material thereof can also be used.
バイヤー法により得られるような安価なアルミナは、通
常は比較的多量のソーダ成分を含有するが、ここではロ
ーソーダアルミナと称せられる、Na2Oの含有量が0.1重
量％以下のものが使用される。ローソーダアルミナであ
っても、なお不純物としてSiやFe等の遷移金属を含有す
るが、本発明においてはこのようなものでも使用でき
る。Inexpensive alumina such as that obtained by the Bayer method usually contains a relatively large amount of soda components, but here, so-called low soda alumina, which has a Na 2 O content of 0.1% by weight or less, is used. R. Even low-soda alumina still contains transition metals such as Si and Fe as impurities, but such substances can also be used in the present invention.
高温で炭素となる化合物としては、特に限定するもので
はないが、たとえばメチルセルロース、ポリエチレンオ
キサイド、ポリビニルアルコール、リグニン、糖類（グ
ルコース等）、炭素等が使用でき、特に水溶性の化合物
が望ましい。なお、ここで炭素は化合物ではないが、こ
こでは高温で炭素となる化合物として扱う。The compound which becomes carbon at high temperature is not particularly limited, but for example, methyl cellulose, polyethylene oxide, polyvinyl alcohol, lignin, sugars (glucose etc.), carbon and the like can be used, and a water-soluble compound is particularly desirable. Although carbon is not a compound here, it is treated here as a compound that becomes carbon at high temperature.
窒素含有化合物としては、特に限定するものではない
が、たとえばグリシン、カルボニルヒドラジド、エチレ
ンジアミン、尿素、メラミン等が使用でき、特に水溶性
の化合物が望ましい。The nitrogen-containing compound is not particularly limited, but glycine, carbonyl hydrazide, ethylenediamine, urea, melamine and the like can be used, and a water-soluble compound is particularly desirable.
本発明においては、以上の原料のほかに塩基性塩化アル
ミニウムを使用する。In the present invention, basic aluminum chloride is used in addition to the above raw materials.
以上の原料は水と共に混合され、つぎに乾燥されて原料
が均一に混合された混合物を得る。乾燥温度は、150〜2
00℃が好ましいが限定するものではない。なお、水溶性
の原料を使用すると混合がより均一に行えるので都合が
よい。The above raw materials are mixed with water and then dried to obtain a mixture in which the raw materials are uniformly mixed. Drying temperature is 150 ~ 2
00 ° C is preferable, but not limited thereto. In addition, it is convenient to use a water-soluble raw material because the mixing can be performed more uniformly.
乾燥されて得られた混合粉末は、窒素を含む非酸化性雰
囲気の中で焼成される。窒素を含む非酸化性雰囲気と
は、窒素ガス、アンモニア等またはこれらを含む非酸化
性ガスが使用される。窒素ガス、アンモニアを含有して
おればアルゴン等の不活性ガス、一酸化炭素ガス等も使
用できる。The dried mixed powder is fired in a non-oxidizing atmosphere containing nitrogen. As the non-oxidizing atmosphere containing nitrogen, nitrogen gas, ammonia or the like or non-oxidizing gas containing these is used. If nitrogen gas or ammonia is contained, an inert gas such as argon, carbon monoxide gas or the like can be used.
焼成過程においては、塩基性塩化アルミニウムの中に含
まれる塩素の作用により、アルミナ中に含有される不純
物、たとえばSi、Fe、場合によってはNa等が塩素化さ
れ、塩化物として気相中に除去される。したがって、純
度の低いアルミニウム源を使用しても高純度な窒化アル
ミニウムを得ることができる。なお、塩基性塩化アルミ
ニウムは比較的高温まで安定であり、不純物の塩素化を
容易に達成することができる。During the firing process, chlorine contained in basic aluminum chloride chlorinates impurities contained in alumina, such as Si, Fe, and Na in some cases, and removes them as chlorides in the gas phase. To be done. Therefore, high-purity aluminum nitride can be obtained even if an aluminum source with low purity is used. In addition, basic aluminum chloride is stable up to a relatively high temperature, and chlorination of impurities can be easily achieved.
前記の混合物の焼成温度は1300〜1700℃の範囲が好まし
いが限定するものではない。The firing temperature of the mixture is preferably in the range of 1300 to 1700 ° C, but is not limited thereto.
なお、本発明において、原料を水と共に混合して均一混
合する際に、同時に基板焼成時にフラックスとして作用
する、酸化イットリウム（Y2O3）や酸化カルシウム（Ca
O）となる化合物を溶かし込んでおくことにより、窒化
アルミニウム粉末中にフラックス成分が均一に、あるい
は固溶した状態で均一に分散した窒化アルミニウム粉末
を得ることができ、基板の焼結に都合がよい。前記の原
料混合物が水溶液状で、あるいはより水溶液に近い状態
で得られると、一層均一混合ができて都合がよい。In the present invention, yttrium oxide (Y 2 O 3 ) and calcium oxide (Ca 2
By dissolving the compound that becomes O) in advance, it is possible to obtain an aluminum nitride powder in which the flux component is uniformly dispersed in the aluminum nitride powder or in a solid solution state, which is convenient for sintering the substrate. Good. When the above-mentioned raw material mixture is obtained in the form of an aqueous solution or in a state closer to the aqueous solution, it is convenient because more uniform mixing can be achieved.
実施例 ローソーダアルミナ、塩基性塩化アルミニウム、高温で
炭素となる化合物、窒素含有化合物と水を混合して水懸
濁液を得た。これをスプレードライヤーで乾燥した後、
窒素ガス気流中で所定温度で焼成して窒化アルミニウム
粉末を得た。Example A water suspension was obtained by mixing low soda alumina, basic aluminum chloride, a compound that becomes carbon at high temperature, and a nitrogen-containing compound with water. After drying this with a spray dryer,
Aluminum nitride powder was obtained by firing at a predetermined temperature in a nitrogen gas stream.
なお、ローソーダアルミナとしては、住友化学工業株式
会社製のAES-11C（平均粒径0.4μｍ）またはALM-41（平
均粒径1.8μｍ）を使用した。As the low soda alumina, AES-11C (average particle size 0.4 μm) or ALM-41 (average particle size 1.8 μm) manufactured by Sumitomo Chemical Co., Ltd. was used.
高温で炭素となる化合物としては、グルコースまたはメ
チルセルロースまたは炭素粉末を使用した。窒素含有化
合物としては尿素を使用した。塩基性塩化アルミニウム
としては、Al2O3換算のアルミニウム含有量が50重量
％、塩基度が84重量％のものを使用した。Glucose, methyl cellulose, or carbon powder was used as the compound that becomes carbon at high temperature. Urea was used as the nitrogen-containing compound. The basic aluminum chloride used had an aluminum content of 50% by weight in terms of Al 2 O 3 and a basicity of 84% by weight.
実施結果を第１表に示した。The execution results are shown in Table 1.
［発明の効果］ この発明は、アルミナまたは／および水酸化アルミニウ
ムおよび塩基性塩化アルミニウムおよび高温で炭素とな
る化合物および／または窒素含有化合物を水と共に混合
して均一に分散させた後、乾燥して得られた混合物を窒
素を含む非酸化性雰囲気中で焼成することを特徴とする
ので、アルミニウム源中の不純物が除去でき、純度の高
い窒化アルミニウムを得ることができる効果がある。 EFFECTS OF THE INVENTION The present invention is that alumina or / and aluminum hydroxide, basic aluminum chloride, a compound that becomes carbon at high temperature, and / or a nitrogen-containing compound are mixed with water and uniformly dispersed, and then dried. Since the obtained mixture is baked in a non-oxidizing atmosphere containing nitrogen, impurities in the aluminum source can be removed, and aluminum nitride with high purity can be obtained.
また、アルミナとして、ローソーダアルミナまたはロー
ソーダアルミナの製造に使用される水酸化アルミニウム
を使用すると、安価な窒化アルミニウムを製造すること
ができる。Further, when alumina of low soda alumina or aluminum hydroxide used for producing low soda alumina is used as alumina, inexpensive aluminum nitride can be produced.
さらに、高温で炭素となる化合物および窒素含有化合物
として、水溶性のものを使用すると、より均一で微細な
窒化アルミニウムの粉末を得ることができる。Furthermore, if a water-soluble compound is used as the compound that becomes carbon at high temperature and the nitrogen-containing compound, a more uniform and fine powder of aluminum nitride can be obtained.
Claims (3)
ムおよび塩基性塩化アルミニウムおよび高温で炭素とな
る化合物および／または窒素含有化合物を水と共に混合
して均一に分散させた後、乾燥して得られた混合物を窒
素を含む非酸化性雰囲気中で焼成することを特徴とする
窒化アルミニウムの製法。1. A mixture obtained by mixing alumina or / and aluminum hydroxide, basic aluminum chloride, a compound that becomes carbon at high temperature and / or a nitrogen-containing compound with water to uniformly disperse the mixture, and then drying. Is produced in a non-oxidizing atmosphere containing nitrogen.
はローソーダアルミナの製造に使用される水酸化アルミ
ニウムを使用することを特徴とする特許請求の範囲第１
項記載の窒化アルミニウムの製法。2. Alumina is low-soda alumina or aluminum hydroxide used in the production of low-soda alumina.
The method for producing aluminum nitride according to the item.
合物として、水溶性のものを使用することを特徴とする
特許請求の範囲第１項または第２項記載の窒化アルミニ
ウムの製法。3. The method for producing aluminum nitride according to claim 1 or 2, wherein a water-soluble compound is used as the compound which becomes carbon at a high temperature and the nitrogen-containing compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12876588A JPH0686286B2 (en) | 1988-05-26 | 1988-05-26 | Manufacturing method of aluminum nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12876588A JPH0686286B2 (en) | 1988-05-26 | 1988-05-26 | Manufacturing method of aluminum nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01298012A JPH01298012A (en) | 1989-12-01 |
| JPH0686286B2 true JPH0686286B2 (en) | 1994-11-02 |
Family
ID=14992918
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12876588A Expired - Fee Related JPH0686286B2 (en) | 1988-05-26 | 1988-05-26 | Manufacturing method of aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0686286B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4753851B2 (en) * | 2005-12-19 | 2011-08-24 | 日本碍子株式会社 | Aluminum nitride powder, aluminum nitride ceramic sintered body, semiconductor manufacturing apparatus member, aluminum nitride light-emitting material, and aluminum nitride powder manufacturing method |
| CN113480828B (en) * | 2021-03-02 | 2022-06-14 | 海南大学 | Aluminum nitride nanoflower/polymer composite material and preparation method thereof |
| CN116730303B (en) * | 2023-07-11 | 2026-02-13 | 河北工业大学 | A method for preparing highly dispersible aluminum nitride spherical particles |
| CN117534478B (en) * | 2023-11-23 | 2025-10-31 | 西安稀有金属材料研究院有限公司 | Preparation method of aluminum nitride nano powder based on dual activation |
-
1988
- 1988-05-26 JP JP12876588A patent/JPH0686286B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01298012A (en) | 1989-12-01 |
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