JPH04321504A - Production of aluminum nitride fiber - Google Patents
Production of aluminum nitride fiberInfo
- Publication number
- JPH04321504A JPH04321504A JP9241691A JP9241691A JPH04321504A JP H04321504 A JPH04321504 A JP H04321504A JP 9241691 A JP9241691 A JP 9241691A JP 9241691 A JP9241691 A JP 9241691A JP H04321504 A JPH04321504 A JP H04321504A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- weight
- guanidine
- aluminum
- nitride fibers
- 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.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 44
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- 150000002357 guanidines Chemical class 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229960000789 guanidine hydrochloride Drugs 0.000 claims description 6
- YJYREIFZLKWHMM-UHFFFAOYSA-N (diaminomethylideneamino) hydrogen carbonate Chemical compound NC(N)=NOC(O)=O YJYREIFZLKWHMM-UHFFFAOYSA-N 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- UBDZFAGVPPMTIT-UHFFFAOYSA-N 2-aminoguanidine;hydron;chloride Chemical compound [Cl-].NC(N)=N[NH3+] UBDZFAGVPPMTIT-UHFFFAOYSA-N 0.000 claims description 4
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 claims description 4
- STIAPHVBRDNOAJ-UHFFFAOYSA-N carbamimidoylazanium;carbonate Chemical compound NC(N)=N.NC(N)=N.OC(O)=O STIAPHVBRDNOAJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005121 nitriding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 1
- 239000011369 resultant mixture Substances 0.000 abstract 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 18
- 150000001875 compounds Chemical class 0.000 description 11
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 9
- 238000010304 firing Methods 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000010292 electrical insulation Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-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
- GURLNXRFQUUOMW-UHFFFAOYSA-K [Al](Cl)(Cl)Cl.[AlH3] Chemical compound [Al](Cl)(Cl)Cl.[AlH3] GURLNXRFQUUOMW-UHFFFAOYSA-K 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229940083094 guanine derivative acting on arteriolar smooth muscle Drugs 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- -1 that is Chemical compound 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】この発明は、窒化アルミニウム繊
維の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention This invention relates to a method for producing aluminum nitride fibers.
【０００２】0002
【従来の技術】窒化アルミニウムは、電気絶縁性と高熱
伝導性を有するとともに、熱膨張性がシリコンのそれに
近く、近年、ＩＣの高集積化・高出力化に対応した高放
熱性材料として注目されている。ただ、従来、利用され
ている窒化アルミニウムは粉末状である。窒化アルミニ
ウムの有効利用を図るためには、繊維状のもの、すなわ
ち窒化アルミニウム繊維が強く望まれている。[Prior Art] Aluminum nitride has electrical insulation properties and high thermal conductivity, and its thermal expansion property is close to that of silicon. In recent years, aluminum nitride has attracted attention as a material with high heat dissipation that is compatible with higher integration and higher output of ICs. ing. However, the aluminum nitride conventionally used is in powder form. In order to effectively utilize aluminum nitride, fibrous materials, that is, aluminum nitride fibers, are strongly desired.
【０００３】窒化アルミニウム繊維は、例えば、アルミ
ニウム含有化合物と炭素含有化合物を混合し、繊維状に
成形した後、窒素を含む非酸化性雰囲気で焼成し還元窒
化することで得られるが、得られた窒化アルミニウム繊
維は、高いＡｌＮ純度で高密度のものである必要がある
。そのため、この場合、還元窒化を行う際には、還元用
の炭素を下式に示す理論値よりも過剰に存在させる必要
がある。[0003] Aluminum nitride fibers can be obtained, for example, by mixing an aluminum-containing compound and a carbon-containing compound, forming the mixture into a fiber, and then firing and reducing and nitriding it in a non-oxidizing atmosphere containing nitrogen. The aluminum nitride fibers need to be of high AlN purity and high density. Therefore, in this case, when performing reductive nitridation, it is necessary to make reducing carbon exist in excess of the theoretical value shown in the formula below.
【０００４】
Ａｌ２ Ｏ ３＋３Ｃ＋Ｎ２ →２ＡｌＮ＋３ＣＯしか
しながら、所定の還元が確実になされる量で還元用の炭
素を過剰に存在させると、焼成を終えた段階で炭素が多
く残留するので、焼成後に残留炭素除去のための熱処理
をさらに行わなければならない。残留炭素の量が多いと
電気的絶縁性が十分でなくなるからである。最初の段階
では還元用炭素の過剰添加を止め、途中の段階で炭素を
後添加して補い残留炭素の量を抑えることも可能ではあ
る。しかしながら、前者は残留炭素除去のための熱処理
を要し、後者は炭素の後添加を要し、製造工程が増える
ため、いずれの場合も今ひとつ実用的であるとは言えな
い。Al2O 3+3C+N2 →2AlN+3COHowever, if carbon for reduction is present in excess in an amount that ensures the specified reduction, a large amount of carbon will remain after firing, so it is difficult to remove residual carbon after firing. Further heat treatment must be performed for this purpose. This is because if the amount of residual carbon is large, electrical insulation will not be sufficient. It is possible to suppress the amount of residual carbon by stopping the excessive addition of reducing carbon in the first stage and supplementing it by adding carbon later in the middle of the process. However, the former requires heat treatment to remove residual carbon, and the latter requires post-addition of carbon, increasing the number of manufacturing steps, so neither case can be said to be very practical.
【０００５】[0005]
【発明が解決しようとする課題】この発明は、上記事情
に鑑み、ＡｌＮ純度が高く緻密で残存炭素の少ない有用
な窒化アルミニウム繊維を容易に得ることのできる方法
を提供することを課題とする。SUMMARY OF THE INVENTION In view of the above circumstances, it is an object of the present invention to provide a method by which useful aluminum nitride fibers with high AlN purity, denseness, and low residual carbon can be easily obtained.
【０００６】[0006]
【課題を解決するための手段】前記課題を解決するため
、請求項１記載の窒化アルミニウム繊維の製造方法は、
アルミニウム多核錯体とグアニジン誘導体とを混合し、
繊維状に成形した後、窒素を含む非酸化性雰囲気で焼成
し、ＡｌＮ純度９４重量％以上の窒化アルミニウム繊維
を得るようにしている。[Means for Solving the Problems] In order to solve the above problems, a method for manufacturing aluminum nitride fibers according to claim 1 includes the following steps:
Mixing an aluminum polynuclear complex and a guanidine derivative,
After being formed into a fiber, it is fired in a non-oxidizing atmosphere containing nitrogen to obtain an aluminum nitride fiber with an AlN purity of 94% by weight or more.
【０００７】以下、この発明の窒化アルミニウム繊維の
製造方法をより具体的に説明する。この発明で用いる原
料の一つであるアルミニウム多核錯体（アルミニウム含
有化合物）としては、塩基性塩化アルミニウム、塩基性
乳酸アルミニウム、塩基性硫酸アルミニウム、塩基性酢
酸アルミニウムなどが挙げられる。この発明で用いる原
料の一つであるグアニジン誘導体としては、炭酸グアニ
ジン、塩酸グアニジン、重炭酸グアニジン、塩酸アミノ
グアニジンなどが挙げられる。これらのグアニジン誘導
体は炭素含有化合であり、還元用の炭素を提供するもの
であることは言うまでもない。The method for producing aluminum nitride fibers of the present invention will be explained in more detail below. Examples of the aluminum polynuclear complex (aluminum-containing compound) that is one of the raw materials used in this invention include basic aluminum chloride, basic aluminum lactate, basic aluminum sulfate, and basic aluminum acetate. Examples of the guanidine derivative that is one of the raw materials used in this invention include guanidine carbonate, guanidine hydrochloride, guanidine bicarbonate, and aminoguanidine hydrochloride. It goes without saying that these guanidine derivatives are carbon-containing compounds and provide carbon for reduction.
【０００８】まず、原料のアルミニウム多核錯体とグア
ニジン誘導体の混合溶液を作るのであるが、この混合溶
液には繊維成形性をもたせるための高分子化合物（例え
ば、ポリエチレンオキサイド）も含ませるようにする。
この高分子化合物は量的に少なくて窒化還元反応には殆
ど影響しないのであるが、混合溶液に所定の粘性をもた
せるとともに紡糸性をもたせるために必要だからである
。この繊維成形性をもたせるための高分子化合物として
は、ポリエチレンオキサイドの他に、ポリビニルアルコ
ールやメチルセルロース等が具体的に挙げられる。First, a mixed solution of a raw material aluminum polynuclear complex and a guanidine derivative is prepared, and this mixed solution also contains a polymer compound (for example, polyethylene oxide) for imparting fiber formability. This is because, although the amount of this polymer compound is small and it hardly affects the nitriding-reduction reaction, it is necessary to give the mixed solution a predetermined viscosity and spinnability. In addition to polyethylene oxide, polyvinyl alcohol, methylcellulose, and the like can be specifically mentioned as the polymer compound for imparting this fiber formability.
【０００９】混合の際のアルミニウム多核錯体とグアニ
ジン誘導体との間のＣ／Ａｌモル比が２．５〜６．０の
範囲となるように両者を配合することが好ましい。とい
うのは、Ｃ／Ａｌモル比が２．５を下回ると９４重量％
以上のＡｌＮ純度や必要な緻密度の確保が難しく、Ｃ／
Ａｌモル比が６．０を上回ると０．５重量％以下の残留
炭素含有量や必要な緻密度の確保が難しいからである。
ＡｌＮ純度が９４重量％未満では熱伝導性が十分である
とは言えず、残留炭素が０．５重量％を越えると電気的
絶縁性が十分であるとは言えない。[0009] It is preferable that the aluminum polynuclear complex and the guanidine derivative be blended so that the C/Al molar ratio is in the range of 2.5 to 6.0. This is because when the C/Al molar ratio is less than 2.5, 94% by weight
It is difficult to secure the above AlN purity and the necessary density, and C/
This is because if the Al molar ratio exceeds 6.0, it is difficult to ensure a residual carbon content of 0.5% by weight or less and a necessary density. If the AlN purity is less than 94% by weight, it cannot be said that the thermal conductivity is sufficient, and if the residual carbon exceeds 0.5% by weight, it cannot be said that the electrical insulation is sufficient.
【００１０】このようにして、原料混合溶液を得て繊維
状に成形した後、この繊維状成形物を窒素を含む非酸化
性雰囲気で焼成し、窒化アルミニウム繊維を得る。窒素
を含む非酸化性雰囲気としては、窒素のみからなる雰囲
気、窒素を含むアルゴン雰囲気、窒素を含む一酸化炭素
雰囲気、アンモニア雰囲気等が挙げられる。焼成温度は
、通常、１４００〜１９００℃程度の範囲である。[0010] After obtaining the raw material mixed solution and molding it into a fibrous shape in this manner, the fibrous molded product is fired in a non-oxidizing atmosphere containing nitrogen to obtain aluminum nitride fibers. Examples of the non-oxidizing atmosphere containing nitrogen include an atmosphere consisting only of nitrogen, an argon atmosphere containing nitrogen, a carbon monoxide atmosphere containing nitrogen, an ammonia atmosphere, and the like. The firing temperature is usually in the range of about 1400 to 1900°C.
【００１１】なお、この発明で用いられる化合物や処理
条件等は、上記例示のものに限らないことは言うまでも
ない。[0011] It goes without saying that the compounds and processing conditions used in this invention are not limited to those exemplified above.
【００１２】0012
【作用】この発明によれば、焼成後の残存炭素除去のた
めの熱処理や途中段階での炭素の後添加を行わずとも、
残留炭素が少なく（０．５重量％以下）、ＡｌＮ純度が
高く（９４重量％以上）て緻密（相対密度９７％以上）
な窒化アルミニウム繊維が容易に得られる。これは、Ａ
ｌ含有化合物にアルミニウム多核錯体を炭素供給源にグ
アニジン誘導体を用い両出発原料を混合させる段階を経
る場合は、両者がＡｌＮ前駆物を生成して、還元用炭素
とＡｌ含有化合物の酸素が近接し炭素がそれほど過剰で
なくても還元窒化が進み易いからであると考えられる。[Operation] According to the present invention, even without heat treatment to remove residual carbon after firing or post-addition of carbon at an intermediate stage,
Low residual carbon (0.5% by weight or less), high AlN purity (94% by weight or more), and dense (relative density 97% or more)
aluminum nitride fibers can be easily obtained. This is A
When going through the step of mixing both starting materials using an aluminum polynuclear complex for the l-containing compound and a guanidine derivative for the carbon source, both produce an AlN precursor, and the reducing carbon and the oxygen of the Al-containing compound come close to each other. This is thought to be because reductive nitridation tends to proceed even if carbon is not excessively large.
【００１３】[0013]
【実施例】以下、この発明の実施例を説明する。
−実施例１−
ポリエチレンオキサイド１重量％溶液に重炭酸グアニジ
ンと塩基性塩化アルミニウムを溶解し、繊維状に成形・
乾燥し繊維状成形物を得た。なお、重炭酸グアニジンと
塩基性塩化アルミニウムとの間のＣ／Ａｌモル比は３．
０である。また、ポリエチレンオキサイドは平均分子量
４００万以上（アルコックスＥ−１６０明成化学工業（
株）製）のものを用いた。[Embodiments] Examples of the present invention will be described below. -Example 1- Guanidine bicarbonate and basic aluminum chloride were dissolved in a 1% by weight solution of polyethylene oxide, and formed into a fiber shape.
It was dried to obtain a fibrous molded product. Note that the C/Al molar ratio between guanidine bicarbonate and basic aluminum chloride is 3.
It is 0. In addition, polyethylene oxide has an average molecular weight of 4 million or more (Alcox E-160 Meisei Chemical Industry Co., Ltd.)
Co., Ltd.) was used.
【００１４】つぎに、作成した繊維状成形物を、Ｎ２
気流中、１７００℃の温度、３時間の焼成で還元窒化し
、窒化アルミニウム繊維を得た。得られた繊維は、Ａｌ
Ｎ純度９７重量％、残存炭素量０．１０重量％、密度９
８％であった。
−実施例２−
ポリエチレンオキサイド１重量％溶液に塩酸アミノグア
ニジンと塩基性乳酸アルミニウムを溶解し、繊維状に成
形・乾燥し繊維状成形物を得た。なお、塩酸アミノグア
ニジンと塩基性乳酸アルミニウムとの間のＣ／Ａｌモル
比は４．７である。この他は、実施例１と同様にして、
窒化アルミニウム繊維を得た。[0014] Next, the produced fibrous molded product was heated with N2
Reduction nitridation was performed by firing in an air stream at a temperature of 1700° C. for 3 hours to obtain aluminum nitride fibers. The obtained fiber is Al
N purity 97% by weight, residual carbon content 0.10% by weight, density 9
It was 8%. -Example 2- Aminoguanidine hydrochloride and basic aluminum lactate were dissolved in a 1% by weight solution of polyethylene oxide, molded into a fibrous form, and dried to obtain a fibrous molded product. Note that the C/Al molar ratio between aminoguanidine hydrochloride and basic aluminum lactate is 4.7. Other than this, the same procedure as in Example 1 was carried out.
Aluminum nitride fibers were obtained.
【００１５】得られた繊維は、ＡｌＮ純度９６重量％、
残存炭素量０．１３重量％、密度９８．５％であった。
−実施例３−
ポリエチレンオキサイド０．５重量％溶液に塩酸グアニ
ジンと塩基性塩化アルミニウムを溶解し、繊維状に成形
・乾燥し繊維状成形物を得た。なお、塩酸グアニジンと
塩基性塩化アルミニウムとの間のＣ／Ａｌモル比は３．
５である。この他は、実施例１と同様にして、窒化アル
ミニウム繊維を得た。The obtained fiber had an AlN purity of 96% by weight,
The amount of residual carbon was 0.13% by weight, and the density was 98.5%. -Example 3- Guanidine hydrochloride and basic aluminum chloride were dissolved in a 0.5% by weight solution of polyethylene oxide, molded into a fibrous form and dried to obtain a fibrous molded product. Note that the C/Al molar ratio between guanidine hydrochloride and basic aluminum chloride is 3.
It is 5. Other than this, aluminum nitride fibers were obtained in the same manner as in Example 1.
【００１６】得られた繊維は、ＡｌＮ純度９７重量％、
残存炭素量０．０９重量％、密度９８．５％であった。
−実施例４−
ポリエチレンオキサイド０．８重量％溶液に塩酸グアニ
ジンと塩基性塩化アルミニウムを溶解し、繊維状に成形
・乾燥し繊維状成形物を得た。なお、塩酸グアニジンと
塩基性塩化アルミニウムとの間のＣ／Ａｌモル比は２．
５であった。また、ポリエチレンオキサイドは平均分子
量４００万以上（アルコックスＥ−１６０明成化学工業
（株）製）のものを用いた。The obtained fiber had an AlN purity of 97% by weight,
The amount of residual carbon was 0.09% by weight, and the density was 98.5%. - Example 4 - Guanidine hydrochloride and basic aluminum chloride were dissolved in a 0.8% by weight solution of polyethylene oxide, molded into a fibrous form and dried to obtain a fibrous molded product. Note that the C/Al molar ratio between guanidine hydrochloride and basic aluminum chloride is 2.
It was 5. The polyethylene oxide used had an average molecular weight of 4 million or more (Alcox E-160 manufactured by Meisei Chemical Industry Co., Ltd.).
【００１７】得られた繊維状成形物を、Ｎ２ 気流中、
１９００℃の温度、３時間の焼成で還元窒化し、窒化ア
ルミニウム繊維を得た。得られた繊維は、ＡｌＮ純度９
８重量％、残存炭素量０．０９重量％、密度９９％であ
った。
−比較例１−
ポリエチレンオキサイド１重量％溶液にグルコースと塩
基性塩化アルミニウムを溶解し、繊維状に成形・乾燥し
繊維状成形物を得た。なお、グルコースと塩基性塩化ア
ルミニウムとの間のＣ／Ａｌモル比は３．０である。こ
れ以外は、実施例１と同様にして、窒化アルミニウム繊
維を得た。[0017] The obtained fibrous molded product was placed in a N2 gas stream.
Reduction nitridation was performed by firing at a temperature of 1900° C. for 3 hours to obtain aluminum nitride fibers. The obtained fiber has an AlN purity of 9
The carbon content was 8% by weight, the amount of residual carbon was 0.09% by weight, and the density was 99%. - Comparative Example 1 - Glucose and basic aluminum chloride were dissolved in a 1% by weight solution of polyethylene oxide, molded into a fibrous form and dried to obtain a fibrous molded product. Note that the C/Al molar ratio between glucose and basic aluminum chloride is 3.0. Except for this, aluminum nitride fibers were obtained in the same manner as in Example 1.
【００１８】得られた繊維は、ＡｌＮ純度９６重量％、
残存炭素量１．１重量％、密度８０％であった。密度が
低いと非常に脆く壊れやすい。
−参考例１−
重炭酸グアニジンと塩基性塩化アルミニウムとの間のＣ
／Ａｌモル比が２．０である他は、実施例１と同様にし
て窒化アルミニウム繊維を得た。The obtained fiber had an AlN purity of 96% by weight,
The amount of residual carbon was 1.1% by weight, and the density was 80%. If the density is low, it becomes very brittle and breaks easily. -Reference Example 1- C between guanidine bicarbonate and basic aluminum chloride
Aluminum nitride fibers were obtained in the same manner as in Example 1 except that the /Al molar ratio was 2.0.
【００１９】得られた繊維は、ＡｌＮ純度が８７重量％
と低かった。
−参考例２−
重炭酸グアニジンと塩基性塩化アルミニウムとの間のＣ
／Ａｌモル比が７．０である他は、実施例１と同様にし
て窒化アルミニウム繊維を得た。得られた繊維は、残存
炭素量が１．０重量％、密度が８７％と十分なものにな
らなかった。The obtained fiber had an AlN purity of 87% by weight.
It was low. -Reference Example 2- C between guanidine bicarbonate and basic aluminum chloride
Aluminum nitride fibers were obtained in the same manner as in Example 1 except that the /Al molar ratio was 7.0. The obtained fiber had a residual carbon content of 1.0% by weight and a density of 87%, which was not sufficient.
【００２０】[0020]
【発明の効果】以上に述べたように、この発明にかかる
製造方法によれば、Ａｌ含有化合物にアルミニウム多核
錯体を炭素源にグアニジン誘導体を用い混合させる段階
を経るため、焼成後の残存炭素除去のための熱処理や途
中段階での炭素の後添加を行わずとも、残留炭素の少な
い高ＡｌＮ純度（９４重量％以上）で緻密な窒化アルミ
ニウム繊維が容易に得られる。[Effects of the Invention] As described above, according to the production method of the present invention, the step of mixing an aluminum polynuclear complex with an Al-containing compound using a guanidine derivative as a carbon source makes it possible to remove residual carbon after firing. Dense aluminum nitride fibers with high AlN purity (94% by weight or more) with little residual carbon can be easily obtained without performing any heat treatment or post-addition of carbon during the process.
【００２１】残存炭素量が０．５重量％以下の窒化アル
ミニウム繊維は電気絶縁性が高く有用性が高い。アルミ
ニウム多核錯体とグアニジン誘導体との間のＣ／Ａｌモ
ル比が２．５〜６．０の範囲の場合は、９４重量％以上
のＡｌＮ純度で残存炭素量が０．５重量％以下の窒化ア
ルミニウム繊維を確実に得ることができる。[0021] Aluminum nitride fibers having a residual carbon content of 0.5% by weight or less have high electrical insulation properties and are highly useful. When the C/Al molar ratio between the aluminum polynuclear complex and the guanidine derivative is in the range of 2.5 to 6.0, aluminum nitride with an AlN purity of 94% by weight or more and a residual carbon content of 0.5% by weight or less Fibers can be obtained reliably.
Claims (4)
導体とを混合し、繊維状に成形した後、窒素を含む非酸
化性雰囲気で焼成し、ＡｌＮ純度９４重量％以上の窒化
アルミニウム繊維を得るようにする窒化アルミニウム繊
維の製造方法。Claim 1: Nitriding in which an aluminum polynuclear complex and a guanidine derivative are mixed, formed into a fiber, and then fired in a non-oxidizing atmosphere containing nitrogen to obtain aluminum nitride fiber with an AlN purity of 94% by weight or more. Method for producing aluminum fiber.
炭素量が０．５重量％以下である請求項１記載の窒化ア
ルミニウム繊維の製造方法。2. The method for producing aluminum nitride fibers according to claim 1, wherein the residual carbon content of the obtained aluminum nitride fibers is 0.5% by weight or less.
アニジン誘導体との間のＣ／Ａｌモル比が２．５〜６．
０の範囲となるように配合する請求項１または２記載の
窒化アルミニウム繊維の製造方法。3. The C/Al molar ratio between the aluminum polynuclear complex and the guanidine derivative during mixing is 2.5 to 6.
3. The method for producing aluminum nitride fibers according to claim 1 or 2, wherein the aluminum nitride fibers are blended so as to be in the range of 0.
、重炭酸グアニジン、塩酸アミノグアニジン、炭酸グア
ニジンのうちの少なくとも一つである請求項１から３ま
でのいずれかに記載の窒化アルミニウム繊維の製造方法
。4. The method for producing aluminum nitride fibers according to claim 1, wherein the guanidine derivative is at least one of guanidine hydrochloride, guanidine bicarbonate, aminoguanidine hydrochloride, and guanidine carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9241691A JPH04321504A (en) | 1991-04-23 | 1991-04-23 | Production of aluminum nitride fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9241691A JPH04321504A (en) | 1991-04-23 | 1991-04-23 | Production of aluminum nitride fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04321504A true JPH04321504A (en) | 1992-11-11 |
Family
ID=14053815
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9241691A Pending JPH04321504A (en) | 1991-04-23 | 1991-04-23 | Production of aluminum nitride fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04321504A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
| KR20170094123A (en) * | 2014-12-16 | 2017-08-17 | 니폰 케미콘 가부시키가이샤 | Method for producing metal compound particle group, metal compound particle group, and electrode for electricity storage device containing metal compound particle group |
-
1991
- 1991-04-23 JP JP9241691A patent/JPH04321504A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
| KR20170094123A (en) * | 2014-12-16 | 2017-08-17 | 니폰 케미콘 가부시키가이샤 | Method for producing metal compound particle group, metal compound particle group, and electrode for electricity storage device containing metal compound particle group |
| US11398626B2 (en) | 2014-12-16 | 2022-07-26 | Nippon Chemi-Con Corporation | Method of producing metal compound particle group, metal compound particle group, and electricity storage device electrode containing metal compound particle group |
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