JPH01224268A - Production of sintered aluminum nitride - Google Patents
Production of sintered aluminum nitrideInfo
- Publication number
- JPH01224268A JPH01224268A JP63051076A JP5107688A JPH01224268A JP H01224268 A JPH01224268 A JP H01224268A JP 63051076 A JP63051076 A JP 63051076A JP 5107688 A JP5107688 A JP 5107688A JP H01224268 A JPH01224268 A JP H01224268A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- thermal conductivity
- room temperature
- sintered body
- rare earth
- 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
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000000843 powder Substances 0.000 claims abstract description 22
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 11
- 239000000654 additive Substances 0.000 claims description 3
- 150000002222 fluorine compounds Chemical class 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 238000005121 nitriding Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 9
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 abstract description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 abstract description 6
- 229910001632 barium fluoride Inorganic materials 0.000 abstract description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract description 5
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 abstract description 5
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 abstract description 4
- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 abstract description 4
- 229910001637 strontium fluoride Inorganic materials 0.000 abstract description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 abstract 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000005452 bending Methods 0.000 description 12
- 229910001873 dinitrogen Inorganic materials 0.000 description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001938 gadolinium oxide Inorganic materials 0.000 description 2
- 229940075613 gadolinium oxide Drugs 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 229910001954 samarium oxide Inorganic materials 0.000 description 2
- 229940075630 samarium oxide Drugs 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 241000208195 Buxaceae Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 101800000560 Protein M1' Proteins 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000002747 voluntary 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)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は窒化アルミニウム焼結体の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for manufacturing an aluminum nitride sintered body.
近年、半導体工業の急速な技術革新によりＩＣ。 In recent years, due to rapid technological innovation in the semiconductor industry, IC.
ＬＳＩをはじめとする大規模集積回路は高集積化高出力
化が行われ、これに伴うシリコン素子の単位面積機りの
発熱量が大幅に増加してきた。そこで、シリコン素子の
通電動作による発熱のためシリコン素子の正常な動作を
妨ける問題が生じ始め ゛ている。それに伴って熱伝導
性の良い絶縁性基板材料が要求されている。Large-scale integrated circuits such as LSIs have become highly integrated and have high output, and as a result, the amount of heat generated per unit area of silicon devices has increased significantly. Therefore, a problem has begun to arise in which the normal operation of the silicon element is disturbed due to the heat generated by the current-carrying operation of the silicon element. Accordingly, insulating substrate materials with good thermal conductivity are required.
従来、絶縁性基板材料としては、一般にアルミナ焼結体
が最も多く使用されている。しかしながら、最近ではア
ルミナ基板は熱放散に関しては満足しているとは言えず
、さらに熱放散性（熱伝導性）の優れた絶縁性基板材料
の開発が要求されるよう罠なってきた。このような絶縁
基板材料としては熱伝導性が良い（熱伝導率が大きい）
、電気絶縁性である、熱膨張率がシリコン単結晶の値に
近い、機械的強度が大きい等の特性が要求される。Conventionally, alumina sintered bodies have generally been most commonly used as insulating substrate materials. However, recently, alumina substrates cannot be said to be satisfactory in terms of heat dissipation, and there has been a growing demand for the development of insulating substrate materials with even better heat dissipation (thermal conductivity). Good thermal conductivity for such an insulating substrate material (high thermal conductivity)
It is required to have properties such as electrical insulation, a coefficient of thermal expansion close to that of a silicon single crystal, and high mechanical strength.
ところで、良好な熱伝導性を有することが知られている
窒化アルミニウムは熱膨張率が約４．３Ｘ１０”−’／
’Ｃ（室温から４００℃の平均値）でアルミナ焼結体の
約７ Ｘ １０−’／”ＣＫ比べて小さく、シリコン素
子の熱膨張率３．５〜４．０Ｘ１０″／℃に近い。また
機械的強度も曲げ強さで約５０Ｋｇ／ｒｍ”程度を有し
、アルミナ焼結体の値２０〜３０ Ｋｑ／Ｉ！１ｍ”
Ｋ比べ高強度である電気絶縁性に優れた材料である。By the way, aluminum nitride, which is known to have good thermal conductivity, has a coefficient of thermal expansion of approximately 4.3X10"-'/
'C (average value from room temperature to 400°C) is smaller than that of an alumina sintered body, which is approximately 7 x 10'/'CK, and is close to the thermal expansion coefficient of a silicon element, which is 3.5 to 4.0 x 10'/'C. In addition, the mechanical strength is approximately 50 Kg/rm" in terms of bending strength, and the value of alumina sintered body is 20 to 30 Kq/I!1m"
It is a material with high strength and excellent electrical insulation properties compared to K.
従来、窒化アルミニウム（ＡＪ！Ｎ）焼結体は窒化アル
ミニウムの粉末を成形、焼結して得られるのであるが、
窒化アルミニウムは難焼結性物質であるため、緻密な焼
結体を得ることが困難である。Conventionally, aluminum nitride (AJ!N) sintered bodies are obtained by molding and sintering aluminum nitride powder.
Since aluminum nitride is a difficult-to-sinter substance, it is difficult to obtain a dense sintered body.
そして現在までに焼結助剤を加え、常圧焼結法やホット
プレス法により緻密な窒化アルミニウム焼結体を得る試
みがなされている。昭和５９年窯業協会年会予稿集のＰ
２Ｏ３には酸化イツトリウム（ＹｚＯｌ）を焼結助剤と
して加える窒化アルミニウム焼結体の製造方法が示され
ている。この方法によると熱伝導率が１００Ｗ／ｍｋ（
室温）の窒化アルミニウム焼結体が得られている。Up to now, attempts have been made to obtain a dense aluminum nitride sintered body by adding a sintering aid and using pressureless sintering or hot pressing. P of the proceedings of the 1981 Ceramics Association Annual Meeting
2O3 discloses a method for producing an aluminum nitride sintered body in which yttrium oxide (YzOl) is added as a sintering aid. According to this method, the thermal conductivity is 100W/mk (
An aluminum nitride sintered body at room temperature) was obtained.
しかしながら、近年め集積回路技術の発達に伴い、さら
に高熱伝導性を有する熱放散用基板材料が求められてい
る。However, with the recent development of integrated circuit technology, there has been a demand for heat dissipating substrate materials having even higher thermal conductivity.
本発明の目的は、高熱伝導性を有し、さらに種々の有用
な性質を有する窒化アルミニウム焼結体の製造方法を提
供することにある。An object of the present invention is to provide a method for producing an aluminum nitride sintered body having high thermal conductivity and various useful properties.
本発明の窒化アルミニウム焼結体の製造方法は、窒化ア
ルミニウム粉末に添加剤として希土類元素の酸化物のう
ち少くとも一種とアルカリ土類元素のフッ化物のうち少
くとも一種とを配合した混合粉末を形成後、非酸化性雰
囲気で焼成することを特徴とする。The method for producing an aluminum nitride sintered body of the present invention includes a mixed powder containing at least one kind of rare earth element oxide and at least one alkaline earth element fluoride as an additive to aluminum nitride powder. After formation, it is characterized by being fired in a non-oxidizing atmosphere.
希土類元素の酸化物は、酸化ランタン、酸化セリウム、
酸化ネオジウム、酸化サマリウム、酸化ガドリニウムが
好ましい。Oxides of rare earth elements include lanthanum oxide, cerium oxide,
Neodymium oxide, samarium oxide, and gadolinium oxide are preferred.
アルカリ土類元素のフッ化物はフッ化カルシウム、フッ
′化ストロンチウム、フッ化バリクムカ好ましい。Preferred examples of the alkaline earth element fluoride include calcium fluoride, strontium fluoride, and fluoride.
希土類元素の酸化物の添加量の合計は０．０５〜１５重
量％が好ましく、アルカリ土類元素のフッ化物の添加量
の合計は０．０５〜１２重量％が好ましい。The total amount of oxides of rare earth elements added is preferably 0.05 to 15% by weight, and the total amount of fluorides of alkaline earth elements added is preferably 0.05 to 12% by weight.
窒化アルミニウム原料は純度として高純度のも■、例え
ば９８チ以上のもＯが好ましいが、９５〜９８チ程度の
ものも使用可能である。平均粒径は１０μｍ以下、好ま
しくは２μｍ程度のものが良い。The aluminum nitride raw material preferably has a high purity, for example, 98% or more, but it is also possible to use aluminum nitride having a purity of about 95 to 98%. The average particle size is preferably 10 μm or less, preferably about 2 μm.
添加剤としては希土類元素の酸化物のうち少くとも一種
とアルカリ土類元素のフッ化物のうち少くとも一種との
両方を加えることが好ましい。それは、希土類元素の酸
化物とアルカリ土類元素のフッ化物とを適量複合使用す
る事により熱伝導率を著しく増大させることができるか
らである。As additives, it is preferable to add both at least one kind of oxide of rare earth elements and at least one kind of fluoride of alkaline earth elements. This is because thermal conductivity can be significantly increased by using an appropriate amount of rare earth element oxide and alkaline earth element fluoride in combination.
希土類元素の酸化物は、例えば、酸化ランタン。Examples of rare earth element oxides include lanthanum oxide.
酸化セリウム、酸化ネオジウム、酸化サマリウム。Cerium oxide, neodymium oxide, samarium oxide.
酸化ガドリニウムが好ましく、又、アルカリ土類元素の
フッ化物は、フッ化カルシウム、７ツ化ストロンチウム
、フッ化バリウムが好ましい。Gadolinium oxide is preferred, and the alkaline earth element fluoride is preferably calcium fluoride, strontium heptadide, or barium fluoride.
特に、希土類元素の酸化物の添加量の合計量を０．０５
〜１５重量％及びアルカリ土類元素の添加量の合計量を
０．０５〜１２重量％にする事により熱伝導率が１４０
Ｗ／ｍｋ （室温）以上となり、従来の窒化アルミニウ
ム焼結体より大きな値が得られる。In particular, the total amount of rare earth element oxides added is 0.05
-15% by weight and the total amount of alkaline earth elements added is 0.05-12% by weight, the thermal conductivity is 140%.
W/mk (room temperature) or higher, which is larger than the conventional aluminum nitride sintered body.
希土類元素の酸化物の添加量の合計は０．０５重ｊｋチ
以下では熱伝導率が１４０（Ｗ／ｍｋ）以下で効果が少
なく、１５重量−以上では異相が多くなるので熱伝導率
が１４０ （Ｗ／ｍ ｋ ）以下で小さくなる。If the total amount of rare earth element oxides added is less than 0.05 weight jk, the thermal conductivity will be less than 140 (W/mk), and the effect will be small, and if it is more than 15 weight, different phases will increase, so the thermal conductivity will be 140. (W/m k ) or less.
アルカリ土類元素のフッ化物の添加量の合計は０．０５
重ｘｉ以下では熱伝導率が１４０（Ｗ／ｍｋ）以下で効
果が少なく、１２重景−以上では異相が多くなるので熱
伝導率が１４０ （Ｗ／ｍｋ ）以下で小さくなる。The total amount of fluoride added to alkaline earth elements is 0.05
When the weight is below xi, the effect is small when the thermal conductivity is below 140 (W/mk), and when it is above 12 x x i, there are many different phases, so the thermal conductivity becomes small when it is below 140 (W/mk).
以上の理由により、希土類元素の酸化物の添加量の合計
は０．０５〜１５重量％、アルカリ土類元素のフッ化物
の添加量の合計は０．０５〜１２重量％が好ましい。For the above reasons, the total amount of rare earth element oxides added is preferably 0.05 to 15% by weight, and the total amount of alkaline earth element fluorides added is preferably 0.05 to 12% by weight.
次Ｋ、焼結は非酸化性雰囲気中で高温焼結することが必
要である。酸化性雰囲気中で焼結すると窒化アルミニウ
ムが酸化してしまい緻密な焼結体が得られない。非酸化
性雰囲気としては窒素ガス。Next, sintering requires high temperature sintering in a non-oxidizing atmosphere. If sintered in an oxidizing atmosphere, aluminum nitride will be oxidized and a dense sintered body will not be obtained. Nitrogen gas is used as a non-oxidizing atmosphere.
ヘリウムガス、アルゴンガス、−液化炭素ガス。Helium gas, argon gas, - liquefied carbon gas.
水素ガス、真空雰囲気などが使用できるが、中でモ窒素
ガス、アルゴンガス、ヘリクムガス、真空算囲気が便利
で好ましい。焼結は１５００〜２０００℃で行われ、特
［１６００〜２０００℃が有効であるが、特にこれらの
温度範囲に限定されるものでは無い、また焼結は常圧焼
結法でも良いし、加圧焼結法によって本良い。加圧焼結
法としてはホットプレス法（−軸加工焼結法）とＨＩＰ
法（熱間静水圧加圧焼結法）のどちらでも可能である。Hydrogen gas, vacuum atmosphere, etc. can be used, and nitrogen gas, argon gas, helium gas, and vacuum atmosphere are convenient and preferred. Sintering is performed at a temperature of 1,500 to 2,000°C, and 1,600 to 2,000°C is particularly effective, but it is not limited to these temperature ranges. Made using pressure sintering method. Pressure sintering methods include hot press method (-shaft processing sintering method) and HIP
Either method (hot isostatic pressing sintering method) is possible.
実施例１
平均粒径が２μｍの窒化アルミニウム粉末ＫＬａ２０３
とＣａ Ｆｚを添加し、次いでこの混合物粉末を室温で
２トン／−の圧力を加えて成形体とした。この成形体を
焼結炉において窒素ガス雰囲気下で２０００℃で１０時
間常圧焼結を行った。Example 1 Aluminum nitride powder KLa203 with an average particle size of 2 μm
and CaFz were added thereto, and then a pressure of 2 tons/- was applied to this powder mixture at room temperature to form a compact. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第１図は第１の実施例による窒化アルミニウム焼結体の
室温での熱伝導率を示す特性図でおる。FIG. 1 is a characteristic diagram showing the thermal conductivity at room temperature of the aluminum nitride sintered body according to the first example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−６／’Ｃ１曲げ強度は
約２．６トン／ＣＭ１”以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10-6/'C1, and the bending strength was about 2.6 tons/CM1'' or more.
尚、Ｌａ２Ｏ３ＣａＦｌ系は、成形後の取扱いに充分な
る注意を要さないと、成形体が膨潤し、ノ・ンドリンク
性が悪くなる。Note that if the La2O3CaFl type product is not handled with sufficient care after molding, the molded product will swell and the non-linkability will deteriorate.
実施例２
平均粒径が２μｍの窒化アルミニウム粉末ＫＬａｚＯ１
とＣａＦ２． ＳｒＦ２． ＢａＦ２の少くとも一種を
添加し、次いでこの混合物粉末を室温で２トン／ａｎ″
の圧力を加えて成形体とした。この成形体を焼結炉にお
いて窒素ガス雰囲気下で２０００℃で１０時間常圧焼結
を行った。Example 2 Aluminum nitride powder KLazO1 with an average particle size of 2 μm
and CaF2. SrF2. At least one type of BaF2 is added, and then the mixture powder is mixed at room temperature with 2 tons/an''
A molded body was obtained by applying a pressure of . This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第１表に第２の実施例による窒化アルミニウム焼結体の
室温での相対密度と熱伝導率を示す。Table 1 shows the relative density and thermal conductivity at room temperature of the aluminum nitride sintered body according to the second example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４３Ｘ１０−６／’Ｃ１曲げ強度は約
２．６トン／ａＩｌ”以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 43 x 10-6/'C1, and the bending strength was about 2.6 tons/al'' or more.
尚、ＬａｚＯｓ ＣａＦ２ 、 ＬａｗＯｓ ５ｒ
Ｆｚ系は、成形後の取扱いに充分なる注意を要さないと
、成形体が膨潤し、ハンドリング性が悪くなる。In addition, LazOs CaF2, LawOs 5r
If the Fz type product is not handled with sufficient care after molding, the molded product will swell and the handling properties will deteriorate.
第 １ 表 木印は比較例である。Chapter 1 Table The wooden seal is a comparative example.
実施例３
平均粒径が２μｍの窒化アルミニウム粉末にＣｅＯ２と
ＣａＦｌを添加し、次いでこの混合物粉末を室温で２ト
ン／口３の圧力を加えて成形体とした。この成形体を焼
結炉において窒素ガス雰囲気下で２０００℃で１０時間
常圧焼結を行った。Example 3 CeO2 and CaFl were added to aluminum nitride powder with an average particle size of 2 μm, and then this mixed powder was formed into a compact by applying a pressure of 2 tons/port 3 at room temperature. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第２図は第３の実施例による窒化アルミニウム焼結体の
室温での熱伝導率を示す特性図である。FIG. 2 is a characteristic diagram showing the thermal conductivity at room temperature of the aluminum nitride sintered body according to the third example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−’／℃、曲げ強度は約
２．６トン／−以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10-'/°C, and the bending strength was about 2.6 tons/- or more.
実施例４
平均粒径が２μｍの窒化アルミニウム粉末にＣｅＣｈと
ＣａＦｌ、 ５ｒＦｚ、 ＢａＦ２の少くとも一種を添
加し、次いでこの混合物粉末を室温で２トン／−の圧力
を加えて成形体とした。この成形体を焼結炉において窒
素ガス雰囲気下で２０００℃で１０時間常圧焼結を行っ
た。Example 4 At least one of CeCh, CaFl, 5rFz, and BaF2 was added to aluminum nitride powder having an average particle size of 2 μm, and then this mixed powder was formed into a compact by applying a pressure of 2 tons/− at room temperature. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第２表に第４の実施例による窒化アルミニウム焼結体の
室温での相対密度と熱伝導率を示す。Table 2 shows the relative density and thermal conductivity at room temperature of the aluminum nitride sintered body according to the fourth example.
本発明の製造方法により室温での熱伝導率が１４ｏＷ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−’／’Ｃ１曲げ強度は
約２，６トン／ａｘＬ”以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 14oW/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10-'/'C1 bending strength was about 2.6 tons/axL'' or more.
実施例５
平均粒径が２μｍの窒化アルミニウム粉末にＮｄ、０゜
とＣａＦｓを添加し、次いでこの混合物粉末を室温で２
トン／ｄの圧力を加えて成形体とした。この成形体を焼
結炉において窒素ガス雰囲気下で２０００℃で１０時間
常圧焼結を行った。Example 5 Nd, 0° and CaFs were added to aluminum nitride powder with an average particle size of 2 μm, and then the mixed powder was heated at room temperature for 2 μm.
A pressure of ton/d was applied to form a compact. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第３図は第５図の実施例による窒化アルミニウム焼結体
の室温での熱伝導率を示す特性図である。FIG. 3 is a characteristic diagram showing the thermal conductivity at room temperature of the aluminum nitride sintered body according to the embodiment shown in FIG.
本発明の製造方法により室温での熱伝導車が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０”−’／’Ｃ１曲げ強度
は約２．６トン／−以上であった。By the manufacturing method of the present invention, the heat conduction vehicle at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10"-'/'C1 bending strength was about 2.6 tons/- or more.
実施例６ 平均粒径が２μｍの窒化アルミニウム粉末にＮｄ、Ｏ。Example 6 Nd and O in aluminum nitride powder with an average particle size of 2 μm.
とＣａＦｌ、 ５ｒＦｚ、 ＢａＦ２の少くとも一種を
添加し、次いでこの混合物粉末を室温で２トン／億８の
圧力を加えて成形体とした。この成形体を焼結炉におい
て窒素ガス雰囲気下で２０００℃で１０時間常圧焼結を
行った。At least one of CaFl, 5rFz, and BaF2 was added thereto, and then this mixture powder was formed into a compact by applying a pressure of 2 tons/80 million at room temperature. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第３表に第６の実施例による窒化アルミニウム焼結体の
室温での相対密度と熱伝導率を示す。Table 3 shows the relative density and thermal conductivity at room temperature of the aluminum nitride sintered body according to the sixth example.
本発明の製造方法により室温での熱伝導率がｔ４ｏＷ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−６／’Ｃ１曲げ強度は
約２．６トン／−以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is t4oW/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10-6/'C1 bending strength was about 2.6 tons/- or more.
第 ３ 表 ＊印は比較例である。Table 3 *marks are comparative examples.
実施例７
平均粒径が２μｍの窒化アルミニウム粉末にＳｍ２Ｏ３
とＣａＦ２を添加し、次いでこの混合物粉末を室温で２
トン／３″の圧力を加えて成形体とした。この成形体を
焼結炉において窒素ガス雰囲気下で２０００℃で１０時
間常圧焼結を行った。Example 7 Sm2O3 in aluminum nitride powder with an average particle size of 2 μm
and CaF2, and then the mixture powder was heated at room temperature for 2
A pressure of ton/3" was applied to form a compact. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第４図は第７の実施例による窒化アルミニウム焼結体の
室温での熱伝導率を示す特性図である。FIG. 4 is a characteristic diagram showing the thermal conductivity at room temperature of the aluminum nitride sintered body according to the seventh example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−’／℃、曲げ強度は約
２．６トン／−以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10-'/°C, and the bending strength was about 2.6 tons/- or more.
実施例８
平均粒径が２μｍの窒化アルミニウム粉末Ｋ Ｓｍ＊
ＯｓとＣａＦｌ、 ５ｒＦ１． ＢａＦｚの少くとも一
種を添加し、次いでこの混合物粉末を室温で２トン／ｃ
ｍ” Ｃ）圧力を加えて成形体とした。この成形体を焼
結炉において窒素ガス雰囲気下で２０００℃で１０時間
常圧焼結を行った。Example 8 Aluminum nitride powder K Sm* with an average particle size of 2 μm
Os and CaFl, 5rF1. At least one type of BaFz is added, and then the mixture powder is mixed at room temperature at 2 tons/c.
C) Pressure was applied to form a molded body. This molded body was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第４表に第８の実施例による窒化アルミニウム焼結体の
室温での相対密度と熱伝導率を示す。Table 4 shows the relative density and thermal conductivity at room temperature of the aluminum nitride sintered body according to the eighth example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−’／’Ｃ１曲げ強度は
約２．６トン／−以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3×10-'/'C1 bending strength was about 2.6 tons/- or more.
第 ４ 表
実施例９
平均粒径が２μｍの窒化アルミニウム粉末ＫＧｄｓＯｓ
、！−ＣａＦｘｔ添加し、次いでこの混合物粉末を室温
で２トン／（！！Ｉ”の圧力を加えて成形体とした。こ
の成形体を焼結炉において窒素ガス雰囲気下で２０００
℃で１０時間常圧焼結を行った。Table 4 Example 9 Aluminum nitride powder KGdsOs with an average particle size of 2 μm
,! -CaFxt was added, and then this mixture powder was made into a compact by applying a pressure of 2 tons/(!! I" at room temperature. This compact was heated to 2000 m
Normal pressure sintering was performed at ℃ for 10 hours.
第５図は第９の実施例による窒化アルミニウム焼結体の
室温での熱伝導率を示す特性図である。FIG. 5 is a characteristic diagram showing the thermal conductivity at room temperature of the aluminum nitride sintered body according to the ninth example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ １０−’／℃、曲げ強度は
約２．６トン／ａｎ″以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3 x 10-'/°C, and the bending strength was about 2.6 tons/an'' or more.
実施例１０
平均粒径が２μｍの窒化アルミニウム粉末にＧｄｚ０３
とＣａＦｚ、 ５ｒＦ１ 、 ＢａＦｚの少くとも一種
を添加し、次いでこの混合粉末を室温で２トン／（ｍ”
の圧力を加えて成形体とした。この成形体を焼結炉にお
いて窒素ガス雰囲気下で２０００℃で１０時間常圧焼結
を行った。Example 10 Gdz03 was added to aluminum nitride powder with an average particle size of 2 μm.
and at least one of CaFz, 5rF1, and BaFz, and then this mixed powder was mixed at room temperature at a rate of 2 tons/(m”
A molded body was obtained by applying a pressure of . This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第５表に第１０の実施例による窒化アルミニウム焼結体
の室温での相対密度と熱伝導率を示す。Table 5 shows the relative density and thermal conductivity at room temperature of the aluminum nitride sintered body according to the tenth example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０−’／’Ｃ１曲げ強度は
約２．６トン／−以上であった。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3×10-'/'C1 bending strength was about 2.6 tons/- or more.
第 ５ 表 ＊印は比較例である。Table 5 *marks are comparative examples.
実施例１１
平均粒径が２μｍの窒化アルミニウム粉末Ｋ Ｌ ａ
２０ 、＋ＣｅＯ２、Ｎｄ２Ｏ５、ＳｍｚＯｓ 、 Ｇ
ｄｔＯｓを１〜５樵と、ＣａＦｔ、 ＳｒＦ２． Ｂａ
Ｆｚを１〜３種添加し、次いでこの混合物粉末を室温で
２トン／Ｑ！ｌ”の圧力を加えて成形体とした。この成
形体を焼結炉において窒素ガス雰囲気下で２０００℃で
１０時間常圧焼結を行った。Example 11 Aluminum nitride powder K La with an average particle size of 2 μm
20, +CeO2, Nd2O5, SmzOs, G
dtOs, CaFt, SrF2. Ba
1 to 3 types of Fz are added, and then this mixed powder is mixed at room temperature at a rate of 2 tons/Q! A pressure of 1" was applied to obtain a compact. This compact was subjected to normal pressure sintering in a sintering furnace at 2000° C. for 10 hours in a nitrogen gas atmosphere.
第６表に第１１の実施例による窒化アルミニウム焼結体
の室温での相対密度と熱伝導率を示す。Table 6 shows the relative density and thermal conductivity at room temperature of the aluminum nitride sintered body according to the eleventh example.
本発明の製造方法により室温での熱伝導率が１４０Ｗ／
ｍｋ以上の高熱伝導性窒化アルミニウム焼結体が得られ
た。熱膨張率は約４．３Ｘ１０＝／１：：、曲げ強度は
約２．６トン／ａｎ”以上でありた。By the manufacturing method of the present invention, the thermal conductivity at room temperature is 140W/
An aluminum nitride sintered body with high thermal conductivity of mk or more was obtained. The coefficient of thermal expansion was about 4.3×10=/1::, and the bending strength was about 2.6 tons/an” or more.
本発明の製造方法で製造した窒化アルミニウム焼結体は
高密度で熱伝導性に優れ、熱的特性、電気的特性９機械
的特性にも良好であったため、半導体工業等の放熱材料
としての応用以外にるつげ。The aluminum nitride sintered body produced by the production method of the present invention has high density and excellent thermal conductivity, and has good thermal properties, electrical properties, and mechanical properties, so it can be applied as a heat dissipation material in the semiconductor industry, etc. Other than boxwood.
蒸着容器、耐熱ジグ高温部材等の高温材料としての応用
も可能であるなど、工業的に多くの利点を有するもので
ある。It has many industrial advantages, such as being able to be used as a high-temperature material for vapor deposition containers, heat-resistant jigs, high-temperature members, and the like.
第１図乃至第５図はそれぞれ本発明の第１．第３、第５
．第７．第９の実施卸による窒化アルミニウム焼結体の
室温での熱伝導率を示す特性図である。
代理人 弁理士 内 原 音
￥１図
＾Ｆｚ（重量比）
ｃａｈ（重量比）
ＣａＦｚ （重量比）
Ｃ（ｚＦｚ （重量比少
ＣａＦｚ（重量比］
手続補正書（自発）1 to 5 respectively show the first embodiment of the present invention. 3rd, 5th
．． 7th. FIG. 9 is a characteristic diagram showing the thermal conductivity at room temperature of an aluminum nitride sintered body according to a ninth embodiment. Agent Patent Attorney Uchihara Oto ￥1 Figure ＾ Fz (weight ratio) cah (weight ratio) CaFz (weight ratio) C(zFz (weight ratio small CaFz (weight ratio) Procedural amendment (voluntary)
Claims (1)
化物の群の中から選ばれた少なくとも一種とアルカリ土
類元素のフッ化物の群の中から選ばれた少くとも一種と
を用いることを特徴とする窒化アルミニウム焼結体の製
造方法。Nitriding characterized by using at least one selected from the group of oxides of rare earth elements and at least one selected from the group of fluorides of alkaline earth elements as additives to aluminum nitride powder. Method for producing aluminum sintered body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63051076A JPH01224268A (en) | 1988-03-03 | 1988-03-03 | Production of sintered aluminum nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63051076A JPH01224268A (en) | 1988-03-03 | 1988-03-03 | Production of sintered aluminum nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01224268A true JPH01224268A (en) | 1989-09-07 |
Family
ID=12876718
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63051076A Pending JPH01224268A (en) | 1988-03-03 | 1988-03-03 | Production of sintered aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01224268A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61209959A (en) * | 1985-03-13 | 1986-09-18 | 株式会社東芝 | Manufacture of aluminum nitride |
| JPS6241766A (en) * | 1985-08-13 | 1987-02-23 | 株式会社トクヤマ | Aluminum nitride sintered body and manufacture |
| JPS6252180A (en) * | 1985-08-30 | 1987-03-06 | 株式会社トクヤマ | Aluminum nitride composition |
-
1988
- 1988-03-03 JP JP63051076A patent/JPH01224268A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61209959A (en) * | 1985-03-13 | 1986-09-18 | 株式会社東芝 | Manufacture of aluminum nitride |
| JPS6241766A (en) * | 1985-08-13 | 1987-02-23 | 株式会社トクヤマ | Aluminum nitride sintered body and manufacture |
| JPS6252180A (en) * | 1985-08-30 | 1987-03-06 | 株式会社トクヤマ | Aluminum nitride composition |
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