JPH01126276A - Production of ceramic sintered body - Google Patents
Production of ceramic sintered bodyInfo
- Publication number
- JPH01126276A JPH01126276A JP62286346A JP28634687A JPH01126276A JP H01126276 A JPH01126276 A JP H01126276A JP 62286346 A JP62286346 A JP 62286346A JP 28634687 A JP28634687 A JP 28634687A JP H01126276 A JPH01126276 A JP H01126276A
- Authority
- JP
- Japan
- Prior art keywords
- ceramic powder
- metal
- ceramic
- powder
- sintered body
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 150000002736 metal compounds Chemical class 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- -1 alkoxide compound Chemical class 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical group Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 10
- 150000004703 alkoxides Chemical class 0.000 abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 abstract description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000005484 gravity Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- KEQVPIDOPAGWCP-UHFFFAOYSA-N ethanolate;yttrium(3+) Chemical compound [Y+3].CC[O-].CC[O-].CC[O-] KEQVPIDOPAGWCP-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 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 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- HHFAWKCIHAUFRX-UHFFFAOYSA-N ethoxide Chemical compound CC[O-] HHFAWKCIHAUFRX-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical group [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】 利用分野 本発明は、セラミック焼結体の製法に関する。[Detailed description of the invention] Field of use The present invention relates to a method for manufacturing a ceramic sintered body.
詳しくは、金属化合物の焼結助剤を混合してセラミック
粉を焼結する工程において、該助剤用金属のアルコキシ
ド化合物の非水性溶液を該セラミック粉に均一混合して
、該セラミック粉表面に該金属の化合物を微細かつ均一
に付着せしめた材料を焼結する、均質なセラミック焼結
体の容易な製法に関する。Specifically, in the step of sintering ceramic powder by mixing a sintering aid of a metal compound, a non-aqueous solution of an alkoxide compound of the metal for the aid is uniformly mixed with the ceramic powder, and the surface of the ceramic powder is coated. The present invention relates to an easy method for producing a homogeneous ceramic sintered body by sintering a material to which the metal compound is finely and uniformly adhered.
従来の技術および問題点
一般に、セラミックは高温で焼成されるが、その際に焼
結を促進させるために種々の金属化合物が焼結助剤とし
て添加される。各セラミック原料に適当な焼結助剤は、
当業界によく知られている。Prior Art and Problems Generally, ceramics are fired at high temperatures, and various metal compounds are added as sintering aids to promote sintering. Sintering aids suitable for each ceramic raw material are:
Well known in the industry.
例えばチッ化アルミニウム（以下にＡＱＮということ′
がある）焼結体の製造においては、イツトリウム、アル
カリ土類金属またはランタン族金属等の化合物を０．１
〜１０重量％程度添加し１７００〜２０００℃で焼成さ
れている。焼結助剤は試薬級の粉体であり、焼結を容易
にするため主成分のＡＱＮ粉体の粒径も２ミクロン以下
である場合が多い。したがって、主成分であるＡＱＮと
焼結助剤粉体との混合は、困難であり、通常ボールミル
等で長時間混合処理を行わなければならない。アトライ
ター、振動ミルなど高効率の混合機を用いれば混合時間
は短縮できるが、設備的に高価であり、装置からのコン
タミも多くなる。For example, aluminum nitride (hereinafter referred to as AQN)
) In the production of sintered bodies, compounds such as yttrium, alkaline earth metals, or lanthanum group metals are
It is added in an amount of about 10% by weight and fired at 1700 to 2000°C. The sintering aid is a reagent-grade powder, and in order to facilitate sintering, the particle size of the main component, AQN powder, is often 2 microns or less. Therefore, it is difficult to mix AQN, which is the main component, and the sintering aid powder, and usually requires a long mixing process using a ball mill or the like. Mixing time can be shortened by using a highly efficient mixer such as an attritor or a vibration mill, but the equipment is expensive and contamination from the equipment increases.
第４図は、湿式ボールミル混合法による焼結助剤の添加
実験の結果を示す混合時間とＡＱＮ焼結体の嵩比重の関
係図である。ナイロン製ボールミル容器に５ｍｍ、１２
１９９．５％のアルミナボールを用い、ｎ−ブタノール
を溶媒とした。Ａ、！Ｎ原料は東芝セラミック製を用い
、焼結助剤はＹ ｔ Ｏ３を３重量％とした。このよう
にしてボールミルで混合されたスラリーを乾燥し、１０
０ ＭＰａで単軸加圧成形し、チッ素雰囲気下にて１８
００℃で２時間焼成した。焼成体の嵩比重はアルキメデ
ス法で測定した。緻密な焼成体を得るのに約７２時間混
合しなければならず、Δｆ２Ｎセラミックの製造工程上
大きな制約となる。しかも装置からのコンタミも多く、
アルミナボールの摩耗成分は主成分であるＡｌ２Ｎ原料
の約５ｆｆｉｆｆｉ％にも達する（７２時間混合にて）
。FIG. 4 is a diagram showing the relationship between the mixing time and the bulk specific gravity of the AQN sintered body, showing the results of a sintering aid addition experiment using a wet ball mill mixing method. 5mm, 12 in a nylon ball mill container
199.5% alumina balls were used, and n-butanol was used as the solvent. A,! The N raw material was manufactured by Toshiba Ceramics, and the sintering aid was 3% by weight of Y t O3. The slurry thus mixed in a ball mill was dried and
Uniaxial pressure molding at 0 MPa and 18
It was baked at 00°C for 2 hours. The bulk specific gravity of the fired body was measured by the Archimedes method. It takes about 72 hours of mixing to obtain a dense fired body, which is a major constraint on the manufacturing process of Δf2N ceramics. Moreover, there is a lot of contamination from the equipment.
The abrasion component of alumina balls reaches approximately 5ffiffi% of the main component Al2N raw material (after 72 hours of mixing)
.
上記の問題点は、他のセラミック焼結体の製造において
も全く同様である。すなわち、ボールミル混合等による
機械的な助剤添加法は、ミクロ的に不均一になる可能性
があり、セラミックスの内部不均一の原因になりやすい
。従ってセラミックの製造において、焼結助剤が十分に
均一に混合でき、しかも短時間で処理でき、コンタミも
少なく、特殊な装置が不要な方法が必要視されていた。The above problems are exactly the same in the production of other ceramic sintered bodies. That is, mechanical additive addition methods such as ball mill mixing may result in microscopic non-uniformity, which is likely to cause internal non-uniformity in the ceramic. Therefore, in the production of ceramics, there has been a need for a method that allows the sintering aid to be sufficiently and uniformly mixed, that can be processed in a short time, that causes less contamination, and that does not require special equipment.
問題点を解決するための手段
本発明者は、該焼結助剤の金属のアルコキシド化合物の
非水性溶液を焼結性セラミック粉に均一混合し、該セラ
ミック粉表面に存在するＯＨ基および／または付着水の
作用によって微細な金属化合物を析出等によって付着さ
せそして乾燥して該セラミック粉表面に均一に付着せし
めた材料が、上記の焼結体の製法に極めて有利であるこ
とを見出した。Means for Solving the Problems The present inventor uniformly mixed a non-aqueous solution of a metal alkoxide compound of the sintering aid into sinterable ceramic powder, and solved the OH groups and/or It has been found that a material in which a fine metal compound is deposited by precipitation or the like under the action of deposited water and dried to be uniformly deposited on the surface of the ceramic powder is extremely advantageous for the above method of manufacturing the sintered body.
従って本発明によって、焼結性セラミック粉に金属化合
物の焼結助剤を混合して焼結する方法において：該金属
のアルコキシド化合物を実質的に非水性溶液の形態にて
該セラミック粉と均一混合し、そして該セラミック粉の
表面に該金属の化合物を微細かつ均一に付着せしめた材
料を焼結することを特徴とする、セラミック焼結体の製
法が提供される。なお、上記の「実質的に非水性溶液」
とは、該非水性溶剤中に含有される僅かな水分等によっ
て溶液中に金属化合物微粉子が若干析出している溶液も
使用できる意味である。Therefore, according to the present invention, in a method of mixing a sinterable ceramic powder with a sintering aid of a metal compound and sintering the mixture, the alkoxide compound of the metal is homogeneously mixed with the ceramic powder in the form of a substantially non-aqueous solution. There is also provided a method for producing a ceramic sintered body, which is characterized by sintering a material in which the metal compound is finely and uniformly adhered to the surface of the ceramic powder. In addition, the above-mentioned "substantially non-aqueous solution"
This means that a solution in which a small amount of metal compound fine particles are precipitated in the solution due to a small amount of water contained in the non-aqueous solvent can also be used.
発明の詳しい記述
本発明にて使用される金属アルコキシド化合物のアルコ
キシル基部分としては、非水性溶剤（例えば相当するア
ルコール）に容易に溶解するものが使用される。例えば
炭素数が１〜５程度の低級アルコキシドが有利に使用で
きるが、特に限定はされない。通常はエトキシドまたは
イソプロポキシドが用いられる。DETAILED DESCRIPTION OF THE INVENTION As the alkoxyl moiety of the metal alkoxide compound used in the present invention, one that is easily soluble in a non-aqueous solvent (for example, a corresponding alcohol) is used. For example, lower alkoxides having about 1 to 5 carbon atoms can be advantageously used, but are not particularly limited. Usually ethoxide or isopropoxide is used.
一般に金属のアルコキシドは、加水分解によって金属酸
化物またはその水和物となるが、本発明では特別に水を
アルコキシドに加えることは行わない。ＡＱＮを例とし
て記述するとＡ（！Ｎ粉体の表面のＯＨ基および付着水
分を利用して、Ａ１２Ｎ粒子表面に酸化イツトリウムを
形成させている。第１図の説明図に示すようにＡｆ２Ｎ
粒子表面にＹ、０３が形成されるとηえられる。すなわ
ち、ＡＣＮ粉体ニ限うず実質的にすべてのセラミック用
粉体は、大気中の水分により表面に付着水またはＯＨ基
の存在が認められている。ＡＱＮ粉も第２図に示す赤外
線吸収スペクトルの分析結果により、表面にＯＨ基が存
在していることが明らかになっている。Generally, metal alkoxides become metal oxides or hydrates thereof through hydrolysis, but in the present invention, water is not specifically added to the alkoxides. To describe AQN as an example, yttrium oxide is formed on the surface of A12N particles using the OH groups and attached moisture on the surface of A(!N powder.
When Y,03 is formed on the particle surface, η is obtained. That is, in virtually all ceramic powders, including ACN powders, it is recognized that water or OH groups are present on the surface due to moisture in the atmosphere. The analysis results of the infrared absorption spectrum shown in FIG. 2 reveal that the AQN powder also has OH groups on its surface.
また溶媒として使用したエタノール中にも小債の水分が
含まれているため、これらの水分とイツトリウムエトキ
シドが反応し、イツトリウムの酸化物が形成されること
も考えられる。なお、セラミック用粉体に加水分解され
ていない金属アルコキシドが付着して残存していても、
差支えない。In addition, since the ethanol used as a solvent also contains moisture in the small bonds, it is possible that this moisture reacts with yttrium ethoxide to form yttrium oxide. Furthermore, even if unhydrolyzed metal alkoxide remains on the ceramic powder,
No problem.
本発明のアルコキシドを用いた助剤添加の場合、湿式ボ
ールミル等の方法よりも、短時間で混合が行われる。す
なわち、セラミックの粉体同士の混合は、微細な粒子は
ど粒子間相互作用が大きく、一部で凝集し易く完全な分
散状態は得にくいため、均一な混合が行いにくい。しか
し金属アルコキシドを用いた場合、イツトリウムエトキ
シドがエタノール中で均一に実質的に溶液状に分散して
おりＡｆ２Ｎ粉体に対しても容易に均一に分Ｉ牧する。In the case of adding an auxiliary agent using the alkoxide of the present invention, mixing can be carried out in a shorter time than by a method such as a wet ball mill. That is, when mixing ceramic powders with each other, it is difficult to achieve uniform mixing because the interaction between fine particles is large and they tend to aggregate in some areas, making it difficult to obtain a complete dispersion state. However, when a metal alkoxide is used, yttrium ethoxide is uniformly and substantially dispersed in solution in ethanol, and is easily and uniformly divided into Af2N powder.
上記においてＡｆｆＮセラミックの焼結助剤としてイツ
トリウム元素について記述したが、アルカリ土類、ラン
タン族元素等のアルコキシドも同様に適用できる。さら
にＡ７２Ｎ以外のセラミックス（例えばＺｒＯ＊、 ５
ｉＪａ、 Ａ１＊Ｏｓ、 ＳｉＣ，Ｔｉ１ｔ等）におい
て、同様に本発明が適用できる。Although yttrium element has been described above as a sintering aid for AffN ceramics, alkoxides of alkaline earth elements, lanthanum group elements, etc. can be similarly applied. Furthermore, ceramics other than A72N (e.g. ZrO*, 5
The present invention is similarly applicable to iJa, A1*Os, SiC, Tilt, etc.).
なお、本発明に従って微細な金属化合物（例えば粒径０
．０１−１ミクロン程度）を焼結性セラミック粉表面上
に均一に付着させた材料は、（イ）常温にて加圧・成形
した後に焼結するか（ロ）高温加圧焼成して焼結するか
、（ハ）いわゆるＨＩＰ焼結する等の公知の方法によっ
て容易に焼結できる。In addition, according to the present invention, fine metal compounds (for example, particle size 0
．． The material in which particles (approximately 0.01-1 micron) are uniformly adhered to the surface of sinterable ceramic powder can be either (a) sintered after being pressurized and shaped at room temperature, or (b) sintered by high-temperature pressure firing. or (c) it can be easily sintered by a known method such as so-called HIP sintering.
実施例
ＡＩＮ原料として、徳山曹達（株）製Ｆグレード粉体を
使用した。焼結助剤としては、高純度化学研究新製のイ
ツトリウムエトキシドを用いた。Example F grade powder manufactured by Tokuyama Soda Co., Ltd. was used as an AIN raw material. As the sintering aid, yttrium ethoxide manufactured by Kojundo Kagaku Kenkyushin was used.
表Ｉに示す所定ｍのイツトリウムエトキシドを１００ｍ
σのエチルアルコール
クスターラーで３０分撹拌して溶液２を得た。100 m of yttrium ethoxide of the specified m shown in Table I
Solution 2 was obtained by stirring for 30 minutes with a σ ethyl alcohol stirrer.
アルミナ製ポットに該溶成〆およびＡ１２Ｎ粉体（表１
の通り）を投入し、２０時間混合した。こうして得られ
たスラリーを乾燥後、１２ ｍｍφの金型を用いｔｏｏ
ＭＰａでプレス成形した。該成形体を、カーボンるつ
ぼ中でチッ素雰囲気下１８００℃で２時間焼成した。焼
成体のかさ比重等を表２に示す。The melted finish and A12N powder were placed in an alumina pot (Table 1).
) and mixed for 20 hours. After drying the slurry thus obtained, it was molded using a 12 mm diameter mold.
Press molding was performed at MPa. The molded body was fired at 1800° C. for 2 hours in a nitrogen atmosphere in a carbon crucible. Table 2 shows the bulk specific gravity of the fired body.
／ＩＮのかさ密度は約３．２６であるから、十分緻密な
／ＩＮセラミックが得られたことが確認された。Since the bulk density of /IN was approximately 3.26, it was confirmed that a sufficiently dense /IN ceramic was obtained.
孝」−
原料組成（全体を約１００ｇとして）
ＡＩＮ−ＹｔＯ＋ Ｙ（ＱＣ，Ｈ５）３ ＡＩ
ＮＯ，５重量％ ０．９９２４ｇ ９
９．５ｇ１、０重量％ １．９８４８ｇ
９９．０ｇ３、０重量％ ５．９５４３ｇ
９７．０ｇ表２
焼結体
０、５重量％ １０１１３％ ３，Ｑ重量％吸水率（１
） １．６５ ０．７７ ０．７１かさ比重
３．１１ ３．２０ ３．２４第３図に、
得られたＡ１２Ｎ焼結体の粉末Ｘ線回折（ＸＲＤ）パタ
ーンを示す。なお、イツトリウム元素として同当量の酸
化イツトリウムを従来法である湿式ボールミルにて７２
時間混合し、同様に焼結したＡ１２Ｎ焼結体も同様なＸ
ＲＤパターンを示すことを確認した。- Raw material composition (total about 100g) AIN-YtO+ Y(QC,H5)3 AI
NO, 5% by weight 0.9924g 9
9.5g1, 0% by weight 1.9848g
99.0g3, 0% by weight 5.9543g
97.0gTable 2 Sintered body 0,5 wt% 10113% 3,Q wt% water absorption rate (1
) 1.65 0.77 0.71 Bulk specific gravity 3.11 3.20 3.24 In Figure 3,
The powder X-ray diffraction (XRD) pattern of the obtained A12N sintered body is shown. In addition, the same amount of yttrium oxide as the yttrium element was prepared using a wet ball mill, which is a conventional method.
The A12N sintered body mixed for a time and sintered in the same manner also had the same
It was confirmed that it showed an RD pattern.
作用および効果
本発明において、焼結助剤の金属のアルコキシド化合物
の非水性溶液を焼結性セラミック粉に均一混合し、該セ
ラミック粉表面に存在するＯＨ基および／または付着水
を利用して微細な金属化合物を析出等によって該セラミ
ック粉表面に均一に付着せしめる作用によって、下記の
ような優れた代表的な効果が達成される。Functions and Effects In the present invention, a non-aqueous solution of a metal alkoxide compound as a sintering aid is uniformly mixed with sinterable ceramic powder, and fine particles are formed by using the OH groups and/or adhering water on the surface of the ceramic powder. By the action of uniformly adhering a metal compound to the surface of the ceramic powder by precipitation or the like, the following excellent typical effects can be achieved.
すなわち、（１）焼結助剤を十分均一に混合することが
できるため、通常のボールミル混合に比べ、短時間で処
理ができる。（２）原理的に液相反応で助剤添加をする
ため、ミクロ的に均一な混合状態が得られる。（３）特
殊な装置を使わずに混合操作が行える。（４）均一な混
合のため添加する焼結助剤は必要最小限で済むので、助
剤量を減らすことができる。（５）助剤添加操作以外は
、通常の操作がそのまま適用できる。（６）本発明によ
り製造したＡ７２Ｎセラミックスは、十分に緻密化およ
び均質化しており、従来法と比較して同等以上の品質が
得られる。That is, (1) since the sintering aid can be mixed sufficiently uniformly, the processing can be completed in a shorter time than in normal ball mill mixing. (2) Since the auxiliary agent is added by a liquid phase reaction in principle, a microscopically uniform mixing state can be obtained. (3) Mixing operations can be performed without using special equipment. (4) The amount of sintering aid added can be reduced to the minimum necessary for uniform mixing, so the amount of the aid can be reduced. (5) Except for the operation of adding the auxiliary agent, the usual operations can be applied as they are. (6) The A72N ceramics produced according to the present invention are sufficiently densified and homogenized, and the quality equivalent to or higher than that obtained by conventional methods can be obtained.
第１図は、本発明における焼結助剤添加の説明図である
。第２図は、チッ化アルミニウム粉の水分を示す赤外線
吸収スペクトルである。第３図は、本発明によるチッ化
アルミニウム焼結体の粉末Ｘ線回折パターンである。第
４図は、従来法にょるヂッ化アルミニウム焼結体のかさ
比重と混合時間の関係を示すグラフである。
特許出願人 株式会社 イナックス第１図
第２図
第３図
第４図
ｏ２ｏＰａＩ７ａＰｏｉｉ。
混合時間FIG. 1 is an explanatory diagram of the addition of a sintering aid in the present invention. FIG. 2 is an infrared absorption spectrum showing the moisture content of aluminum nitride powder. FIG. 3 is a powder X-ray diffraction pattern of the aluminum nitride sintered body according to the present invention. FIG. 4 is a graph showing the relationship between bulk specific gravity and mixing time of a sintered aluminum didide body according to a conventional method. Patent applicant Inax Co., Ltd. Figure 1 Figure 2 Figure 3 Figure 4 o2oPaI7aPoii. mixing time
Claims (2)
合して焼結する方法において；該金属のアルコキシド化
合物を実質的に非水性溶液の形態にて該セラミック粉と
均一混合し、そして該セラミック粉の表面に該金属の化
合物を微細かつ均一に付着せしめた材料を焼結すること
を特徴とする、セラミック焼結体の製法。(1) In a method of mixing a sinterable ceramic powder with a sintering aid of a metal compound and sintering it; homogeneously mixing the metal alkoxide compound with the ceramic powder in the form of a substantially non-aqueous solution; A method for producing a ceramic sintered body, characterized by sintering a material in which the metal compound is finely and uniformly adhered to the surface of the ceramic powder.
、特許請求の範囲第１項の製法。(2) The manufacturing method according to claim 1, wherein the sinterable ceramic powder is aluminum nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62286346A JPH01126276A (en) | 1987-11-11 | 1987-11-11 | Production of ceramic sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62286346A JPH01126276A (en) | 1987-11-11 | 1987-11-11 | Production of ceramic sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01126276A true JPH01126276A (en) | 1989-05-18 |
Family
ID=17703198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62286346A Pending JPH01126276A (en) | 1987-11-11 | 1987-11-11 | Production of ceramic sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01126276A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01317155A (en) * | 1988-03-04 | 1989-12-21 | Mitsubishi Kasei Corp | Production of ceramic compact |
| JPH02233546A (en) * | 1989-03-07 | 1990-09-17 | Mitsubishi Kasei Corp | Ceramic material and production of ceramic using the same |
| JPH04362066A (en) * | 1991-06-10 | 1992-12-15 | Toshiba Corp | Production of ceramic sintered body |
| JP2009235181A (en) * | 2008-03-26 | 2009-10-15 | Hitachi Metals Ltd | Method for manufacturing fluorescent material |
| JP2013512794A (en) * | 2009-12-02 | 2013-04-18 | セラムテック ゲゼルシャフト ミット ベシュレンクテル ハフツング | Functional extrudate made of high thermal conductive ceramic |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56149378A (en) * | 1980-04-21 | 1981-11-19 | Toyota Motor Co Ltd | Manufacture of silicon nitride sintered body |
| JPS60210574A (en) * | 1984-03-30 | 1985-10-23 | 工業技術院長 | Manufacture of high strength heat-resistant ceramic sinteredbody |
| JPS61251578A (en) * | 1985-04-30 | 1986-11-08 | 住友電気工業株式会社 | Manufacture of silicon nitride sintered body |
| JPS61251571A (en) * | 1985-04-26 | 1986-11-08 | 日立金属株式会社 | Manufacture of ceramic formed body |
| JPS61281069A (en) * | 1985-06-05 | 1986-12-11 | 日立金属株式会社 | Manufacture of ceramic sintered body |
| JPS6221764A (en) * | 1985-07-18 | 1987-01-30 | 住友電気工業株式会社 | Manufacture of aluminum nitride |
| JPS62235262A (en) * | 1986-04-07 | 1987-10-15 | 住友電気工業株式会社 | Manufacture of aluminum nitride sintered body |
| JPS63242972A (en) * | 1987-03-31 | 1988-10-07 | 株式会社東芝 | Manufacture of aluminum nitride sintered body |
-
1987
- 1987-11-11 JP JP62286346A patent/JPH01126276A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56149378A (en) * | 1980-04-21 | 1981-11-19 | Toyota Motor Co Ltd | Manufacture of silicon nitride sintered body |
| JPS60210574A (en) * | 1984-03-30 | 1985-10-23 | 工業技術院長 | Manufacture of high strength heat-resistant ceramic sinteredbody |
| JPS61251571A (en) * | 1985-04-26 | 1986-11-08 | 日立金属株式会社 | Manufacture of ceramic formed body |
| JPS61251578A (en) * | 1985-04-30 | 1986-11-08 | 住友電気工業株式会社 | Manufacture of silicon nitride sintered body |
| JPS61281069A (en) * | 1985-06-05 | 1986-12-11 | 日立金属株式会社 | Manufacture of ceramic sintered body |
| JPS6221764A (en) * | 1985-07-18 | 1987-01-30 | 住友電気工業株式会社 | Manufacture of aluminum nitride |
| JPS62235262A (en) * | 1986-04-07 | 1987-10-15 | 住友電気工業株式会社 | Manufacture of aluminum nitride sintered body |
| JPS63242972A (en) * | 1987-03-31 | 1988-10-07 | 株式会社東芝 | Manufacture of aluminum nitride sintered body |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01317155A (en) * | 1988-03-04 | 1989-12-21 | Mitsubishi Kasei Corp | Production of ceramic compact |
| JPH02233546A (en) * | 1989-03-07 | 1990-09-17 | Mitsubishi Kasei Corp | Ceramic material and production of ceramic using the same |
| JPH04362066A (en) * | 1991-06-10 | 1992-12-15 | Toshiba Corp | Production of ceramic sintered body |
| JP2009235181A (en) * | 2008-03-26 | 2009-10-15 | Hitachi Metals Ltd | Method for manufacturing fluorescent material |
| JP2013512794A (en) * | 2009-12-02 | 2013-04-18 | セラムテック ゲゼルシャフト ミット ベシュレンクテル ハフツング | Functional extrudate made of high thermal conductive ceramic |
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