JPH044978B2 - - Google Patents
Info
- Publication number
- JPH044978B2 JPH044978B2 JP59030402A JP3040284A JPH044978B2 JP H044978 B2 JPH044978 B2 JP H044978B2 JP 59030402 A JP59030402 A JP 59030402A JP 3040284 A JP3040284 A JP 3040284A JP H044978 B2 JPH044978 B2 JP H044978B2
- Authority
- JP
- Japan
- Prior art keywords
- ammonium carbonate
- zirconyl
- aqueous solution
- zirconia
- precipitate
- 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 - Lifetime
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 23
- BDSSZTXPZHIYHM-UHFFFAOYSA-N 2-phenoxypropanoyl chloride Chemical group ClC(=O)C(C)OC1=CC=CC=C1 BDSSZTXPZHIYHM-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims 1
- 239000002244 precipitate Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 5
- 239000001099 ammonium carbonate Substances 0.000 description 5
- 239000012452 mother liquor Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 4
- 235000012501 ammonium carbonate Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 150000003754 zirconium Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 2
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- WRAGBEWQGHCDDU-UHFFFAOYSA-M C([O-])([O-])=O.[NH4+].[Zr+] Chemical compound C([O-])([O-])=O.[NH4+].[Zr+] WRAGBEWQGHCDDU-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- -1 oxygen ion Chemical class 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 description 1
Description
【発明の詳細な説明】
本発明はジルコニア微粉末の製造方法に関す
る。更に詳述すれば、本発明は炭酸ジルコニルア
ンモニウムの加熱分解によつて生ずる沈澱物の粒
子間結合が微弱化された塊状粒子を形成し、乾
燥、焼成後に機械的粉砕を必要としない微細なジ
ルコニア粉末の製造方法を提供するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fine zirconia powder. More specifically, the present invention produces fine zirconia particles that form lumpy particles with weakened interparticle bonds of precipitates produced by thermal decomposition of zirconyl ammonium carbonate, and do not require mechanical crushing after drying and firing. A method for producing powder is provided.
ジルコニアは単斜晶系、正方晶系および立方晶
系の３種類の結晶構造があり、耐蝕性、強靭性、
酸素イオン伝導性等の材料にない特性を有してい
ることから、酸素センサー、電子部品、高温耐久
部材等いろいらな用途に応用され、素材として今
後増々重要視されることが予想される。 Zirconia has three types of crystal structures: monoclinic, tetragonal, and cubic, and has excellent corrosion resistance, toughness,
Because it has properties not found in other materials, such as oxygen ion conductivity, it is expected to be used in a variety of applications such as oxygen sensors, electronic components, and high-temperature durable materials, and will become increasingly important as a material in the future.
従来ジルコニウム塩水溶液を水熱加圧下で120
〜300℃で処理することによりジルコニアのハイ
ドロゾルをえる方法は米国特許2984628号で公知
となつており、またジルコニウム塩水溶液を長時
間煮沸することによりジルコニア微粒子スラリー
がえられることもInorg.Chem.第３巻146貢
（1964年）で公知である。更に特開昭58−791818
号には過酸化水素を用いて80〜300℃に加熱処理
してジルコニアのコロイトゾル、微粉末の製造方
法が開示されている。しかしながらこれらは高温
高圧下で長時間の反応を必要とし、また生成微粒
子の分離操作も繁雑であり、いずれも工業的生産
には適さない非能率なものである。 Conventional zirconium salt aqueous solution was heated to 120% under hydrothermal pressure.
A method of obtaining a zirconia hydrosol by treatment at ~300°C is known in US Pat. No. 2,984,628, and it is also known in Inorg.Chem. It is known as 3 volumes, 146 tributes (1964). Furthermore, JP-A-58-791818
No. 3 discloses a method for producing zirconia coroitosol and fine powder by heat treatment at 80 to 300°C using hydrogen peroxide. However, these require a long reaction time at high temperature and high pressure, and the separation operation of the produced fine particles is also complicated, and both are inefficient and unsuitable for industrial production.
本発明者は以上の点に鑑み、工業的な生産に適
するジルコニア微粉末の製造方法について種々研
究を重ねた結果、炭酸ジルコニルアンモニウムを
出発原料とした製造方法において、有機物の共存
下炭酸ジルコニルアンモニウム水溶液を60〜100
℃の加熱分解温度で１〜５時間の処理条件で生成
沈澱物の分離、洗篠操作が非常に簡単で、しかも
生成粒子の凝集が微弱なジルコニア微粉末をえる
ことに成功した。 In view of the above points, the present inventor has conducted various studies on the production method of zirconia fine powder suitable for industrial production, and as a result, in the production method using zirconyl ammonium carbonate as a starting material, an aqueous solution of zirconyl ammonium carbonate in the coexistence of organic matter has been developed. 60~100
Under the treatment conditions of 1 to 5 hours at a thermal decomposition temperature of .degree. C., it was possible to obtain fine zirconia powder in which separation of the precipitate produced and washing operations were very simple, and the agglomeration of the produced particles was weak.
本発明でのジルコニアとは純粋な酸化ジルコニ
ウムおよび一般にジルコニアと呼ばれる程度の数
％までの酸化ハフニウム、その他の安定剤や不純
物を含有する広義のジルコニアを指す。 Zirconia in the present invention refers to pure zirconium oxide and zirconia in a broad sense containing up to several percent of hafnium oxide and other stabilizers and impurities, which is generally referred to as zirconia.
本発明において原料として使用される炭酸ジル
コニルアンモニウムは公知の物質であり、次の様
な方法で製造される。 Zirconyl ammonium carbonate used as a raw material in the present invention is a known substance, and is produced by the following method.
塩化ジルコニル、硝酸ジルコニル、硫酸ジルコ
ニル、有機ジルコニル等の水可溶性ジルコニウム
塩類の水溶液と炭酸アンモニウムや重炭酸アンモ
ニウムの水溶液とを混合しPH７〜9.5程度に調整
すると透明の水溶液となる。 A transparent aqueous solution is obtained by mixing an aqueous solution of water-soluble zirconium salts such as zirconyl chloride, zirconyl nitrate, zirconyl sulfate, and organic zirconyl with an aqueous solution of ammonium carbonate or ammonium bicarbonate and adjusting the pH to about 7 to 9.5.
このようにしてえられる炭酸ジルコニルアンモ
ニウムを本発明は原料とするが、炭酸ジルコニル
アンモニウムの製造工程の途中のジルコニア塩類
を水に溶解した段階、およびPH７〜9.5に調整し
た段階の２点で過工程を入れることにより出発
物質ジルコニウム塩に含まれているシリカ等の不
純物を除去しうるという利点もある。 Zirconyl ammonium carbonate obtained in this way is used as a raw material in the present invention, but it is subjected to an over-processing process at two points during the manufacturing process of zirconyl ammonium carbonate: at the stage where zirconia salts are dissolved in water, and at the stage at which the pH is adjusted to 7 to 9.5. There is also the advantage that impurities such as silica contained in the starting material zirconium salt can be removed by adding .
前記した方法で製造した炭酸ジルコニルアンモ
ニウム水溶液は60℃以上に加熱すると分解して炭
酸ガスとアンモニアを発生し沈澱を生成する。し
かし水溶媒中のみでは沈澱物の母液との分離は非
常に困難である。デカンテーシヨン法で洗篠後蒸
発乾固または遠心沈降等の手段によつて分離した
沈澱物は、乾燥、焼成後の粒子凝集が強固で機械
的粉砕を必要とするものしかえられなつた。 When the aqueous solution of zirconyl ammonium carbonate produced by the method described above is heated to 60° C. or higher, it decomposes, generating carbon dioxide gas and ammonia, and forming a precipitate. However, it is very difficult to separate the precipitate from the mother liquor only in an aqueous solvent. The precipitates separated by decantation, washing, evaporation to dryness, centrifugal sedimentation, etc., have solid particle aggregation after drying and calcination, and require mechanical pulverization.
しかしながら本発明による方法、即ち、メタノ
ール、エタノール、プロパノール、ブタノール等
のアルコール類、アセトン、エチルメチルケトン
等のケトン類等の有機物を加熱分解段階で炭酸ジ
ルコニルアンモニウム水溶液と共存させて60〜
100℃の加熱温度で処理する方法により、処理時
間１〜５時間という短時間で100％分解が進行し、
生成した沈澱物は母液との分離およびその後の洗
篠が非常に簡単であつた。また、本発明の方法に
よつてえられた沈澱物は200℃以下での乾燥後或
は更に500〜800℃での焼成後も機械的粉砕の不要
な非常にほぐれやすい粒子からなる粉末であつ
た。 However, in the method according to the present invention, organic substances such as alcohols such as methanol, ethanol, propanol, and butanol, and ketones such as acetone and ethyl methyl ketone are allowed to coexist with an aqueous solution of zirconyl ammonium carbonate in the thermal decomposition step.
By processing at a heating temperature of 100℃, 100% decomposition progresses in a short processing time of 1 to 5 hours.
The produced precipitate was very easily separated from the mother liquor and washed afterwards. Further, the precipitate obtained by the method of the present invention is a powder consisting of particles that are easily loosened and does not require mechanical crushing even after drying at 200°C or lower or even after calcination at 500 to 800°C. Ta.
以下本発明をさらに具体的に実施例によつて説
明する。 EXAMPLES The present invention will be explained in more detail below using Examples.
実施例 １
オキシ塩化ジルコニル１モルを純水１に溶解
させ、該水溶液を過した後液に炭酸アンモニ
ウムPH8.5になるまで撹拌しながら添加し、炭酸
ジルコニルアンモニウム水溶液を製造した。Example 1 One mole of zirconyl oxychloride was dissolved in one part of pure water, and after the aqueous solution was filtered, it was added to the solution with stirring until the ammonium carbonate pH reached 8.5 to produce an aqueous solution of zirconyl ammonium carbonate.
こうしてえられた炭酸ジルコニルアンモニウム
水溶液に容量でほゞ同量のメタノールを加えた後
70℃に昇温し還流下３時間の加熱分解を行つた。 After adding approximately the same volume of methanol to the aqueous zirconyl ammonium carbonate solution obtained in this way,
The temperature was raised to 70°C and thermal decomposition was carried out under reflux for 3 hours.
この段階で透明な液が白濁し沈澱が生成した。
生成した沈澱は過操作によつて母液と分離し、
えられたケーキは純水で洗篠し、200℃で乾燥し
た。乾燥粉末は非常にほぐれやすく、800℃での
焼成後も機械的粉砕は不要な微粉末がえられた。 At this stage, the clear liquid became cloudy and a precipitate was formed.
The formed precipitate is separated from the mother liquor by over-operation,
The resulting cake was washed with pure water and dried at 200°C. The dry powder was very easy to loosen, and even after firing at 800°C, a fine powder was obtained that did not require mechanical pulverization.
実施例 ２
硝酸ジルコニル0.5モルを純水１に溶解させ、
該水溶液を過した後、液に炭酸水素アンモニ
ウムをPH８になるまで撹拌しながら添加し炭酸ジ
ルコニルアンモニウム水溶液を製造した。Example 2 Dissolve 0.5 mole of zirconyl nitrate in 1 part of pure water,
After the aqueous solution was filtered, ammonium hydrogen carbonate was added to the solution while stirring until the pH reached 8 to produce an aqueous zirconyl ammonium carbonate solution.
こうしてえられた炭酸ジルコニウムアンモニウ
ム水溶液に容量でほゞ同量のｎ−ブタノールを加
えた後90℃に昇温し、還流下１時間の加熱分解を
行つた。 After adding approximately the same volume of n-butanol to the thus obtained aqueous zirconium ammonium carbonate solution, the temperature was raised to 90°C, and thermal decomposition was carried out under reflux for 1 hour.
生成した沈澱物は母液と過操作によつて分離
し、えられたケーキは純水で洗篠し、200℃で乾
燥後600℃で焼成した。乾燥後および焼成後の粉
末は非常にほぐれやすい微粉末であつた。 The resulting precipitate was separated from the mother liquor by over-operation, and the resulting cake was washed with pure water, dried at 200°C, and then calcined at 600°C. The powder after drying and firing was a fine powder that was very easily loosened.
実施例 ３
オキシ塩化ジルコニル１モルを純水１に溶解
させ、該水溶液を過した後後に炭酸アンモニ
ウムPH8.5になるまで撹拌しながら添加し、炭酸
ジルコニルアンモニウム水溶液を製造した。Example 3 One mole of zirconyl oxychloride was dissolved in one part of pure water, and after the aqueous solution was filtered, it was added to the solution with stirring until the pH of ammonium carbonate reached 8.5, thereby producing an aqueous solution of zirconyl ammonium carbonate.
こうしてえられた炭酸ジルコニルアンモニウム
水溶液に容量でほゞ同量のアセトンを加えた後65
℃に昇温し、還流下３時間の加熱分解を行つた。 After adding approximately the same volume of acetone to the aqueous zirconyl ammonium carbonate solution obtained in this way, 65
The temperature was raised to 0.degree. C., and thermal decomposition was carried out under reflux for 3 hours.
この段階で透明な液が白濁し沈澱が生成した。
生成した沈澱は過操作によつて母液と分離し、
えられたケーキは純水で洗篠し、200℃で乾燥し
た。乾燥粉末は非常にほぐれやすく、800℃での
焼成後も機械的粉砕は不要な微粉末がえられた。 At this stage, the clear liquid became cloudy and a precipitate was formed.
The formed precipitate is separated from the mother liquor by over-operation,
The resulting cake was washed with pure water and dried at 200°C. The dry powder was very easy to loosen, and even after firing at 800°C, a fine powder was obtained that did not require mechanical pulverization.
Claims (1)
ルコール類および／またはケトン類よりなる有機
物の共存下での水溶液中で行い、分解生成物であ
る固相部分を分離、乾燥、焼成することを特徴と
するジルコニア微粉末の製造方法。 ２ 有機物がメタノール、エタノール、プロパノ
ールおよびブタノールからなるアルコール類また
はアセトンおよびエチルメチルケトンからなるケ
トン類のうち少なくとも１種であることを特徴と
する特許請求の範囲第１項記載の方法。[Claims] 1. Carrying out thermal decomposition of zirconyl ammonium carbonate in an aqueous solution in the coexistence of an organic substance consisting of alcohols and/or ketones, and separating, drying, and calcining the solid phase portion that is the decomposition product. A method for producing fine zirconia powder, characterized by: 2. The method according to claim 1, wherein the organic substance is at least one of alcohols consisting of methanol, ethanol, propanol, and butanol, or ketones consisting of acetone and ethyl methyl ketone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3040284A JPS60176921A (en) | 1984-02-22 | 1984-02-22 | Production of zirconia fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3040284A JPS60176921A (en) | 1984-02-22 | 1984-02-22 | Production of zirconia fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60176921A JPS60176921A (en) | 1985-09-11 |
| JPH044978B2 true JPH044978B2 (en) | 1992-01-30 |
Family
ID=12302940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3040284A Granted JPS60176921A (en) | 1984-02-22 | 1984-02-22 | Production of zirconia fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60176921A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778671A (en) * | 1986-07-14 | 1988-10-18 | Corning Glass Works | Preparation of unagglomerated metal oxide particles with uniform particle size |
| KR930011269B1 (en) * | 1987-10-23 | 1993-11-29 | 닛뽕쇼꾸바이가가꾸고오교 가부시끼가이샤 | Ceramic green sheet |
| JP2742449B2 (en) * | 1989-07-21 | 1998-04-22 | 株式会社日本触媒 | High performance zirconia sol and method for producing the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56145118A (en) * | 1980-04-11 | 1981-11-11 | Agency Of Ind Science & Technol | Preparation of finely divided particles of zirconium oxide |
| JPS58172233A (en) * | 1982-03-31 | 1983-10-11 | Etsuro Kato | Manufacture of spherical fine zirconia particle |
-
1984
- 1984-02-22 JP JP3040284A patent/JPS60176921A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56145118A (en) * | 1980-04-11 | 1981-11-11 | Agency Of Ind Science & Technol | Preparation of finely divided particles of zirconium oxide |
| JPS58172233A (en) * | 1982-03-31 | 1983-10-11 | Etsuro Kato | Manufacture of spherical fine zirconia particle |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60176921A (en) | 1985-09-11 |
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