JPH0472773B2 - - Google Patents
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- Publication number
- JPH0472773B2 JPH0472773B2 JP23335284A JP23335284A JPH0472773B2 JP H0472773 B2 JPH0472773 B2 JP H0472773B2 JP 23335284 A JP23335284 A JP 23335284A JP 23335284 A JP23335284 A JP 23335284A JP H0472773 B2 JPH0472773 B2 JP H0472773B2
- Authority
- JP
- Japan
- Prior art keywords
- zirconium
- water
- oxide powder
- zirconium oxide
- reaction
- 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
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- 239000000843 powder Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 150000003754 zirconium Chemical class 0.000 claims description 20
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 14
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical group Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- 150000003746 yttrium Chemical class 0.000 claims description 3
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 239000012153 distilled water Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- ZFSFDELZPURLKD-UHFFFAOYSA-N azanium;hydroxide;hydrate Chemical group N.O.O ZFSFDELZPURLKD-UHFFFAOYSA-N 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000009610 hypersensitivity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- LUMVCLJFHCTMCV-UHFFFAOYSA-M potassium;hydroxide;hydrate Chemical compound O.[OH-].[K+] LUMVCLJFHCTMCV-UHFFFAOYSA-M 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Description
【発明の詳細な説明】
〔発明の目的〕
本発明は、酸化ジルコニウム微粉末の製造方法
に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] The present invention relates to a method for producing fine zirconium oxide powder.
従来酸化ジルコニウム微粉末の製造方法は、
ZrO2濃度換算で50〜100ｇ／のジルコニウム塩
水溶液中へアルカリ添加し、中和洗浄、過を行
つていた。
The conventional manufacturing method of zirconium oxide fine powder is as follows:
An alkali was added to an aqueous solution of zirconium salt in an amount of 50 to 100 g in terms of ZrO 2 concentration, and the solution was neutralized, washed, and filtered.
さらに過ケーキを仮焼後、破砕し、酸化ジル
コニウムを得ていた。 Furthermore, after calcining the overcake, it was crushed to obtain zirconium oxide.
しかしながら、上記方法ではゲル状になり易
く、従つて過性が悪く、過洗浄に長時間を要
する欠点を有していた。
However, the above-mentioned method has the disadvantage that it tends to become gel-like, has poor cleaning properties, and requires a long period of time for over-cleaning.
また、このため洗浄も不十分になり易く、仮焼
時における凝集をもたらし、粒子が粗大化し好ま
しいものが得られなかつた。 Furthermore, cleaning tends to be insufficient, resulting in agglomeration during calcination, resulting in coarse particles, making it impossible to obtain a desired product.
さらに破砕等の工程が必然的に必要となり、こ
れによる不純物の混入の問題を生じるなど種々の
問題を生じていた。 Furthermore, a process such as crushing is inevitably required, which causes various problems such as the problem of contamination with impurities.
本発明者等は、上記欠点を排除すべく鋭意検討
した結果、水溶性ジルコニウム塩とアルカリ水
を、ジルコニウム塩の濃度としてZrO2換算300〜
450ｇ／で反応させ微粉末を得ることを発明し
た。
As a result of intensive studies to eliminate the above drawbacks, the present inventors determined that water-soluble zirconium salt and alkaline water have a concentration of zirconium salt of 300 to 300 in terms of ZrO2 .
It was invented that a fine powder can be obtained by reacting at 450 g/kg.
また具体的実施態様として、
水溶性ジルコニウム塩をアルカリ水の中へ添加
し、反応させる方法。 Further, as a specific embodiment, a method in which a water-soluble zirconium salt is added to alkaline water and reacted.
水溶性ジルコニウム塩に対し、アルカリ濃度を
0.5モル以上の過剰で反応させる方法。 Alkali concentration for water-soluble zirconium salt
A method of reacting with an excess of 0.5 mole or more.
ジルコニウム塩がオキシ塩化ジルコニウム、硝
酸ジルコニウム、硫酸ジルコニウム塩のいずれか
一種以上である方法。 A method in which the zirconium salt is one or more of zirconium oxychloride, zirconium nitrate, and zirconium sulfate.
反応後過した後、アルコール洗浄する方法。 A method of washing with alcohol after the reaction.
反応後、洗浄、過し、仮焼する際、仮焼の昇
温速度を50〜150℃／Hrである方法。 A method in which the heating rate for calcination is 50 to 150°C/Hr during washing, filtering, and calcination after the reaction.
アルコールが、C2〜C5アルコールである方法。 A method in which the alcohol is a C2 to C5 alcohol.
反応時に、安定化剤であるカルシウム、マグネ
シウム、イツトリウムの塩のうち一種以上を含む
方法。 A method in which one or more of calcium, magnesium, and yttrium salts are included as stabilizers during the reaction.
を発明した。invented.
以下本発明について詳細に説明する。 The present invention will be explained in detail below.
本発明で用いるジルコニウムは水溶性ジルコニ
ウム塩であり、オキシ塩化ジルコニウム、硝酸ジ
ルコニウム、硫酸ジルコニウムのいずれか一種以
上であることが好ましい。 The zirconium used in the present invention is a water-soluble zirconium salt, and is preferably one or more of zirconium oxychloride, zirconium nitrate, and zirconium sulfate.
水溶性ジルコニウム塩は、アルカリ水と反応さ
せる。 The water-soluble zirconium salt is reacted with alkaline water.
アルカリ水と水溶性ジルコニウム塩と反応させ
る場合には、ZrO2換算で300〜450ｇ／の濃度
で反応させる。ZrO2濃度が高いと第１図に示す
ごとく過性が良く、その後処理が容易なため微
細なZrO2を得ることが容易なためである。ただ
450ｇ／以上になるとゲル状態がひどくなり、
反応し難くなる。 When alkaline water is reacted with a water-soluble zirconium salt, the reaction is carried out at a concentration of 300 to 450 g/ZrO 2 . This is because when the ZrO 2 concentration is high, the transient property is good as shown in FIG. 1, and the subsequent processing is easy, so it is easy to obtain fine ZrO 2 . just
If it exceeds 450 g/g, the gel state will become worse.
It becomes difficult to react.
水溶性ジルコニウムとアルカリ水との反応は、
水溶性ジルコニウム塩とアルカリ水と同時に反応
槽に入れるか、好ましくはアルカリ水中に水溶性
ジルコニウム塩とを反応させる。 The reaction between water-soluble zirconium and alkaline water is
The water-soluble zirconium salt and alkaline water are put into a reaction tank at the same time, or preferably the water-soluble zirconium salt is reacted in alkaline water.
この方法により、より過性の良いZrO2粉を
得ることができる。 By this method, ZrO 2 powder with better permeability can be obtained.
また、アルカリ水の濃度は、水溶性ジルコニウ
ム塩に対し、0.5モル以上の過剰で反応させるこ
とが好ましい。 Further, the concentration of alkaline water is preferably 0.5 mole or more in excess of the water-soluble zirconium salt.
即ち、水溶性ジルコニウム塩の濃度をより高
く、アルカリ水の濃度をより濃い状態で一時に反
応を生ぜしめることが一番好ましい反応なのであ
る。 That is, the most preferable reaction is to carry out the reaction at the same time with a higher concentration of water-soluble zirconium salt and a higher concentration of alkaline water.
アルカリ水は、NH4OH水、NaOH水、KOH
水等が用いられるが、アルカリ金属を嫌う用途の
場合はNH4OH水が好ましい。 Alkaline water is NH4OH water, NaOH water, KOH
Water or the like is used, but NH 4 OH water is preferable for applications that do not like alkali metals.
また、構造材等として用いる場合あるいはその
他機能材と用いる場合に、安定剤又は準安定剤を
必要とする場合は、イツトリウム、マグネシウ
ム、イツトリウムの塩のうち、いずれか一種以上
を含ませる。この添加は、水溶性ジルコニウム塩
とアルカリ水との反応時に添加することが好まし
い。より微細なZrO2粉を得ることができるため
である。 In addition, if a stabilizer or metastabilizer is required when used as a structural material or other functional material, one or more of yttrium, magnesium, and yttrium salts is included. This addition is preferably carried out during the reaction of the water-soluble zirconium salt and alkaline water. This is because finer ZrO 2 powder can be obtained.
水溶性ジルコニウム塩とアルカリ水との反応温
度は、20〜40℃の範囲で行うことが好ましい。 The reaction temperature of the water-soluble zirconium salt and alkaline water is preferably carried out in a range of 20 to 40°C.
反応は１〜３時間程度攪拌し、熟成させる。 The reaction is stirred and aged for about 1 to 3 hours.
生成した水酸化ジルコニウムは、蒸留水を添加
し５〜20分攪拌し、10〜30分静置し上澄液を排出
し、過し洗浄を行う。この洗浄は６〜10回行わ
れる。該洗浄後好ましくはアルコール洗浄する。
二次凝集を防止するためである。これは第２図に
示すごとく過ケーキ中のZrO2濃度が高いこと
から、好ましいことが容易に把握できる。 Distilled water is added to the generated zirconium hydroxide, stirred for 5 to 20 minutes, left to stand for 10 to 30 minutes, and the supernatant liquid is drained and washed by filtration. This washing is carried out 6-10 times. After this washing, it is preferable to wash with alcohol.
This is to prevent secondary aggregation. It can be easily understood that this is preferable since the ZrO 2 concentration in the overcake is high as shown in FIG.
この場合のアルコールは、C2〜C5アルコール
である。このアルコールの中で好ましくは、イソ
プロピルアルコールである。 The alcohol in this case is a C2 - C5 alcohol. Among these alcohols, isopropyl alcohol is preferred.
アルコール洗浄後過し、仮焼を行う。 After washing with alcohol, it is filtered and calcined.
仮焼の昇温速度は50〜150℃／Hrであることが
好ましい。二次凝集を極力避けるためである。 The heating rate for calcination is preferably 50 to 150°C/Hr. This is to avoid secondary aggregation as much as possible.
仮焼温度は700〜900℃である。仮焼保持時間は
２〜６時間である。 The calcination temperature is 700-900°C. The calcining holding time is 2 to 6 hours.
以上の内容を実施することにより、以下の効果
が得られる。
By implementing the above contents, the following effects can be obtained.
(1) 極めて過性の良い水酸化ジルコニウムが得
られるため、活性の高い超微粉末のZrO2を得
ることができる。(1) Since zirconium hydroxide with extremely good permeability can be obtained, highly active ultrafine powder ZrO 2 can be obtained.
ZrO2粉の粒子径が100〜220Åの微粉が得ら
れる。 A fine powder of ZrO 2 powder with a particle size of 100-220 Å is obtained.
また比表面積は20〜50m2／ｇのものが得られ
る。 Further, a specific surface area of 20 to 50 m 2 /g can be obtained.
細孔容積は0.200c.c.／ｇ〜0.260c.c.／ｇのもの
が得られる。 Pore volumes of 0.200 cc/g to 0.260 cc/g can be obtained.
(2) また得られるZrO2粉は微粉であり、かつ活
性の高いZrO2粉が得られる。(2) Furthermore, the obtained ZrO 2 powder is a fine powder and highly active ZrO 2 powder can be obtained.
(3) さらに構造材等に用いる場合は、極めて高い
強度をもたらす。(3) Furthermore, when used in structural materials, etc., it provides extremely high strength.
(4) 過性が20〜40倍であるため生産性が高い。(4) Productivity is high because the hypersensitivity is 20 to 40 times higher.
実施例 １
蒸留水165mlにオキシ塩化ジルコニウム
（ZrOCl2・8H2Ｏ）325ｇを加えて溶解させた水溶
液（350ml）をアンモニア水（NH329wt％）200
mlの中へ添加し、温度30℃で２時間攪拌熟成す
る。そのスラリーの中へ750mlの蒸留水を添加後
10分間攪拌、20分間静置して上澄液を排出、この
操作をくり返し行い洗浄を行つた後、ブフナーロ
ートで過、取り出したケーキをイソプロピルア
ルコール900mlで再度洗浄過し、ケーキを取り
出し石英ボートに入れ100℃／hrで昇温、700℃で
４時間加熱焙焼を行い、酸化ジルコニウムで110
ｇを得た。Example 1 An aqueous solution (350 ml) in which 325 g of zirconium oxychloride (ZrOCl 2.8H 2 O) was added and dissolved in 165 ml of distilled water was mixed with 200 ml of ammonia water (NH 3 29 wt%).
ml and aged with stirring at a temperature of 30°C for 2 hours. After adding 750ml of distilled water into the slurry
Stir for 10 minutes, let stand for 20 minutes, drain the supernatant liquid, repeat this operation, wash, filter through a Buchner funnel, wash the removed cake again with 900 ml of isopropyl alcohol, remove the cake and place it in a quartz boat. The temperature was raised at 100℃/hr, heated and roasted at 700℃ for 4 hours, and zirconium oxide was heated to 110℃.
I got g.
得られた粉体のＸ線回折線の半価幅（111）面
によるSherrerの式を用いた粒子径は170Åであ
り、電子顕微鏡での結果は200Åであつた（第３
図）。これら粉体の比表面積は27m2／ｇ細孔容積
0.228c.c.／ｇであつた。 The particle diameter using Sherrer's equation based on the half-width (111) plane of the X-ray diffraction line of the obtained powder was 170 Å, and the result with an electron microscope was 200 Å (3rd
figure). The specific surface area of these powders is 27m 2 /g pore volume
It was 0.228cc/g.
実施例 ２
蒸留水165mlにオキシ塩化ジルコニウム
（ZrOCl2・8H2Ｏ）325ｇ、塩化イツトリウム
（YCl3・6H2Ｏ）16.1ｇを加えて溶解させた水溶
液370mlを、アンモニア水（NH328wt％）210ml
の中へ添加し、温度30℃で２時間攪拌熟成する。Example 2 370 ml of an aqueous solution obtained by adding and dissolving 325 g of zirconium oxychloride (ZrOCl 2.8H 2 O) and 16.1 g of yttrium chloride (YCl 3.6H 2 O) in 165 ml of distilled water was added to aqueous ammonia (NH 3 28 wt%). 210ml
and stirred and aged for 2 hours at a temperature of 30°C.
熟成後、そのスラリーの中へ750mlの蒸留水を
添加後10分間攪拌、20分間静置し上澄液を排出、
この操作をくり返し行い洗浄を行つた後、ブフナ
ーロートで過、取り出されたケーキはイソプロ
ピルアルコール900mlで洗浄過後ケーキを取り
出し石英ボートに入れ100℃／hrで昇温、700℃で
４時間加熱焙焼を行い、準安定化ジルコニア122
ｇを得た。得られた粉体のＸ線回折線の半価幅
（111）面より、Sherrerの式を用いた粒子径は120
Åであり、電子顕微鏡での結果は150Åであつた
（第４図）。これら粉体の比表面積は44m2／ｇ、細
孔容積0.246c.c.／ｇであつた。 After aging, add 750ml of distilled water to the slurry, stir for 10 minutes, let stand for 20 minutes, and drain the supernatant liquid.
After repeating this operation and washing, the cake was filtered through a Buchner funnel, and the removed cake was washed with 900 ml of isopropyl alcohol.The cake was taken out and placed in a quartz boat, heated at a rate of 100°C/hr, and roasted at 700°C for 4 hours. and metastabilized zirconia 122
I got g. From the half width (111) plane of the X-ray diffraction line of the obtained powder, the particle diameter using Sherrer's formula is 120
The electron microscopic result was 150 Å (Fig. 4). These powders had a specific surface area of 44 m 2 /g and a pore volume of 0.246 cc/g.
実施例 ３
硝酸ジルコニウム〔ZrO（NO3）2・2H2Ｏ〕240
ｇを蒸留水225mlを加えて溶解させた水溶液をア
ンモニア水（NH329wt％）200mlの中へ添加、温
度30℃で２時間攪拌する。熟成が終了後これらス
ラリーの中へ750ml蒸留水を添加、10分間攪拌、
20分間静置して上澄み液を排出する。この操作を
くり返し８回行い洗浄を行つた後、ブフナーロー
トで過、取り出したケーキはイソプロピルアル
コール700ml洗浄過し取り出したケーキを石英
ボートに入れ100℃／hrで昇温し700℃で４時間焙
焼を行い、酸化ジルコニウム108ｇを得た。Example 3 Zirconium nitrate [ZrO(NO 3 ) 2・2H 2 O] 240
An aqueous solution prepared by adding g to 225 ml of distilled water and dissolving it was added to 200 ml of aqueous ammonia (NH 3 29 wt%) and stirred at a temperature of 30°C for 2 hours. After aging, add 750ml of distilled water to the slurry and stir for 10 minutes.
Let stand for 20 minutes and drain the supernatant. After repeating this operation 8 times and washing, the cake was filtered through a Buchner funnel, the removed cake was washed with 700 ml of isopropyl alcohol, the removed cake was placed in a quartz boat, heated at 100°C/hr, and then roasted at 700°C for 4 hours. Firing was performed to obtain 108 g of zirconium oxide.
得られた粉体はＸ線回折線の半価幅（111面）
によるSherrerの式を用いた粒子径170Å、電子顕
微鏡の結果200Å、また比表面積は25m2／ｇ、細
孔容積0.235c.c.／ｇであつた。 The obtained powder has a half width of X-ray diffraction line (111 planes)
The particle size was found to be 170 Å using the Sherrer's formula, 200 Å as determined by electron microscopy, the specific surface area was 25 m 2 /g, and the pore volume was 0.235 cc/g.
第１図はZrO2濃度と過時間の関係、第２図
はZrO2濃度と中和洗浄ケーキ中のZrO2含有量の
関係、第３図は実施例１で得られたZrO2粒子の
顕微鏡写真、第４図は実施例２で得られたZrO2
＋Y2O3粒子の顕微鏡写真を示す。
Figure 1 shows the relationship between ZrO 2 concentration and elapsed time, Figure 2 shows the relationship between ZrO 2 concentration and ZrO 2 content in the neutralized and washed cake, and Figure 3 shows the microscope of ZrO 2 particles obtained in Example 1. The photograph, Figure 4, shows ZrO 2 obtained in Example 2.
A micrograph of +Y 2 O 3 particles is shown.
Claims (1)
コニウム塩の濃度としてZrO2換算300〜450ｇ／
で、反応させ微粉末を得ることを特徴とする酸
化ジルコニウム微粉末の製造方法。 ２ 水溶性ジルコニウム塩をアルカリ水の中へ添
加し、反応させることを特徴とする特許請求の範
囲第１項記載の酸化ジルコニウム微粉末の製造方
法。 ３ 水溶性ジルコニウム塩に対し、アルカリ濃度
を0.5モル以上の過剰で反応させることを特徴と
する特許請求の範囲第１項記載の酸化ジルコニウ
ム微粉末の製造方法。 ４ ジルコニウム塩がオキシ塩化ジルコニウム、
硝酸ジルコニウム、硫酸ジルコニウム塩のいずれ
か一種以上であることを特徴とする特許請求の範
囲第１項記載の酸化ジルコニウム微粉末の製造方
法。 ５ 反応後過した後、アルコール洗浄すること
を特徴とする特許請求の範囲第１項記載の酸化ジ
ルコニウム微粉末の製造方法。 ６ 反応後洗浄、過し、仮焼する際、仮焼の昇
温速度を50〜150℃／Hrであることを特徴とする
特許請求の範囲第１項記載の酸化ジルコニウム微
粉末の製造方法。 ７ アルコールがC2〜C5アルコールであること
を特徴とする特許請求の範囲第５項記載の酸化ジ
ルコニウム微粉末の製造方法。 ８ 反応時に、安定化剤であるカルシウム、マグ
ネシウム、イツトリウムの塩のうち一種以上を含
むことを特徴とする特許請求の範囲第１項記載の
酸化ジルコニウム微粉末の製造方法。[Claims] 1 Water-soluble zirconium salt and alkaline water, the concentration of zirconium salt is 300 to 450 g/ZrO 2
A method for producing fine zirconium oxide powder, characterized in that a fine powder is obtained by the reaction. 2. The method for producing fine zirconium oxide powder according to claim 1, characterized in that a water-soluble zirconium salt is added to alkaline water and reacted. 3. The method for producing fine zirconium oxide powder according to claim 1, wherein the reaction is carried out at an excess alkali concentration of 0.5 molar or more with respect to the water-soluble zirconium salt. 4 Zirconium salt is zirconium oxychloride,
2. The method for producing fine zirconium oxide powder according to claim 1, wherein the zirconium oxide powder is at least one of zirconium nitrate and zirconium sulfate. 5. The method for producing fine zirconium oxide powder according to claim 1, which comprises washing with alcohol after the reaction. 6. The method for producing fine zirconium oxide powder according to claim 1, characterized in that during washing, filtering, and calcining after the reaction, the heating rate for calcining is 50 to 150°C/Hr. 7. The method for producing fine zirconium oxide powder according to claim 5, wherein the alcohol is a C2 to C5 alcohol. 8. The method for producing fine zirconium oxide powder according to claim 1, which contains at least one of calcium, magnesium, and yttrium salts as stabilizers during the reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23335284A JPS61111919A (en) | 1984-11-07 | 1984-11-07 | Production of zirconium oxide fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23335284A JPS61111919A (en) | 1984-11-07 | 1984-11-07 | Production of zirconium oxide fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61111919A JPS61111919A (en) | 1986-05-30 |
| JPH0472773B2 true JPH0472773B2 (en) | 1992-11-19 |
Family
ID=16953799
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23335284A Granted JPS61111919A (en) | 1984-11-07 | 1984-11-07 | Production of zirconium oxide fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61111919A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01188461A (en) * | 1988-01-20 | 1989-07-27 | Noboru Aiko | Al2o3-zro2 ceramic |
| DE4106535A1 (en) * | 1991-03-01 | 1992-09-03 | Degussa | MONOCLIN'S ZIRCONOXIDE, PROCESS FOR ITS PRODUCTION AND USE |
| US6524548B1 (en) | 1994-12-17 | 2003-02-25 | Degussa Ag | Zirconium dioxide powder, method of its production and use |
-
1984
- 1984-11-07 JP JP23335284A patent/JPS61111919A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61111919A (en) | 1986-05-30 |
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