JPH04325413A - Oriented zinc oxide powder and its manufacture - Google Patents
Oriented zinc oxide powder and its manufactureInfo
- Publication number
- JPH04325413A JPH04325413A JP12288391A JP12288391A JPH04325413A JP H04325413 A JPH04325413 A JP H04325413A JP 12288391 A JP12288391 A JP 12288391A JP 12288391 A JP12288391 A JP 12288391A JP H04325413 A JPH04325413 A JP H04325413A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- oriented
- powder
- oxide powder
- line intensity
- 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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 64
- 239000000843 powder Substances 0.000 claims description 40
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 33
- 229940007718 zinc hydroxide Drugs 0.000 claims description 33
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims description 33
- 238000002441 X-ray diffraction Methods 0.000 abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract 4
- 239000002245 particle Substances 0.000 description 30
- 238000000034 method Methods 0.000 description 18
- 239000013078 crystal Substances 0.000 description 8
- 239000011787 zinc oxide Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 7
- 229960001763 zinc sulfate Drugs 0.000 description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- -1 etc. Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、配向性酸化亜鉛粉末及
びその製造方法に関するものである。更に詳しくは、高
度に配向した（００２）配向性酸化亜鉛粉末及びその製
造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to oriented zinc oxide powder and a method for producing the same. More specifically, the present invention relates to highly oriented (002) oriented zinc oxide powder and a method for producing the same.
【０００２】0002
【従来の技術】酸化亜鉛は、半導性、圧電性、光導電性
等種々の機能を兼ね備えており、機能性粉末あるいは機
能性焼結体として広く利用されている。例えば、酸化亜
鉛粉末は電子写真用感光剤、顔料等に、又酸化亜鉛焼結
体はガスセンサー、バリスター、ターゲット等に利用さ
れるものである。従来酸化亜鉛粉末の工業的製造方法と
しては、乾式法と湿式法があり、乾式法には、溶融させ
た金属亜鉛を加熱し、でてくる亜鉛蒸気を空気で酸化さ
せるフランス法、亜鉛鉱石にコークスなどを加え、ばい
焼し発生する亜鉛蒸気を空気で酸化するアメリカ法があ
り、湿式法としては、塩化亜鉛等の溶液にソーダ灰等を
加えて製造する方法等が知られている。しかしながら、
いずれの方法によっても（００２）が高度に配向した酸
化亜鉛粉末を得ることは極めて困難であった。又、例え
ば機能性セラミックスの利用において、焼結体中の結晶
粒子の結晶軸を配向させることにより、その優れた特性
を更に発揮させることが出来、従来から配向性セラミッ
クスに関し種々の方法が試みられている。焼結体は、原
料粉末を乾式加圧成形、鋳込み成形等により成形し、得
られた成形体を焼成することにより得られるが、上記の
ような粉末を原料にして（００２）が高度に配向した酸
化亜鉛焼結体を得ることは極めて困難であった。BACKGROUND OF THE INVENTION Zinc oxide has various functions such as semiconductivity, piezoelectricity, and photoconductivity, and is widely used as a functional powder or a functional sintered body. For example, zinc oxide powder is used for electrophotographic photosensitizers, pigments, etc., and zinc oxide sintered bodies are used for gas sensors, varistors, targets, etc. Conventional industrial methods for producing zinc oxide powder include a dry method and a wet method. There is an American method in which zinc vapor produced by roasting is oxidized with air by adding coke, etc., and a known wet method is one in which soda ash or the like is added to a solution of zinc chloride or the like. however,
It was extremely difficult to obtain zinc oxide powder in which (002) was highly oriented by any method. In addition, for example, when using functional ceramics, by orienting the crystal axes of the crystal grains in the sintered body, its excellent properties can be further exhibited, and various methods have been tried in the past regarding oriented ceramics. ing. The sintered body is obtained by molding raw material powder by dry pressure molding, casting molding, etc., and firing the obtained molded body. It was extremely difficult to obtain a zinc oxide sintered body.
【０００３】0003
【発明が解決しようとする問題点】本発明の目的は、高
度に配向した（００２）配向性酸化亜鉛粉末及びそれを
簡単な方法でかつ容易に製造し得る方法を提供すること
にある。SUMMARY OF THE INVENTION An object of the present invention is to provide a highly oriented (002) oriented zinc oxide powder and a method for producing the same in a simple and easy manner.
【０００４】0004
【問題点を解決するための手段】本発明者等は、配向性
酸化亜鉛を検討し、酸化亜鉛粉末の製造に関し鋭意検討
した結果、（００１）配向性含硫酸水酸化亜鉛粉末を原
料とすることにより容易に（００２）配向性の薄板状酸
化亜鉛粉末が得られることを見出し本発明を完成した。
すなわち、本発明は、
（１）Ｘ線回析による（００２）回析線強度／（１０１
）回析線強度比が２以上である、（００２）配向性酸化
亜鉛粉末。
（２）Ｘ線回析による（００１）回析線強度／（００２
）回析線強度比が５以上である（００１）配向性含硫酸
水酸化亜鉛粉末を仮焼することにより得られる、Ｘ線回
析による（００２）回析線強度／（１０１）回析線強度
比が２以上である（００２）配向性酸化亜鉛粉末の製造
方法。[Means for Solving the Problems] As a result of studying oriented zinc oxide and intensively studying the production of zinc oxide powder, the present inventors have determined that (001) oriented sulfuric acid-containing zinc hydroxide powder is used as a raw material. The present invention was completed based on the discovery that a thin plate-like zinc oxide powder with (002) orientation can be easily obtained by this method. That is, the present invention provides (1) (002) diffraction line intensity/(101) by X-ray diffraction.
) A (002) oriented zinc oxide powder having a diffraction line intensity ratio of 2 or more. (2) (001) diffraction line intensity/(002) by X-ray diffraction
) (002) diffraction line intensity/(101) diffraction line by X-ray diffraction obtained by calcining a (001) oriented sulfuric acid-containing zinc hydroxide powder having a diffraction line intensity ratio of 5 or more A method for producing (002) oriented zinc oxide powder having an intensity ratio of 2 or more.
【０００５】を要旨とするものである。The gist is as follows.
【０００６】以下本発明を詳細に説明する。The present invention will be explained in detail below.
【０００７】[0007]
【作用】本発明の配向性は、通常の粉末法のＸ線回析装
置によるＸ線回析図形を用いて各々の面指数の回析線強
度の比から求めたものである。[Operation] The orientation of the present invention is determined from the ratio of the diffraction line intensities of each plane index using an X-ray diffraction pattern obtained by an ordinary powder method X-ray diffraction apparatus.
【０００８】結晶の配向性は、Ｘ線回析法により調べる
ことが可能である。すなわち、結晶が材料中に３次元的
に規則的に配列している場合、そのＸ線回析図形は単結
晶の場合と同等な異方性を生じるはずであり、一方、結
晶が材料中にランダムに配列している場合、その得られ
るＸ線回析図形は粉末Ｘ線と同等である。[0008] Crystal orientation can be examined by X-ray diffraction. In other words, if crystals are regularly arranged in a three-dimensional manner in a material, the X-ray diffraction pattern should exhibit anisotropy equivalent to that of a single crystal. When arranged randomly, the resulting X-ray diffraction pattern is equivalent to powder X-rays.
【０００９】本発明の酸化亜鉛粉末は、薄板状の含硫酸
水酸化亜鉛を仮焼し得られるものであり、酸化亜鉛結晶
粒子が薄板状に集合したものである。本発明で言う平均
粒子径及び平均粒子厚さは、該薄板状集合体の平均粒子
径及び平均粒子厚さを走査型電子顕微鏡（ＳＥＭ）によ
る観察から求めたものである。The zinc oxide powder of the present invention is obtained by calcining thin plate-shaped sulfuric acid-containing zinc hydroxide, and is a collection of zinc oxide crystal particles in the form of a thin plate. The average particle diameter and average particle thickness referred to in the present invention are those determined from observation of the average particle diameter and average particle thickness of the thin plate-like aggregate using a scanning electron microscope (SEM).
【００１０】本発明に於いては、含硫酸水酸化亜鉛粉末
を原料とすることが（００２）が高度に配向した酸化亜
鉛を得るために必須であり、さらに該含硫酸水酸化亜鉛
粉末の（００１）回析線強度／（００２）回析線強度比
が５以上であることが必要である。In the present invention, it is essential to use the sulfuric acid-containing zinc hydroxide powder as a raw material in order to obtain highly oriented zinc oxide (002), and furthermore, the (002) of the sulfuric acid-containing zinc hydroxide powder is It is necessary that the ratio of 001) diffraction line intensity/(002) diffraction line intensity is 5 or more.
【００１１】前記回析線強度比が５未満の場合は、（０
０２）回析線強度／（１０１）回析線強度比が２以上で
ある（００２）配向性酸化亜鉛粉末を得ることは困難で
あり、５以上に特に上限はなく高い方が望ましい。特に
８以上が望ましい。[0011] When the diffraction line intensity ratio is less than 5, (0
It is difficult to obtain (002) oriented zinc oxide powder with a ratio of 02) diffraction line strength/(101) diffraction line intensity of 2 or more, and there is no particular upper limit to 5 or more, and a higher one is preferable. Particularly desirable is 8 or more.
【００１２】本発明に用いる含硫酸水酸化亜鉛粉末とは
基本構造Ｚｎ４ ＳＯ４ （ＯＨ）６ で表され
る薄板状の化合物であり、上記した条件を満たせば、ど
の様な方法で得た含硫酸水酸化亜鉛粉末も用いることが
出来る。The sulfuric acid-containing zinc hydroxide powder used in the present invention is a thin plate-like compound represented by the basic structure Zn4SO4(OH)6. Zinc hydroxide powder can also be used.
【００１３】例えば、硫酸亜鉛水溶液から含硫酸水酸化
亜鉛を製造するに当たり、該亜鉛イオンに対し．１．０
〜２．０倍のモル比の水酸イオンを生じる塩基を加え、
その後得られた含硫酸水酸化亜鉛スラリーを熟成し、こ
れを濾過、洗浄の後乾燥することにより得ることが出来
る。For example, when producing sulfuric acid-containing zinc hydroxide from an aqueous zinc sulfate solution, for the zinc ion. 1.0
Adding a base that produces hydroxyl ions at a molar ratio of ~2.0 times,
The resulting sulfuric acid-containing zinc hydroxide slurry is aged, filtered, washed, and then dried.
【００１４】この硫酸亜鉛水溶液に加える水溶液系で水
酸イオン（ＯＨ−）を与える塩基としては、水酸化ナト
リウム、水酸化カリウム、アンモニア等使用することが
出来るが、不純物が混入しにくいことからアンモニアの
使用が好ましい。この場合、硫酸亜鉛水溶液から含硫酸
水酸化亜鉛を製造するに当たり、該亜鉛イオンに対し１
．０〜２．０倍のモル比の水酸イオンを生じる塩基を加
える必要がある。As a base that gives hydroxide ions (OH-) in an aqueous solution system to be added to this aqueous zinc sulfate solution, sodium hydroxide, potassium hydroxide, ammonia, etc. can be used, but ammonia is less likely to be contaminated with impurities. It is preferable to use In this case, when producing sulfuric acid-containing zinc hydroxide from a zinc sulfate aqueous solution, 1
．． It is necessary to add a base that produces hydroxyl ions in a molar ratio of 0 to 2.0 times.
【００１５】該モル比が１．０未満の場合、得られる薄
板状粒子がランダムに凝集し高度に配向した含硫酸水酸
化亜鉛粉末を得ることが困難となる。又、２．０を越え
る場合も、含硫酸水酸化亜鉛の溶解度が大きくなり、高
度に配向した含硫酸水酸化亜鉛粉末を得ることが困難と
なる。従って、特に１．５±０．２の範囲が望ましい。
また、反応系の濃度は出来るだけ希薄はものが好ま
しく、反応系中の亜鉛濃度として０．２モル／リットル
程度以下が好ましい。[0015] When the molar ratio is less than 1.0, the resulting thin plate-like particles will randomly aggregate, making it difficult to obtain a highly oriented sulfuric acid-containing zinc hydroxide powder. Further, if it exceeds 2.0, the solubility of the sulfuric acid-containing zinc hydroxide increases, making it difficult to obtain a highly oriented sulfuric acid-containing zinc hydroxide powder. Therefore, a range of 1.5±0.2 is particularly desirable. Further, the concentration of the reaction system is preferably as dilute as possible, and the zinc concentration in the reaction system is preferably about 0.2 mol/liter or less.
【００１６】０．２モル／リットルを越える場合、粒子
の分散性が低下し高配向な含硫酸水酸化亜鉛粉末が得難
い。If the amount exceeds 0.2 mol/liter, the dispersibility of the particles decreases, making it difficult to obtain highly oriented sulfuric acid-containing zinc hydroxide powder.
【００１７】次に、本発明に於いては上記方法により得
られた含硫酸水酸化亜鉛スラリーを熟成することが必要
である。Next, in the present invention, it is necessary to age the sulfuric acid-containing zinc hydroxide slurry obtained by the above method.
【００１８】熟成のない場合、粒子の凝集が激しく高配
向な含硫酸水酸化亜鉛粉末を得ることは困難である。[0018] In the absence of aging, the particles are severely agglomerated and it is difficult to obtain a highly oriented sulfuric acid-containing zinc hydroxide powder.
【００１９】又、熟成には配向比の増加、粒径の増大の
作用があり、適性な時間を選定することにより、用途に
適した配向度及び粒度の含硫酸水酸化亜鉛粉末を容易に
製造し得ることが可能である。[0019] Furthermore, aging has the effect of increasing the orientation ratio and particle size, and by selecting an appropriate time, it is possible to easily produce sulfuric acid-containing zinc hydroxide powder with the degree of orientation and particle size suitable for the application. It is possible to do so.
【００２０】つづいて、上記本発明の含硫酸水酸化亜鉛
スラリーを濾過、水洗後乾燥することにより、Ｘ線回析
による（００１）回析線強度／（００２）回析線強度比
が５以上である（００１）配向性含硫酸水酸化亜鉛粉末
を得ることが出来る。[0020] Subsequently, the sulfuric acid-containing zinc hydroxide slurry of the present invention is filtered, washed with water, and then dried to obtain a (001) diffraction line intensity/(002) diffraction line intensity ratio of 5 or more by X-ray diffraction. A (001) oriented sulfuric acid-containing zinc hydroxide powder can be obtained.
【００２１】乾燥温度は３００℃以下であれば特に制限
はないが、温度により得られる含硫酸水酸化亜鉛（Ｚｎ
４ ＳＯ４ （ＯＨ）６ ・ｎＨ２ Ｏ）の水
和量ｎが異なり、１００〜２００℃が好ましい。３００
℃を越える場合、得られる含硫酸水酸化亜鉛の分解が起
こり易く好ましくない。The drying temperature is not particularly limited as long as it is 300°C or less, but sulfuric acid-containing zinc hydroxide (Zn
The hydration amount n of 4SO4(OH)6·nH2O) is different, and is preferably 100 to 200°C. 300
If the temperature exceeds .degree. C., decomposition of the resulting sulfuric acid-containing zinc hydroxide tends to occur, which is not preferable.
【００２２】上記本発明の条件を満足する含硫酸水酸化
亜鉛粉末を原料とし、仮焼することにより、本発明の条
件を満足する（００２）配向性酸化亜鉛粉末を容易に得
ることが出来る。By using the sulfuric acid-containing zinc hydroxide powder that satisfies the conditions of the present invention as a raw material and calcining it, it is possible to easily obtain (002) oriented zinc oxide powder that satisfies the conditions of the present invention.
【００２３】本発明に於ける仮焼温度は、８００〜１４
００℃の範囲が好ましい。[0023] The calcination temperature in the present invention is 800 to 14
A range of 00°C is preferred.
【００２４】８００℃未満の場合、（００２）回析線強
度／（１０１）回析線強度比が２以上である（００２）
配向性酸化亜鉛粉末を得ることが困難であり、又、ＳＯ
４ が残留し好ましくない。一方、１４００℃を越える
と粒子間の焼結が著しく粗粒化し好ましくない。特に、
８５０〜１１００℃が望ましい。[0024] When the temperature is less than 800°C, the ratio of (002) diffraction line intensity/(101) diffraction line intensity is 2 or more (002)
It is difficult to obtain oriented zinc oxide powder, and SO
4 remains, which is not desirable. On the other hand, if the temperature exceeds 1400°C, the sintering between the particles becomes extremely coarse, which is not preferable. especially,
850-1100°C is desirable.
【００２５】以上の方法により、Ｘ線回析による（００
２）回析線強度／（１０１）回析線強度比が２以上であ
る（００２）配向性酸化亜鉛粉末を得ることが出来る。By the above method, (00
2) A (002) oriented zinc oxide powder having a diffraction line intensity/(101) diffraction line intensity ratio of 2 or more can be obtained.
【００２６】本発明の方法で得られる（００２）配向性
酸化亜鉛粉末は、平均粒子径１〜１００μｍ、平均粒子
厚さ０．０２〜０．５μｍ、平均粒子径／平均粒子厚さ
比が２０以上であることが望ましい。The (002) oriented zinc oxide powder obtained by the method of the present invention has an average particle diameter of 1 to 100 μm, an average particle thickness of 0.02 to 0.5 μm, and an average particle diameter/average particle thickness ratio of 20. The above is desirable.
【００２７】平均粒子径が１μｍ未満の場合、（００２
）回析線強度／（１０１）回析線強度比が２以上である
（００２）配向性酸化亜鉛粉末を得ることは困難である
。又、１００μｍを越える場合、（００２）回析線強度
／（１０１）回析線強度比が２以上である（００２）配
向性酸化亜鉛粉末を得ることは困難である。又、平均粒
子厚さが０．０２未満の場合、（００２）回析線強度／
（１０１）回析線強度比が２以上である（００２）配向
性酸化亜鉛粉末を得ることは困難であり、０．５μｍを
越える場合も（００２）回析線強度／（１０１）回析線
強度比が２以上である（００２）配向性酸化亜鉛粉末を
得ることは困難である。又、本発明に於いては上記粉末
の平均粒子径／平均粒子厚さ比が２０以上であることが
望ましいし、特に５０以上が望ましい。When the average particle diameter is less than 1 μm, (002
) It is difficult to obtain a (002) oriented zinc oxide powder with a diffraction line intensity/(101) diffraction line intensity ratio of 2 or more. Moreover, when it exceeds 100 μm, it is difficult to obtain (002) oriented zinc oxide powder with a ratio of (002) diffraction line intensity/(101) diffraction line intensity of 2 or more. In addition, when the average particle thickness is less than 0.02, (002) diffraction line intensity/
It is difficult to obtain (002) oriented zinc oxide powder with a (101) diffraction line intensity ratio of 2 or more, and even when the ratio exceeds 0.5 μm, (002) diffraction line intensity/(101) diffraction line It is difficult to obtain (002) oriented zinc oxide powder with an intensity ratio of 2 or more. Further, in the present invention, the average particle diameter/average particle thickness ratio of the powder is preferably 20 or more, and particularly preferably 50 or more.
【００２８】２０未満の場合、（００２）回析線強度／
（１０１）回析線強度比が２以上である（００２）配向
性酸化亜鉛粉末を得ることは困難である。[0028] If it is less than 20, (002) diffraction line intensity/
It is difficult to obtain a (002) oriented zinc oxide powder with a (101) diffraction line intensity ratio of 2 or more.
【００２９】[0029]
【実施例】以下実施例を述べるが、本発明はこれに限定
されるものではない。[Examples] Examples will be described below, but the present invention is not limited thereto.
【００３０】Ｘ線回析の測定は自動Ｘ線粉末回析装置（
ＰｈｉｌｉｐｓＰＷ１７２９）を使用した。測定条件は
、ＣｕＫα線、Ｘ線管電圧４０ＫＶ、電流５０ｍＡ、走
査速度２°／ｍｉｎで行った。X-ray diffraction measurements are performed using an automatic X-ray powder diffraction device (
Philips PW1729) was used. The measurement conditions were CuKα rays, an X-ray tube voltage of 40 KV, a current of 50 mA, and a scanning speed of 2°/min.
【００３１】実施例１
（００１）回析線強度／（００２）回析線強度比９．５
の（００１）配向性含硫酸水酸化亜鉛を下記の方法で得
た。Example 1 (001) diffraction line intensity/(002) diffraction line intensity ratio 9.5
(001) oriented sulfuric acid-containing zinc hydroxide was obtained by the following method.
【００３２】０．５モルの硫酸亜鉛を３０℃純水１０ｇ
に溶解させ、この硫酸亜鉛水溶液に１．４７モル／リッ
トルのアンモニア水５１０ｋｇを２時間で添加し、その
後撹拌下７２時間３０℃で熟成した。得られたスラリー
のＰＨは８．１であった。次に、得られたスラリーを濾
過し、純水２０ｋｇで洗浄した。つづいて、得られたケ
ーキを空気中１１０℃で２４時間乾燥させ、５９ｇの粉
末を得た。0.5 mol of zinc sulfate in 10 g of 30°C pure water
510 kg of 1.47 mol/liter ammonia water was added to this zinc sulfate aqueous solution over 2 hours, and then aged at 30° C. for 72 hours with stirring. The pH of the resulting slurry was 8.1. Next, the obtained slurry was filtered and washed with 20 kg of pure water. Subsequently, the obtained cake was dried in air at 110° C. for 24 hours to obtain 59 g of powder.
【００３３】得られた粉末は、ＳＥＭ観察により高分散
な６μｍ程度の六角板状の結晶であった。The obtained powder was found to be highly dispersed hexagonal plate-shaped crystals of about 6 μm according to SEM observation.
【００３４】この粉末は、Ｘ線回析で調べたところ基本
構造Ｚｎ４ ＳＯ４ （ＯＨ）６ で表される含
硫酸水酸化亜鉛であり、（００１）回析線強度／（００
２）回析線強度比にして９．５で表されるような非常に
（００１）が高度に配向した配向性含硫酸水酸化亜鉛で
あった。When examined by X-ray diffraction, this powder was found to be sulfuric acid-containing zinc hydroxide with the basic structure Zn4 SO4 (OH)6, and the ratio of (001) diffraction line intensity/(00
2) It was highly (001) oriented sulfuric acid-containing zinc hydroxide as expressed by a diffraction line intensity ratio of 9.5.
【００３５】次に、この配向性含硫酸水酸化亜鉛粉末を
９００℃で２時間仮焼した。Next, this oriented sulfuric acid-containing zinc hydroxide powder was calcined at 900° C. for 2 hours.
【００３６】得られた粉末は、Ｘ線回析で調べたところ
（００２）回析線強度／（１０１）回析線強度比９であ
る（００２）配向性酸化亜鉛粉末であり、ＳＥＭ観察に
より０．３μｍ程度の粒子が集合した平均粒子径５〜１
０μｍで平均厚さ０．２μｍ程度の薄板状粒子であり、
本発明の要件を満足するものであった。この粉末のＸ線
回析図形を図１に示した。
実施例２
実施例１で得られた配向性含硫酸水酸化亜鉛粉末を１０
００℃で２時間仮焼した。The obtained powder was examined by X-ray diffraction and was found to be (002) oriented zinc oxide powder with a ratio of (002) diffraction line intensity/(101) diffraction line intensity of 9, and by SEM observation. Average particle size of particles of about 0.3 μm aggregated 5 to 1
It is a thin plate-like particle with an average thickness of about 0.2 μm at 0 μm,
This satisfied the requirements of the present invention. The X-ray diffraction pattern of this powder is shown in FIG. Example 2 The oriented sulfuric acid-containing zinc hydroxide powder obtained in Example 1 was
It was calcined at 00°C for 2 hours.
【００３７】得られた粉末は、Ｘ線回析で調べたところ
（００２）回析線強度／（１０１）回析線強度比９．５
である（００２）配向性酸化亜鉛粉末であり、ＳＥＭ観
察により０．５μｍ程度の粒子が集合した平均粒子径１
０〜２０μｍで平均厚さ０．３μｍ程度の薄板状粒子で
あり、本発明の要件を満足するものであった。この粉末
のＸ線回析図形を図２に示した。
実施例３
（００１）回析線強度／（００２）回析線強度比６．７
の（００１）配向性含硫酸水酸化亜鉛を下記の方法で得
た。When the obtained powder was examined by X-ray diffraction, the ratio of (002) diffraction line intensity/(101) diffraction line intensity was 9.5.
It is a (002) oriented zinc oxide powder, and according to SEM observation, the average particle size of particles of about 0.5 μm is 1.
They were thin plate-like particles with a size of 0 to 20 μm and an average thickness of about 0.3 μm, which satisfied the requirements of the present invention. The X-ray diffraction pattern of this powder is shown in FIG. Example 3 (001) diffraction line intensity/(002) diffraction line intensity ratio 6.7
(001) oriented sulfuric acid-containing zinc hydroxide was obtained by the following method.
【００３８】０．５モルの硫酸亜鉛を３０℃純水１０ｇ
に溶解させ、この硫酸亜鉛水溶液に１．４７モル／リッ
トルのアンモニア水５１０ｋｇを２時間で添加し、その
後撹槇下１０時間３０℃で熟成した。得られたスラリー
のＰＨは８．１であった。次に、得られたスラリーを濾
過し、純水２０ｋｇで洗浄した。つづいて、得られたケ
ーキを空気中１１０℃で２４時間乾燥させ、５９ｇの粉
末を得た。得られた粉末は、ＳＥＭ観察により２〜３μ
ｍ程度の六角板状の結晶であった。0.5 mol of zinc sulfate in 10 g of 30°C pure water
510 kg of 1.47 mol/liter ammonia water was added to this aqueous zinc sulfate solution over 2 hours, and then aged at 30° C. for 10 hours under stirring. The pH of the obtained slurry was 8.1. Next, the obtained slurry was filtered and washed with 20 kg of pure water. Subsequently, the obtained cake was dried in air at 110° C. for 24 hours to obtain 59 g of powder. The obtained powder has a particle size of 2 to 3μ according to SEM observation.
It was a hexagonal plate-shaped crystal with a diameter of about m.
【００３９】この粉末は、Ｘ線回析で調べたところ基本
構造Ｚｎ４ ＳＯ４ （ＯＨ）６ で表される含
硫酸水酸化亜鉛であり、（００１）回析線強度／（００
２）回析線強度比が６．７である（００１）が高度に配
向した配向性含硫酸水酸化亜鉛であった。 次に、上
記配向性含硫酸水酸化亜鉛粉末を１０００℃で２時間仮
焼した。When examined by X-ray diffraction, this powder was found to be sulfuric acid-containing zinc hydroxide with the basic structure Zn4SO4(OH)6, and the ratio of (001) diffraction line intensity/(00
2) The (001) having a diffraction line intensity ratio of 6.7 was highly oriented oriented sulfuric acid-containing zinc hydroxide. Next, the above-mentioned oriented sulfuric acid-containing zinc hydroxide powder was calcined at 1000° C. for 2 hours.
【００４０】得られた粉末は、Ｘ線回析で調べたところ
（００２）回析線強度／（１０１）回析線強度比が３．
５である（００２）配向性酸化亜鉛粉末であり、ＳＥＭ
観察により０．４μｍ程度の粒子が集合した平均粒子径
３〜５μｍで平均厚さ０．２μｍ程度の薄板状粒子であ
り、本発明の要件を満足するものであった。この粉末の
Ｘ線回析図形を図３に示した。
比較例１
（００１）回折線強度／（１０１）回折線強度比が０．
５の試薬酸化亜鉛粉末を１０００℃で２時間仮焼した。When the obtained powder was examined by X-ray diffraction, the ratio of (002) diffraction line intensity/(101) diffraction line intensity was 3.
5 (002) oriented zinc oxide powder, SEM
Observation revealed that the particles were thin plate-like particles with an average particle size of 3 to 5 μm and an average thickness of about 0.2 μm, which were a collection of particles of about 0.4 μm, which satisfied the requirements of the present invention. The X-ray diffraction pattern of this powder is shown in FIG. Comparative Example 1 (001) diffraction line intensity/(101) diffraction line intensity ratio is 0.
The reagent zinc oxide powder of No. 5 was calcined at 1000° C. for 2 hours.
【００４１】得られた粉末は、Ｘ線回折で調べたところ
（００２）回折線強度／（１０１）回折線強度が０．５
程度の酸化亜鉛粉末であり、本発明の要件を満足するも
のは得られなかった。When the obtained powder was examined by X-ray diffraction, the (002) diffraction line intensity/(101) diffraction line intensity was 0.5.
However, no zinc oxide powder was obtained that satisfied the requirements of the present invention.
【００４２】この粉末のＸ線回折図を図４に示した。
比較例２
（００１）回析線強度／（００２）回析線強度比が３と
配向性の小さい含硫酸水酸化亜鉛粉末を９００℃で２時
間仮焼した。The X-ray diffraction pattern of this powder is shown in FIG. Comparative Example 2 A sulfuric acid-containing zinc hydroxide powder having a (001) diffraction line intensity/(002) diffraction line intensity ratio of 3 and a low orientation was calcined at 900°C for 2 hours.
【００４３】得られた粉末は、Ｘ線回析で調べたところ
（００２）回析線強度／（１０１）回析線強度比が１．
３程度の酸化亜鉛粉末であり、本発明の要件を満足する
ものは得られなかった。この粉末のＸ線回析図を図５に
示した。When the obtained powder was examined by X-ray diffraction, the ratio of (002) diffraction line intensity/(101) diffraction line intensity was 1.
It was a zinc oxide powder of about 3.5%, and no powder satisfying the requirements of the present invention could be obtained. The X-ray diffraction diagram of this powder is shown in FIG.
【００４４】[0044]
【発明の効果】本発明は、配向性酸化亜鉛粉末及びその
製造方法を提供するものであり、本発明により高度に配
向した（００２）配向性酸化亜鉛粉末を容易に得ること
が可能となる。Effects of the Invention The present invention provides an oriented zinc oxide powder and a method for producing the same, and the present invention makes it possible to easily obtain a highly oriented (002) oriented zinc oxide powder.
【００４５】例えば、この酸化亜鉛を原料とし高度に配
向した配向性酸化亜鉛焼結体を得ることが出来る。For example, a highly oriented oriented zinc oxide sintered body can be obtained using this zinc oxide as a raw material.
【図１】実施例１の方法で得られたＸ線回析図である。FIG. 1 is an X-ray diffraction diagram obtained by the method of Example 1.
【図２】実施例２の方法で得られたＸ線回析図である。FIG. 2 is an X-ray diffraction diagram obtained by the method of Example 2.
【図３】実施例３の方法で得られたＸ線回析図である。FIG. 3 is an X-ray diffraction diagram obtained by the method of Example 3.
【図４】比較例１の方法で得られたＸ線回析図である。FIG. 4 is an X-ray diffraction diagram obtained by the method of Comparative Example 1.
【図５】比較例２の方法で得られたＸ線回析図である。FIG. 5 is an X-ray diffraction diagram obtained by the method of Comparative Example 2.
Claims (2)
１０１）回析線強度比が２以上である、（００２）配向
性酸化亜鉛粉末。Claim 1: (002) diffraction line intensity/(
101) (002) oriented zinc oxide powder having a diffraction line intensity ratio of 2 or more.
００２）回析線強度比が５以上である（００１）配向性
含硫酸水酸化亜鉛粉末を仮焼することを特徴とする、Ｘ
線回析による（００２）回析線強度／（１０１）回析線
強度比が２以上である（００２）配向性酸化亜鉛粉末の
製造方法。Claim 2: (001) diffraction line intensity/(
002) X, characterized by calcining a (001) oriented sulfuric acid-containing zinc hydroxide powder having a diffraction line intensity ratio of 5 or more.
A method for producing (002) oriented zinc oxide powder having a (002) diffraction line intensity/(101) diffraction line intensity ratio of 2 or more by line diffraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12288391A JPH04325413A (en) | 1991-04-26 | 1991-04-26 | Oriented zinc oxide powder and its manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12288391A JPH04325413A (en) | 1991-04-26 | 1991-04-26 | Oriented zinc oxide powder and its manufacture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04325413A true JPH04325413A (en) | 1992-11-13 |
Family
ID=14846999
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12288391A Pending JPH04325413A (en) | 1991-04-26 | 1991-04-26 | Oriented zinc oxide powder and its manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04325413A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002121067A (en) * | 2000-10-10 | 2002-04-23 | Kyocera Corp | Zinc oxide-based sintered compact and method of producing the same |
| US11276515B2 (en) | 2019-02-22 | 2022-03-15 | Panasonic Intellectual Property Management Co., Ltd. | Varistor and method for producing same |
-
1991
- 1991-04-26 JP JP12288391A patent/JPH04325413A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002121067A (en) * | 2000-10-10 | 2002-04-23 | Kyocera Corp | Zinc oxide-based sintered compact and method of producing the same |
| JP4502493B2 (en) * | 2000-10-10 | 2010-07-14 | 京セラ株式会社 | Zinc oxide sintered body and method for producing the same |
| US11276515B2 (en) | 2019-02-22 | 2022-03-15 | Panasonic Intellectual Property Management Co., Ltd. | Varistor and method for producing same |
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