JPH01219014A - Production of dielectric material powder - Google Patents
Production of dielectric material powderInfo
- Publication number
- JPH01219014A JPH01219014A JP4609388A JP4609388A JPH01219014A JP H01219014 A JPH01219014 A JP H01219014A JP 4609388 A JP4609388 A JP 4609388A JP 4609388 A JP4609388 A JP 4609388A JP H01219014 A JPH01219014 A JP H01219014A
- Authority
- JP
- Japan
- Prior art keywords
- dielectric material
- crystal
- component
- powder
- point
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 239000003989 dielectric material Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 238000007496 glass forming Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 claims abstract description 5
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 3
- 229910052790 beryllium Inorganic materials 0.000 claims abstract 2
- 229910052749 magnesium Inorganic materials 0.000 claims abstract 2
- 229910052705 radium Inorganic materials 0.000 claims abstract 2
- 229910052719 titanium Inorganic materials 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 28
- 101100215617 Arabidopsis thaliana ADO3 gene Proteins 0.000 abstract description 12
- 229910052776 Thorium Inorganic materials 0.000 abstract 1
- 229910052788 barium Inorganic materials 0.000 abstract 1
- 229910052735 hafnium Inorganic materials 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- 229910052726 zirconium Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 22
- 239000002994 raw material Substances 0.000 description 9
- 239000003985 ceramic capacitor Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000010306 acid treatment Methods 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、セラミックコンデンサなどの電子部品となる
誘電体素子の製造に適する誘電体材料粉末の製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing dielectric material powder suitable for producing dielectric elements that become electronic components such as ceramic capacitors.
（従来の技術）
従来から、セラミックコンデンサなどとして使用されて
いるＢａＴ１０３．５ｒＴｉ（ｈなどやこれらセラミッ
クコンデンサにキュリー点のシフターなどとして添加さ
れるＣａＴｉＯ２、ＢａＺｒ０ ｚなどの酸化物系誘電
体材料粉末の製造方法としては、固相反応法が一般的に
用いられている。この固相反応法をＢａＴｉＯ３を例と
して説明すると、たとえばＴｉＯ２とＢａＣ０３とを出
発原料として使用し、これらを充分に混合した後、１０
００℃〜１２００℃程度の温 ・度で仮焼して結晶化
させ、得られた焼成物を粉砕、後処理して粉末とする方
法である。また、この固相反応性以外に、共沈法、アル
コキシド法、水熱合成法などが知られている。(Prior art) Oxide-based dielectric material powders such as BaT103.5rTi(h) used in ceramic capacitors, CaTiO2, BaZr0z, etc., which are added to these ceramic capacitors as Curie point shifters, etc. As a manufacturing method, a solid phase reaction method is generally used. To explain this solid phase reaction method using BaTiO3 as an example, for example, TiO2 and BaC03 are used as starting materials, and after mixing them thoroughly, , 10
This is a method of calcining and crystallizing at a temperature of about 00°C to 1200°C, and crushing and post-processing the obtained fired product to form a powder. In addition to this solid phase reactivity, coprecipitation methods, alkoxide methods, hydrothermal synthesis methods, and the like are known.
そして、これらの方法によって得た誘電体材料粉末をバ
インダ成分などとともに混合し、所定の形状の成形体を
作製した後、焼成して焼結させることによって目的とす
る誘電体素子を得ている。Then, the dielectric material powder obtained by these methods is mixed with a binder component and the like to produce a molded body of a predetermined shape, and then fired and sintered to obtain the desired dielectric element.
（発明が解決しようとする課題）
しかしながら、上述した固相反応法は、経済性、量産性
などに優れている半面、得られる粉末の粒径が２μｆｉ
ｌ〜３μｌと比較的大きく、また粒度の分布幅も広いと
いう問題があった。また、固相反応性以外の共沈法、ア
ルコキシド法、水熱合成法などによって製造される誘電
体材料粉末は、粒径が０．５μｍ＝１．５μｍ程度と比
較的微細な粉末であり、粒径的にはセラミックコンデン
サ用として適しているが、やはり上述した固相反応法と
同様に粒度分布幅が広く、粒径のばらつきが大きいとい
う問題があった。このように、粒径が不均一であると、
焼結させた際に得られる焼結体の機械的強度が部分的に
不均一となり、素子の寿命を短くする原因となるため、
より粒径の均一な誘電体材料粉末が求められている。(Problems to be Solved by the Invention) However, while the solid phase reaction method described above is excellent in economy and mass production, the particle size of the obtained powder is 2 μfi.
There was a problem that the particle size was relatively large at 1 to 3 μl, and the particle size distribution was wide. In addition, dielectric material powder produced by a coprecipitation method, an alkoxide method, a hydrothermal synthesis method, etc. other than solid phase reactivity is a relatively fine powder with a particle size of about 0.5 μm = 1.5 μm, Although it is suitable for use in ceramic capacitors in terms of particle size, it still has the problem of a wide particle size distribution and large variations in particle size, similar to the solid phase reaction method described above. In this way, if the particle size is non-uniform,
When sintered, the mechanical strength of the sintered body obtained becomes partially uneven, which can shorten the life of the element.
There is a demand for dielectric material powder with more uniform particle size.
また、近年、電子機器の小型化に伴いセラミックコンデ
ンサなどの素子も小型大容量のものが望まれている。こ
のセラミックコンデンサなどの素子の小型大容量化を実
現する一つの手段として積層型セラミックコンデンサが
知られており、積層数を増してさらに大容量化すること
が試みられている。しかし、積層数を増加させることは
誘電体層間に設けられる内部電極数をも増加させること
となり著しいコストの上昇を招いてしまう。これは、Ｂ
ａＴ１０３、ＢａＺｒ０３、ＣａＴｉＯ３、ＳｒＴｉＯ
３などの焼結温度が１３００℃〜１４００℃と高いため
、内部電極として高価なＰｔ’ＰＰｄを使用せざる得な
いためである。Furthermore, in recent years, with the miniaturization of electronic devices, elements such as ceramic capacitors are desired to have a small size and a large capacity. Multilayer ceramic capacitors are known as one means of realizing smaller size and larger capacity of elements such as ceramic capacitors, and attempts are being made to increase the number of laminated layers to further increase the capacity. However, increasing the number of laminated layers also increases the number of internal electrodes provided between dielectric layers, resulting in a significant increase in cost. This is B
aT103, BaZr03, CaTiO3, SrTiO
This is because the sintering temperature of No. 3 and the like is as high as 1300° C. to 1400° C., so that expensive Pt'PPd must be used as the internal electrode.
これに対する解決策の一つとして誘電体材料粉末を微細
化して焼結温度を低下させ、内部電極にＡｇなどの比較
的安価な材料の使用を可能にする方法が考えられている
が、上述したような従来法によって製造された誘電体材
料粉末は、上記要求を満足していないため、この方法に
適した高品位で微細な誘電体材料粉末が強く求められて
いる。One possible solution to this problem is to reduce the sintering temperature by making the dielectric material powder finer, making it possible to use relatively inexpensive materials such as Ag for the internal electrodes. Since the dielectric material powder produced by the conventional method does not satisfy the above requirements, there is a strong demand for a high-grade, fine dielectric material powder suitable for this method.
本発明は、このような従来技術の課題に対処するべくな
されたもので、粒径が微細で、かつ粒度分布の均一な誘
電体材料粉末を安定して得ることを可能にした誘電体材
料粉末の製造方法を提供することを目的としている。The present invention was made to address the problems of the prior art, and provides a dielectric material powder that makes it possible to stably obtain dielectric material powder with fine particle size and uniform particle size distribution. The purpose is to provide a manufacturing method for.
［発明の構成］
（課題を解決するための手段）
本発明の誘電体材料粉末の製造方法は、上記目的を達成
するために、誘電体材料の基本成分としてＡＯ酸成分Ａ
はＢａＳＢｅＳｑｇ、 Ｃａ５Ｓｒ、 Ｒａから選ばれ
た少なくとも一種の元素を示す。以下同じ。）オヨヒＤ
０２成分（Ｄ ハＴＩ、 Ｚｒ５Ｈｆ、 Ｔｈから選ば
れた少なくとも一種の元素を示す。以下同じ。）とガラ
ス形成成分としてＢ２Ｏ３成分およびＡＯ酸成分を少な
くとも含有する原料混合物を加熱溶融する工程と、この
溶融物を急冷して非晶質体とする工程と、この非晶質体
に熱処理を施してＡＤ（ｈで表される誘電体材料結晶を
析出させる工程と、この熱処理工程によって得た焼成物
を粉砕する工程と、得られた粉末を希酸で処理してガラ
ス形成成分を除去し、ＡＤＯ３で表される誘電体材料の
結晶粉末を抽出する工程とを有することを特徴としてい
る。[Structure of the Invention] (Means for Solving the Problems) In order to achieve the above object, the method for producing a dielectric material powder of the present invention uses an AO acid component A as a basic component of the dielectric material.
represents at least one element selected from BaSBeSqg, Ca5Sr, and Ra. same as below. ) Oyohi D
02 component (D represents at least one element selected from TI, Zr5Hf, and Th; the same applies hereinafter); a step of heating and melting a raw material mixture containing at least a B2O3 component and an AO acid component as glass-forming components; A process of rapidly cooling the melt to form an amorphous body, a process of subjecting the amorphous body to a heat treatment to precipitate dielectric material crystals represented by AD (h), and a fired product obtained by this heat treatment process. The method is characterized by comprising a step of pulverizing the powder, and a step of treating the obtained powder with a dilute acid to remove glass-forming components and extracting a crystalline powder of a dielectric material represented by ADO3.
（作 用）
本発明においては、まずＡＯ−ＤＯ２−Ｂ２０３系の原
料混合物を溶融した後、急冷することにって非晶質体を
作製する。そして、この非晶質体に熱処理を施すことに
よってＡＤＯ３の結晶を析出させる。このＡＤＯ３結晶
の析出反応は、固相内での原子拡散に支配されるため、
ゆっくりと反応が進み、析出するＡＤＯ３結晶を非常に
微細な粒子とすることが可能となる。また、析出させる
結晶粒子の粒径の熱処理温度依存性が緩かであるため、
熱処理条件や原料混合物中の成分組成を変化させること
で、粒径の制御を容易に行うことが可能である。(Function) In the present invention, an amorphous body is produced by first melting an AO-DO2-B203-based raw material mixture and then rapidly cooling it. Then, by subjecting this amorphous body to heat treatment, crystals of ADO3 are precipitated. This precipitation reaction of ADO3 crystals is dominated by atomic diffusion within the solid phase, so
The reaction proceeds slowly, making it possible to form the precipitated ADO3 crystals into very fine particles. In addition, since the grain size of the crystal grains to be precipitated has a gentle dependence on the heat treatment temperature,
By changing the heat treatment conditions and the component composition in the raw material mixture, it is possible to easily control the particle size.
この熱処理条件は、目的とする誘電体材料によって異な
るが、通常６００℃〜８５０℃程度の温度条件下で、１
時間〜８時間程度行う。The conditions for this heat treatment vary depending on the intended dielectric material, but are usually 600°C to 850°C.
Do this for about 8 hours.
また、原料混合物中の各成分組成は、第１図に示す三角
成分図中におけるＡ０５０ｍｏ１％−８２０３５０ｔｏ
。In addition, the composition of each component in the raw material mixture is A050mo1%-820350to in the triangular component diagram shown in FIG.
.
１％の点ａと００２５５ｍｏ１％−ＡＯ４５ｍｏ１％の
点すとＢ０２４５ｍｏｌ１％−ＡＯ５５ｍｏ１％の点Ｃ
とで囲まれた範囲内（図中斜線で示す。）の組成を有す
るものが好ましい。1% point a and 00255mol1%-AO45mol1% point B0245mol1%-AO55mol1% point C
It is preferable to have a composition within the range surrounded by (indicated by diagonal lines in the figure).
これは、非晶質体を熱処理した際に、まずＡＢ２０４（
あるいはＡＯ・ Ｂ２０３）相が析出する。This is because when an amorphous material is heat-treated, AB204 (
Alternatively, the AO/B203) phase precipitates.
これは示差熱分析およびＸ線回折の結果などからＡＤＯ
３に優先して析出することを確認している。This is confirmed by differential thermal analysis and X-ray diffraction results.
It has been confirmed that this precipitates preferentially to 3.
したがってＡＤＯ３の基本成分となるＡＯがＢ２Ｏ３と
等量モルより少ない場合、ＡＯはＢ２Ｏ３と化合してＡ
Ｂ２０４となり易いため、目的とするＡＤＯ３の析出量
が減少し、残部がＤＯ２として析出してしまう。このＤ
Ｏ２は後工程の希酸処理によって除去することが比較的
困難であるため、最終生成物であるＡＤＯ３中に残存し
やすい。また、８２０３ｍの減少と共に溶融温度の上昇
を招き経済性が悪化する。以上の影響を考慮すると、第
１図中の点ａと点すとを結ぶ線上の組成およびそれより
ＡＯが過剰となる組成が好ましい組成範囲となる。Therefore, if AO, which is the basic component of ADO3, is less than the equivalent mole of B2O3, AO will combine with B2O3 and A
Since it tends to become B204, the amount of the target ADO3 to be precipitated decreases, and the remainder is precipitated as DO2. This D
Since O2 is relatively difficult to remove by dilute acid treatment in the post-process, it tends to remain in the final product ADO3. Furthermore, as the length of 8203 m decreases, the melting temperature increases, resulting in poor economic efficiency. Considering the above effects, the preferred composition range is the composition on the line connecting point a and point 2 in FIG. 1 and the composition where AO is in excess.
一方、ＡＯがＢ２Ｏ３のモル数より過剰である場合には
、ＡＯが非晶質体中に残存し、ＡＤＯ３＋ＡＢ２０４
＋ＡＯが析出する。このＡＯはＡＢ２０４と共・ に希
酸処理によって容易に除去することが可能であるが、Ａ
Ｏの析出量の増加に伴ってＡＤＯ３の収率が低下し、ま
た希酸処理工程への負担が増大し、生産性が損われるた
め、第１図中の点ａと点Ｃとを結ぶ線上の組成およびそ
れよりＤＯ２が過剰となる組成が好ましい組成範囲とな
る。On the other hand, when AO is in excess of the number of moles of B2O3, AO remains in the amorphous body, and ADO3+AB204
+AO is precipitated. This AO can be easily removed together with AB204 by dilute acid treatment;
As the amount of precipitated O increases, the yield of ADO3 decreases, and the burden on the dilute acid treatment process increases, which impairs productivity. A preferred composition range is a composition in which DO2 is in excess.
したがって、第１図中の点ａと点すと点Ｃとで囲まれた
範囲内の成分組成を有する原料混合物を使用することが
好ましい。さらに、化学量論比としテハ、点ａと点ｄ１
すなわち００２５０ｍｏ１％−ＡＯ５（１ｍｏ１％の点
とを結ぶ線上の組成であり、この線上の組成が最も望ま
しい成分組成となる。Therefore, it is preferable to use a raw material mixture having a component composition within the range surrounded by point a, point C, and point C in FIG. 1. Furthermore, as a stoichiometric ratio, the point a and the point d1
That is, it is the composition on the line connecting 00250mol%-AO5 (1mol%), and the composition on this line is the most desirable component composition.
（実施例）
以下、本発明の方法をＢ ａ （Ｔ ｉ ｘ Ｚ ｒ
１−ｘ ） ｏ３の製造に適、用した一実施例について
説明する。なお、ここでＺｒはＢａＴｉＯ３のキュリー
点をシフトさせる成分で、ＴＩに対してｘ−０，８０〜
１．０程度の範囲で選択的に置換するものである。(Example) Hereinafter, the method of the present invention will be described as B a (T i x Z r
1-x) An example applied to the production of o3 will be described. Note that Zr is a component that shifts the Curie point of BaTiO3, and is
This is selective substitution within a range of approximately 1.0.
まず、ガラス形成物質としてＢａｏ−Ｂ２Ｏ３を用い、
原料混合物を溶融冷却して得られる非晶質体において、
Ｂａ（Ｔｌｘｚｒｌ−ｘ）０３：Ｂａｏ−Ｂ２Ｏ３がモ
ル比でｓｏ：ｓｏ左なるように、それぞれの出発原料で
あるＴｉＯ２、ＺｒＯ２、Ｈ３ＢＯ３、ＢａＣ０３を所
定世評量し、これらを充分に混合した後、白金ルツボに
収容し、１３００℃〜１４００℃の温度条件で加熱溶融
した。この溶融物を白金ルツボ底部のノズルから流出さ
せ、直径２００１１１１０％回転数５０Ｏｒ、ｐ、ｍ−
、線圧５ｔ、ｏｎの水冷双ロール上に注いで急冷して薄
板状の非晶質体とした。First, using Bao-B2O3 as a glass forming substance,
In the amorphous body obtained by melting and cooling the raw material mixture,
After measuring the respective starting materials TiO2, ZrO2, H3BO3, and BaC03 in predetermined amounts so that the molar ratio of Ba(Tlxzrl-x)03:Bao-B2O3 is so:so, and mixing these thoroughly, It was placed in a platinum crucible and heated and melted at a temperature of 1300°C to 1400°C. This melt was flowed out from the nozzle at the bottom of the platinum crucible, with a diameter of 20011110% and a rotation speed of 50 Or, p, m-
The mixture was poured onto water-cooled twin rolls with a linear pressure of 5 t on and rapidly cooled to form a thin plate-like amorphous body.
次に、この非晶質体をボールミルまたは振動ミルによっ
て微粉砕し、所定の容器に充填して電気炉内に収容し、
７５０℃〜８５０℃で５時間熱処理を行い、Ｂａ （Ｔ
Ｉ、 Ｚｒ１−ｘ） ０３結晶を含む焼成物を作製した
。この焼成物を２０メツシユ以下となるように粉砕し、
１０％酢酸溶液で処理してガラス形成物質の溶解除去を
行った。なお、この際の結晶粉末の量は、酢酸溶液に対
して２０重量％とし、８０℃の液中で行った。次いで、
この酸処理後の処理物に対して繰返し水洗を行い、ｐＨ
が６以上となったところで水洗を終了して、脱水および
乾燥を行い、Ｂａ （ＴｉｘＺｒｌ−、） ０３結晶機
粒子を得た。Next, this amorphous material is pulverized using a ball mill or a vibration mill, and is filled into a predetermined container and placed in an electric furnace.
Heat treatment was performed at 750°C to 850°C for 5 hours, and Ba (T
A fired product containing Zr1-x)03 crystals was produced. This fired product is crushed to a size of 20 mesh or less,
The glass-forming substances were dissolved and removed by treatment with a 10% acetic acid solution. The amount of crystal powder at this time was 20% by weight based on the acetic acid solution, and the test was carried out in a liquid at 80°C. Then,
After this acid treatment, the treated product is repeatedly washed with water and the pH
Washing with water was completed when the value of 6 or more was reached, and dehydration and drying were performed to obtain Ba (TixZrl-,) 03 crystallizer particles.
得られたＢａ （ＴｉＸＺｒ１−ｘ） ０３粉末は、測
定の結果、平均粒径０．５μｍ１粒度分布（３σ） ０
．０８であった。As a result of measurement, the obtained Ba (TiXZr1-x) 03 powder has an average particle size of 0.5 μm1 particle size distribution (3σ) 0
．． It was 08.
一方、本発明との比較のため、共沈法によってＢａ（Ｔ
ｉ工Ｚ ｒ １□）０３粉末を作製し、この粉末につい
ても同様な測定を行ったところ、平均粒径１．６μｍ１
粒度分布（３σ）０，５であり、上記実施例によるＢａ
（ＴｉｘＺｒ、、 ） ０１粉末が粒径のそろった均
一なものであることを確認した。またこの結果は、各Ｂ
ａ （ＴｌｘＺｒｌ−ｘ） Ｏ、粉末の電子顕微鏡写真
からもいっそう明らかとなった。On the other hand, for comparison with the present invention, Ba(T
i-Tech Z r 1□)03 powder was prepared and similar measurements were performed on this powder, and the average particle size was 1.6 μm1.
The particle size distribution (3σ) is 0.5, and Ba according to the above example
(TixZr, , ) It was confirmed that the 01 powder was uniform with a uniform particle size. Also, this result shows that each B
a (TlxZrl-x) O, which became even clearer from the electron micrograph of the powder.
次に、上記実施例によって得たＢａ （ＴｉｘＺｒｌ−
ｘ）０３粉末を用い、焼結体を作製したところ、均質で
焼結強度が高く、非常に安定した長寿命の素子を得るこ
とができた。Next, Ba (TixZrl-
When a sintered body was produced using x)03 powder, it was possible to obtain an element that was homogeneous, had high sintering strength, and was extremely stable and had a long life.
なお、上記実施例においては、出発原料となる原料混合
物の組成や熱処理条件を変えることによって容易に粒径
を制御することができ、これらの組合わせにより、必要
に応じて０．０１μｍ〜数μＩの範囲で粒径を制御する
ことが可能である。In the above examples, the particle size can be easily controlled by changing the composition of the raw material mixture serving as the starting material and the heat treatment conditions. It is possible to control the particle size within the range of .
また、上記実施例では、本発明の製造方法をＢａ （Ｔ
ｉｘＺｒ１□）０３の製造に適用した例について説明し
たが、ＡＤＯ３のＡが１３６５Ｍｇ 、 Ｃａ、 Ｓｒ
やＲａで、ＤがＨｆ’やＴｈの場合でも同様な結果が得
られた。Furthermore, in the above examples, the manufacturing method of the present invention is described as Ba (T
We have explained an example applied to the production of ixZr1□)03, but when A of ADO3 is 1365Mg, Ca, Sr
Similar results were obtained when D was Hf' or Th.
［発明の効果］
以上説明したように本発明の誘電体材料粉末の製造方法
によれば、微細で粒度分布の幅が狭い均質な誘電体材料
粉末が得られ、また原料混合物の組成範囲や非晶質体へ
の熱処理条件を変えることにより粒径の制御が容易にで
き、希望する粒径の微粒子粉末を比較的大きいものから
、非常に微細なものまでコストを上げることなく安定し
て得ることが可能である。[Effects of the Invention] As explained above, according to the method for producing dielectric material powder of the present invention, a fine and homogeneous dielectric material powder with a narrow particle size distribution can be obtained, and the composition range of the raw material mixture and the Particle size can be easily controlled by changing the heat treatment conditions for the crystalloid, and it is possible to stably obtain fine particles of the desired particle size, from relatively large to extremely fine, without increasing costs. is possible.
第１図は本発明に係る原料混合物の各出発原料の組成を
示す三角成分図である。
出願人 東芝硝子株式会社
代理人 弁理士 須 山 佐 −
輸お
二角ｌ ＊ ｔ！ｌ （ｍｏ １％）
第１図FIG. 1 is a triangular component diagram showing the composition of each starting material of the raw material mixture according to the present invention. Applicant Toshiba Glass Co., Ltd. Agent Patent Attorney Sasa Suyama - Export Nikaku l * t! l (mo 1%) Figure 1
Claims (1)
、Ｂｅ、Ｍｇ、Ｃａ、Ｓｒ、Ｒａから選ばれた少なくと
も一種の元素を示す。）およびＤＯ＿２成分（ＤはＴｉ
、Ｚｒ、Ｈｒ、Ｔｈから選ばれた少なくとも一種の元素
を示す。）とガラス形成成分としてＢ＿２Ｏ＿３成分お
よびＡＯ成分とを含有する原料混合物を加熱溶融する工
程と、この溶融物を急冷して非晶質体とする工程と、こ
の非晶質体に熱処理を施してＡＤＯ＿３で表される誘電
体材料結晶を析出させる工程と、この熱処理工程によっ
て得た焼成物を粉砕する工程と、得られた粉末を希酸で
処理してガラス形成成分を除去し、ＡＤＯ＿３で表され
る誘電体材料の結晶粉末を抽出する工程とを有すること
を特徴とする誘電体材料粉末の製造方法。(1) AO component (A is Ba) as the basic component of dielectric material
, Be, Mg, Ca, Sr, and Ra. ) and DO_2 component (D is Ti
, Zr, Hr, and Th. ) and a B_2O_3 component and an AO component as glass-forming components by heating and melting, rapidly cooling this melt to form an amorphous body, and heat-treating this amorphous body. A process of precipitating dielectric material crystals represented by ADO_3, a process of pulverizing the fired product obtained by this heat treatment process, and a process of treating the obtained powder with dilute acid to remove glass-forming components, A method for producing a dielectric material powder, the method comprising: extracting a crystalline powder of a dielectric material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4609388A JPH01219014A (en) | 1988-02-29 | 1988-02-29 | Production of dielectric material powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4609388A JPH01219014A (en) | 1988-02-29 | 1988-02-29 | Production of dielectric material powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01219014A true JPH01219014A (en) | 1989-09-01 |
Family
ID=12737374
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4609388A Pending JPH01219014A (en) | 1988-02-29 | 1988-02-29 | Production of dielectric material powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01219014A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004331492A (en) * | 2003-04-18 | 2004-11-25 | Asahi Glass Co Ltd | Method of manufacturing lead titanate zirconate fine particle |
| JP2007326735A (en) * | 2006-06-07 | 2007-12-20 | Asahi Glass Co Ltd | Manufacturing method of fine particle of ceria-zirconia solid solution |
| JP2008143733A (en) * | 2006-12-08 | 2008-06-26 | Asahi Glass Co Ltd | Production method of zirconia microparticle |
| JP2011105542A (en) * | 2009-11-17 | 2011-06-02 | Asahi Glass Co Ltd | Method for producing titanate compound particle and titanate compound particle |
-
1988
- 1988-02-29 JP JP4609388A patent/JPH01219014A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004331492A (en) * | 2003-04-18 | 2004-11-25 | Asahi Glass Co Ltd | Method of manufacturing lead titanate zirconate fine particle |
| JP2007326735A (en) * | 2006-06-07 | 2007-12-20 | Asahi Glass Co Ltd | Manufacturing method of fine particle of ceria-zirconia solid solution |
| JP2008143733A (en) * | 2006-12-08 | 2008-06-26 | Asahi Glass Co Ltd | Production method of zirconia microparticle |
| JP2011105542A (en) * | 2009-11-17 | 2011-06-02 | Asahi Glass Co Ltd | Method for producing titanate compound particle and titanate compound particle |
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