JP3018683B2 - Method for producing lead-containing ceramics - Google Patents
Method for producing lead-containing ceramicsInfo
- Publication number
- JP3018683B2 JP3018683B2 JP31834091A JP31834091A JP3018683B2 JP 3018683 B2 JP3018683 B2 JP 3018683B2 JP 31834091 A JP31834091 A JP 31834091A JP 31834091 A JP31834091 A JP 31834091A JP 3018683 B2 JP3018683 B2 JP 3018683B2
- Authority
- JP
- Japan
- Prior art keywords
- setter
- lead
- ceramics
- ceramic
- firing
- 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
- 239000000919 ceramic Substances 0.000 title claims description 51
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000000203 mixture Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 6
- 230000003746 surface roughness Effects 0.000 claims description 3
- 238000010304 firing Methods 0.000 description 21
- 239000011230 binding agent Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 11
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 8
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 6
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 239000004926 polymethyl methacrylate Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は鉛を含有するセラミック
スの製造方法に関し、特に鉛を含有するＰＺＴ（チタン
酸ジルコン酸鉛）、ＰＴ（チタン酸鉛）系セラミックス
等の焼成工程において、セラミックスに発生する反りを
低減し、バインダーの飛散を容易にし、ワレ不良の少な
い、鉛系セラミックスで発生し易いＰｂＯの蒸発や、焼
成したセラミックスの特性ばらつきを抑えるために、焼
成中の鉛の雰囲気を制御した鉛を含有するセラミックス
の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing lead-containing ceramics, and more particularly to a method for firing lead-containing ceramics such as PZT (lead zirconate titanate) and PT (lead titanate) ceramics. Controlling the atmosphere of lead during firing in order to reduce the warpage that occurs, facilitate the scattering of the binder, reduce the cracking defect, and suppress the evaporation of PbO, which is likely to occur in lead-based ceramics, and the variation in the characteristics of fired ceramics The present invention relates to a method for producing a ceramic containing lead.
【０００２】[0002]
【従来の技術】板状のセラミックスの成形体を焼成する
場合に、一般に焼結体には反りが発生する。これを低減
するためにセラミックス成形体と同じ組成のセラミック
スの板を、積み上げたセラミックス成形体の上下どちら
か、もしくは両方に配置していた。このセラミックス板
はセッターと呼ばれているが、このセッターはラップ等
によって反りを極力少なくし、この面精度により焼成時
のセラミックスの成形体の反りを低減させている。この
反り低減のメカニズムは次の通りである。上側に配置さ
れたセッターはその重量で、セラミックスが押さえつけ
られ、そりが少なくなる。下側に配置されたセッターは
セラミックスが、焼成時に高温下で柔らかくなり成形体
の自重でセッターの面にそって変形することにより、成
形体独自の反りがなくなる。ＰｂＯの雰囲気に起因す
る、セラミックスの特性ばらつきの対策としては、白金
もしくはマグネシア、アルミナ等の密閉容器中でＰｂＯ
の雰囲気が飛散しないようにして焼成している。2. Description of the Related Art Generally, when a plate-shaped ceramic compact is fired, the sintered compact is warped. In order to reduce this, a ceramic plate having the same composition as the ceramic molded body is arranged on one or both sides of the stacked ceramic molded body, or both. The ceramic plate is called a setter, and the setter minimizes the warpage by wrapping and the like, and the surface accuracy reduces the warpage of the ceramic molded body during firing. The mechanism of this warpage reduction is as follows. The weight of the setter arranged on the upper side suppresses the ceramics, and the warpage is reduced. The ceramics of the setter arranged on the lower side are softened at a high temperature at the time of firing and deformed along the surface of the setter by the weight of the formed body, so that the warpage unique to the formed body is eliminated. As a countermeasure against the variation in the characteristics of ceramics due to the atmosphere of PbO, PbO is sealed in a sealed container of platinum, magnesia, alumina or the like.
The baking is performed so that the atmosphere is not scattered.
【０００３】[0003]
【発明が解決しようとする課題】上記従来技術によれ
ば、セラミックスの鉛の蒸発は一応押さえることはでき
るが、複数のセラミックスの板を積み上げて焼成する場
合には、積み段数間の特性ばらつきが発生し焼成ロット
内のばらつきを大きくしていた。すなわち重いＰｂＯの
雰囲気は、焼成容器の底に集まり積み段が下のセラミッ
クスほど、濃い鉛雰囲気で焼成されて特性ばらつきの原
因になっていた。また、特に鉛が蒸発し易い組成のセラ
ミックスでは、密閉容器で焼成しても鉛が蒸発し特性が
劣化する問題があった。このような場合には鉛雰囲気を
放出するＰｂＯの粉末等を焼成匣の中にいれて焼成を行
っている。この場合にも上記の鉛雰囲気の、高さ方向の
濃度勾配に起因する特性ばらつきが発生し、問題になっ
ていた。以上のような問題は、特にセラミックフィルタ
ーやセラミック発振子のように、０．５％以下の音速ば
らつきが問題になるような圧電体セラミックスでは特に
重要である。また、従来の方法ではバインダーを含有す
る成形体の上下をセラミックス板で挟んでしまうため、
バインダーが飛散しにくくなり、一部残留したバインダ
ーによってセラミックスが還元されたり、特性が低下し
たりする問題点があった。さらに、セッターは焼成工程
において何度も使用するため、セッター自体にそりが発
生するようになる問題があり、この問題の解決のために
セッターの厚さはある程度厚くして、そりを発生しにく
くしている。ところがこれに付随してセッターの重量が
重くなりすぎ、セラミックスの焼成過程において成形体
にワレが発生するという問題点があった。According to the above prior art, the evaporation of lead in ceramics can be suppressed for the time being, but when a plurality of ceramic plates are stacked and fired, the characteristic variation between the number of stacking stages is reduced. This occurred and the variation among firing lots was large. That is, the atmosphere of heavy PbO gathered at the bottom of the firing container, and the lower the stacking stage, the lower the firing temperature of the ceramics, and the higher the firing temperature, the more the characteristics of the ceramics fluctuated. Further, in particular, in the case of ceramics having a composition in which lead easily evaporates, there is a problem in that even when fired in a closed container, lead evaporates and characteristics are deteriorated. In such a case, firing is performed by placing a PbO powder or the like that releases a lead atmosphere in a firing box. In this case as well, characteristic variations due to the concentration gradient in the height direction of the above-mentioned lead atmosphere occur, which has been a problem. The above problems are particularly important for piezoelectric ceramics such as a ceramic filter or a ceramic oscillator in which a variation in sound speed of 0.5% or less becomes a problem. In addition, in the conventional method, since the upper and lower sides of the molded body containing the binder are sandwiched between ceramic plates,
There has been a problem that the binder is not easily scattered, and the ceramics are reduced by the partially remaining binder, or the characteristics are deteriorated. Furthermore, since the setter is used many times in the firing process, there is a problem that warpage occurs in the setter itself.In order to solve this problem, the thickness of the setter is increased to some extent, and it is difficult to generate warpage. are doing. However, accompanying this, the weight of the setter becomes too heavy, and there is a problem that cracks occur in the molded body during the firing process of the ceramics.
【０００４】本発明は、上記従来技術の有する問題点に
鑑みてなされたもので、セラミックスに焼結工程で発生
する反りを低減し、同時にバインダーの飛散を容易に
し、ワレ不良を少なくし、特性のばらつきを少なくする
鉛を含有するセラミックスの製造方法を提供することを
目的としている。The present invention has been made in view of the above-mentioned problems of the prior art, and has been made to reduce the warpage generated in a sintering process on ceramics, at the same time facilitate the scattering of a binder, reduce cracking defects, and improve the characteristics. It is an object of the present invention to provide a method for producing lead-containing ceramics, which reduces the variation of the ceramics.
【０００５】[0005]
【問題点を解決するための手段】本発明は、鉛を含有す
るセラミックスの成形体を１枚以上積み上げて焼結する
工程を有する鉛を含有するセラミックスの製造方法にお
いて、焼結工程を積み上げた前記成形体の上、下又は成
形体の間の少なくとも１個所に、板状のセッターを配置
して行い、該セッターの組成は鉛の重量比が化学量論比
と一致していないことを特徴とする。セッターの表面粗
さが５μm 以上であるか、または５％以上の気孔率であ
ることが好ましい。SUMMARY OF THE INVENTION The present invention relates to a method for producing lead-containing ceramics, comprising the step of sintering and sintering at least one lead-containing ceramic compact. A plate-like setter is arranged at least at one position above, below, or between the molded bodies, and the composition of the setter is such that the weight ratio of lead does not match the stoichiometric ratio. And It is preferable that the setter has a surface roughness of 5 μm or more or a porosity of 5% or more.
【０００６】[0006]
【作用】本発明は、セッターの鉛の重量比を化学量論比
よりも減少させることにより、セッターが匣の中の鉛雰
囲気を減少させることができる。またセッターの鉛の重
量比を化学量論比よりも増加させることにより、セッタ
ーから酸化鉛の雰囲気を意図的に放出することが可能と
なり、焼成時の鉛雰囲気のコントロールが可能となる。
セッターの気孔率を５％以上とし、セッターの層内にポ
アを形成することにより、焼成過程においてセラミック
スの成形体に含まれる有機バインダーの分解ガスが、ポ
アを通じて飛散することが可能となる。多孔質のセッタ
ーにすることにより、セッターの密度は小さくなりセッ
ターの重量は低減できる。これによりセラミックス焼成
時に成形体にかかる加重を低減することができる。ま
た、表面粗さを粗くしても、気孔率の大きいのと同様の
効果が得られる。The present invention allows the setter to reduce the lead atmosphere in the box by reducing the lead weight ratio of the setter below the stoichiometric ratio. By increasing the weight ratio of lead in the setter to above the stoichiometric ratio, the atmosphere of lead oxide can be intentionally released from the setter, and the lead atmosphere during firing can be controlled.
By setting the porosity of the setter to 5% or more and forming pores in the layer of the setter, it becomes possible for the decomposition gas of the organic binder contained in the ceramic molded body to be scattered through the pores during the firing process. By using a porous setter, the density of the setter can be reduced and the weight of the setter can be reduced. As a result, the load applied to the compact during firing of the ceramics can be reduced. Further, even if the surface roughness is increased, the same effect as that of a large porosity can be obtained.
【０００７】[0007]
【実施例】以下本発明を実施例により詳しく説明する。
ＰＺＴ系圧電体セラミックスの製造に適用した例を以下
に説明する。実施例１ セッターを、図１に示す鉛を含有するセラミックスの製
造方法の工程に従って作製する。セッターは作成しよう
とする圧電体セラミックスと同一組成系とし、Ｐｂ
X （Ｔｉ0.48Ｚｒ0.52）Ｏ3 ＋１．０ｗｔ％Ｎｂ2 Ｏ5
で表される組成になるように、ＰｂＯ，ＴｉＯ2 ，Ｚｒ
Ｏ2 ，Ｎｂ2 Ｏ5をそれぞれ秤量し、ボールミルで湿式
混合した（工程ａ）。ここで鉛量Ｘは１．０１や０．９
９のように化学量論比からずれた組成になるようにそれ
ぞれ秤量した。得られたスラリーを脱水し電気炉中で９
００℃で仮焼し（工程ｂ）、仮焼粉末とポリビニルアル
コール（ＰＶＡ）系のバインダーを圧電体の仮焼粉末に
対して５ｗｔ％と、粒度５０μｍのポリメタアクリル酸
メチル（ＰＭＭＡ）系のバインダーを圧電体の仮焼粉末
に対し３〜２０ｗｔ％加えボールミルで湿式混合した
（工程ｃ）。混合したスラリーはスプレードライヤーに
よって乾燥・造粒した（工程ｄ）。得られたスプレー粉
末をプレス成形によって薄板状に成形した（工程ｅ）。
成形圧力は１ton/ cm2、外形寸法は３５mm×３５mm×厚
さ２．５mmである。この成形体を電気炉中で１２００〜
１２５０℃の温度で焼成し（工程ｆ）、気孔率５〜６０
％の多孔質焼結体を得た。この多孔質焼結体をセッター
として使うために、＃４００の研磨粉を用いてラップし
平面度を出した。The present invention will be described in more detail with reference to the following examples.
An example in which the present invention is applied to the production of a PZT-based piezoelectric ceramic will be described below. Example 1 A setter is manufactured according to the steps of the method for manufacturing a lead-containing ceramic shown in FIG. The setter has the same composition as the piezoelectric ceramic to be made,
X (Ti 0.48 Zr 0.52 ) O 3 +1.0 wt% Nb 2 O 5
PbO, TiO 2 , Zr so that the composition represented by
O 2 and Nb 2 O 5 were weighed and wet-mixed with a ball mill (step a). Here, the lead amount X is 1.01 or 0.9
Each was weighed so that the composition deviated from the stoichiometric ratio as shown in FIG. The obtained slurry is dewatered and placed in an electric furnace for 9 hours.
Calcined at 00 ° C. (step b), and calcined powder and polyvinyl alcohol (PVA) -based binder are 5 wt% based on the calcined powder of the piezoelectric substance, and polymethyl methacrylate (PMMA) -based with a particle size of 50 μm is used. The binder was added in an amount of 3 to 20% by weight based on the calcined powder of the piezoelectric body, and was wet-mixed with a ball mill (step c). The mixed slurry was dried and granulated by a spray drier (step d). The obtained spray powder was formed into a thin plate by press molding (step e).
The molding pressure is 1 ton / cm 2 , and the outer dimensions are 35 mm × 35 mm × 2.5 mm in thickness. This molded body is placed in an electric furnace at 1200
Firing at a temperature of 1250 ° C. (step f), porosity 5-60
% Of a porous sintered body was obtained. In order to use this porous sintered body as a setter, it was wrapped with # 400 abrasive powder to obtain flatness.
【０００８】次いで、鉛を含有するセラミックスの製造
方法の図１に示す製造工程に従って成形体を作製する。
焼成しようとする圧電体セラミックスは、ＰｂX （Ｔｉ
0.48Ｚｒ0.52）Ｏ3 ＋１．０ｗｔ％Ｎｂ2 Ｏ5 で表され
る組成となるようにＰｂＯ，ＴｉＯ2 ，ＺｒＯ2 ，Ｎｂ
2 Ｏ5 をそれぞれ秤量し混合し（工程ａ）、上記セッタ
ーの作製と同様に仮焼する（工程ｂ）。この仮焼粉末を
ＰＭＭＡ系のバインダーを使用しない以外は、セッター
の作製と同様の操作手順により、バインダーと混合し
（工程ｃ）、造粒し（工程ｄ）、１ton/cm2 の圧力でプ
レス成形し（工程ｅ）、２５mm×２５mm×厚さ０．８mm
の寸法の成形体にした。この成形体の焼成は、図２に示
すように、成形体１の上下に、セッター２，２を配置
し、マグネシア製の匣に入れ、１２００〜１２５０℃で
行った（工程ｆ）。この組成のセラミックスでは上側の
セッターを鉛過剰にし、下側のセッターの鉛を減少させ
た方がばらつきを小さくすることができた。こうして得
られた焼成体についてワレ不良率、電気機械結合係数
（Ｋｐ）（％）、誘電率について試験した結果を表１に
示した。なお表１に従来例として、焼成しようとするＰ
ＺＴと同一組成のセッターを用いて焼成した結果も５欄
に合わせて示した。Next, a compact is produced according to the production process shown in FIG. 1 of the method for producing lead-containing ceramics.
The piezoelectric ceramic to be fired is Pb x (Ti
0.48 Zr 0.52 ) O 3 +1.0 wt% Nb 2 O 5 PbO, TiO 2 , ZrO 2 , Nb
Each of 2 O 5 is weighed and mixed (step a), and calcined in the same manner as in the preparation of the setter (step b). This calcined powder is mixed with a binder (step c), granulated (step d) and pressed at a pressure of 1 ton / cm 2 in the same operation procedure as in the preparation of the setter, except that a PMMA-based binder is not used. Formed (step e), 25mm x 25mm x 0.8mm thick
A molded article having the following dimensions: As shown in FIG. 2, the sintering of the compact was performed by placing the setters 2 and 2 above and below the compact 1 and placing them in a magnesia box at 1200 to 1250 ° C. (step f). In the ceramics of this composition, the dispersion could be reduced by making the upper setter lead-excessive and reducing the lead in the lower setter. Table 1 shows the results of tests on the fired body obtained in this way for cracking defect rate, electromechanical coupling coefficient (Kp) (%), and dielectric constant. Table 1 shows a conventional example of P to be fired.
The results of firing using a setter having the same composition as ZT are also shown in column 5.
【０００９】[0009]
【表１】 [Table 1]
【００１０】実施例２ 組成を、ＰｂX （Ｔｉ0.20Ｚｒ0.80）Ｏ3 ＋１．０ｗｔ
％Ｎｂ2 Ｏ5 で表される組成に適用した以外は実施例１
と同様にして工程ａ〜ｆにより、セッター及び成形体を
成形し、焼成し、試験した。この組成はＰＺＴ系のジル
コン酸鉛に近い組成で、極めて鉛の蒸発が発生しやすい
組成である。 Example 2 The composition was changed to Pb x (Ti 0.20 Zr 0.80 ) O 3 +1.0 wt.
Example 1 except that the composition represented by% Nb 2 O 5 was applied.
In steps a to f, a setter and a molded body were molded, fired, and tested in the same manner as in the above. This composition is close to PZT-based lead zirconate, and is a composition in which lead evaporation is extremely likely to occur.
【００１１】[0011]
【表２】 [Table 2]
【００１２】このような組成では、表２からわかるよう
に、上下のセッターとも鉛過剰の方がばらつきが少なく
なった。なお、上記実施例では圧電体であるＰＺＴで説
明したが、ＰＺＴ系以外の圧電体、又は圧電体以外の誘
電体や、絶縁体、磁性体その他の構造用セラミックス等
で鉛を含有するセラミックスに適用してもよい。また、
焼成時に鉛を過剰にしたセッターを使用するか、減少し
たセッターを使用するかは、焼成しようとするセラミッ
クスの組成や、匣の密閉度、匣内の対流等によって最適
なものを選ぶ。また、ポアをセッター中に形成する方法
は、樹脂の粉末を混合するだけでなく、有機バインダー
の混合比を多くしたり、発泡性の薬剤を混合して成形す
る等の方法でもよい。また成形方法も実施例ではスプレ
ードライヤーによる造粒粉をプレスする例を示したが、
ドクターブレード法や引き上げ成形法等のシート工法、
押し出し成形やインジェクション成形、鋳込み成形等の
成形方法において、上記の焼成後ポアを作る物質を混入
させてもよい。さらにポアを作る混入物質は、実施例で
はスラリー中に混合して造粒したが、造粒粉に乾式で樹
脂粉を混合する工法をとってもよい。また、上記実施例
では単板のセラミックスで説明したが、内部電極を含む
積層体では特にバインダーが飛散しにくく、バインダー
の残留が問題になる場合が多いが、本発明は積層セラミ
ックスの焼成においても有効である。With such a composition, as can be seen from Table 2, the variation in excess of lead was smaller in both the upper and lower setters. In the above-described embodiment, PZT, which is a piezoelectric material, has been described. However, piezoelectric materials other than PZT, dielectric materials other than piezoelectric materials, insulators, magnetic materials, and other ceramics containing lead, etc. May be applied. Also,
Whether to use a setter with an excessive amount of lead during firing or a reduced setter is selected according to the composition of the ceramic to be fired, the degree of sealing of the box, the convection in the box, and the like. Further, the method of forming the pores in the setter is not only to mix the resin powder, but also to increase the mixing ratio of the organic binder or to mix and mix the foaming agent and the like. In addition, the molding method also shows an example in which granulated powder is pressed by a spray dryer in the examples,
Sheet construction methods such as doctor blade method and pull-up molding method,
In a molding method such as extrusion molding, injection molding, cast molding, or the like, the above-mentioned material that forms pores after firing may be mixed. Further, in the embodiment, the contaminants forming the pores are mixed into the slurry and granulated, but a method of mixing the granulated powder with the resin powder in a dry manner may be employed. Further, in the above embodiment, a single-plate ceramic has been described. However, in a laminate including internal electrodes, the binder is particularly difficult to be scattered, and the remaining of the binder often becomes a problem. It is valid.
【００１３】[0013]
【発明の効果】本発明によれば、セッターの鉛量を化学
量論比から減少することにより、セッターで鉛雰囲気を
吸収させることが可能になる。また鉛量を化学量論比か
ら増加することにより、セッターから鉛雰囲気を放出さ
せることが可能になる。これによって焼成時の匣内の雰
囲気コントロールを、セッターによって行うことが可能
になり、同時に反りの低減も実現することが可能にな
る。さらに匣内の雰囲気コントロールは、どの鉛量のセ
ッターをどの位置に配置するかによって、面内だけでな
く高さ方向にも雰囲気濃度のコントロールが可能にな
り、きわめて特性ばらつきが小さいセラミックスを製造
することが可能である。またバインダーの分解ガスがス
ムーズにポアを通じて飛散するため、本発明により焼成
したセラミックスは、バインダーの残留にともなうセラ
ミックスの劣化や還元をなくすことができる。また、セ
ッターの重量の低減に伴い、セラミックスのワレ不良も
減少させることができる。According to the present invention, the lead atmosphere can be absorbed by the setter by reducing the lead content of the setter from the stoichiometric ratio. By increasing the amount of lead from the stoichiometric ratio, it becomes possible to release the lead atmosphere from the setter. This makes it possible to control the atmosphere in the box during firing by the setter, and at the same time, to reduce warpage. In addition, the atmosphere in the box can be controlled not only in the plane but also in the height direction by controlling the amount of lead setter and the position of the setter. It is possible. Further, since the decomposition gas of the binder is smoothly scattered through the pores, the ceramic fired according to the present invention can eliminate the deterioration and reduction of the ceramic due to the residual binder. Further, with the reduction in the weight of the setter, cracking failure of the ceramics can be reduced.
【図１】本発明に係るセラミックスの製造方法の工程を
説明する図である。FIG. 1 is a view for explaining steps of a method for producing a ceramic according to the present invention.
【図２】上記工程の内の焼成工程を説明する図である。FIG. 2 is a diagram illustrating a firing step of the above steps.
１ 成形体 ２ セッター 1 molded body 2 setter
───────────────────────────────────────────────────── フロントページの続き (72)発明者 米田 康信 京都府長岡京市天神二丁目26番10号株式 会社 村田製作所内 (56)参考文献 特開 平４−187569（ＪＰ，Ａ) 特開 平４−321565（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C04B 35/64 ────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Yasunobu Yoneda 2-26-10 Tenjin, Nagaokakyo-shi, Kyoto Murata Manufacturing Co., Ltd. (56) References JP-A-4-187569 (JP, A) JP-A-4 -321565 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C04B 35/64
Claims (4)
枚以上積み上げて焼結する工程を有する鉛を含有するセ
ラミックスの製造方法において、焼結工程を積み上げた
前記成形体の上、下又は成形体の間の少なくとも１個所
に、板状のセッターを配置して行い、該セッターの組成
は鉛の重量比が化学量論比と一致していないことを特徴
とするセラミックスの製造方法。1. A lead-containing ceramic formed body is
In a method for producing lead-containing ceramics having a step of stacking and sintering at least one sheet, a plate-like setter is disposed at least at one place above, below, or between the formed bodies stacked in the sintering step. Wherein the weight ratio of lead does not coincide with the stoichiometric ratio in the composition of the setter.
電極を有する積層体であることを特徴とする請求項１記
載のセラミックスの製造方法。2. The method according to claim 1, wherein the lead-containing ceramic is a laminate having an internal electrode.
ある請求項１または請求項２記載のセラミックスの製造
方法。3. The method according to claim 1, wherein the setter has a surface roughness of 5 μm or more.
請求項１または請求項２記載の鉛を含有するセラミック
スの製造方法。4. The method for producing a lead-containing ceramic according to claim 1, wherein the setter has a porosity of 5% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31834091A JP3018683B2 (en) | 1991-11-05 | 1991-11-05 | Method for producing lead-containing ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31834091A JP3018683B2 (en) | 1991-11-05 | 1991-11-05 | Method for producing lead-containing ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05124872A JPH05124872A (en) | 1993-05-21 |
| JP3018683B2 true JP3018683B2 (en) | 2000-03-13 |
Family
ID=18098077
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31834091A Expired - Lifetime JP3018683B2 (en) | 1991-11-05 | 1991-11-05 | Method for producing lead-containing ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3018683B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4766827B2 (en) * | 2003-06-26 | 2011-09-07 | 京セラ株式会社 | Method for manufacturing piezoelectric laminate |
| WO2012133529A1 (en) | 2011-03-30 | 2012-10-04 | 日本碍子株式会社 | Method for manufacturing piezoelectric substrate |
-
1991
- 1991-11-05 JP JP31834091A patent/JP3018683B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05124872A (en) | 1993-05-21 |
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