JPH07267729A - Production of grain boundary insulated semiconductor porcelain - Google Patents
Production of grain boundary insulated semiconductor porcelainInfo
- Publication number
- JPH07267729A JPH07267729A JP6080899A JP8089994A JPH07267729A JP H07267729 A JPH07267729 A JP H07267729A JP 6080899 A JP6080899 A JP 6080899A JP 8089994 A JP8089994 A JP 8089994A JP H07267729 A JPH07267729 A JP H07267729A
- Authority
- JP
- Japan
- Prior art keywords
- grain boundary
- germanium
- compacts
- molded body
- semiconductor porcelain
- 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.)
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- Compositions Of Oxide Ceramics (AREA)
- Ceramic Capacitors (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、粒界絶縁型半導体磁器
における結晶粒子の均一性を改善するための製造方法に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a manufacturing method for improving the uniformity of crystal grains in a grain boundary insulating semiconductor ceramic.
【０００２】[0002]
【従来の技術】従来の磁器コンデンサ用の粒界絶縁型半
導体磁器の典型的な製造方法は、チタン酸ストロンチウ
ム等の主成分とＮｂ2 Ｏ5 等の原子価制御剤と結晶粒子
を安定させる効果のあるＧｅの酸化物（ＧｅＯ2 ）とか
ら成る半導体磁器材料の成形体を形成する工程と、成形
体を還元性雰囲気中で焼成して焼結体を得る工程と、焼
結体の表面にＢｉ2 Ｏ3 、Ｐｂ3 Ｏ4 、Ｂ2 Ｏ3 等の粒
界絶縁化物質のペーストを塗布して大気中で熱処理を施
して半導体磁器を得る工程とから成る。2. Description of the Related Art A typical method for manufacturing a grain boundary insulation type semiconductor porcelain for a conventional porcelain capacitor has an effect of stabilizing crystal grains with a main component such as strontium titanate, a valence control agent such as Nb 2 O 5 and the like. On the surface of the sintered body, a step of forming a molded body of a semiconductor porcelain material composed of a Ge oxide (GeO 2 ) having a certain amount of heat, a step of firing the molded body in a reducing atmosphere to obtain a sintered body. A step of applying a paste of a grain boundary insulating material such as Bi 2 O 3 , Pb 3 O 4 , B 2 O 3 and performing heat treatment in the atmosphere to obtain a semiconductor porcelain.
【０００３】[0003]
【発明が解決しようとする課題】ところで、結晶粒子を
制御する作用を有するＧｅＯ2 は、焼成工程において還
元され、成形体から外部に放出される。このため、焼成
工程中にＧｅを成形体中に均一に分布させることが困難
であり、結晶粒子のバラツキが生じ、所望の電気的特性
を得ることができないことがある。また、放出される分
量を見込んでＧｅＯ2 を過剰に添加する必要があり、原
料コストが高くなった。By the way, GeO 2 , which has the function of controlling the crystal grains, is reduced in the firing step and released from the molded body to the outside. For this reason, it is difficult to uniformly distribute Ge in the compact during the firing step, and variations in crystal particles occur, which may make it impossible to obtain desired electrical characteristics. Further, it is necessary to add GeO 2 excessively in consideration of the amount to be released, which increases the raw material cost.
【０００４】そこで、本発明の目的は、Ｇｅの作用の均
一性を保つことができ、且つ製造コストの低減を図るこ
とができる粒界絶縁型半導体磁器の製造方法を提供する
ことにある。Therefore, an object of the present invention is to provide a method of manufacturing a grain boundary insulation type semiconductor ceramic which can maintain the uniformity of the action of Ge and can reduce the manufacturing cost.
【０００５】[0005]
【課題を解決するための手段】上記目的を達成するため
の本発明は、ゲルマニウム又はこの化合物を含む粒界絶
縁型半導体磁器材料の成形体を形成する工程と、前記成
形体をゲルマニウム蒸気の雰囲気中で焼成する工程とを
有する粒界絶縁型半導体磁器の製造方法に係わるもので
ある。なお、請求項２に示すように固体のゲルマニウム
を成形体に接触しないように包囲体に配置し、加熱する
ことによって焼成することが望ましい。The present invention for achieving the above object comprises a step of forming a molded body of a grain boundary insulating semiconductor ceramic material containing germanium or a compound thereof, and an atmosphere of germanium vapor in the molded body. The present invention relates to a method for manufacturing a grain boundary insulating type semiconductor ceramic having a step of firing in the inside. It is desirable that the solid germanium is placed in the enclosure so as not to come into contact with the molded body and heated to be fired.
【０００６】[0006]
【発明の作用及び効果】本発明に従ってゲルマニウム蒸
気の雰囲気で焼成すると、成形体又は焼結体内部からの
ゲルマニウムの放出が抑制され、ゲルマニウムの作用を
均一に得ることが可能になり、結晶粒子の均一性を高
め、電気的特性の改善及び電気的特性のバラツキを低減
できる。請求項２の方法によれば、蒸発したゲルマニウ
ムが焼成後の冷却過程で凝固して球形の塊（固体）にな
るので、容易に回収して再び使用することができる。従
って、原料コストの低減を図ることができる。Calculating according to the present invention in the atmosphere of germanium vapor suppresses the release of germanium from the inside of the molded body or the sintered body, and makes it possible to obtain the function of germanium uniformly, and It is possible to improve uniformity, improve electrical characteristics, and reduce variations in electrical characteristics. According to the method of claim 2, the evaporated germanium solidifies into a spherical mass (solid) in the cooling process after firing, so that it can be easily recovered and reused. Therefore, the raw material cost can be reduced.
【０００７】[0007]
【実施例】次に、本発明の実施例に係わる粒界絶縁型半
導体磁器コンデンサの製造方法を説明する。ＳｒＴｉＯ
3 （チタン酸ストロンチウム）１００．００重量部、Ｎ
ｂ2 Ｏ5 （酸化ニオブ）０．２５重量部及び、ＧｅＯ2
（酸化ゲルマニウム）０．０５重量部の混合物に、水を
加えてボールミルで１５時間攪拌し、これを乾燥して原
料粉末を得た。次に、この原料粉末の１００重量部に対
して、１０〜１５重量部のポリビニルアルコール水溶液
を有機結合材として加えて混練し、造粒したものを約１
トン／cm2 の圧力で成形し、直径１２．５ｍｍ、厚さ
０．３ｍｍの円板状成形体を得た。Next, a method of manufacturing a grain boundary insulating type semiconductor ceramic capacitor according to an embodiment of the present invention will be described. SrTiO
3 (Strontium titanate) 100.00 parts by weight, N
b 2 O 5 (niobium oxide) 0.25 parts by weight and GeO 2
Water was added to a mixture of 0.05 parts by weight of (germanium oxide), the mixture was stirred with a ball mill for 15 hours, and dried to obtain a raw material powder. Next, to 100 parts by weight of this raw material powder, 10 to 15 parts by weight of an aqueous polyvinyl alcohol solution was added as an organic binder, kneaded, and granulated to about 1 part.
It was molded at a pressure of ton / cm 2 to obtain a disk-shaped molded body having a diameter of 12.5 mm and a thickness of 0.3 mm.
【０００８】次に、図１及び図２に示すようにアルミナ
から成る容器即ちサヤ１とアルミナから成る蓋２との組
合わせから成る実質的に気密な包囲体３を用意し、サヤ
１の中にＺｒＯ2 板から成る載置板４を置き、この板４
の上に多数の上述の半導体磁器材料の成形体５を積層状
配置し、更に成形体５に接触しないように固体のゲルマ
ニウム球６を複数個分散配置し、Ｎ2 ＋Ｈ2 から成る還
元性雰囲気中で気密的に蓋２を覆せて炉に入れた。な
お、包囲体３は完全に気密である必要はない。Next, as shown in FIGS. 1 and 2, a substantially airtight enclosure 3 comprising a container made of alumina, that is, a sheath 1 and a lid 2 made of alumina is prepared. Place the mounting plate 4 made of ZrO 2 plate on the
A large number of the above-mentioned semiconductor porcelain compacts 5 are stacked on top of each other, and a plurality of solid germanium spheres 6 are dispersed so as not to contact the compacts 5, and a reducing atmosphere of N 2 + H 2 is provided. The lid 2 was airtightly covered and placed in a furnace. The enclosure 3 does not have to be completely airtight.
【０００９】次に、包囲体３の内及び外をＮ2 （９６容
積％）＋Ｈ2 （４容積％）の還元性雰囲気（非酸化性雰
囲気）中で、包囲体３と共に成形体５及びゲルマニウム
球６を１４００℃、３時間加熱（焼成）して円板状半導
体磁器（焼結体）を得た。この工程において、ゲルマニ
ウム球６からゲルマニウムの蒸発が生じ、包囲体３の中
にゲルマニウム蒸気が均一に分布した雰囲気が得られ
た。成形体５はゲルマニウム蒸気に接しているので、成
形体又は焼結体に含まれているＧｅＯ2 が還元されて気
相のＧｅとなって外部へ放出されることが抑制され、ゲ
ルマニウムの作用を均一に保持した状態で焼成が行わ
れ、均一化された結晶粒子が得られた。Next, the inside and outside of the enclosure 3 are in a reducing atmosphere (non-oxidizing atmosphere) of N 2 (96% by volume) + H 2 (4% by volume) together with the enclosure 3 and the compact 5 and germanium. The sphere 6 was heated (fired) at 1400 ° C. for 3 hours to obtain a disc-shaped semiconductor ceramic (sintered body). In this step, germanium was evaporated from the germanium spheres 6 and an atmosphere in which germanium vapor was uniformly distributed in the enclosure 3 was obtained. Since the compact 5 is in contact with the germanium vapor, GeO 2 contained in the compact or the sintered compact is suppressed from being reduced to Ge in the gas phase and released to the outside, and the action of germanium is suppressed. Firing was performed in a state of being uniformly held, and uniformed crystal particles were obtained.
【００１０】次に、得られた半導体磁器の表面に周知の
粒界絶縁化用の金属酸化物ペースト、具体的には、Ｂｉ
2 Ｏ3 が４０重量部、Ｐｂ3 Ｏ4 が４６重量部、Ｂ2 Ｏ
3 が７重量部の割合の金属酸化物とバインダとしての樹
脂に溶剤を添加してペーストを作り、このペーストを半
導体磁器の表面に塗布し、１１５０℃で２時間の熱拡散
処理を行って結晶粒子を絶縁化した。Next, on the surface of the obtained semiconductor porcelain, a known metal oxide paste for grain boundary insulation, specifically, Bi
40 parts by weight of 2 O 3, 46 parts by weight of Pb 3 O 4 , B 2 O
3 is 7 parts by weight of a metal oxide and a resin as a binder to which a solvent is added to form a paste, and the paste is applied to the surface of the semiconductor porcelain and subjected to thermal diffusion treatment at 1150 ° C. for 2 hours to crystallize. The particles were insulated.
【００１１】次に、図３に示す結晶粒界絶縁化後の半導
体磁器の一対の主面に導電性ペーストとして銀ペースト
を塗布して８００℃で１時間焼付けて一対の電極１１、
１２を形成して同一製造条件の１００個の半導体磁器コ
ンデンサを完成させた。Next, a silver paste as a conductive paste is applied to the pair of main surfaces of the semiconductor porcelain after crystal grain boundary insulation shown in FIG. 3 and baked at 800 ° C. for 1 hour to form a pair of electrodes 11.
12 was formed to complete 100 semiconductor ceramic capacitors under the same manufacturing conditions.
【００１２】次に、完成した１００個のコンデンサの見
掛けの比誘電率ε、誘電損失tan δ、破壊電圧ＢＤＶ、
絶縁抵抗ＩＲを測定してその平均値を求めたところ、ε
は５６０００、tan δは０．３６％、ＢＤＶは３００
Ｖ、ＩＲは１６００ＭΩであった。また、１００個のコ
ンデンサの静電容量を測定し、このバラツキを求めたと
ころ４．７６％であった。なお、ε及びtan δは、温度
２５℃、印加電圧値１Ｖ、周波数１ｋＨｚの条件で測定
し、ＢＤＶはコンデンサ電極１１、１２間に１ｍＡの電
流が流れた時の電圧値であり、ＩＲは２５℃で２５Ｖの
直流電圧を１５秒間印加した後に測定し、静電容量のバ
ラツキは（標準偏差値／平均値）×１００％の式で求め
た。Next, the apparent relative permittivity ε, dielectric loss tan δ, breakdown voltage BDV of 100 completed capacitors,
The insulation resistance IR was measured and the average value was calculated.
Is 56000, tan δ is 0.36%, BDV is 300
V and IR were 1600 MΩ. Further, the capacitance of 100 capacitors was measured, and the variation was found to be 4.76%. Note that ε and tan δ are measured under the conditions of a temperature of 25 ° C., an applied voltage value of 1 V and a frequency of 1 kHz, BDV is a voltage value when a current of 1 mA flows between the capacitor electrodes 11 and 12, and IR is 25 It was measured after applying a direct current voltage of 25 V at 15 ° C. for 15 seconds, and the variation in capacitance was calculated by the formula of (standard deviation value / average value) × 100%.
【００１３】比較のために、ゲルマニウム球６を包囲体
３の中に置く代りに、半導体磁器材料中に加えるＧｅＯ
2 （酸化ゲルマニウム）の量を０．１５重量部に増やし
た他は実施例と全く同一の方法で磁器コンデンサを作
り、同一の方法で特性を測定したところ、εは５４００
０、tan δは０．３６、ＢＤＶは２７０Ｖ、ＩＲは１４
００ＭΩ、静電容量のバラツキは６．８５％であった。For comparison, instead of placing the germanium sphere 6 in the enclosure 3, GeO is added in the semiconductor porcelain material.
A porcelain capacitor was manufactured by the same method as in the example except that the amount of 2 (germanium oxide) was increased to 0.15 parts by weight, and the characteristics were measured by the same method.
0, tan δ is 0.36, BDV is 270V, IR is 14
The variation in capacitance was 00 MΩ and the capacitance was 6.85%.
【００１４】上記の実施例と比較例との対比から明らか
なように本実施例によれば、ε、ＢＤＶ、及びＩＲが高
くなり、静電容量のバラツキが小さくなる。これはゲル
マニウム蒸気中で焼成したための効果である。また、本
実施例では、焼成後の冷却過程で気相のＧｅが球状に凝
固し、これを回収することができた。この回収されたＧ
ｅは再使用可能なものであった。従って、材料費の低減
を図ることができる。As is clear from the comparison between the above embodiment and the comparative example, according to this embodiment, ε, BDV, and IR are increased, and the variation in capacitance is reduced. This is the effect of firing in germanium vapor. In addition, in this example, the vapor phase Ge was spherically solidified in the cooling process after firing and could be recovered. This recovered G
e was reusable. Therefore, the material cost can be reduced.
【００１５】[0015]
【変形例】本発明は上述の実施例に限定されるものでな
く、例えば次の変形が可能なものである。 （１） 主成分はＳｒＴｉＯ3 に限ることなく、ＡＢＯ
3 （但しＡはＳｒ、Ｃａ、Ｂａ、Ｍｇの内の１種又は複
数種の元素、ＢはＴｉ、Ｚｒの１種又は複数種の元素）
で示すことができるチタン酸ストロンチウム系の成分と
することができる。 （２） 半導体化剤（原子化制御剤）としては、Ｎｂ2
Ｏ5 の代りに又はこれに加えて、Ｗ、Ｔａ、Ｙ、希土類
元素（Ｌａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｄｙ、Ｐｍ、Ｅ
ｕ、Ｇｄ、Ｔｂ、Ｈｏ、Ｅｒ、Ｔｍ、Ｙｂ、Ｌｕ等）等
の酸化物（ＷＯ3 、Ｔａ2 Ｏ5 、Ｌａ2 Ｏ3 、Ｃｅ
Ｏ2 、Ｎｄ2 Ｏ3 、Ｙ2 Ｏ3 、Ｓｍ2 Ｏ5 、Ｐｒ
6 Ｏ11、Ｄｙ2 Ｏ3 等）の１種又は複数種を１００重量
部のＳｒＴｉＯ3 又は前述のＡＢＯ3 から成る主成分に
対して好ましくは０．１〜５．０重量部の範囲で使用す
ることができる。 （３） 磁器材料に対するその他の添加物としてＡｌ2
Ｏ3 、ＳｉＯ2 、ＣｕＯ、ＭｎＯ2 、Ａｇ2 Ｏから選択
された１種又は複数種を１００重量部のＳｒＴｉＯ3 又
は前述のＡＢＯ3 から成る主成分に対して好ましくは
０．０５〜０．５０重量部の範囲で添加することができ
る。 （４） 粒界の絶縁化物質として、Ｂｉ2 Ｏ3 、Ｐｂ3
Ｏ4 、Ｂ2 Ｏ3 の代りに、これ等とＭｎＯ2 、ＣｕＯ、
Ｔｌ2 Ｏ3 、Ｓｂ2 Ｏ5 、Ｆｅ2 Ｏ3 等の金属酸化物か
ら選択された１種又は複数種を使用して金属酸化物ペー
ストを作り、これを磁器に塗布することができる。 （５） ＳｒＴｉＯ3 の代りに、これが得られる割合に
出発材料としてＳｒＣＯ3 、ＴｉＯ2 を使用することが
できる。 （６） 成形体を形成する前に大気雰囲気（酸化性雰囲
気）中、１０００〜１２００℃で１〜５時間仮焼し、仮
焼後の原料粉末を使用して成形体を作ることができる。 （７） 磁器原料に含めるＧｅＯ2 の量を、１００重量
部のＳｒＴｉＯ3 又は前述のＡＢＯ3 に対して好ましく
は０．０１〜５．０重量部の範囲で変えることができ
る。 （８） 磁器の製造条件を種々変えることができる。例
えば、還元性雰囲気（非酸化性雰囲気）での焼成を１３
００〜１５００℃、１〜５時間とすることができる。ま
た、前述の金属酸化物ペーストの塗布後の拡散処理を８
００〜１３００℃、１〜５時間とすることができる。MODIFICATION The present invention is not limited to the above-mentioned embodiments, and the following modifications are possible. (1) The main component is not limited to SrTiO 3 , but ABO
3 (However, A is one or more elements of Sr, Ca, Ba and Mg, B is one or more elements of Ti and Zr)
Can be used as the strontium titanate-based component. (2) Nb 2 as a semiconducting agent (atomization control agent)
Instead of or in addition to O 5 , W, Ta, Y, rare earth elements (La, Ce, Pr, Nd, Sm, Dy, Pm, E
u, Gd, Tb, Ho, Er, Tm, Yb, Lu and the like oxides (WO 3 , Ta 2 O 5 , La 2 O 3 , Ce).
O 2 , Nd 2 O 3 , Y 2 O 3 , Sm 2 O 5 , Pr
6 O 11 , Dy 2 O 3, etc.) is used preferably in the range of 0.1 to 5.0 parts by weight with respect to 100 parts by weight of SrTiO 3 or the above main component consisting of ABO 3. can do. (3) Al 2 as other additive to porcelain material
O 3, SiO 2, CuO, preferably with respect to the main component consisting of MnO 2, Ag 2 O is selected from one or more of SrTiO 3 or above of ABO 3 in 100 parts by weight of 0.05 to 0. It can be added in the range of 50 parts by weight. (4) Bi 2 O 3 , Pb 3 as an insulating material at the grain boundary
Instead of O 4 , B 2 O 3 , these and MnO 2 , CuO,
It is possible to prepare a metal oxide paste using one or more kinds selected from metal oxides such as Tl 2 O 3 , Sb 2 O 5 , Fe 2 O 3 and the like, and apply the paste to a porcelain. (5) Instead of SrTiO 3 , SrCO 3 or TiO 2 can be used as a starting material in a proportion to obtain it. (6) Before forming the molded body, the molded body can be calcined in the air atmosphere (oxidizing atmosphere) at 1000 to 1200 ° C. for 1 to 5 hours, and the calcined raw material powder can be used to form the molded body. (7) The amount of GeO 2 contained in the porcelain raw material can be changed within the range of preferably 0.01 to 5.0 parts by weight with respect to 100 parts by weight of SrTiO 3 or the above ABO 3 . (8) The manufacturing conditions of porcelain can be variously changed. For example, firing in a reducing atmosphere (non-oxidizing atmosphere) 13
The temperature can be set to 00 to 1500 ° C. for 1 to 5 hours. In addition, the diffusion process after applying the metal oxide paste described above
The temperature can be set to 00 to 1300 ° C. and 1 to 5 hours.
【図１】本発明の実施例に係わる成形体とゲルマニウム
球を収容した包囲体を示す断面図である。FIG. 1 is a cross-sectional view showing a molded body according to an embodiment of the present invention and an enclosure containing a germanium ball.
【図２】図１の包囲体の中を蓋をとって示す平面図であ
る。FIG. 2 is a plan view showing the inside of the enclosure of FIG. 1 with a lid removed.
【図３】完成した磁器コンデンサを示す正面図である。FIG. 3 is a front view showing a completed porcelain capacitor.
１ サヤ ５ 成形体 ６ ゲルマニウム球 1 Saya 5 Molded body 6 Germanium ball
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｇ 4/12 ３２５ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI technical display location H01G 4/12 325
Claims (2)
絶縁型半導体磁器材料の成形体を形成する工程と、 前記成形体をゲルマニウム蒸気の雰囲気中で焼成する工
程とを有する粒界絶縁型半導体磁器の製造方法。1. A grain boundary insulating semiconductor porcelain having a step of forming a molded body of a grain boundary insulating semiconductor ceramic material containing germanium or a compound thereof, and a step of firing the molded body in an atmosphere of germanium vapor. Production method.
囲体の中に前記成形体を配置すると共に、前記成形体に
接触しないように固体のゲルマニウム（Ｇｅ）を配置
し、前記成形体と前記ゲルマニウムとを前記包囲体と共
に加熱する工程である請求項１記載の粒界絶縁型半導体
磁器の製造方法。2. In the firing step, the molded body is arranged in a substantially sealed enclosure, and solid germanium (Ge) is arranged so as not to come into contact with the molded body. The method of manufacturing a grain boundary insulating semiconductor ceramic according to claim 1, which is a step of heating the germanium and the germanium together with the envelope.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6080899A JPH07267729A (en) | 1994-03-28 | 1994-03-28 | Production of grain boundary insulated semiconductor porcelain |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6080899A JPH07267729A (en) | 1994-03-28 | 1994-03-28 | Production of grain boundary insulated semiconductor porcelain |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07267729A true JPH07267729A (en) | 1995-10-17 |
Family
ID=13731220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6080899A Withdrawn JPH07267729A (en) | 1994-03-28 | 1994-03-28 | Production of grain boundary insulated semiconductor porcelain |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07267729A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515782A (en) * | 2011-12-22 | 2012-06-27 | 许昌学院 | Method for sintering Chinese Jun porcelain at oxidizing atmosphere with addition of nano-material |
-
1994
- 1994-03-28 JP JP6080899A patent/JPH07267729A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515782A (en) * | 2011-12-22 | 2012-06-27 | 许昌学院 | Method for sintering Chinese Jun porcelain at oxidizing atmosphere with addition of nano-material |
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| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
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