JPS58183936A - Granulation of ceramic powder - Google Patents

Granulation of ceramic powder

Info

Publication number
JPS58183936A
JPS58183936A JP57065184A JP6518482A JPS58183936A JP S58183936 A JPS58183936 A JP S58183936A JP 57065184 A JP57065184 A JP 57065184A JP 6518482 A JP6518482 A JP 6518482A JP S58183936 A JPS58183936 A JP S58183936A
Authority
JP
Japan
Prior art keywords
polyvinyl alcohol
granules
particle
spray drying
emulsion
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.)
Granted
Application number
JP57065184A
Other languages
Japanese (ja)
Other versions
JPS6327051B2 (en
Inventor
Migiwa Ando
安藤 汀
Yukiaki Ito
伊藤 幸昭
Akira Sawaki
沢木 昭
Masayuki Yano
正行 矢野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Tokushu Togyo KK
Niterra Co Ltd
Original Assignee
NGK Spark Plug Co Ltd
Nippon Tokushu Togyo KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by NGK Spark Plug Co Ltd, Nippon Tokushu Togyo KK filed Critical NGK Spark Plug Co Ltd
Priority to JP57065184A priority Critical patent/JPS58183936A/en
Publication of JPS58183936A publication Critical patent/JPS58183936A/en
Publication of JPS6327051B2 publication Critical patent/JPS6327051B2/ja
Granted legal-status Critical Current

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Landscapes

  • Glanulating (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

PURPOSE:To obtain a granule easily collapsible during press molding and excellent in mold releasability, by a method wherein a mixture of a high molecular emulsion and polyvinyl alcohol are compounded in the fine particle of a ceramics stock material as a particle binder and the obtained sludge is subjected to spray drying. CONSTITUTION:A mixture consisting of, on the basis of a solid component, 1-4% high molecular emulsion (e.g., polyacrylic ester) and 0.1-0.8% polyvinyl alcohol is compounded in the fine particle of a ceramics stock material as a particle binder and the obtained sludge is subjected to spray drying. Because thus obtained granule is easily collapsible during press molding and mold releasability thereof is excellent, a molded product is reduced in surface defficiency and one with high density is obtained.

Description

【発明の詳細な説明】 本発明は、装置によるプレス成形に際して金型に対する
充填密度が高く、離型性に優れ九セラ建ツクス粉体の造
粒方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for granulating a nine-cell powder that has a high packing density in a mold and has excellent mold releasability during press molding using an apparatus.

金型のプレス成形に使用されるセラ2ツタスの原料粉末
の顆粒(以下顆粒と略称する)Kは充填密度を高めて緻
密な焼結体を得る丸めの高い真円度と、同じく焼結晶の
表面を平滑にする丸めの優れた離聾性が要求され、特に
厚膜印刷を用いた集積回路基板として戴く使用されてい
るアル建す基板において強く要求されている。
The raw material powder granules (hereinafter referred to as granules) K used for press forming of molds have a high roundness that increases the packing density to obtain a dense sintered body, and also have a high roundness of sintered crystals. Excellent deafening properties with smooth rounding of the surface are required, and this is especially strongly required for aluminum substrates used as integrated circuit boards using thick film printing.

上記アル建す基板はアル建す含有量デJ−Pり慢の高純
度アル建すll器が使用されているが、集積密度を^め
るえめ、基板上に集積回路配線の幅および配−間隙の微
細化が要求され、これに付随して該基板表面の平滑性お
よびビット等の欠陥に対する許容値が逐次厳しくなって
来ている。
The above-mentioned aluminum substrate is made of high-purity aluminum with a high aluminum content. - There is a demand for finer gaps, and along with this, tolerances for smoothness of the substrate surface and defects such as bits are gradually becoming stricter.

上記基板の表面に発生する欠陥は、原料の微粒子を一旦
泥漿化して噴霧乾燥によって製造され九顆粒が、硬くて
潰れ難い場合においてプレス成形品の顆粒外に生ずる凹
部によるか、プレス成形時において金INK付着して成
形体から引剥がされる顆粒あるいは該顆粒の破砕片によ
るため、上記原料微粒子を噴務乾燥によって顆粒化する
有機質の結合剤には造粒され九顆粒を潰れ易くし、しか
も高い離型性を具えるという相反する特性が要求され、
両特性を同時に満足させる結合剤は得られなかつえ。
Defects that occur on the surface of the substrate described above may be due to recesses that occur outside the granules of the press-formed product when the fine particles of the raw material are once made into a slurry and are manufactured by spray drying, and the granules are hard and difficult to crush. Because of the granules attached to the INK and peeled off from the compact, or the crushed pieces of the granules, the organic binder used to granulate the raw material fine particles by jet drying is granulated, making the granules easy to crush, and having a high separation. The contradictory characteristics of having moldability are required,
It has not been possible to obtain a binder that satisfies both properties at the same time.

本発明は上記の相反する問題点を同時に解決し、プレス
成形に際して潰れ轟く、しかも離型性に優れ九顆粒を噴
霧乾燥によって造粒することに成功したもので、セy(
ツタの原料微粒子に、高分子の乳化液をポリビニルアル
コールの混合物を粒子結合剤として泥漿中に配合するこ
とを4I徴とじ九ものである。
The present invention simultaneously solves the above-mentioned contradictory problems and has succeeded in granulating nine granules by spray drying that do not collapse and roar during press molding and have excellent mold release properties.
The 4I method involves blending a polymeric emulsion into a slurry using a mixture of polyvinyl alcohol as a particle binder and fine particles of ivy as a raw material.

本発明において上記の粒子結合剤として為分子の乳化液
とポリビニルアルコールを併用する理由は、先ず1I1
1t1i性が粒子結合剤の金部金属面およびアル建す磁
器面に対する親′和性によって大きな影替を受けると考
えて先ず、従来粒子結合剤として知られる各種のポリ!
−の上記金蓋金属面(鋼材)とセツイツタ基1[K対す
る舖れ性について一定しえ処、図に示されるようにポリ
アクリル酸エステル(1) 、ポリ酢酸ビニル(C)、
ポリメタクリル酸エステル(D) 、ポリアクリルv(
E)等の高分子乳化液はいずれもアル賓すffi器と濡
れ難い反面、金属とは槁れ易く、一方ヂリビニルアルコ
ール(ム)は逆の特性を呈することが4’1lljll
た。このように金属と濡れ易い高分子の乳化液を用いて
造粒し九顆粒が一蓋性に劣る反面、軟質で潰れ易く、一
方ポリビニルアルコールによって造粒し九顆粒は硬くて
潰れ細い欠点を有する反面、離型性に優れているだけで
はなく、造粒に際して外部へ滲出して薄膜を形成する独
得の高い造膜性を具えていることをも発見し九ことに基
づくものである。
In the present invention, the reason for using the Tamemolecular emulsion and polyvinyl alcohol together as the particle binder is as follows.
Considering that the 1t1i property is greatly affected by the particle binder's affinity for the metal surface of the metal part and the porcelain surface of the aluminum plate, we first applied various types of polyols known as conventional particle binders.
- The metal surface of the metal lid (steel material) and the setter group 1 [K] have a certain degree of fragility, as shown in the figure, polyacrylic acid ester (1), polyvinyl acetate (C),
Polymethacrylic acid ester (D), polyacrylic v (
While polymer emulsions such as E) are difficult to wet with alcoholic FFI devices, they are easy to rub against metals, while divinyl alcohol (M) exhibits the opposite characteristics.
Ta. In this way, the nine granules granulated using an emulsion of a polymer that is easily wetted with metal have the disadvantage that they are soft and easily crushed, while the nine granules granulated using polyvinyl alcohol are hard, crushable, and thin. On the other hand, this is based on the discovery that it not only has excellent mold releasability, but also has a unique high film-forming property that oozes out to the outside and forms a thin film during granulation.

実施例 アルオナ(18和軽金属AI−/j)     j−無
水珪II(林純薬試薬1級)       JOf次酸
カルシウム(米用薬品試薬1級)7/f縦酸マグネシウ
ム(片山化学試薬7級)   参コfを原料粉末とし、
これにボリビエルアルスール(日本合成(J−77) 
Jjf 、高分子の乳化液としてポリアクリル酸エステ
ルの10%を含む乳化剤(以下同様)(日本純系ジエリ
マー8E−j10コ)lOJfからなる粒子結合剤と、
水コtを加えて内容積4tのボール建ルによって73時
間の混合、粉砕を行なって泥漿となし、これをガス温g
170℃、ディスク径/10−φ、4100′RPIL
%毎秒J輔の条件によって噴霧乾燥を行なって得九本発
明による顆粒と、上記粒子結合剤としてポリビニルアル
コールを除きポリアクリル酸エステルのみとしてこれを
l0Jtとした他は同条件として造粒し九顆粒(比較品
l)およびポリアクリル酸エステルを使用せずポリビニ
ルアルコールのみを779として同条件で造粒しえ顆粒
(比較品コ)を、/l0OK4/dCJ金型プレスによ
ってコタ×コタX2mtの基板に成形し、これら3櫨の
成形品を電気炉中/jJO℃、1時間の焼成を行なって
得た焼結晶について##特性を一定した結果をls1表
に示す。
Examples Alona (18 Wa Light Metal AI-/j) j-Anhydrous silicon II (Hayashi Pure Chemical Reagent Grade 1) JOf Calcium Suboxide (Rice Pharmaceutical Reagent Grade 1) 7/f Magnesium Vertical Acid (Katayama Chemical Reagent Grade 7) Sanko f is used as a raw material powder,
In this, Bolivier Arsul (Nippon Gosei (J-77)
Jjf, an emulsifier containing 10% of polyacrylic acid ester as a polymer emulsion (the same applies hereinafter) (Japanese pure dielimer 8E-j10); a particle binder consisting of lOJf;
Add t of water, mix and crush for 73 hours in a bowl with an internal volume of 4 t to form a slurry, which is then mixed at a gas temperature of g.
170℃, disk diameter/10-φ, 4100'RPIL
The granules according to the present invention were obtained by spray drying under the conditions of 10% per second, and the 9 granules were granulated under the same conditions except that polyacrylic acid ester was used as the particle binder except for polyvinyl alcohol, and 10Jt was used as the particle binder. (Comparative product 1) and granules granulated under the same conditions using only polyvinyl alcohol (779) without using polyacrylic acid ester (Comparative product 2) were molded onto a Kota x Kota x 2m substrate using a /l0OK4/dCJ mold press. Table ls1 shows the results of the baked crystals obtained by molding and firing these three molded products in an electric furnace at JJO° C. for 1 hour with constant ## characteristics.

/ / 上表によって、粒子結合剤としてポリビニルアルコール
とポリアクリル酸エステルの両者を併用し九本発明品は
表面欠陥が少なく、高密度のアルミナ基板が得られ九I
DK対し、ポリアクリル酸エステルのみの比較品(1)
は離蓋性が悪く金型の連続使用回数は本発明品O17i
o Kも達せず、またポリビニルアルコールのみを用い
九比較品−)は離型性に優れているが表面欠陥が着しく
多く、vli度も低かつえ。
/ / According to the above table, by using both polyvinyl alcohol and polyacrylic acid ester as particle binders, the product of the present invention has fewer surface defects and a high-density alumina substrate can be obtained.
Comparison product (1) with only polyacrylic acid ester compared to DK
The product O17i of the present invention has poor release properties and the number of continuous use of the mold is poor.
o K was not reached, and the comparative product using only polyvinyl alcohol had excellent mold releasability, but had many surface defects and low VLI.

本発明において上記の効果を奏する理由は、泥漿中にポ
リアクリル酸エステルと共に配合されたポリビニルアル
コールが、噴霧乾燥によって造粒されるとき前に述べ九
特有の高い造膜性によって顆粒の外部に滲出し、セラミ
ックスの原料微粒子と上記乳化剤とから亀る屑を薄く被
横し、金属と親和性が低く1III性に富んだ薄膜から
なる外層とを構成し、これがプレス加工において要求さ
れる潰れ易さと離製性の両者を同時に満足させるためで
ある。
The reason why the above effects are achieved in the present invention is that when the polyvinyl alcohol blended with the polyacrylic acid ester in the slurry is granulated by spray drying, it oozes out to the outside of the granules due to the high film-forming properties unique to the above-mentioned nine. The outer layer is thinly coated with debris from the ceramic raw material fine particles and the emulsifier, and has a low affinity for metals and is rich in IIII properties. This is to satisfy both requirements of releasability at the same time.

上記成臘品の切断面および表面に、冒つ嵩ot% 1x
fpw7 ル:1− ル1貧’1%、ホウ9191%、
水Jり7−からなるポリビニルアルコール染色液に塗布
し、倍率1gll0拡大鏡によって調べた処、成形体の
表面はPvム薄膜が紫色Kitり顆粒は粒界のくぼみを
生じないように潰れて平滑となり、内IIO大部分の顆
粒社周調四方から受ける圧力によって瞬接する顆粒と相
接し、周l1IiIK連続する多画体七址していた。
Add bulk ot% 1x to the cut surface and surface of the above finished product.
fpw7 le:1-le1po'1%, hou9191%,
When applied to a polyvinyl alcohol staining solution consisting of water and examined with a magnifying glass of 1gll0, the surface of the molded product was found to have a purple Pvum thin film. As a result, most of the granules in the inner IIO came into contact with the granules that came into instant contact with each other due to the pressure received from all four directions, forming a continuous multi-layer structure.

また、ポリビニルアルコールに配合する乳化液としては
上記ポリアクリル酸エステルの他ポリ酢醗ビニル樹脂、
あるいはポリアクリルwk樹脂その他があり、いずれも
ポリアクリル酸エステルと同様の効果を奏することが確
かめられた。
In addition to the above-mentioned polyacrylic acid ester, the emulsifying liquid to be mixed with polyvinyl alcohol includes polyacetic acid vinyl resin,
Alternatively, there are polyacrylic wk resins and others, and it has been confirmed that all of them have the same effects as polyacrylic esters.

しかして、上記ポリビニルアルコールおよび乳化箪Oセ
ラミツタス原料に対する混合割合は重量比でポリビニル
アルコールat−alqk、乳化液の固形分l−夢一の
範囲内で、前者ポリビニルアルコールが上限のat−を
超えた場合は造粒された顆粒が硬すぎてプレス成形時に
おいて金型と当接する表面OII粒が潰れ離く、表面欠
陥を生じ、逆に下限に満たないときは顆粒内110セラ
ミックスの微粒子を包んだ乳化液が金型に付着して成形
体から引き剥がされ表面欠陥を生じ、一方乳化液を固形
分ペースで7−参−としたのは/−以下では顆粒がプレ
ス時潰れ難く表面欠陥を生じ、事−を超える時は焼成切
れが多くなるため、上記の範囲内に限定する必要がある
Therefore, the mixing ratio of the above-mentioned polyvinyl alcohol and the emulsion tank O ceramitus raw material was within the range of polyvinyl alcohol at-alqk and emulsion solid content l-Yumeichi in terms of weight ratio, and the former polyvinyl alcohol exceeded the upper limit at- In this case, the granules are too hard and the surface OII grains in contact with the mold are crushed and separated during press molding, resulting in surface defects.On the other hand, when the lower limit is not reached, the 110 ceramic fine particles inside the granules are wrapped. The emulsion adheres to the mold and is peeled off from the molded body, causing surface defects.On the other hand, when the solid content of the emulsion is set to 7-3, the granules are difficult to crush during pressing and cause surface defects. If the temperature exceeds , the number of firing defects will increase, so it is necessary to limit the temperature to within the above range.

【図面の簡単な説明】[Brief explanation of the drawing]

図面は本発明に使用するポリビニルアルコールと各種乳
化液および各種ポリマーO,アル電す基板および金証金
属に対する接触角を示す点グラフである。 1 1− ″」 金型名刀1(引n卑ヤ)乙のギ勝気9色手続補正書(自
発) 昭和17年7327日 l事件の表示 昭和!7牛特許m  第4!II参号 −1発明の名称 セラ々ツタス粉体O造粒方法 3補正をする者 事件と0WsS  %許出願人 (pre)日本籍殊陶業株式金社 代R:I小用修次 偶代 履 人 よ補正の対象 明細書中、発1jIO詳細な説明の−。 「コ4fJを「コJfJに訂正します。 以上
The drawing is a point graph showing the contact angles of polyvinyl alcohol used in the present invention, various emulsions, various polymers O, aluminum substrates, and gold proof metals. 1 1- ″” Mold name sword 1 (Hinbaiya) Otsu no Gi Katsuki 9 color procedural amendment (voluntary) 1945 7327 l Incident Showa! 7 cow patent m 4th! II Part No.-1 Name of the Invention Ceratus Tutus Powder O Granulation Method 3 Person Who Makes Amendment Case and 0WsS % Applicant (pre) Nippon Shishu Togyo Co., Ltd. In the specification subject to amendment, please refer to the detailed explanation of 1jIO. I am correcting ``ko4fJ'' to ``koJfJ.''

Claims (1)

【特許請求の範囲】[Claims] セラ建ツクス原料の微粒子に、高分子の乳化液を固形分
ペースでl−≠−と、ポリビニルアルコールa/ −6
7−の混合物を粒子結合剤として配合してなる泥漿を噴
霧乾燥することを特徴としたセラミックス粉体O造粒方
法。
Add a polymer emulsion to the fine particles of the ceramic material at a solid content pace of 1-≠- and polyvinyl alcohol a/-6.
7- A ceramic powder O granulation method characterized by spray-drying a slurry formed by blending the mixture of 7- as a particle binder.
JP57065184A 1982-04-19 1982-04-19 Granulation of ceramic powder Granted JPS58183936A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57065184A JPS58183936A (en) 1982-04-19 1982-04-19 Granulation of ceramic powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57065184A JPS58183936A (en) 1982-04-19 1982-04-19 Granulation of ceramic powder

Publications (2)

Publication Number Publication Date
JPS58183936A true JPS58183936A (en) 1983-10-27
JPS6327051B2 JPS6327051B2 (en) 1988-06-01

Family

ID=13279572

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57065184A Granted JPS58183936A (en) 1982-04-19 1982-04-19 Granulation of ceramic powder

Country Status (1)

Country Link
JP (1) JPS58183936A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4875354A (en) * 1986-01-17 1989-10-24 Trond Nilsen Machine for adjustable longitudinal corrugating of sheet materials
WO1994024203A1 (en) * 1993-04-19 1994-10-27 Kabushiki Kaisha Meiji Gomu Kasei Method of manufacturing fine piezoelectric ceramic balls for piezoelectric elastomer
CN111205096A (en) * 2020-03-05 2020-05-29 山东国瓷功能材料股份有限公司 Spray granulation method and preparation method of microwave medium powder

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5023408A (en) * 1973-07-04 1975-03-13

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5023408A (en) * 1973-07-04 1975-03-13

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4875354A (en) * 1986-01-17 1989-10-24 Trond Nilsen Machine for adjustable longitudinal corrugating of sheet materials
WO1994024203A1 (en) * 1993-04-19 1994-10-27 Kabushiki Kaisha Meiji Gomu Kasei Method of manufacturing fine piezoelectric ceramic balls for piezoelectric elastomer
CN111205096A (en) * 2020-03-05 2020-05-29 山东国瓷功能材料股份有限公司 Spray granulation method and preparation method of microwave medium powder

Also Published As

Publication number Publication date
JPS6327051B2 (en) 1988-06-01

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