JPH02153866A - Production of uniform sintered compact - Google Patents
Production of uniform sintered compactInfo
- Publication number
- JPH02153866A JPH02153866A JP63306738A JP30673888A JPH02153866A JP H02153866 A JPH02153866 A JP H02153866A JP 63306738 A JP63306738 A JP 63306738A JP 30673888 A JP30673888 A JP 30673888A JP H02153866 A JPH02153866 A JP H02153866A
- Authority
- JP
- Japan
- Prior art keywords
- molded article
- sintered body
- molding
- sintered compact
- present
- 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
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 230000002706 hydrostatic effect Effects 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims description 13
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 239000011148 porous material Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052580 B4C Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野コ
本発明は均質焼結体の製造方法に係り、更に詳しくは、
構造部材、軸受部材、耐摩耗部材あるいは摺動部材など
に有用な高緻密で均質なセラミックス焼結体の製造方法
に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for manufacturing a homogeneous sintered body, and more specifically,
The present invention relates to a method for manufacturing highly dense and homogeneous ceramic sintered bodies useful for structural members, bearing members, wear-resistant members, sliding members, etc.
［従来の技術］
従来より、セラミックス原料と焼結助剤を混合し、次い
でこれに結合剤、可塑剤、分散剤、消泡剤、滑剤等の有
機質成形助剤を添加した後、第３図に示す工程に従い、
プレス成形、スリップキャスト成形、押出し成形あるい
は射出成形等の各種の成形法によりセラミックス成形体
が成形されている。[Prior Art] Conventionally, ceramic raw materials and sintering aids are mixed, and then organic forming aids such as binders, plasticizers, dispersants, antifoaming agents, and lubricants are added thereto. Follow the steps shown in
Ceramic molded bodies are molded by various molding methods such as press molding, slip cast molding, extrusion molding, or injection molding.
次いで上記例れかの成形法によって得られた成形体は、
乾燥後５００°Ｃ程度の温度に加熱して成形助剤が除去
された後焼成することにより焼結体が製造されている。Next, the molded article obtained by any of the above molding methods is
After drying, the sintered body is produced by heating to a temperature of about 500°C to remove the forming aid, and then firing.
［発明が解決しようとする課題］
しかしながら、上記した第３図の従来の焼結体の製造方
法にあっては、成形体の成形助剤を除去後そのまま焼成
しているため、成形助剤除去後の成形体（仮焼体）中に
は成形助剤除去に伴なって形成された気孔が残存するこ
とになる０通常セラミックス成形体には成形法にもよる
が、約１〜２０重量％程度の成形助剤か含まれており、
１ノかも成形助剤は成形体中に均一に分散しているわけ
ではなく偏って存在していることか多く、また、ｍｓ、
塵等の有機質の異物が成形体中に混入し、成形助剤除去
後の成形体には粗大な気孔か残ることになる。従って、
これを焼成すると、得られる焼結体にはそのまま粗大気
孔か残り、強度にバラツキのある焼結体が製造されるこ
とになるという問題かある。[Problems to be Solved by the Invention] However, in the conventional method for manufacturing the sintered body shown in FIG. The pores formed due to the removal of the forming aid will remain in the subsequent molded body (calcined body). Usually ceramic molded bodies contain about 1 to 20% by weight, depending on the molding method. Contains a certain amount of molding aid,
The molding aid is not uniformly dispersed in the molded product, but is often present unevenly, and ms,
Organic foreign matter such as dust gets mixed into the molded product, and coarse pores remain in the molded product after the molding aid is removed. Therefore,
When this is fired, coarse pores remain in the resulting sintered body, resulting in a sintered body with varying strength.
［課題を解決するための手段］
そこで、本発明者は焼結体に粗大な気孔が残存せず、均
質な焼結体を得るべく種々検討を行なった結果、本発明
を完成したものである。[Means for Solving the Problems] Therefore, the present inventor conducted various studies in order to obtain a homogeneous sintered body in which no coarse pores remain in the sintered body, and as a result, the present invention was completed. .
即ち、本発明は、第１図に示すように、セラミックス成
形体の有機質成形助剤を加熱除去後焼成することにより
焼結体を製造する方法において、前記助剤を加熱除去し
た成形体に流動性を付与した後静水圧加圧を施し、好ま
しくは乾燥し、次いで焼成することを特徴とする均質焼
結体の製造方法を提供するものである。That is, as shown in FIG. 1, the present invention provides a method for producing a sintered body by heating and removing an organic forming aid from a ceramic molded body and then firing the molded body, in which the molded body from which the aid has been removed by heating is flowed. The present invention provides a method for producing a homogeneous sintered body, which comprises imparting properties to the homogeneous sintered body, applying isostatic pressure, preferably drying, and then firing.
［作用コ
本発明において特に重要なポイントは、成形助剤を加熱
除去した成形体に流動性を付与した後に静水圧加圧処理
を施すことである。′成形助剤を加熱除去した成形体に
流動性を付与することにより、該成形体中の粒子同士の
滑りか円滑になり、これに静水圧加圧処理を施すことに
より成形体中に不均一に存在する気孔が潰され、その結
果、焼成して得られる焼結体は強度のバラツキが小さく
、緻密で均質なものとなる。[Operations] A particularly important point in the present invention is to impart fluidity to the molded product from which the molding aid has been removed by heating, and then to perform the hydrostatic pressure treatment. 'By imparting fluidity to the molded body from which the molding aid has been removed by heating, the particles in the molded body can smoothly slide against each other, and by applying hydrostatic pressure treatment to this, unevenness in the molded body can be eliminated. As a result, the sintered body obtained by firing has small variations in strength, and is dense and homogeneous.
ここで流動性を付与するものとしては水、アルコール等
を用い、それらを蒸気化するか或いはスプレーにて行な
うことか好ましい。流動性の付与は、例えば水分を添加
する場合には４重量％以下か好ましく、１〜４重量％が
更に好ましい。水分添加量か４重量％を超えると、乾燥
時にクラックが発生し易く、また乾燥時間が長くなると
いう問題がある。Here, it is preferable to use water, alcohol, etc. to impart fluidity, and to vaporize them or spray them. For example, when water is added, the fluidity is preferably 4% by weight or less, more preferably 1 to 4% by weight. If the amount of water added exceeds 4% by weight, there is a problem that cracks are likely to occur during drying and the drying time becomes longer.
又、上記の流動性を付与する手段としては所定の湿度下
（調湿下）に該成形体を置き、水蒸気を成形体の気孔内
に浸入させることにより行なうことが好ましい、具体的
には、恒温・恒湿器を用い、温度２５〜４０℃、湿度８
０〜９８％下でｌＯ〜２０時間成形体を処理することに
より行なうことが好ましい。In addition, as a means for imparting the above-mentioned fluidity, it is preferable to place the molded product under a predetermined humidity (humidity control) and allow water vapor to penetrate into the pores of the molded product. Specifically, Using a constant temperature/humidifier, temperature 25-40℃, humidity 8
It is preferable to carry out this by treating the molded body at 0 to 98% for 10 to 20 hours.
成形体に流動性を付与した後に行なう静水圧加圧処理工
程は、流動性付与後の成形体をゴム等の可撓性の容器（
ゴム型）に封入し、これに液体を経て均一な圧力を付与
するものてあり、成形体の全般に均一な圧力をかけるこ
とができる。この静水圧加圧処理工程において付与する
圧力は、１．０００〜１００，０００ ｋｇ／ｃｍ”が
好ましく、２，０００〜７．０００ ｋｇ／ｃ朧２が更
で好ましい。In the isostatic pressure treatment step, which is performed after imparting fluidity to the molded body, the molded body after imparting fluidity is placed in a flexible container such as rubber (
This method applies uniform pressure to the entire molded product through liquid. The pressure applied in this hydrostatic pressure treatment step is preferably 1.000 to 100,000 kg/cm'', more preferably 2,000 to 7.000 kg/cm2.
圧力が１，０００ ｋｇ／ｃｍ”より小さいと、成形体
中の気孔か漬れにくくなって、均質で緻密な焼結体か得
られ難くなり、一方、１００，０口Ｏｋｇ／ｃｍ”を超
えると、成形歪みが大きくなり、乾燥時にクラックを生
じ易くなり好ましくない。If the pressure is less than 1,000 kg/cm", the pores in the compact will be difficult to soak, making it difficult to obtain a homogeneous and dense sintered body; on the other hand, if the pressure exceeds 100,0 kg/cm" This is not preferable because molding distortion becomes large and cracks are likely to occur during drying.
次に、静水圧加圧処理を施された成形体は、次いで好ま
しくは乾燥された後、焼成される。Next, the molded body subjected to the hydrostatic pressure treatment is preferably dried and then fired.
焼成条件はセラミックスの種類、使用目的などに応じて
適宜決定される。例えば、窒化珪素焼結体を製造する場
合、常圧焼成では１６００〜１８００℃、加圧焼成では
１７００〜２０００℃で窒素ガス雰囲気中での焼成が好
ましい。尚、より高緻密な焼結体を得るため、熱間静水
圧プレス（ＨＩＰ）を行なってもよい。また炭化珪素焼
結体を製造する場合は１９００〜２２００℃でアルゴン
雰囲気中での焼成が好ましい。さらに部分安定化ジルコ
ニア焼結体を製造する場合は１３００〜１５００℃で空
気雰囲気中での焼成か好ましい
本発明に用いるセラミックス原料としては従来公知のセ
ラミックス材料を用いることかでき、例えば窒化珪素、
炭化珪素、ジルコニア、サイアロン、アルミナ、スピネ
ル、ムライト、炭化硼素等が使用できる。Firing conditions are appropriately determined depending on the type of ceramic, purpose of use, etc. For example, when manufacturing a silicon nitride sintered body, firing in a nitrogen gas atmosphere is preferred at 1600 to 1800°C for normal pressure firing, and at 1700 to 2000°C for pressure firing. Incidentally, in order to obtain a more dense sintered body, hot isostatic pressing (HIP) may be performed. Further, when producing a silicon carbide sintered body, firing is preferably performed at 1900 to 2200°C in an argon atmosphere. Further, in the case of manufacturing a partially stabilized zirconia sintered body, it is preferable to sinter it at 1300 to 1500°C in an air atmosphere.As the ceramic raw material used in the present invention, conventionally known ceramic materials can be used, such as silicon nitride,
Silicon carbide, zirconia, sialon, alumina, spinel, mullite, boron carbide, etc. can be used.
なお、本発明におけるセラミックス成形体の製造方法と
しては何ら限定されるものではなく、従来例で述べた如
く、例えばプレス成形、スリラフキャスト成形、押出し
成形あるいは射出成形等各種の成形法を適用することが
できる。Note that the method for producing the ceramic molded body in the present invention is not limited in any way, and various molding methods such as press molding, slip rough cast molding, extrusion molding, or injection molding may be applied, as described in the conventional examples. be able to.
［実施例］
以下、′本発明を実施例に基き更に詳細に説明するが、
本発明はこれらの実施例に限られるものではない。[Examples] Hereinafter, the present invention will be explained in more detail based on Examples.
The present invention is not limited to these examples.
（実施例１）
平均粒径０．５μｍのα型窒化珪素粉末１００重量部に
焼結助剤としてＭ ｇ Ｏ，Ｚ ｒ ０２ 、 Ｙ２Ｏ
３の各粉末を夫々４重量部、２重量部、７重量部の割合
で混合し、それに水分６０重量部を加え、バッチ式粉砕
機により混合粉砕した後、目開き２０ｐｍの篩通しをし
て平均粒子径０．７ｇｍのスラリーを得た。このスラリ
ーにバインダーとしてポリビニルアルコール（ＰＶＡ）
２重量部を添加し、噴霧乾燥機を用いて造粒粉体とした
。(Example 1) MgO, Zr02, Y2O were added as sintering aids to 100 parts by weight of α-type silicon nitride powder with an average particle size of 0.5 μm.
The powders of 3 were mixed at a ratio of 4 parts by weight, 2 parts by weight, and 7 parts by weight, respectively, 60 parts by weight of water was added thereto, and the mixture was mixed and ground using a batch-type grinder, and then passed through a sieve with an opening of 20 pm. A slurry with an average particle size of 0.7 gm was obtained. Polyvinyl alcohol (PVA) was added to this slurry as a binder.
2 parts by weight were added to form a granulated powder using a spray dryer.
この造粒粉体を金型に入れ、圧力２００ ｋｇ／ｃｍ２
で一軸圧縮し、φ１８０Ｘ３０ｔｍｍの成形体を作製し
た。This granulated powder was put into a mold and the pressure was 200 kg/cm2.
This was uniaxially compressed to produce a molded body with a diameter of 180 x 30 tmm.
次に、第１図のフローチャートに示すように、得られた
成形体を１００℃で２時間乾燥した後、５００°Ｃに加
熱し、成形助剤を除去した。これを温度４０°Ｃ１湿度
９８％の恒温・恒湿器の中に１６時間入れて水分２重量
％を添加した０次いでこの成形体をラバープレス成形法
により、圧力３ 、０００ ｋｇ／ｃｍ２で１分間静水
圧加圧した後、温度１００℃で５時間乾燥した。Next, as shown in the flowchart of FIG. 1, the obtained molded body was dried at 100°C for 2 hours, and then heated to 500°C to remove the molding aid. This was placed in a constant temperature/humidity chamber at a temperature of 40°C and a humidity of 98% for 16 hours, and 2% water by weight was added.Then, this molded body was molded using a rubber press at a pressure of 3,000 kg/cm2. After applying hydrostatic pressure for a minute, it was dried at a temperature of 100° C. for 5 hours.
次に、これを１気圧の窒素雰囲気下、温度１７００°Ｃ
′ｃ１時間焼成することにより焼結体（本発明の焼結体
）を得た。Next, this was heated to 1,700°C under a nitrogen atmosphere of 1 atm.
A sintered body (sintered body of the present invention) was obtained by firing for 1 hour.
なお、比較のため、第３図に示す従来法によりφ１８０
Ｘ３０ｔｍｍ成形品の焼結体を得た。For comparison, the conventional method shown in Figure 3
A sintered body having a size of 30 tmm was obtained.
上記で得られた本発明の焼結体と従来法の焼結体のそれ
ぞれについて超音波探傷□検査を行なったところ、従来
法の焼結体についてはｌ ００ ＪＬｍ程度の欠陥か３
個検出されたのに対して、本発明の焼結体には欠陥か検
出されなかった。When the sintered body of the present invention obtained above and the sintered body of the conventional method were subjected to ultrasonic flaw detection □ inspection, it was found that the sintered body of the conventional method had defects of about 100 JLm or 3
However, no defects were detected in the sintered body of the present invention.
また、焼結体の強度のバラツキを調べるため、夫々のワ
イブル係数を測定したところ、第２図のような結果を得
た。In addition, in order to examine variations in the strength of the sintered bodies, the Weibull coefficients of each were measured, and the results shown in FIG. 2 were obtained.
すなわち、第２図から明らかな通り、本発明の焼結体は
従来の焼結体に比し、ワイブル係数が大となり、強度の
バラツキか少ないことがわかる。That is, as is clear from FIG. 2, the sintered body of the present invention has a larger Weibull coefficient and less variation in strength than the conventional sintered body.
［発明の効果］
以上説明したように１本発明の均質焼結体の製造方法に
よれば、成形助剤を加熱除去後の成形体に流動性を付与
し次いでその成形体に静水圧加圧を施しているため、加
熱除去後に形成される成形体中の粗大気孔か漬れ、引続
く焼成工程により均質で緻密な焼結体を得ることかでき
る。[Effects of the Invention] As explained above, according to the method for producing a homogeneous sintered body of the present invention, fluidity is imparted to the molded body after the molding aid is removed by heating, and then hydrostatic pressure is applied to the molded body. As a result, coarse pores in the molded body formed after heat removal are soaked, and a homogeneous and dense sintered body can be obtained through the subsequent firing process.
第１図 第３図Figure 1 Figure 3
第１図は本発明の製造工程を示すフローチャート、第２
図は本発明の焼結体と従来の焼結体のそれぞれについて
ワイブル係数を示すとともに曲げ強度に対する破壊確率
を示すグラフ、第３図は従来の製造工程を示すフローチ
ャートである。Figure 1 is a flowchart showing the manufacturing process of the present invention, Figure 2 is a flowchart showing the manufacturing process of the present invention.
The figure is a graph showing the Weibull coefficient and the fracture probability with respect to bending strength for the sintered body of the present invention and the conventional sintered body, and FIG. 3 is a flowchart showing the conventional manufacturing process.
Claims (1)
後焼成することにより焼結体を製造する方法において、
前記助剤を加熱除去した成形体に流動性を付与した後静
水圧加圧を施し、次いで焼成することを特徴とする均質
焼結体の製造方法。(1) In a method for producing a sintered body by heating and removing an organic forming aid from a ceramic molded body and then firing it,
A method for producing a homogeneous sintered body, which comprises imparting fluidity to the molded body from which the auxiliary agent has been removed by heating, applying hydrostatic pressure, and then firing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63306738A JPH02153866A (en) | 1988-12-03 | 1988-12-03 | Production of uniform sintered compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63306738A JPH02153866A (en) | 1988-12-03 | 1988-12-03 | Production of uniform sintered compact |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02153866A true JPH02153866A (en) | 1990-06-13 |
| JPH0512302B2 JPH0512302B2 (en) | 1993-02-17 |
Family
ID=17960709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63306738A Granted JPH02153866A (en) | 1988-12-03 | 1988-12-03 | Production of uniform sintered compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02153866A (en) |
-
1988
- 1988-12-03 JP JP63306738A patent/JPH02153866A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0512302B2 (en) | 1993-02-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |