JPH035282B2 - - Google Patents
Info
- Publication number
- JPH035282B2 JPH035282B2 JP26196485A JP26196485A JPH035282B2 JP H035282 B2 JPH035282 B2 JP H035282B2 JP 26196485 A JP26196485 A JP 26196485A JP 26196485 A JP26196485 A JP 26196485A JP H035282 B2 JPH035282 B2 JP H035282B2
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- hollow
- powder
- mold
- ceramic
- 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 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 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 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010987 cubic zirconia Substances 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 230000036316 preload Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Landscapes
- Press-Shaping Or Shaping Using Conveyers (AREA)
- Devices For Post-Treatments, Processing, Supply, Discharge, And Other Processes (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 本発明は、セラミツクスの加工方法に関する。[Detailed description of the invention] Industrial applications The present invention relates to a method for processing ceramics.
従来の技術及びその問題点
セラミツクス焼結体は、一般に耐熱性、耐摩耗
性、耐食性等に優れているので、従来から使用さ
れている金属機械部品に代替し得る構造用セラミ
ツクス製品としての開発が進められている。しか
しながら、セラミツクス焼結体は、一般に硬脆材
料である為、ダイヤモンド等の超硬砥粒による煩
雑な加工を必要とし、しかも構造用部品等に用い
られるセラミツクスは、複雑な形状の製品とする
ことは不可能である。焼結前の圧粉体を金型成
形、射出成形等によりほぼ所定の形状に対応する
形状に成形した後、焼結する試みも行なわれてい
るが、圧粉体の密度、焼結温度等によつて収縮の
度合が大巾に変動するので、均一で寸法精度の高
い焼結機械部品は得られない。Conventional technology and its problems Ceramic sintered bodies generally have excellent heat resistance, abrasion resistance, corrosion resistance, etc., so it is important to develop structural ceramic products that can replace conventionally used metal mechanical parts. It is progressing. However, since ceramic sintered bodies are generally hard and brittle materials, they require complicated processing using carbide abrasive grains such as diamond, and ceramics used for structural parts, etc., are products with complex shapes. is impossible. Attempts have also been made to mold the green compact before sintering into a shape that almost corresponds to a predetermined shape using die molding, injection molding, etc., and then sinter it, but the density of the green compact, the sintering temperature, etc. Since the degree of shrinkage varies widely depending on the material, it is not possible to obtain sintered mechanical parts that are uniform and have high dimensional accuracy.
問題点を解決するための手段
本発明者は、上記の如き従来の技術の問題点に
鑑みて種々研究を重ねた結果、或る種のセラミツ
クス焼結体が、特定の温度域において変形抵抗が
低くなる、即ち比較的低い応力で巨大な伸びを生
ずるという超塑性現象を示すことを見出した。本
発明は、この様なセラミツクス焼結体における超
塑性現象を利用して、以下の如き加工方法を提供
するものである。Means for Solving the Problems The present inventor has conducted various studies in view of the problems of the conventional technology as described above, and has found that a certain type of ceramic sintered body has low deformation resistance in a specific temperature range. It has been found that a superplastic phenomenon occurs in which a huge elongation occurs at a relatively low stress. The present invention utilizes such a superplastic phenomenon in a ceramic sintered body to provide the following processing method.
「型内に配置した超塑性セラミツクス中空焼結
体の中空部に難焼結性粉体を充填し、中空焼結体
が超塑性現象を示す温度域において難焼結性粉体
を加圧することにより、中空焼結体を型に対応す
る形状に変化させることを特徴とする超塑性セラ
ミツクス焼結体の加工方法。」
本発明の対象となる超塑性セラミツクス中空焼
結体の材料としては、Y2O3、MgO、CaO、CeO2
等の添加成分を含む部分安定化ジルコニア、アル
ミナ、窒化珪素等が例示される。部分安定化ジル
コニアの場合には、立方晶系ジルコニア微結晶を
20体積％以上含有し且つ結晶粒径が2μｍ以下で
あることが好ましく、1μｍ以下であることがよ
り好ましい。中空焼結体は、常法に従つて原料粉
体を成形し、焼成したものを使用すれば良い。 "Filling the hollow part of a superplastic ceramic hollow sintered body placed in a mold with hard-to-sinter powder, and pressurizing the hard-to-sinter powder in a temperature range where the hollow sintered body exhibits a superplastic phenomenon. A method for processing a superplastic ceramic sintered body, which is characterized by changing the hollow sintered body into a shape corresponding to a mold by 2O3 , MgO, CaO , CeO2
Examples include partially stabilized zirconia, alumina, and silicon nitride containing additive components such as. In the case of partially stabilized zirconia, cubic zirconia microcrystals are used.
It is preferable that the content is 20% by volume or more and the crystal grain size is 2 μm or less, more preferably 1 μm or less. The hollow sintered body may be one obtained by molding and firing raw material powder according to a conventional method.
中空焼結体の中空部に充填される難焼結性粉体
としては、SiC、Ｃ、BN、Al2O3、ムライト等が
例示され、粒度は、１〜100μｍ程度とすること
が好ましい。 Examples of the hard-to-sinter powder filled in the hollow part of the hollow sintered body include SiC, C, BN, Al 2 O 3 , mullite, etc., and the particle size is preferably about 1 to 100 μm.
超塑性現象を示す温度域は、部分安定化ジルコ
ニア中空焼結体の場合、1000℃程度以上である
が、本発明における加工は、通常1200〜1600℃程
度、より好ましくは1400〜1500℃程度で行なう。
加工温度が1200℃程度未満では、変形もしくは加
工速度が遅くなつて実用的でない。一方1600℃℃
を上回る場合には、ジルコニア結晶粒径の成長が
著しく、臨界粒径を越えて粗大化して室温におい
て単斜晶となつてしまうので、応力誘起変態によ
る強化機構が期待できなくなる。この場合、変形
加工は、容易となるものの、成形体の強度は著し
く低下する。 The temperature range in which the superplastic phenomenon occurs is about 1000°C or higher in the case of partially stabilized zirconia hollow sintered bodies, but processing in the present invention is usually carried out at about 1200 to 1600°C, more preferably about 1400 to 1500°C. Let's do it.
If the processing temperature is less than about 1200°C, deformation or processing speed will become slow, making it impractical. Meanwhile 1600℃℃
If the zirconia crystal grain size exceeds 1, the growth of the zirconia crystal grain size is remarkable, and the grain size exceeds the critical grain size and becomes coarse, forming a monoclinic crystal at room temperature, so that a strengthening mechanism based on stress-induced transformation cannot be expected. In this case, although the deformation process becomes easy, the strength of the molded product is significantly reduced.
中空焼結体の材料がAl2O3である場合には、加
工温度は1500〜1650℃程度とし、Si3N4の場合に
は、1450〜1750℃程度とする。 When the material of the hollow sintered body is Al2O3 , the processing temperature is about 1500 to 1650 °C, and when it is Si3N4 , it is about 1450 to 1750°C.
中空焼結体の中空部に充填された難焼結性粉体
に対して加えられる圧力は、30〜200メガパスカ
ル（MPa）程度とすることが好ましい。加工時
の変形若しくはひずみ速度は、温度が高い程大と
することが出来るが、通常1200〜1600℃の温度範
囲において10-2／sec以下であることが好ましい。
具体的には、変形若しくはひずみ速度は、部分安
定化ジルコニアについては、温度が1450℃の場
合、１×10-4〜６×10-4／sec程度とすることが
好ましい。変形若しくはひずみ速度が、10-2／
secを上回る場合には、焼結体の結晶粒界におけ
るキヤビテイーの生成及び成長が著るしくなり、
加工中に焼結体が破壊したり、焼結体の強度が低
下したりする。 The pressure applied to the hard-to-sinter powder filled in the hollow part of the hollow sintered body is preferably about 30 to 200 megapascals (MPa). The deformation or strain rate during processing can be increased as the temperature is higher, but it is usually preferably 10 -2 /sec or less in the temperature range of 1200 to 1600°C.
Specifically, the deformation or strain rate is preferably about 1×10 −4 to 6×10 −4 /sec when the temperature is 1450° C. for partially stabilized zirconia. The deformation or strain rate is 10 -2 /
If it exceeds sec, the formation and growth of cavities at the grain boundaries of the sintered body becomes remarkable,
The sintered body may break during processing or its strength may decrease.
以下、図面を参照しつつ本発明を具体的に説明
する。 Hereinafter, the present invention will be specifically described with reference to the drawings.
第１図において、超塑性セラミツクス中空焼結
体１は、半割り型３及び５からなる型内に配置さ
れている。中空焼結体１内には、難焼結性粉体７
が充填されており、該粉体の上下には、それぞれ
往復動可能な上部加圧棒９及び下部加圧棒１１が
配置されている。 In FIG. 1, a superplastic ceramic hollow sintered body 1 is placed in a mold consisting of half molds 3 and 5. In FIG. Inside the hollow sintered body 1 is a hard-to-sinter powder 7.
is filled with the powder, and an upper pressure rod 9 and a lower pressure rod 11 that can reciprocate are arranged above and below the powder, respectively.
加工に際しては、上部加圧棒９及び／または下
部加圧棒１１を移動させて難焼結性粉体７を予備
圧縮することにより、粉体７を密充填し、中空焼
結体１を固定し、かつ上下の加工棒９及び１１の
圧力が均等に伝わる様にした後、中空焼結体を所
定の温度に保持した状態で、上部加圧棒９及び／
又は下部加圧棒１１を所定の速度で移動させて粉
体７を更に圧縮させると、粉体を媒介した圧力に
より中空焼結体１が半割り型３及び５の凹部１３
及び１５に向けて膨脹変形し、第２図に示す如
く、バルジ１７を有する製品が得られる。 During processing, the upper pressure rod 9 and/or the lower pressure rod 11 are moved to pre-compress the hard-to-sinter powder 7 to tightly pack the powder 7 and fix the hollow sintered body 1. After making sure that the pressure of the upper and lower working rods 9 and 11 is evenly transmitted, the upper pressing rods 9 and/or
Alternatively, when the lower pressure rod 11 is moved at a predetermined speed to further compress the powder 7, the hollow sintered body 1 is compressed into the recesses 13 of the half-split molds 3 and 5 due to the pressure mediated by the powder.
The product is expanded and deformed toward 15, and a product having a bulge 17 as shown in FIG. 2 is obtained.
尚、半割り型３及び５、上部加圧棒９及び下部
加圧棒１１としては、アルミナ、炭化珪素、ムラ
イト等の耐熱材料からなるものを使用し、加工時
に中空焼結体１と反応しない様に加工温度に応じ
て適切な材料を選択すれば良い。 The half molds 3 and 5, the upper pressure rod 9 and the lower pressure rod 11 are made of heat-resistant materials such as alumina, silicon carbide, mullite, etc., and do not react with the hollow sintered body 1 during processing. It is only necessary to select an appropriate material according to the processing temperature.
本発明方法を実施するに際しての雰囲気は、特
に限定されないが、酸化物セラミツクスの場合に
は、通常は大気中で行なえば良い。 The atmosphere in which the method of the present invention is carried out is not particularly limited, but in the case of oxide ceramics, it is usually sufficient to carry out the process in the atmosphere.
本発明方法は、上記のバルジ部形成以外にも、
種々の形状の加工が可能である。例えば、中空焼
結体１の側部にほぼ同径の膨出部１９を形成した
後、その先端部分２１を切断することにより、Ｔ
字管を形成することも可能である（第３図参照）。
この他にも、種々の形態の製品を得ることが可能
であり、本発明が、特定形状の製品の製造にのみ
限定されるものでないことは言うまでもない。 In addition to the above-mentioned bulge formation, the method of the present invention also includes the following:
It is possible to process various shapes. For example, the T
It is also possible to form a double tube (see FIG. 3).
It goes without saying that it is possible to obtain products in various other shapes, and the present invention is not limited to the manufacture of products of a specific shape.
発明の効果 本発明によれば、以下の如き効果が奏される。Effect of the invention According to the present invention, the following effects are achieved.
(i) 構造用部品としては複雑な形状を有するセラ
ミツクス製品がはじめて製造可能となつた。(i) For the first time, it became possible to manufacture ceramic products with complex shapes as structural parts.
(ii) 成形用型の内面を鏡面仕上げとしておくこと
により、セラミツクス製品の面精度を容易に向
上させることが出来る。(ii) By giving the inner surface of the mold a mirror finish, the surface precision of ceramic products can be easily improved.
(iii) 従つて、構造用部材、機械部品等へのセラミ
ツクス製品の利用範囲を大巾に拡大することが
出来る。(iii) Therefore, the scope of use of ceramic products for structural members, mechanical parts, etc. can be greatly expanded.
実施例
以下実施例を示し、本発明の特徴とするところ
をより一層明らかにする。Examples Examples will be shown below to further clarify the features of the present invention.
実施例 １
Y2O3を３モル％固溶し、平均粒子径0.3μｍの
正方晶系ジルコニア結晶を70体積％含有するジル
コニア中空焼結体（内径７mm、外径10mm、長さ50
mm）の中空部に平均粒径約10μｍの炭化珪素粉末
1.5ｇを充填した後、型内に配置し、外径７mmの
炭化珪素製加圧棒により上下から10Kgの予圧を加
えた。この状態で、大気中で温度1450℃で押し込
み速度0.2mm／minで炭化珪素粉末充填部分を10
mm圧縮した。 Example 1 Zirconia hollow sintered body (inner diameter 7 mm, outer diameter 10 mm, length 50
Silicon carbide powder with an average particle size of approximately 10μm in the hollow part of mm)
After filling 1.5 g, it was placed in a mold, and a preload of 10 kg was applied from above and below using a silicon carbide pressure rod with an outer diameter of 7 mm. In this state, the silicon carbide powder filled part was injected 10 times at a pushing speed of 0.2 mm/min at a temperature of 1450°C in the air.
mm compressed.
その結果、ジルコニア焼結体は、型の内部形状
に密着する様に膨出して、その中央部の外径は、
15mmとなつた。 As a result, the zirconia sintered body bulges out to closely fit the internal shape of the mold, and the outer diameter of the central part is
It became 15mm.
第１図及び第２図は、本発明方法の実施の１例
を示す断面図、第３図は、本発明方法により得ら
れるセラミツクス加工製品の１例を示す断面図で
ある。
１……中空焼結体、３，５……半割り型、７…
…難焼結性粉体、９……上部加圧棒、１１……下
部加圧棒、１３，１５……半割り型３，５の凹
部、１７……バルジ、１９……膨出部、２１……
膨出部１９の先端部。
1 and 2 are cross-sectional views showing an example of the method of the present invention, and FIG. 3 is a cross-sectional view showing an example of a ceramic processed product obtained by the method of the present invention. 1...Hollow sintered body, 3, 5...Half-split mold, 7...
... Difficult to sinter powder, 9 ... Upper pressure rod, 11 ... Lower pressure rod, 13, 15 ... Recessed part of half-split molds 3 and 5, 17 ... Bulge, 19 ... Swelling part, 21...
The tip of the bulge 19.
Claims (1)
体の中空部に難焼結性粉体を充填し、中空焼結体
が超塑性現象を示す温度域において難焼結性粉体
を加圧することにより、中空焼結体を型に対応す
る形状に変化させることを特徴とする超塑性セラ
ミツクス焼結体の加工方法。1 Filling the hollow part of a superplastic ceramic hollow sintered body placed in a mold with a hard-to-sinter powder, and pressurizing the hard-to-sinter powder in a temperature range where the hollow sintered body shows a superplastic phenomenon. A method for processing a superplastic ceramic sintered body, characterized by changing a hollow sintered body into a shape corresponding to a mold.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26196485A JPS62119005A (en) | 1985-11-20 | 1985-11-20 | Method of processing super-plastic ceramics sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26196485A JPS62119005A (en) | 1985-11-20 | 1985-11-20 | Method of processing super-plastic ceramics sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62119005A JPS62119005A (en) | 1987-05-30 |
| JPH035282B2 true JPH035282B2 (en) | 1991-01-25 |
Family
ID=17369101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26196485A Granted JPS62119005A (en) | 1985-11-20 | 1985-11-20 | Method of processing super-plastic ceramics sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62119005A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1989010337A1 (en) * | 1988-04-29 | 1989-11-02 | Dow Chemical Company Limited | Superplastic sintered magnesium-oxide ceramic |
-
1985
- 1985-11-20 JP JP26196485A patent/JPS62119005A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62119005A (en) | 1987-05-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |