JPH0774106B2 - Method for manufacturing powder sintered products such as ceramics - Google Patents
Method for manufacturing powder sintered products such as ceramicsInfo
- Publication number
- JPH0774106B2 JPH0774106B2 JP5208950A JP20895093A JPH0774106B2 JP H0774106 B2 JPH0774106 B2 JP H0774106B2 JP 5208950 A JP5208950 A JP 5208950A JP 20895093 A JP20895093 A JP 20895093A JP H0774106 B2 JPH0774106 B2 JP H0774106B2
- Authority
- JP
- Japan
- Prior art keywords
- ceramics
- sintering
- sintered product
- powder
- calculated
- 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 - Fee Related
Links
- 238000000034 method Methods 0.000 title claims description 26
- 239000000843 powder Substances 0.000 title claims description 21
- 239000000919 ceramic Substances 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 238000005245 sintering Methods 0.000 claims description 21
- 230000000007 visual effect Effects 0.000 claims description 5
- 239000013078 crystal Substances 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011179 visual inspection Methods 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、セラミックス等粉末焼
結品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 a powder sintered product such as ceramics.
【０００２】[0002]
【従来の技術】種々の材料の粉末を生成し、その粉末を
構成している材質の融点以下の温度で加熱して強固な結
合を作り出し、部品として利用しようという試みは以前
から取り組まれ、特に金属粉末を利用したものは既に粉
末冶金として完全に実用化領域にある。また、この方法
は金属のみならず、セラミックスのように高融点で、溶
解や鋳造では製造困難な材料においては欠かせない工法
の一つである。2. Description of the Related Art Attempts have been made for a long time to produce powders of various materials, heat them at a temperature lower than the melting point of the materials forming the powders to create a strong bond, and use them as parts. Those using metal powders are already in the practical application area as powder metallurgy. Further, this method is one of the indispensable construction methods not only for metals but also for materials that have a high melting point such as ceramics and are difficult to manufacture by melting or casting.
【０００３】ところで、セラミックスなどの粉末を焼結
する際、その焼結工程において成形品を構成する粉末は
加熱に伴い周囲の粉末と原子的な結合をして行くが、焼
結品の特性はそのときの加熱条件により大きく左右され
ることが知られている。すなわち、焼結工程において、
熱のかかり具合が不完全の場合は粉末粒子間の結合が不
完全なものとなり、焼結品の強度は極めて小さいものと
なる。By the way, when a powder of ceramics or the like is sintered, the powder constituting the molded product is atomically bonded to the surrounding powder due to heating in the sintering process. It is known that the heating conditions at that time largely depend. That is, in the sintering process,
If the degree of heat application is incomplete, the bond between the powder particles will be incomplete, and the strength of the sintered product will be extremely low.
【０００４】一方、焼結工程中に過剰に熱が加わると粒
子間の結合は強固なものとなるが、結晶粒が粗大化する
という問題が生じる。On the other hand, if excessive heat is applied during the sintering process, the bonds between the particles become strong, but the problem that the crystal grains become coarse occurs.
【０００５】通常、このような焼結品の破断現象をミク
ロ的に見た場合、結晶粒が破断するのではなく、結晶粒
と結晶粒の界面、すなわち結晶粒界を亀裂が進展し、破
断に及ぶことが知られている。Usually, when microscopically observing the rupture phenomenon of such a sintered product, the crystal grains do not rupture, but a crack develops at the interface between the crystal grains, that is, at the crystal grain boundary, and the fracture occurs. It is known to extend to
【０００６】このように、焼結工程において熱が過剰に
加わった場合でも焼結品の強度が低下することがあり、
これによって焼結には最適の条件が存在することが理解
される。[0006] As described above, the strength of the sintered product may decrease even if heat is excessively applied in the sintering process.
It is understood from this that optimum conditions exist for sintering.
【０００７】[0007]
【発明が解決しようとする課題】しかし、この焼結の最
適条件というのは普遍的なものではなく、焼結品の形状
や表面積、体積、重量等によって変化し、それを決定す
るのは試行錯誤による以外に適当な方法がなかった。However, the optimum conditions for this sintering are not universal, and they vary depending on the shape, surface area, volume, weight, etc. of the sintered product, and it is a trial to determine it. There was no suitable method except by mistake.
【０００８】このため、従来はその都度、強度や伸び等
の機械的特性、結晶粒径などの評価が必要となり、作業
が煩雑であるという問題があった。Therefore, conventionally, it is necessary to evaluate mechanical properties such as strength and elongation, crystal grain size and the like each time, and there is a problem that the work is complicated.
【０００９】本発明は、かかる問題を解決するためにな
されたもので、その目的とするところは、試行錯誤によ
る多大な手間を要することなく、高品位な粉末焼結品を
容易に得ることが可能なセラミックス等粉末焼結品の製
造方法を提供することにある。The present invention has been made in order to solve such a problem, and an object thereof is to easily obtain a high-quality powder-sintered product without requiring a great deal of effort by trial and error. An object of the present invention is to provide a method for producing a powder-sintered product such as ceramics.
【００１０】[0010]
【課題を解決するための手段】前記目的を達成するため
に、本発明のセラミックス等粉末焼結品の製造方法にお
いては、セラミックス等の粉末成形品の焼結に際し、焼
結工程中のサンプルをテレビカメラ等の視認装置や非接
触の測長手段により焼結品の寸法を測定し、このとき算
出される単位時間当たりの寸法変動や寸法から算出可能
な因子の単位時間当たりの変動を求め、その値があらか
じめ設定された値以下となったときに焼結が完了したと
判断して降温することを特徴とする。In order to achieve the above object, in the method for producing a powder sintered product such as ceramics of the present invention, a sample in the sintering process is used when sintering a powder molded product such as ceramics. The size of the sintered product is measured by a visual device such as a TV camera or a non-contact length measuring unit, and the dimensional fluctuation per unit time calculated at this time and the fluctuation per unit time of the factor calculable from the size are obtained. It is characterized in that when the value becomes equal to or less than a preset value, it is judged that the sintering is completed and the temperature is lowered.
【００１１】[0011]
【作用】本発明方法は、前述のごとく構成したことによ
り、焼結工程中のサンプルの外形寸法等を所定の視認装
置または非接触の測長手段により測定するとともに、焼
結中のサンプルの寸法変動等を求め、このときの寸法変
動等があらかじめ設定された値以下となった時点で工程
を完了することで、手間を要さず容易に良好な粉末焼結
品を得ることができる。The method of the present invention is configured as described above, so that the outer dimensions of the sample during the sintering process can be measured by a predetermined visual device or non-contact length measuring means, and the size of the sample during sintering can be measured. By obtaining the variation or the like and completing the process when the dimension variation or the like at this time becomes equal to or less than the preset value, it is possible to easily obtain a good powder sintered product without any trouble.
【００１２】すなわち、成形品の焼結には、一般に温度
や時間等の最適条件が存在するが、この最適条件は焼結
品の形状や重量等によって変化し、これを決定するため
には試行錯誤による繰り返し以外にはなく、多大の手間
を要するのが実情であるが、本発明方法においては、こ
れを焼結品の外形寸法を測定することで焼結条件を決定
しようとするものである。That is, there are generally optimum conditions such as temperature and time for the sintering of a molded product, but these optimum conditions vary depending on the shape, weight, etc. of the sintered product. In reality, it requires a lot of trouble other than repetition due to an error, but in the method of the present invention, the sintering conditions are determined by measuring the external dimensions of the sintered product. .
【００１３】[0013]
【実施例】以下、本発明方法を図面に示す実施例に従っ
て説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The method of the present invention will be described below with reference to the embodiments shown in the drawings.
【００１４】本発明方法の特徴的なことは、セラミック
ス等の粉末成形品の焼結に際し、焼結工程中のサンプル
をテレビカメラ等の視認装置や非接触の測長手段により
焼結品の寸法を測定し、このとき算出される単位時間当
たりの寸法変動や寸法から算出可能な因子の単位時間当
たりの変動を求め、その値があらかじめ設定された値以
下となったときに焼結が完了したと判断して降温するよ
うにしたことである。A characteristic of the method of the present invention is that when a powder molded product such as ceramics is sintered, the size of the sintered product is measured by a visual inspection device such as a television camera or a non-contact length measuring device during the sintering process. Was measured, and the dimensional fluctuation per unit time calculated at this time and the fluctuation per unit time of the factor that can be calculated from the dimension were calculated.Sintering was completed when the value fell below a preset value. It was decided to lower the temperature.
【００１５】そして、本発明方法を実施するための製造
装置では、図１に示すごとく、炉体８の上部に、周囲を
水冷した覗き窓９が設けられている。この覗き窓９に
は、石英ガラスが嵌め込まれており、さらに炉内は高温
のため光輝状態になっているので、視認性を向上させる
ためにフィルタ１０が設けられている。覗き窓９の上部
には、テレビカメラ１１が設けられており、覗き窓９を
通して炉内が観察できるようになっている。炉内には、
テレビカメラ１１により視認できる範囲にサンプル１３
が載置される。In the manufacturing apparatus for carrying out the method of the present invention, as shown in FIG. 1, a viewing window 9 whose periphery is water-cooled is provided on the upper part of the furnace body 8. Quartz glass is fitted into the viewing window 9, and since the inside of the furnace is in a bright state due to high temperature, a filter 10 is provided to improve visibility. A television camera 11 is provided above the observation window 9 so that the inside of the furnace can be observed through the observation window 9. In the furnace,
Sample 13 within the range visible by the TV camera 11
Is placed.
【００１６】前記テレビカメラ１１は、画像処理用のコ
ンピュータ１４と接続されており、テレビカメラ１１か
ら取り込まれた画像は、この画像処理用のコンピュータ
１４に送られ、２値化処理されてリアルタイムでその寸
法が計測される。The television camera 11 is connected to a computer 14 for image processing, and an image captured from the television camera 11 is sent to the computer 14 for image processing, binarized, and in real time. Its dimensions are measured.
【００１７】ここで、本発明方法を実施する工程の一例
では、図２に示すように、セラミックス等の粉末と、有
機結合剤とを混練する。Here, in an example of the step of carrying out the method of the present invention, as shown in FIG. 2, powder of ceramics or the like and an organic binder are kneaded.
【００１８】粉末には、例えば平均粒径０．８μｍ、比
表面積６ｍ2 ／ｇのＹ2 Ｏ3 ｍｏｌ％添加部分安定化ジ
ルコニアを用いる。有機結合剤には、ポリエチレングリ
コール、ポリ酢酸ビニル等を用いる。As the powder, for example, partially stabilized zirconia containing Y 2 O 3 mol% and having an average particle diameter of 0.8 μm and a specific surface area of 6 m 2 / g is used. Polyethylene glycol, polyvinyl acetate, or the like is used as the organic binder.
【００１９】前記粉末に有機結合剤を４５ｖｏｌを添加
し、混練する。混練後、３０ｍｍ×３０ｍｍの平板に成
形する。この成形品を、例えば３５０℃まで２４時間で
昇温して脱脂し、有機結合剤を除去する。脱脂後、１０
０℃／ｈｒの条件にて昇温し、１５５０℃に達したら、
その温度にキープする。45 vol of an organic binder is added to the powder and kneaded. After kneading, a flat plate of 30 mm × 30 mm is formed. This molded product is heated to, for example, 350 ° C. for 24 hours to degrease it, and the organic binder is removed. After degreasing, 10
When the temperature is raised under the condition of 0 ° C / hr and reaches 1550 ° C,
Keep at that temperature.
【００２０】このとき、毎分当たりの寸法変化率を測定
し、あらかじめ設定された所定の変化率、例えば０．０
１％／ｍｉｎに達したとき、降温を開始する。At this time, the rate of dimensional change per minute is measured, and a predetermined rate of change, for example, 0.0
When the temperature reaches 1% / min, the temperature reduction is started.
【００２１】図３は、以上の実施例における炉内温度と
寸法変化率との関係を示している。FIG. 3 shows the relationship between the temperature in the furnace and the dimensional change rate in the above embodiment.
【００２２】なお、毎分当たりの寸法変化率は、成形品
の寸法をＬ、焼結品の寸法をＬ′、焼結時間をΔｔとす
ると、次の数１で算出される。The dimensional change rate per minute is calculated by the following formula 1 where L is the dimension of the molded product, L'is the dimension of the sintered product, and Δt is the sintering time.
【数１】 [Equation 1]
【００２３】次に、図４は本発明方法の他の実施例にお
ける炉内温度と焼結品の寸法との関係を示すもので、前
述の寸法変化率の代わりに寸法収縮率を用いている。Next, FIG. 4 shows the relationship between the temperature in the furnace and the size of the sintered product in another embodiment of the method of the present invention, in which the dimensional shrinkage rate is used instead of the dimensional change rate. .
【００２４】この実施例では、原料粉末と有機結合剤と
の混合比から、焼結品の完了寸法を算出する。ついで、
現在焼結中の成形品の寸法を測定し、測定された寸法が
焼結品の完了寸法に達しているか，否かを演算処理して
判定する。そして、この実施例では焼結中の成形品の１
辺の寸法があらかじめ設定された例えば２４．７ｍｍに
達したとき、降温を開始する。In this embodiment, the completed size of the sintered product is calculated from the mixing ratio of the raw material powder and the organic binder. Then,
The dimensions of the molded article that is currently being sintered are measured, and it is determined whether or not the measured dimension has reached the completed dimension of the sintered article by arithmetic processing. And, in this example, one of the molded products being sintered
When the side dimension reaches a preset value, for example, 24.7 mm, the temperature reduction is started.
【００２５】なお、前記成形品から焼結品への寸法収縮
率は、次の数２で算出される。The dimensional shrinkage ratio from the molded product to the sintered product is calculated by the following equation 2.
【数２】 [Equation 2]
【００２６】以上の各実施例において、焼結品の３点曲
げ強度を測定したところ、１１０ｋｇ／ｍｍ2 、結晶粒
径１．０μｍと高強度であり、これによって結晶粒の粗
大化のない良好な焼結品を製造することができた。In each of the above examples, the three-point bending strength of the sintered product was measured and found to be 110 kg / mm 2 , and the crystal grain size was 1.0 μm, which was a high strength. It was possible to manufacture various sintered products.
【００２７】なお、以上は本発明の一例であり、材質も
Ｙ2 Ｏ3 −部分安定化ジルコニアに限定されるものでは
なく、Ｓｉ3 Ｎ4 、ＳｉＣ等のセラミックス、および従
来の粉末冶金に使用されている金属粉や超硬でも可能で
ある。また、視認装置についてもテレビカメラに限定さ
れるものではなく、ＣＣＤ等の利用やレーザの反射を利
用した測長等でも可能である。The above is one example of the present invention, and the material is not limited to Y 2 O 3 -partially stabilized zirconia, but is used for ceramics such as Si 3 N 4 and SiC, and conventional powder metallurgy. It is also possible to use metal powders or super hard materials. Further, the visual recognition device is not limited to the television camera, and it is also possible to use a CCD or the like or a length measurement using reflection of a laser.
【００２８】[0028]
【発明の効果】以上説明したように、本発明方法によれ
ば、セラミックス等の粉末成形品の焼結に際し、焼結工
程中のサンプルをテレビカメラ等の視認装置や非接触の
測長手段により焼結品の寸法を測定し、このとき算出さ
れる単位時間当たりの寸法変動や寸法から算出可能な因
子の単位時間当たりの変動を求め、その値があらかじめ
設定された値以下となったときに焼結が完了したと判断
して降温することにより、試行錯誤による多大なロスを
生じることなく、容易に良好な粉末焼結品を得ることが
できる。As described above, according to the method of the present invention, when a powder molded article such as ceramics is sintered, the sample during the sintering process is measured by a visual device such as a television camera or a non-contact length measuring means. When the dimensions of the sintered product are measured, the dimensional variation per unit time calculated at this time and the variation per unit time of the factors that can be calculated from the dimensions are calculated, and when the value becomes less than or equal to the preset value By determining that the sintering is completed and lowering the temperature, it is possible to easily obtain a good powder sintered product without causing a large loss due to trial and error.
【図１】本発明方法を実施するための製造装置の一例を
示す図である。FIG. 1 is a diagram showing an example of a manufacturing apparatus for carrying out the method of the present invention.
【図２】本発明方法を実施するための工程図である。FIG. 2 is a process chart for carrying out the method of the present invention.
【図３】本発明方法の一実施例における炉内温度と焼結
品の寸法変化率との関係を示す図である。FIG. 3 is a diagram showing a relationship between a temperature in a furnace and a rate of dimensional change of a sintered product in one embodiment of the method of the present invention.
【図４】本発明方法の他の実施例における炉内温度と焼
結品の寸法との関係を示す図である。FIG. 4 is a diagram showing the relationship between the furnace temperature and the size of a sintered product in another example of the method of the present invention.
８ 炉体 ９ 覗き窓 １１ テレビカメラ １２ サンプル設置台 １３ サンプル １４ コンピュータ 8 Furnace Body 9 Peep Window 11 Television Camera 12 Sample Stand 13 Sample 14 Computer
Claims (1)
し、焼結工程中のサンプルをテレビカメラ等の視認装置
や非接触の測長手段により焼結品の寸法を測定し、この
とき算出される単位時間当たりの寸法変動や寸法から算
出可能な因子の単位時間当たりの変動を求め、その値が
あらかじめ設定された値以下となったときに焼結が完了
したと判断して降温することを特徴とするセラミックス
等粉末焼結品の製造方法。1. When sintering a powder molded product such as ceramics, the dimensions of the sintered product are measured by measuring the sample during the sintering process with a visual device such as a television camera or a non-contact length measuring means. The dimensional fluctuation per unit time and the fluctuation per unit time of the factors that can be calculated from the dimension are calculated, and when the value is below a preset value, it is judged that the sintering is completed and the temperature is lowered. A method for producing a powdered sintered product such as a characteristic ceramics.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63295143A JPH0625022B2 (en) | 1988-11-22 | 1988-11-22 | Ceramic blade manufacturing method |
| JP5208950A JPH0774106B2 (en) | 1988-11-22 | 1993-07-30 | Method for manufacturing powder sintered products such as ceramics |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63295143A JPH0625022B2 (en) | 1988-11-22 | 1988-11-22 | Ceramic blade manufacturing method |
| JP5208950A JPH0774106B2 (en) | 1988-11-22 | 1993-07-30 | Method for manufacturing powder sintered products such as ceramics |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63295143A Division JPH0625022B2 (en) | 1988-11-22 | 1988-11-22 | Ceramic blade manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0648843A JPH0648843A (en) | 1994-02-22 |
| JPH0774106B2 true JPH0774106B2 (en) | 1995-08-09 |
Family
ID=26517135
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63295143A Expired - Fee Related JPH0625022B2 (en) | 1988-11-22 | 1988-11-22 | Ceramic blade manufacturing method |
| JP5208950A Expired - Fee Related JPH0774106B2 (en) | 1988-11-22 | 1993-07-30 | Method for manufacturing powder sintered products such as ceramics |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63295143A Expired - Fee Related JPH0625022B2 (en) | 1988-11-22 | 1988-11-22 | Ceramic blade manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (2) | JPH0625022B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0465437U (en) * | 1990-10-16 | 1992-06-08 | ||
| JP5086507B2 (en) * | 2001-09-28 | 2012-11-28 | 三菱重工業株式会社 | Manufacturing method of fuel cell tube and ceramic manufacturing apparatus |
| US9464004B2 (en) * | 2011-02-28 | 2016-10-11 | Corning Incorporated | Method for manufacturing ceramic honeycombs with reduced shrinkage |
-
1988
- 1988-11-22 JP JP63295143A patent/JPH0625022B2/en not_active Expired - Fee Related
-
1993
- 1993-07-30 JP JP5208950A patent/JPH0774106B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0648843A (en) | 1994-02-22 |
| JPH02141456A (en) | 1990-05-30 |
| JPH0625022B2 (en) | 1994-04-06 |
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| LAPS | Cancellation because of no payment of annual fees |