JP2001122665A - Method for manufacturing boron carbide atmospheric sintered compact - Google Patents
Method for manufacturing boron carbide atmospheric sintered compactInfo
- Publication number
- JP2001122665A JP2001122665A JP30487199A JP30487199A JP2001122665A JP 2001122665 A JP2001122665 A JP 2001122665A JP 30487199 A JP30487199 A JP 30487199A JP 30487199 A JP30487199 A JP 30487199A JP 2001122665 A JP2001122665 A JP 2001122665A
- Authority
- JP
- Japan
- Prior art keywords
- boron carbide
- temperature
- sintering
- sintered compact
- atmospheric
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、高緻密かつ高曲げ
強度の炭化ほう素常圧焼結体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 high-density and high-flexural strength boron carbide atmospheric pressure sintered body.
【０００２】[0002]
【従来の技術】炭化ほう素焼結体は高硬度かつ軽量であ
り、またその優れた耐摩耗性の特長を活かして、ブラス
トノズル、ブラッシング材（砥石ならし）、耐摩耗機工
部品等に使用されている。2. Description of the Related Art Boron carbide sintered bodies are high hardness and light weight, and are used for blast nozzles, brushing materials (grinding stones), wear-resistant machine parts, etc. by taking advantage of their excellent wear resistance. ing.
【０００３】従来、炭化ほう素焼結体を製造するには、
ホットプレス法でが広く用いられているが、大型形状品
ないしは複雑形状品の製造や、連続製造には不向きであ
るので、今日では常圧焼結法が検討されている。その一
例を示せば、特開平８−１２４３４号公報、特開平１１
−１５７９３５号公報である。しかしながら、これらの
常圧焼結法では、アルミニウム等の焼結助剤を用いてい
るので、その混合作業の煩雑さや、得られた常圧焼結体
には焼結助剤成分が残留し、また曲げ強度の均質性にも
劣るという問題があった。Conventionally, to produce a boron carbide sintered body,
Although the hot press method is widely used, it is not suitable for production of large-sized or complicated-shaped products or continuous production. One example is described in JP-A-8-12434 and JP-A-11-11.
157935. However, in these normal pressure sintering methods, since a sintering aid such as aluminum is used, the sintering aid component remains in the troublesome mixing operation and the obtained normal pressure sintered body, In addition, there is a problem that the homogeneity of bending strength is poor.
【０００４】更には、上記先行技術の実施例に従って炭
化ほう素常圧焼結体を製造してみると、比較的良好な緻
密化品が製造されたが、外皮（外周部）が先行して緻密
化するので内部気孔が抜けきれず、十分に高い緻密化品
は得られなかった。Further, when a boron carbide atmospheric pressure sintered body is manufactured in accordance with the above-mentioned prior art embodiment, a relatively good densified product is manufactured, but the outer skin (outer peripheral portion) is first made dense. Therefore, the internal pores could not be completely removed, and a sufficiently high densified product could not be obtained.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、上記に鑑み
てなされたものであり、その目的は、焼結助剤を用いな
くても、高緻密かつ高曲げ強度の炭化ほう素焼結体を常
圧焼結によって製造することである。SUMMARY OF THE INVENTION The present invention has been made in view of the above, and an object of the present invention is to provide a high-density and high-flexural strength boron carbide sintered body without using a sintering aid. It is manufactured by normal pressure sintering.
【０００６】[0006]
【課題を解決するための手段】すなわち、本発明は、炭
化ほう素粉末の予備成形体を非酸化性雰囲気中で常圧焼
結するにあたり、温度２１５０℃から２２００℃の間の
昇温速度を５〜１００℃／ｈｒとして昇温した後、更に
２２００℃をこえる最終焼結温度までに温度を高めるこ
とを特徴とする炭化ほう素常圧焼結体の製造方法であ
る。That is, the present invention provides a method for sintering a preformed body of boron carbide powder at normal pressure in a non-oxidizing atmosphere at a temperature rising rate between 2150 ° C and 2200 ° C. A method for producing a normal-pressure boron carbide sintered body, characterized in that after raising the temperature at 5 to 100 ° C./hr, the temperature is further raised to a final sintering temperature exceeding 2200 ° C.
【０００７】[0007]
【発明の実施の形態】以下、更に詳しく本発明について
説明する。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail.
【０００８】本発明で使用される炭化ほう素粉末は、市
販品で十分であるが、中でも平均粒径０．５〜２μｍ、
特に１．０μｍ以下であり、しかも比表面積５ｍ2／ｇ
以上、特に１５ｍ2／ｇ以上の微粉末であることが好ま
しい。その市販品としては、シュタルク社（Ｈ．Ｃ．Ｓ
ｔａｒｃｋ社）製「ＨＳグレード」がある。As the boron carbide powder used in the present invention, commercially available products are sufficient, but among others, the average particle size is 0.5 to 2 μm,
In particular, it is 1.0 μm or less, and the specific surface area is 5 m 2 / g.
As described above, it is particularly preferable that the powder is a fine powder of 15 m 2 / g or more. As a commercial product, Stark Co., Ltd. (HCS
“HS grade” manufactured by Starck Corporation.
【０００９】炭化ほう素粉末の予備成形体は、炭化ほう
素粉末を金型にて一次成形した後、ＣＩＰ（冷間静水プ
レス）成形されたものが好適である。一次成形は保形で
きる程度の圧力で行われ、通常は４〜１０ＭＰａであ
る。また、ＣＩＰ成形は高圧であることが好ましく、一
例は１５０〜３００ＭＰａである。あれば十分である。The preformed body of the boron carbide powder is preferably formed by first forming the boron carbide powder in a mold and then performing CIP (cold isostatic pressing). The primary molding is performed at a pressure sufficient to maintain the shape, and is usually 4 to 10 MPa. Further, the CIP molding is preferably performed under a high pressure, and an example is 150 to 300 MPa. It is enough.
【００１０】焼結は、アルゴン、ヘリウム等の希ガス、
一酸化炭素、水素等の非酸化性雰囲気中で行われる。こ
れらの中でも、アルゴン雰囲気は、取扱性、安全性の点
から好適である。The sintering is performed by using a rare gas such as argon or helium,
This is performed in a non-oxidizing atmosphere such as carbon monoxide and hydrogen. Among them, an argon atmosphere is preferable from the viewpoint of handling properties and safety.
【００１１】本発明においては、非酸化性雰囲気中、２
２００℃をこえる最終焼結温度で焼結されるが、重要な
ことは、雰囲気温度が２１５０℃から２２００℃の間に
おいては、昇温速度を５〜１００℃／ｈｒ、好ましくは
１０〜７５℃／ｈｒとすることである。昇温速度が５℃
／ｈｒ未満では、十分に高い緻密化品を製造するのに時
間がかかりすぎ、また１００℃／ｈｒ超では、上記の外
皮先行焼結が顕著となって、十分に高い緻密化品を製造
することができなくなる。温度２１５０℃から２２００
℃の間における昇温は、等速で行うことが特に好まし
い。In the present invention, in a non-oxidizing atmosphere,
Sintering is performed at a final sintering temperature exceeding 200 ° C., but it is important that when the ambient temperature is between 2150 ° C. and 2200 ° C., the heating rate is 5 to 100 ° C./hr, preferably 10 to 75 ° C. / Hr. Heating rate is 5 ℃
If it is less than / hr, it takes too much time to produce a sufficiently high densified product, and if it exceeds 100 ° C / hr, the above-mentioned sintering preceding sintering becomes remarkable, and a sufficiently high densified product is produced. You will not be able to do it. Temperature 2150 ° C to 2200
It is particularly preferred that the temperature rise between ℃ is carried out at a constant speed.
【００１２】本発明においては、温度２１５０℃に達す
るまでの昇温速度と、温度２２００℃をこえる最終焼結
温度にするまでの昇温速度については、特に制約はな
い。例えば、前者については４００〜１２００℃／ｈ
ｒ、後者については５〜１００℃／ｈｒの速度で昇温す
ることができる。In the present invention, there are no particular restrictions on the rate of temperature rise until the temperature reaches 2150 ° C. and the rate of temperature rise until the final sintering temperature exceeds 2200 ° C. For example, for the former, 400 to 1200 ° C./h
r, the latter can be heated at a rate of 5 to 100 ° C./hr.
【００１３】本発明における最終焼結温度としては、２
２００℃をこえ２３００℃までの任意の温度であること
が好ましく、特に２２２０〜２２５０℃が好適である。
最終焼結温度が２３００℃をこえると異常な粒成長が起
こりやすく、強度低下を招く恐れがある。The final sintering temperature in the present invention is 2
It is preferable that the temperature be any temperature from 200 ° C. to 2300 ° C., and particularly preferably 2220 to 2250 ° C.
If the final sintering temperature exceeds 2300 ° C., abnormal grain growth is likely to occur, which may cause a decrease in strength.
【００１４】[0014]
【実施例】以下、実施例、比較例をあげて更に具体的に
本発明を説明する。The present invention will be described more specifically with reference to examples and comparative examples.
【００１５】実施例１〜３ 比較例１〜３ 炭化ほう素粉末（Ｈ．Ｃ．Ｓｔａｒｃｋ社「ＨＳグレー
ド」）６０ｇを、直径５２ｍｍ円筒に入れ、シリンダー
にて４．９ＭＰａでプレス加圧して一次成形体を製造し
た。次いで、これをＣＩＰ（冷間静水圧プレス）により
面圧２６５ＭＰａをかけ、円柱状の予備成形体を成形し
た。これを黒鉛るつぼ内に入れ、常圧のアルゴン雰囲気
下、焼結炉（富士電波社製：ＦＶＳ−Ｒ−８０／８０
ＦＲＥＴ−２０）にて表１に示す条件で焼結を行った。
なお、最終焼結温度に達した後は、温度調節電源を切
り、アルゴン雰囲気下で自然冷却をした。Examples 1 to 3 Comparative Examples 1 to 3 60 g of boron carbide powder ("HS grade" manufactured by H. C. Starck) was placed in a cylinder having a diameter of 52 mm, and pressurized with a cylinder at 4.9 MPa to perform primary press. A molded body was manufactured. Next, the resultant was subjected to a surface pressure of 265 MPa by CIP (cold isostatic press) to form a cylindrical preform. This was put in a graphite crucible, and a sintering furnace (FVS-R-80 / 80, manufactured by Fuji Electric Co., Ltd.) was placed in an argon atmosphere at normal pressure.
Sintering was performed under the conditions shown in Table 1 by FRET-20).
After the temperature reached the final sintering temperature, the temperature control power was turned off and the product was naturally cooled in an argon atmosphere.
【００１６】得られた常圧焼結体について、アルキメデ
ス法による密度、及び焼結体内部から３×４×３６ｍｍ
の試片を切り出し、ＪＩＳＲ１６０１に準拠して３点曲
げ強度を測定した。それらの結果を表１に示す。The density of the obtained sintered body under normal pressure was measured by Archimedes method, and 3 × 4 × 36 mm
Was cut out, and the three-point bending strength was measured in accordance with JISR1601. Table 1 shows the results.
【００１７】[0017]
【表１】 [Table 1]
【００１８】[0018]
【発明の効果】本発明によれば、高緻密かつ高曲げ強度
であり、しかも焼結助剤成分の残留のない炭化ほう素常
圧焼結体を得ることができる。According to the present invention, a normal-pressure sintered body of boron carbide having high density and high bending strength and having no sintering aid component remaining can be obtained.
Claims (1)
雰囲気中で常圧焼結するにあたり、温度２１５０℃から
２２００℃の間の昇温速度を５〜１００℃／ｈｒとして
昇温した後、更に２２００℃をこえる最終焼結温度まで
に温度を高めることを特徴とする炭化ほう素常圧焼結体
の製造方法。When sintering a preformed body of boron carbide powder at normal pressure in a non-oxidizing atmosphere, the temperature was raised between 2150 ° C. and 2200 ° C. at a rate of 5-100 ° C./hr. Thereafter, the temperature is further increased to a final sintering temperature exceeding 2200 ° C., thereby producing a boron carbide normal pressure sintered body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30487199A JP2001122665A (en) | 1999-10-27 | 1999-10-27 | Method for manufacturing boron carbide atmospheric sintered compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30487199A JP2001122665A (en) | 1999-10-27 | 1999-10-27 | Method for manufacturing boron carbide atmospheric sintered compact |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001122665A true JP2001122665A (en) | 2001-05-08 |
Family
ID=17938290
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30487199A Pending JP2001122665A (en) | 1999-10-27 | 1999-10-27 | Method for manufacturing boron carbide atmospheric sintered compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001122665A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008524108A (en) * | 2004-12-20 | 2008-07-10 | ジョージア・テック・リサーチ・コーポレーション | B4C with improved density and hardness after pressureless sintering and post-HIP |
| JP2008535769A (en) * | 2005-04-11 | 2008-09-04 | ジョージア・テック・リサーチ・コーポレーション | Boron carbide component and method for producing the same |
| US7517491B2 (en) | 2003-06-12 | 2009-04-14 | Georgia Tech Research Corporation | Processes and methods of making boron carbide |
| KR101166723B1 (en) * | 2010-03-26 | 2012-07-19 | 한국세라믹기술원 | Manufacturing method of high density boroncarbide sintered body |
-
1999
- 1999-10-27 JP JP30487199A patent/JP2001122665A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7517491B2 (en) | 2003-06-12 | 2009-04-14 | Georgia Tech Research Corporation | Processes and methods of making boron carbide |
| US7592279B1 (en) | 2003-06-12 | 2009-09-22 | Georgia Tech Research Corporation | Boron carbide and boron carbide components |
| JP2008524108A (en) * | 2004-12-20 | 2008-07-10 | ジョージア・テック・リサーチ・コーポレーション | B4C with improved density and hardness after pressureless sintering and post-HIP |
| US8377369B2 (en) | 2004-12-20 | 2013-02-19 | Georgia Tech Research Corporation | Density and hardness pressureless sintered and post-HIPed B4C |
| JP2008535769A (en) * | 2005-04-11 | 2008-09-04 | ジョージア・テック・リサーチ・コーポレーション | Boron carbide component and method for producing the same |
| KR101166723B1 (en) * | 2010-03-26 | 2012-07-19 | 한국세라믹기술원 | Manufacturing method of high density boroncarbide sintered body |
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