JPH0225865B2 - - Google Patents
Info
- Publication number
- JPH0225865B2 JPH0225865B2 JP58036301A JP3630183A JPH0225865B2 JP H0225865 B2 JPH0225865 B2 JP H0225865B2 JP 58036301 A JP58036301 A JP 58036301A JP 3630183 A JP3630183 A JP 3630183A JP H0225865 B2 JPH0225865 B2 JP H0225865B2
- Authority
- JP
- Japan
- Prior art keywords
- boron carbide
- sintered body
- weight
- temperature
- sintering
- 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
- 238000005245 sintering Methods 0.000 claims description 12
- 229910052580 B4C Inorganic materials 0.000 claims description 11
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 description 5
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
本発明は高密度かつ高強度なB4C焼結体および
その製造方法に関するものである。
炭化硼素はダイヤモンドに次ぐ高硬度材料でし
かも密度が小さく化学的安定性の特徴を有してお
り、その用途として、ノズル、シールリング、ド
レツサー研磨材、強酸取扱い用機器部品などがあ
るが、一方高融点で焼結が困難であり、単に炭化
硼素粉末を融点近くの温度で焼結しても満足な焼
結体は得られない。そこで、従来炭化硼素粉末に
金属を添加し焼結する方法により曲げ強さ60Kg/
mm2以上の焼結体が得られていたが、炭化硼素を
金属で結合しているため高温域での強度また耐摩
耗性に対して著しく劣るという欠点があつた。ま
た金属結合による焼結でなく、炭化硼素の焼結法
として黒鉛型を使用し2100℃以上の温度で加圧焼
結するホツトプレス法にて焼結がなされている
が、この方法は炭化硼素に何ら添加剤を加えるこ
となく焼結可能なので、得られる炭化硼素成形体
は炭化硼素の優れた特性をそのまま有している
が、焼結温度が2000℃を越し、黒鉛型の損耗や装
置の損傷が大きく製造コストが高く、また結晶粒
子の成長が生じ結晶粗大化となり、曲げ強さも約
50Kg/mm2と低く、また衝撃強度も低いためその
用途も限られていた。
本発明では上記欠点を解消し高密度、高強度な
B4C焼結体およびその製造方法を提供せんとする
ものであり、その要旨は窒化珪素1〜10重量%、
残部炭化硼素からなり、その相対理論密度が98.5
%以上で結晶粒度が10μm以下の焼結体および窒
化珪素1〜10重量%、残部炭化硼素からなる原料
粉末をホツトプレス焼結することを特徴とする焼
結体の製造方法である。この場合の焼結温度は
1900〜1950℃が好ましいものである。本発明にし
たがえば焼結が困難であるとされるB4Cを理論密
度の98.5%以上の密度を持つ焼結体にすることが
できる。以下本願発明を開発するに至つた実施例
について述べる。
実施例 1
純度99.5%、平均粒子径3μmのB4C粉末と純度
99.5%平均粒子径5μmのSi3N4粉末を第1表記載
の割合で各種配合したものをボールミル混合機に
より10時間湿式混合粉砕を行つた後、これを充分
に乾燥して焼結用原料とし、50×50(mm)角、高
さ60mmの黒鉛型内に上記各種焼結用原料を充填す
ると共に高周波コイルに挿入し、1850〜2000℃の
温度範囲内で各所定温度にて200Kg/cm2の圧力を
加え60分間保持し次いで圧力を抜いて放冷するこ
とにより50×50×5.5(mm)の目的の焼結体を得
た。各々の焼結体をダイヤモンド砥石で切断後研
削して各4個の3×4×36(mm)の試験片を作成
し、各種試験をして得られた測定値を同じく第1
表に示す。
The present invention relates to a high-density and high-strength B 4 C sintered body and a method for manufacturing the same. Boron carbide is a hard material second only to diamond, and has a low density and chemical stability.Its uses include nozzles, seal rings, dresser abrasives, and equipment parts for handling strong acids. Sintering is difficult due to its high melting point, and a satisfactory sintered body cannot be obtained simply by sintering boron carbide powder at a temperature close to its melting point. Therefore, the conventional method of adding metal to boron carbide powder and sintering it has a bending strength of 60 kg/
A sintered body with a size of mm 2 or more was obtained, but because the boron carbide was bonded with metal, it had the disadvantage of being significantly inferior in strength and wear resistance in high temperature ranges. In addition, instead of sintering by metal bonding, boron carbide is sintered by the hot press method, which uses a graphite mold and sinters under pressure at a temperature of 2100°C or higher. Since sintering is possible without adding any additives, the resulting boron carbide compact retains the excellent properties of boron carbide, but the sintering temperature exceeds 2000℃, causing wear and tear on the graphite mold and damage to equipment. The manufacturing cost is high, and the crystal grains grow, resulting in coarse crystals, and the bending strength is approximately
Its use was limited due to its low impact strength of 50Kg/mm 2 and low impact strength. The present invention eliminates the above drawbacks and provides high density and high strength.
The purpose of the present invention is to provide a B 4 C sintered body and a method for manufacturing the same, and the gist thereof is to contain 1 to 10% by weight of silicon nitride,
The remainder consists of boron carbide, and its relative theoretical density is 98.5.
% or more and a grain size of 10 μm or less, and a raw material powder consisting of 1 to 10% by weight of silicon nitride and the balance boron carbide is hot-press sintered. The sintering temperature in this case is
A temperature of 1900 to 1950°C is preferred. According to the present invention, B 4 C, which is considered difficult to sinter, can be made into a sintered body having a density of 98.5% or more of the theoretical density. Examples that led to the development of the present invention will be described below. Example 1 B 4 C powder with purity of 99.5% and average particle size of 3 μm and purity
A mixture of various Si 3 N 4 powders with a 99.5% average particle size of 5 μm in the proportions listed in Table 1 was wet mixed and pulverized using a ball mill mixer for 10 hours, and then thoroughly dried to obtain a raw material for sintering. Fill a 50 x 50 (mm) square graphite mold with a height of 60 mm with the various sintering materials mentioned above, insert it into a high-frequency coil, and produce 200 kg/kg at each predetermined temperature within the temperature range of 1850 to 2000°C. A pressure of cm 2 was applied and maintained for 60 minutes, then the pressure was released and the mixture was allowed to cool to obtain a desired sintered body measuring 50×50×5.5 (mm). Each sintered body was cut and ground with a diamond grindstone to create four 3 x 4 x 36 (mm) test pieces, and the measured values obtained from various tests were also used for the first
Shown in the table.
【表】
なお、上記第1表中の試料No.1の試験片につい
て2100℃、200Kg/cm2、60分間の条件で焼結した
ものについて対理論密度、粒度、シヤルピー衝撃
値を測定した結果は、対理論密度97.2%、粒度
40μm、シヤルピー衝撃値0.06Kg・m/cm2であつ
た。
実施例 2
実施例1で1950℃の温度で焼結した試料を10×
10×5(mm)の板にダイヤモンド砥石で切断し、
No.200のダイヤモンド砥石で表面研削を行い10×
10(mm)面を内径8mmのノズルを有するサンドブ
ラスト機にて空気圧5Kg/cm2で砥粒(メテコライ
トC、No.40)を噴射距離50mmで噴射させ、重量減
を測定した。その結果を第2表に示す。[Table] The results of measuring the theoretical density, particle size, and Charpy impact value of the test piece of sample No. 1 in Table 1 above, which was sintered at 2100°C, 200Kg/cm 2 , and for 60 minutes. is the theoretical density 97.2%, particle size
The diameter was 40 μm, and the Shalpy impact value was 0.06 Kg·m/cm 2 . Example 2 The sample sintered at a temperature of 1950°C in Example 1 was
Cut into a 10 x 5 (mm) plate with a diamond grindstone,
Surface grinding is done with a No. 200 diamond whetstone to 10×
Abrasive grains (Metecolite C, No. 40) were sprayed at a spray distance of 50 mm at an air pressure of 5 Kg/cm 2 on a 10 (mm) surface using a sandblasting machine having a nozzle with an inner diameter of 8 mm, and the weight loss was measured. The results are shown in Table 2.
【表】
以上の実施例結果から次の事が判る。即ちB4C
粉末にSi3N4粉末を添加して焼結したものは無添
加のものに比べて焼結性が向上しており、1900℃
と比較的低温での焼結にもかかわらず相当高い値
を示している。つまり試料No.1のものでは2000℃
で焼結したものでさえまだ焼結不良だつたので更
に温度を2100℃まで高め焼結したが、それでも上
述の様に本願方法のものよりシヤルピー衝撃値の
点で著しく低い値となつている。一方Si3N4を添
加したものでもSi3N4添加量0.5重量%のものはホ
ツトプレス温度1850〜2000℃においても充分焼結
しておらないところから、1重量%以上は必要で
ある。また、逆に12重量%以上になるとシヤルピ
ー衝撃値が0.15Kg・m/cm2以上のものが得られず
靭性が無くなる。これらのことよりSi3N4添加量
は1〜10重量%が好ましい。
以上述べて来た様に本願発明に係る焼結体は緻
密かつ微細な結晶構造を有したものであり、ノズ
ル、シールリング、ドレツサー研磨材、ジエツト
粉砕機のライナーなどとしての用途に対して満足
すべき強度を有する。[Table] From the results of the above examples, the following can be seen. i.e. B 4 C
Powders sintered with Si 3 N 4 powder added have improved sinterability compared to those without additives, and can be heated at 1900℃.
Despite sintering at a relatively low temperature, this value is quite high. In other words, for sample No. 1, the temperature was 2000℃.
Even those sintered using the method of the present invention were still poorly sintered, so the temperature was further increased to 2100°C for sintering, but as mentioned above, the Charpy impact value was significantly lower than that of the method of the present invention. On the other hand, even when Si 3 N 4 is added, a Si 3 N 4 addition amount of 0.5% by weight is not sufficiently sintered even at a hot press temperature of 1850 to 2000°C, so 1% by weight or more is required. On the other hand, if it exceeds 12% by weight, it will not be possible to obtain a Charpy impact value of 0.15 Kg·m/cm 2 or more and the toughness will be lost. For these reasons, the amount of Si 3 N 4 added is preferably 1 to 10% by weight. As described above, the sintered body according to the present invention has a dense and fine crystal structure, and is satisfactory for use as nozzles, seal rings, dresser abrasives, liners for jet crushers, etc. It has the required strength.
Claims (1)
りその相対理論密度が98.5%以上で、結晶粒度が
10μm以下の焼結体。 2 窒化珪素1〜10重量%、残部炭化硼素からな
る原料粉末をホツトプレス焼結することを特徴と
する焼結体の製造方法。[Scope of Claims] 1 Consisting of 1 to 10% by weight of silicon nitride and the remainder boron carbide, its relative theoretical density is 98.5% or more, and its crystal grain size is
Sintered body of 10μm or less. 2. A method for producing a sintered body, which comprises hot press sintering raw material powder consisting of 1 to 10% by weight of silicon nitride and the balance boron carbide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58036301A JPS59162180A (en) | 1983-03-04 | 1983-03-04 | Boron carbide sintered body having a dense and fine crystal structure and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58036301A JPS59162180A (en) | 1983-03-04 | 1983-03-04 | Boron carbide sintered body having a dense and fine crystal structure and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59162180A JPS59162180A (en) | 1984-09-13 |
| JPH0225865B2 true JPH0225865B2 (en) | 1990-06-06 |
Family
ID=12465991
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58036301A Granted JPS59162180A (en) | 1983-03-04 | 1983-03-04 | Boron carbide sintered body having a dense and fine crystal structure and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59162180A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1641727A4 (en) * | 2003-06-12 | 2009-04-01 | Georgia Tech Res Inst | METHOD AND DEVICE FOR PREPARING BORCARBIDE AND BORCARBIDE COMPONENTS |
| US8377369B2 (en) | 2004-12-20 | 2013-02-19 | Georgia Tech Research Corporation | Density and hardness pressureless sintered and post-HIPed B4C |
| EP1879630A2 (en) | 2005-04-11 | 2008-01-23 | Georgia Tech Research Corporation | Boron carbide component and methods for the manufacture thereof |
-
1983
- 1983-03-04 JP JP58036301A patent/JPS59162180A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59162180A (en) | 1984-09-13 |
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