JPS63156015A - Production of powdery mixture consisting of zirconium oxide and carbide - Google Patents
Production of powdery mixture consisting of zirconium oxide and carbideInfo
- Publication number
- JPS63156015A JPS63156015A JP61304197A JP30419786A JPS63156015A JP S63156015 A JPS63156015 A JP S63156015A JP 61304197 A JP61304197 A JP 61304197A JP 30419786 A JP30419786 A JP 30419786A JP S63156015 A JPS63156015 A JP S63156015A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- oxide
- particle size
- zirconium oxide
- carbide
- 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims description 22
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims description 21
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229910026551 ZrC Inorganic materials 0.000 title claims description 10
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 title claims description 10
- 239000000203 mixture Substances 0.000 title abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 238000002485 combustion reaction Methods 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract 2
- 230000000087 stabilizing effect Effects 0.000 claims abstract 2
- 239000011812 mixed powder Substances 0.000 claims description 18
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 23
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052721 tungsten Inorganic materials 0.000 abstract description 2
- 239000010937 tungsten Substances 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- -1 if necessary Chemical compound 0.000 abstract 2
- 238000000465 moulding Methods 0.000 abstract 2
- 239000006230 acetylene black Substances 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 239000007858 starting material Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 4
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010067 TiC2 Inorganic materials 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、超硬工具や高温構造材用の原料として用いら
れる酸化ジルコニウムと炭化物よりなる混合粉末の製造
方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing a mixed powder of zirconium oxide and carbide, which is used as a raw material for cemented carbide tools and high-temperature structural materials.
従来の技術
従来、酸化ジルコニウム−炭化物複合焼結体用の混合粉
末は、まず金属またはその酸化物に炭素粉末または固形
炭素を混合し、高温で反応させることによって合成した
炭化物粉末と酸化ジルコニウム粉末を十分に混合するこ
とによって製造していた。Conventional technology Conventionally, mixed powder for zirconium oxide-carbide composite sintered bodies has been prepared by mixing carbide powder and zirconium oxide powder, which are synthesized by first mixing metal or its oxide with carbon powder or solid carbon and reacting at high temperature. Manufactured by thorough mixing.
発明が解決しようとする問題点
この方法は、製造工程が長（複雑であるため不純物が混
入しやす＜、シかもエネルギー消費が非常に大きかった
。Problems to be Solved by the Invention This method requires a long manufacturing process (because it is complex, it is easy for impurities to be mixed in), and consumes a lot of energy.
問題点を解決するための手段
本発明の特徴は、ジルコニウム金属粉末（反応後には酸
化ジルコニウムとなる）と、酸化物（反応後には炭化物
になる）と、炭素とからなる混合物の成形体の一部を強
熱点火して燃焼反応を起こさせ、この化学反応によって
炭化物と酸化ジルコニウムの粒子を合成することにある
。Means for Solving the Problems The present invention is characterized by a molded body of a mixture of zirconium metal powder (which becomes zirconium oxide after reaction), oxide (which becomes carbide after reaction), and carbon. The purpose is to ignite the parts at high heat to cause a combustion reaction, and through this chemical reaction, synthesize carbide and zirconium oxide particles.
作用
本発明によれば、成形体に点火するだけで高純度の酸化
ジルコニウムと炭化物よりなる混合粉末が容易に得られ
る。したがって従来の炭化物と酸化ジルコニウムの粉末
を混合する製造方法と比較してきわめて省エネルギーで
あり、しかも得られる粉体もきわめて高純度である。According to the present invention, a mixed powder of high purity zirconium oxide and carbide can be easily obtained by simply igniting a compact. Therefore, compared to the conventional manufacturing method of mixing carbide and zirconium oxide powders, this method is extremely energy-saving, and the resulting powder is also extremely pure.
実施例
実施例１
出発原料として粒径１θμ■以下のジルコニウム粉末、
平均粒径１μｍの二酸化チタン（ＴｉＣ２）粉末、それ
にアセチレンを原料とするカーボンブラックを用い、そ
れらを１ ： １ ：０．９５のモル比で混合後、直径
２０ｇ＋ｏ＋ 、高さ２０ｍｍの柱状にプレス成形した
。成形体への着火は、試料上部に設けたタングステンフ
ィラメントに通電することによって行った。成形体を室
温・真空（Ｉｇａ＋Ｈｇ）雰囲気下で、着火用ヒーター
に通電して反応を開始させた。得られた多孔体をボール
ミルを用いて粉砕した後、Ｘ線回折で同定したところ炭
化チタンと酸化ジルコニウムの回折線しか見られなかっ
た。得られた混合粉末の粒径は、それぞれ０．２〜０．
３μｍであり、出発原料の粒径よりも小さくなっていた
。Examples Example 1 Zirconium powder with a particle size of 1θμ or less as a starting material,
Using titanium dioxide (TiC2) powder with an average particle size of 1 μm and carbon black made from acetylene, they were mixed at a molar ratio of 1:1:0.95, and then press-molded into a column with a diameter of 20g+o+ and a height of 20mm. did. The molded body was ignited by energizing a tungsten filament provided above the sample. The reaction was started by applying electricity to the ignition heater at room temperature and in a vacuum (Iga+Hg) atmosphere. After pulverizing the obtained porous body using a ball mill, it was identified by X-ray diffraction, and only the diffraction lines of titanium carbide and zirconium oxide were observed. The particle size of the obtained mixed powder is 0.2 to 0.0.
The particle size was 3 μm, which was smaller than the particle size of the starting material.
このプロセスの化学反応式は以下のようになる。The chemical reaction equation for this process is as follows.
Ｚｒ＋ＴｉＯｚ＋ｏ、９５ｃｍＺｒＯ２＋Ｔｉにの化学
反応式かられかるようにこの反応は、Ｚｒ金属によるＴ
ｉＯ２の還元を基本にして、還元されたＴｉ金ｇ（融解
して液体になっているものと思われる）がＣと反応して
ＴｉＣになるのである。As can be seen from the chemical reaction formula for Zr+TiOz+o, 95cmZrO2+Ti, this reaction
Based on the reduction of iO2, the reduced Ti gold (which is thought to have melted into a liquid) reacts with C to become TiC.
このときの反応熱が大きいので外部から加熱しなくても
試料が高温（２０００℃程度まで上昇する）になりＺｒ
Ｏ２とＴｉＣからなる混合粉末が得られるのである。Since the heat of reaction at this time is large, the sample reaches a high temperature (up to about 2000°C) even without external heating, and the Zr
A mixed powder consisting of O2 and TiC is obtained.
実施例２
出発原料として粒径１０μ■以下のジルコニウム粉末、
焼成非晶質二酸化ケイ素（ジオツギ製薬製カープレック
スＣ３−５）それにアセチレンを原料とするカーボンブ
ラックを用い、それらを１：１：２のモル比で混合後、
実施例１と同様のプロセスで処理した。但し、本実施例
では５００℃まで加熱して反応を開始させた。得られた
試料を、７００℃に加熱して余ったカーボンを除去した
後、Ｘ線回折を用いて同定したところ炭化ケイ素と酸化
ジルコニウムの回折線しか見られなかった。得られた混
合粉末の粒径は、それぞれ０．１〜０．５μ曽であり、
出発原料の粒径よりも小さくなっていた。Example 2 Zirconium powder with a particle size of 10μ or less as a starting material,
After mixing calcined amorphous silicon dioxide (Carplex C3-5 manufactured by Geotsugi Pharmaceutical) and carbon black made from acetylene at a molar ratio of 1:1:2,
The same process as in Example 1 was used. However, in this example, the reaction was started by heating to 500°C. The obtained sample was heated to 700° C. to remove excess carbon, and then identified using X-ray diffraction, and only diffraction lines of silicon carbide and zirconium oxide were observed. The particle size of the obtained mixed powder is 0.1 to 0.5μ, respectively,
The particle size was smaller than that of the starting material.
実施例３
出発原料として、粒径３２５メツシユ以下のマグネシウ
ムを５ｍｏ１％含有したジルコニウム粉末と、平均粒径
１μ■の五酸化ニオブ（Ｎｂ２０ｓ）それにアセチレン
を原料とするカーボンブラックを用い、本実施例ではさ
らに平均粒径０．５μｍのマグネシウムで安定化した酸
化ジルコニウム粉末を加えた、それらを１ ： ０．３
９ ： ０．７８ ； ０．１のモル比で混合後、実施
例１と同様のプロセスで処理した。得られた混合粉末を
Ｘ線回折を用いて同定したところ炭化ニオブと酸化ジル
コニウムの回折線しか見られなかった。得られた混合粉
末の粒径は、それぞれ０．２〜０．４μ−であり、出発
原料の粒径よりも小さくなっていた。Example 3 As starting materials, zirconium powder containing 5 mo1% of magnesium with a particle size of 325 mesh or less, niobium pentoxide (Nb20s) with an average particle size of 1 μm, and carbon black made from acetylene were used. Furthermore, zirconium oxide powder stabilized with magnesium with an average particle size of 0.5 μm was added, and the mixture was mixed in a ratio of 1:0.3.
After mixing at a molar ratio of 9:0.78;0.1, the same process as in Example 1 was performed. When the obtained mixed powder was identified using X-ray diffraction, only the diffraction lines of niobium carbide and zirconium oxide were observed. The particle size of the obtained mixed powders was 0.2 to 0.4 .mu.-, which was smaller than the particle size of the starting materials.
実施例４
出発原料として、粒径ｌＯμ霞以下のジルコニウム粉末
、平均粒径３μＩの三酸化二チタン（Ｔｉ２０３ ）そ
れにアセチレンを原料とするカーボンブラックを用い、
それらを３：２：３．９のモル比で混合後、実施例１と
同様のプロセスで処理した。得られた混合粉末をＸ線回
折を用いて同定したところ炭化チタンと酸化ジルコニウ
ムの回折線しか見られなかった。得られた混合粉末の粒
径は、それぞれ０．３〜０．５μｍであり、出発原料の
粒径よりも小さくなっていた。Example 4 As starting materials, zirconium powder with a particle size of 1Oμ or less, dititanium trioxide (Ti203) with an average particle size of 3μI, and carbon black made from acetylene were used.
After mixing them in a molar ratio of 3:2:3.9, they were treated in the same process as in Example 1. When the obtained mixed powder was identified using X-ray diffraction, only the diffraction lines of titanium carbide and zirconium oxide were observed. The particle size of the obtained mixed powder was 0.3 to 0.5 μm, which was smaller than the particle size of the starting raw material.
発明の効果
本発明の製造方法によれば、ジルコニウム粉末と酸化物
それに炭素とからなる混合物の成形体の一部に点火して
燃焼反応を起こさせるだけで酸化ジルコニウムと炭化物
からなる混合粉末が作製できる。従って、本発明の製造
方法によれば、従来の炭化物粉末と酸化物粉末を混合す
る製造方法に比較してはるかに低温のプロセスで、つま
り、きわめて小さなエネルギーで酸化ジルコニウムと炭
化物の混合粉末が作製できる。また、得られる混合粉末
は純度が高く、その粒径はいずれも０．１〜０．５μｍ
の範囲で分布していて、出発原料の粒径よりも小さくな
っている。したがって焼結体作製の原料粉末として非常
に適したものである。Effects of the Invention According to the manufacturing method of the present invention, a mixed powder of zirconium oxide and carbide can be produced by simply igniting a part of a compact of a mixture of zirconium powder, oxide, and carbon to cause a combustion reaction. can. Therefore, according to the production method of the present invention, a mixed powder of zirconium oxide and carbide can be produced using a much lower temperature process than the conventional production method of mixing carbide powder and oxide powder, that is, with extremely low energy. can. In addition, the obtained mixed powder has high purity, and its particle size is 0.1 to 0.5 μm.
The particle size is smaller than that of the starting material. Therefore, it is very suitable as a raw material powder for producing a sintered body.
Claims (5)
成形体の一部に点火して燃焼過程を開始させ、その後の
ジルコニウム粉末と酸化物粉末と炭素の反応を、燃焼過
程の結果発生する熱によって進行させることを特徴とす
る酸化ジルコニウムと炭化物よりなる混合粉末の製造方
法。(1) A part of the compact made of zirconium powder, oxide powder, and carbon is ignited to start the combustion process, and the subsequent reaction between the zirconium powder, oxide powder, and carbon is controlled by the heat generated as a result of the combustion process. 1. A method for producing a mixed powder of zirconium oxide and carbide, characterized in that the process proceeds by:
と炭素とからなる成形体に点火して燃焼過程を開始させ
ることを特徴とする特許請求の範囲第１項記載の酸化ジ
ルコニウムと炭化物よりなる混合粉末の製造方法。(2) From zirconium oxide and carbide according to claim 1, the compacted body made of zirconium powder, oxide powder, and carbon is ignited under heating conditions to start a combustion process. A method for producing a mixed powder.
ずれかである特許請求の範囲第１項記載の酸化ジルコニ
ウムと炭化物よりなる混合粉末の製造方法。(3) The method for producing a mixed powder of zirconium oxide and carbide according to claim 1, wherein the oxide powder is either titanium oxide or niobium oxide.
粉末、あるいは酸化物粉末を混合する特許請求の範囲第
１項記載の酸化ジルコニウムと炭化物よりなる混合粉末
の製造方法。(4) A method for producing a mixed powder of zirconium oxide and carbide according to claim 1, wherein a metal powder or oxide powder of a stabilizing element of zirconium oxide is mixed into the compact.
の範囲第１項記載の酸化ジルコニウムと炭化物よりなる
混合粉末の製造方法。(5) A method for producing a mixed powder of zirconium oxide and carbide according to claim 1, wherein zirconium oxide is mixed into a compact.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61304197A JPS63156015A (en) | 1986-12-19 | 1986-12-19 | Production of powdery mixture consisting of zirconium oxide and carbide |
| US07/041,810 US4902457A (en) | 1986-04-07 | 1987-04-07 | Method for manufacturing a porous material or a composite sintered product comprising zirconium oxide and a carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61304197A JPS63156015A (en) | 1986-12-19 | 1986-12-19 | Production of powdery mixture consisting of zirconium oxide and carbide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63156015A true JPS63156015A (en) | 1988-06-29 |
Family
ID=17930186
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61304197A Pending JPS63156015A (en) | 1986-04-07 | 1986-12-19 | Production of powdery mixture consisting of zirconium oxide and carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63156015A (en) |
-
1986
- 1986-12-19 JP JP61304197A patent/JPS63156015A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR920000783B1 (en) | Neodymium titanate and barium neodymium titanate processes for their preparation and thetr applications in ceramic compositions | |
| JPS63156015A (en) | Production of powdery mixture consisting of zirconium oxide and carbide | |
| RU2639244C1 (en) | Method of producing zirconium tungstate powder | |
| JPS62256767A (en) | Manufacture of composite sintered body comprising carbonitride and oxide | |
| JPS62235258A (en) | Manufacture of carbide oxide composite sintered body | |
| JP2747916B2 (en) | Potassium titanate long fiber and method for producing titania fiber using the same | |
| JPS63156069A (en) | Manufacture of mixed powder comprising zirconium oxide, aluminum oxide and carbide | |
| JPH0672048B2 (en) | Method for producing zirconium oxide-based composite sintered body | |
| JPH0672062B2 (en) | Method for producing composite sintered body composed of carbide and complex oxide | |
| JPS63282165A (en) | Powder mixture containing zirconium oxide and boride and production of composite sintered body containing said powder | |
| JPS62288166A (en) | Manufacture of tungsten carbide-oxide composite sintered body | |
| JPH0158131B2 (en) | ||
| JPS62288165A (en) | Manufacture of titanium carbide-oxide composite sintered body | |
| JPS63288960A (en) | Production of (pb, bi) (zr, ti)o3 | |
| JPS6317219A (en) | Production of ceramic powder | |
| JPH075369B2 (en) | Method for producing composite sintered body composed of carbide and two or more kinds of oxides | |
| JPS6221714A (en) | Production of high-purity stabilized zirconia powder | |
| JPS62256766A (en) | Manufacture of composite sintered body comprising nitride and oxide | |
| JPS62288164A (en) | Manufacture of vanadium carbide-oxide composite sintered body | |
| JPH0478580B2 (en) | ||
| JPS6278113A (en) | Production of stabilized zirconia powder | |
| JPS58204813A (en) | Preparation of powdery carbide and nitride of silicon | |
| JPS63147807A (en) | Production of silicon nitride having high content of alpha form | |
| JPS6186427A (en) | Preparation of low melting point glass | |
| JPH06166566A (en) | Production of fine powder of tetragonal zironia containing ceria as solid solution |