JPS63282165A - Powder mixture containing zirconium oxide and boride and production of composite sintered body containing said powder - Google Patents
Powder mixture containing zirconium oxide and boride and production of composite sintered body containing said powderInfo
- Publication number
- JPS63282165A JPS63282165A JP62114156A JP11415687A JPS63282165A JP S63282165 A JPS63282165 A JP S63282165A JP 62114156 A JP62114156 A JP 62114156A JP 11415687 A JP11415687 A JP 11415687A JP S63282165 A JPS63282165 A JP S63282165A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- zirconium oxide
- oxide
- boride
- sintered body
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims description 41
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 239000000203 mixture Substances 0.000 title abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000002485 combustion reaction Methods 0.000 claims abstract description 8
- 229910052796 boron Inorganic materials 0.000 claims abstract description 7
- 239000011812 mixed powder Substances 0.000 claims description 21
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims 2
- 229910026551 ZrC Inorganic materials 0.000 claims 1
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 abstract description 14
- 229910033181 TiB2 Inorganic materials 0.000 abstract description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 230000002250 progressing effect Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 45
- 238000002441 X-ray diffraction Methods 0.000 description 11
- 239000007858 starting material Substances 0.000 description 11
- 239000004408 titanium dioxide Substances 0.000 description 6
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229920006311 Urethane elastomer Polymers 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- -1 - Titanium boride Chemical compound 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 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
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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ホウ化物よりなる混合粉末及び
それらを含む複合焼結体９製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a mixed powder of zirconium oxide and boride used as a raw material for cemented carbide tools and high-temperature structural materials, and a method for producing a composite sintered body 9 containing the same. .
従来の技術
従来、酸化ジルコニウムとホウ化物を含む複合焼結体は
、まず金属またはその酸化物にホウ素粉末を混合し、高
温で反応させることによって合成したホウ化物粉末と酸
化ジルコニウム粉末を十分に混合し、その混合粉末を成
形後、高温高圧下で焼結することによって製造していた
。Conventional technology Conventionally, composite sintered bodies containing zirconium oxide and boride have been produced by first mixing boron powder with metal or its oxide, and then reacting at high temperature to thoroughly mix boride powder and zirconium oxide powder. It was manufactured by molding the mixed powder and then sintering it under high temperature and high pressure.
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
入しやすり、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 (and complex) manufacturing process, which can easily introduce impurities and consumes a large amount of energy.
問題点を解決するための手段
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０／（反応後にはホウ化物になる）ホウ素
とを含む混合物の成形体を作製し、その成形体の一部を
強熱点火して燃焼反応を起こさせ、この化学反応によっ
てホウ化物と酸化ジルコニウムの粒子を合成する。Means for solving the problem A molded body of a mixture containing zirconium metal powder (becomes zirconium oxide after reaction) and boron oxide/boron (becomes boride after reaction) is prepared, and one of the molded bodies is This chemical reaction synthesizes particles of boride and zirconium oxide.
また、加圧下で上記工程を行うことにより、発生する化
学反応熱を利用して合成同時焼結を行う。Further, by performing the above steps under pressure, simultaneous synthesis and sintering is performed using the generated chemical reaction heat.
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
ジルコニウムとホウ化物よりなる混合粉末が容易に得ら
れる。また、加圧下で成形体に点火することによって酸
化ジルコニウムとホウ化物を含む複合焼結体が容易に得
られる。したがって従来のホウ化物と酸化ジルコニウム
の粉末を用いて作成する混合粉末及び複合焼結体の製造
方法と比較してきわめて省エネルギーである。According to the present invention, a mixed powder of high purity zirconium oxide and boride can be easily obtained by simply igniting a compact. Moreover, a composite sintered body containing zirconium oxide and a boride can be easily obtained by igniting the molded body under pressure. Therefore, compared to conventional methods for producing mixed powders and composite sintered bodies using powders of boride and zirconium oxide, this method is extremely energy-saving.
実施例
実施例１
出発原料として粒径１０μ輪以下のジルコニウム粉末、
平均粒径１μｍの二酸化チタン（ＴｉＯｚ）粉末、それ
に粒径が１５μｍ以下の結晶質のホウ素粉末を用い、そ
れらを１：１：２のモル比で混合後、直径２０ｍｍ 、
高さ２０ｍｍの柱状にプレス成形した。成形体への着火
は、試料下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・アルゴン雰囲
気下で、着火用ヒーターに通電して反応を開始させた。Examples Example 1 Zirconium powder with a particle size of 10 μm or less as a starting material,
Using titanium dioxide (TiOz) powder with an average particle size of 1 μm and crystalline boron powder with a particle size of 15 μm or less, after mixing them at a molar ratio of 1:1:2, a diameter of 20 mm,
It was press-molded into a columnar shape with a height of 20 mm. The molded body was ignited by energizing a tungsten filament provided at the bottom of the sample. The molded body was heated to an ignition heater at room temperature under an argon atmosphere to start a reaction.
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ニホウ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０．１〜０．３μＩであり、出発原料の
粒径よりも小さくなっていた。After the obtained porous body was pulverized using a ball mill, it was identified by X-ray diffraction, and only the diffraction lines of titanium diboride and zirconium oxide were observed. The particle size of the obtained mixed powder was 0.1 to 0.3 μI, which was smaller than the particle size of the starting raw 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＋ＴｉＯ２＋２ Ｂ−”ＺｒＯ＊ ＋ＴｉＢｚこ
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 ｉ Ｏ２の還元を基本にして、還元されたＴｉ
金属（融解して液体になっているものと思われる）がＢ
と反応してＴｉＢ２になるのである。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（２０
００℃程度まで上昇する）になりＺｒＯ２とＴ ｉ Ｂ
２からなる混合粉末が得られるのである。Zr+TiO2+2 B-"ZrO* +TiBzAs can be seen from this chemical reaction formula, this reaction is based on the reduction of T i O2 by Zr metal, and the reduced Ti
The metal (which is thought to have melted into a liquid) is B
It reacts with TiB2. The heat of reaction at this time is large, so the sample can reach a high temperature (20
00℃), and ZrO2 and T i B
A mixed powder consisting of 2 is obtained.
実施例２
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とマグネシウムの
合金粉末と、平均粒径１μｍの二酸化チタン（ＴｉＯ２
）それに粒径が１５μ曙以下の結晶質のホウ素粉末を用
い、本実施例ではさらに平均粒径０．５μＩの５ｍｏ１
％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２：１．９５ ： ３．９ ： 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
ころニホウ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。Example 2 As starting materials, an alloy powder of zirconium and magnesium containing 5 mo1% of magnesium with a particle size of 325 mesh or less, and titanium dioxide (TiO2) with an average particle size of 1 μm were used.
) A crystalline boron powder with a particle size of 15 μl or less was used, and in this example, 5 mol of boron powder with an average particle size of 0.5 μl was used.
% magnesium stabilized zirconium oxide powder was added. They are 2:1.95:3.9:0.
After mixing at a molar ratio of 1:1, 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 titanium diboride and zirconium oxide were observed.
得られた混合粉末の粒径は、それぞれ０．１〜０．３μ
Ｉであり、出発原料の粒径よりも小さくなっていた。The particle size of the obtained mixed powder is 0.1 to 0.3μ, respectively.
I, and the particle size was smaller than that of the starting material.
実施例３
出発原料として、粒径１０μｌ以下のジルコニウム粉末
、平均粒径３μｍの三酸化二チタン（Ｔｉ２０２）それ
に粒径が１５μｍ以下の結晶質のホウ素粉末を用い、そ
れらを３ ： ２．０７５ ： ８．３のモル比で秤量
し、さらにジルコニウムに対して５ｗｏ１％のイツトリ
ウムを添加して混合後、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２００℃に加熱た状態で点
火した。得られた混合粉末をＸ線回折を用いて同定した
ところニホウ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
０．１〜０゜５μｍ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 with a particle size of 10 μl or less, dititanium trioxide (Ti202) with an average particle size of 3 μm, and crystalline boron powder with a particle size of 15 μm or less were used, and they were mixed in a ratio of 3:2.075: The mixture was weighed at a molar ratio of 8.3, and further, yttrium was added in an amount of 5w1% to zirconium, mixed, and then treated in the same process as in Example 1. However, in this example, ignition was carried out in a state where it was heated to 200°C. When the obtained mixed powder was identified using X-ray diffraction, only the diffraction lines of titanium diboride and zirconium oxide were observed. The particle size of the obtained mixed powders was 0.1 to 0.5 μm, which was smaller than the particle size of the starting raw materials.
実施例４
出発原料として粒径１０μ−以下のジルコニウム粉末、
粒径ｌθμＩ以下のアルミニウム粉末、平均粒径１μｍ
の二酸化チタン（ＴｉＯ２）粉末、それに粒径が１５μ
ｍ以下の結晶質のホウ素粉末を用い、それらを０．２
： １．６ ： １．４ ： ２．８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。得られた多孔
体を粉砕した後、Ｘ線回折を用いて同定したところニホ
ウ化チタンと酸化ジルコニウム、酸化アルミニウムの回
折線しか見られなかった。Example 4 Zirconium powder with a particle size of 10μ or less as a starting material,
Aluminum powder with particle size lθμI or less, average particle size 1μm
titanium dioxide (TiO2) powder with a particle size of 15μ
Using crystalline boron powder of less than 0.2
After mixing at a molar ratio of : 1.6 : 1.4 : 2.8, the same process as in Example 1 was performed. After the obtained porous body was crushed, it was identified using X-ray diffraction, and only the diffraction lines of titanium diboride, zirconium oxide, and aluminum oxide were observed.
得られた混合粉末の粒径は、それぞれ０．１〜０．２μ
ｍであり、出発原料の粒径よりも非常に小さくなってい
た。The particle size of the obtained mixed powder is 0.1 to 0.2μ, respectively.
m, which was much smaller than the particle size of the starting material.
実施例５
出発原料として粒径１０μｍ以下のジルコニウム粉末、
粒径１０μｍ以下のアルミニウム粉末、平均粒径３μｍ
の三酸化二チタン（ＴｉｓＯ３）粉末、それに粒径が１
５μｍ以下の結晶質のホウ素粉末を用い、それらを０．
６ ： ０．８ ： ０，８ ： ３．２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２００℃に加熱した状態で成形体に点火した
。得られた多孔体を粉砕した後、Ｘ線回折を用いて同定
したところニホウ化チタンと酸化ジルコニウム、酸化ア
ルミ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０．２〜０．５μｍであり、出
発原料の粒径よりも小さくなっていた。Example 5 Zirconium powder with a particle size of 10 μm or less as a starting material,
Aluminum powder with a particle size of 10 μm or less, average particle size of 3 μm
dititanium trioxide (TisO3) powder with a particle size of 1
Crystalline boron powder with a size of 5 μm or less is used and
After mixing at a molar ratio of 6:0.8:0 and 8:3.2, the same process as in Example 1 was performed. However, in this example, the molded body was ignited while being heated to 200°C. After the obtained porous body was crushed, it was identified using X-ray diffraction, and only the diffraction lines of titanium diboride, zirconium oxide, and aluminum oxide were observed. The particle size of the obtained mixed powder was 0.2 to 0.5 μm, which was smaller than the particle size of the starting raw material.
実施例６
出発原料として粒径１０μｍ以下のジルコニウム粉末、
平均粒径１μＩの二酸化チタン（Ｔｉｅｓ）粉末、それ
に粒径が１５μｍ以下の結晶質のホウ素粉末を用い、そ
れらを１：１：２のモル比で混合後、直径１０１１高さ
１０ＩＩＩＩ１１の柱状にプレス成形した。この成形体
を炭化ケイ素製の型材に入れて、ウレタンゴム製の弾性
体を備えた一軸加圧真空ホットプレスを用いて合成同時
焼結を行った。成形体への着火は、試料下部に設けたタ
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・アルゴン雰囲気・５０ＭＰａの圧力条
件下で、着火用ヒーターに通電して反応を開始させた。Example 6 Zirconium powder with a particle size of 10 μm or less as a starting material,
Using titanium dioxide (Ties) powder with an average particle size of 1 μI and crystalline boron powder with a particle size of 15 μm or less, they were mixed at a molar ratio of 1:1:2 and then pressed into a columnar shape with a diameter of 1011 and a height of 10III11. Molded. This molded body was placed in a mold made of silicon carbide, and simultaneously synthesized and sintered using a uniaxial pressure vacuum hot press equipped with an elastic body made of urethane rubber. The molded body was ignited by energizing a tungsten filament provided at the bottom of the sample. The reaction was started by applying electricity to the ignition heater under the conditions of room temperature, argon atmosphere, and 50 MPa pressure.
得られた焼結体をＸ線回折で同定したところニホウ化チ
タンと正方晶と単斜晶の酸化ジルコニウムの回折線しか
見られなかった。このＸ線回折図形から正方晶と単斜晶
の酸化ジルコニウムの割合がほぼ１：１であった。また
、この焼結体の相対密度は９７％であった。When the obtained sintered body was identified by X-ray diffraction, only the diffraction lines of titanium diboride and tetragonal and monoclinic zirconium oxides were observed. From this X-ray diffraction pattern, the ratio of tetragonal and monoclinic zirconium oxides was approximately 1:1. Moreover, the relative density of this sintered body was 97%.
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＋ＴｉＯ２＋２Ｂ−＋ＺｒＯ２＋ＴｉＢ ２この化
学反応式かられかるようにこの反応は、Ｚｒ金属による
ＴｉＯ２の還元を基本にして、還元されたＴｉ金属（融
解して液体になっているものと思われる）がＢと反応し
てＴｉＢ ２になるのである。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、しかもウレタンゴム製の弾
性体を介して加圧しているので、合成したＺ ｒ ０２
粒子と、Ｔｉ８２粒子が焼結してＺｒＯ２とＴｉＢ ２
からなる複合焼結体が得られるのである。Zr+TiO2+2B-+ZrO2+TiB 2As can be seen from this chemical reaction formula, this reaction is based on the reduction of TiO2 by Zr metal, and the reduced Ti metal (which is thought to be melted and turned into a liquid) becomes B. It reacts to become TiB2. The heat of reaction at this time is large, so the sample can reach a high temperature (2000℃) without external heating.
Moreover, since the pressure is applied through an elastic body made of urethane rubber, the synthesized Z r 02
particles and Ti82 particles are sintered to form ZrO2 and TiB2
A composite sintered body consisting of
実施例７
出発原料として、粒径ｌＯμＩ以下のジルコニウム粉末
、平均粒径３μｍの三酸化二チタン（Ｔｉ２０３、）粉
末それに粒径が１５μｍ以下の結晶質のホウ素粉末を用
い、それらを３：２：８のモル比で混合後、実施例６と
同様のプロセスで処理した。Example 7 As starting materials, zirconium powder with a particle size of lOμI or less, dititanium trioxide (Ti203,) powder with an average particle size of 3 μm, and crystalline boron powder with a particle size of 15 μm or less were used, and they were mixed in a ratio of 3:2: After mixing at a molar ratio of 8, the same process as in Example 6 was carried out.
但し、本実施例では２００℃まで加熱して反応を開始さ
せた。得られた焼結体をＸ線回折で同定したところニホ
ウ化チタンと正方晶と単斜晶の酸化ジルコニウムの回折
線しか見られなかつた。このＸ線回折図形から正方晶と
単斜晶の酸化ジルコニウムの割合がほぼ１：１であった
。また、この焼結体の相対密度は９８．７％であった。However, in this example, the reaction was started by heating to 200°C. When the obtained sintered body was identified by X-ray diffraction, only the diffraction lines of titanium diboride and tetragonal and monoclinic zirconium oxides were observed. From this X-ray diffraction pattern, the ratio of tetragonal and monoclinic zirconium oxides was approximately 1:1. Moreover, the relative density of this sintered body was 98.7%.
実施例８
出発原料として、粒径３２５メツシユ以下のマグネシウ
ム５ｍｏ１％含有したジルコニウムとマグネシウムの合
金粉末と、平均粒径１μｍの二酸化チタン（Ｔｉ０２）
それに粒径が１５μｍ以下の結晶質のホウ素粉末を用い
、本実施例ではさらに平均粒径０．５μｍの５ｍｏ１％
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２：１．９５ ： １．９５ ： ０．
１のモル比で混合後、実施例６と同様のプロセスで処理
した。得られた焼結体をＸ線回折で同定したところニホ
ウ化チタン、−ホウ化チタン、チタンそれに酸化ジルコ
ニウムの回折線しか見られなかった。また、この焼結体
の相対密度は９９．５％であった。Example 8 As starting materials, zirconium and magnesium alloy powder containing 5 mo1% of magnesium with a particle size of 325 mesh or less, and titanium dioxide (Ti02) with an average particle size of 1 μm.
Crystalline boron powder with a particle size of 15 μm or less is used for this, and in this example, 5mol% with an average particle size of 0.5 μm is used.
of magnesium-stabilized zirconium oxide powder was added. They are 2:1.95:1.95:0.
After mixing at a molar ratio of 1, the same process as in Example 6 was carried out. When the obtained sintered body was identified by X-ray diffraction, only the diffraction lines of titanium diboride, titanium -boride, titanium, and zirconium oxide were observed. Moreover, the relative density of this sintered body was 99.5%.
実施例９
出発原料として粒径１０μｍ以下のジルコニウム粉末、
粒径１０μｍ以下のアルミニウム粉末、平均粒径０．７
μｍの二酸化チタン（ＴｉＯ２）粉末、それに粒径が１
５μＩ以下の結晶質のホウ素粉末を用い、それらを０．
８ ： ０．４ ： １．１ ： １．１のモル比で混
合後、実施例６と同様のプロセスで処理した。得られた
焼結体をＸ線回折で同定したところニホウ化チタン、−
ホウ化チタン、チタンそれに酸化ジルコニウム（はぼ９
０％が正方晶系であり、残りは単斜晶系）の回折線しか
見られなかった。また、この焼結体の相対密度は９９．
７％であった。Example 9 Zirconium powder with a particle size of 10 μm or less as a starting material,
Aluminum powder with a particle size of 10 μm or less, average particle size of 0.7
μm titanium dioxide (TiO2) powder, and particle size 1
Using crystalline boron powder of 5 μI or less, they were heated to 0.
After mixing at a molar ratio of 8:0.4:1.1:1.1, the same process as in Example 6 was performed. The obtained sintered body was identified by X-ray diffraction as titanium diboride, -
Titanium boride, titanium and zirconium oxide (Habo9
Only diffraction lines of 0% were tetragonal and the rest were monoclinic were observed. Moreover, the relative density of this sintered body is 99.
It was 7%.
発明の効果
本発明の製造方法によれば、ジルコニウム金属粉末と酸
化物粉末とホウ素を含む混合物からなる成形体を作製し
、そ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ホウ化物を含む混合粉末が得
られる。また、この成形体に圧力をかけた状態で点火す
ると、酸化ジルコニウムとホウ化物の合成同時焼結が起
こり、酸化ジルコニウムとホウ化物を含む複合焼結体が
得られる。Effects of the Invention According to the manufacturing method of the present invention, a molded body made of a mixture containing zirconium metal powder, oxide powder, and boron is produced, and a part of the molded body is ignited to cause a combustion reaction. A mixed powder containing zirconium oxide and boride is obtained. Moreover, when this molded body is ignited under pressure, zirconium oxide and boride are simultaneously synthesized and sintered, and a composite sintered body containing zirconium oxide and boride is obtained.
従って、本発明の製造方法によれば、従来の酸化ジルコ
ニウムとホウ化物の混合粉末を製造したり・その混合粉
末を用いて複合焼結体を製造する方法に比較して、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
ギー酸化ジルコニウムとホウ化物を含む混合粉末や複合
焼結体が作製できる。Therefore, the manufacturing method of the present invention requires a much lower temperature process than the conventional method of manufacturing a mixed powder of zirconium oxide and boride or manufacturing a composite sintered body using the mixed powder. In other words, it is possible to produce mixed powders and composite sintered bodies containing extremely low energy zirconium oxide and boride.
Claims (10)
素とを含む成形体を作製し、その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
化物粉末それにホウ素との反応を、燃焼過程の結果発生
する熱によって進行させる酸化ジルコニウムとホウ化物
を含む混合粉末の製造方法。(1) A molded body containing at least zirconium powder, oxide powder, and boron is produced, a part of the molded body is ignited to start the combustion process, and the subsequent reaction with the zirconium powder, oxide powder, and boron is performed. A method for producing a mixed powder containing zirconium oxide and boride, in which the process proceeds with heat generated as a result of a combustion process.
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
ジルコニウムとホウ化物を含む混合粉末の製造方法。(2) A method for producing a mixed powder containing zirconium oxide and a boride according to claim 1, characterized in that the compact is ignited under heating conditions to initiate a combustion process.
１項記載の酸化ジルコニウムとホウ化物を含む混合粉末
の製造方法。(3) The method for producing a mixed powder containing zirconium oxide and a boride according to claim 1, wherein the oxide powder is titanium oxide.
する特許請求の範囲第１項記載の酸化ジルコニウムとホ
ウ化物を含む混合粉末の製造方法。(4) A method for producing a mixed powder containing zirconium oxide and a boride according to claim 1, wherein the compact contains a stabilizing element for zirconium oxide.
の範囲第１項記載の酸化ジルコニウムとホウ化物を含む
混合粉末の製造方法。(5) A method for producing a mixed powder containing zirconium oxide and a boride according to claim 1, which comprises mixing aluminum powder into a compact.
素とを含む成形体を作製し、加圧条件下で、その成形体
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それにホウ素との反応及び生成
した酸化ジルコニウムと炭化物の焼結を、燃焼過程の結
果発生する熱によって進行させる酸化ジルコニウムとホ
ウ化物を含む複合焼結体の製造方法。(6) A molded body containing at least zirconium powder, oxide powder, and boron is produced, a part of the molded body is ignited under pressurized conditions to start the combustion process, and the zirconium powder and oxide are then ignited. A method for producing a composite sintered body containing zirconium oxide and boride, in which the reaction between the powder and boron and the sintering of the generated zirconium oxide and carbide are progressed by heat generated as a result of the combustion process.
開始させることを特徴とする特許請求の範囲第６項記載
の酸化ジルコニウムとホウ化物を含む複合焼結体の製造
方法。(7) A method for producing a composite sintered body containing zirconium oxide and a boride according to claim 6, characterized in that the compact is ignited under heated and pressurized conditions to initiate a combustion process.
６項記載の酸化ジルコニウムとホウ化物を含む複合焼結
体の製造方法。(8) The method for producing a composite sintered body containing zirconium oxide and boride according to claim 6, wherein the oxide powder is titanium oxide.
する特許請求の範囲第６項記載の酸化ジルコニウムとホ
ウ化物を含む複合焼結体の製造方法。(9) A method for producing a composite sintered body containing zirconium oxide and a boride according to claim 6, wherein the compact contains a stabilizing element of zirconium oxide.
求の範囲第６項記載の酸化ジルコニウムとホウ化物を含
む複合焼結体の製造方法。(10) A method for producing a composite sintered body containing zirconium oxide and a boride according to claim 6, wherein aluminum powder is mixed into the compact.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62114156A JPS63282165A (en) | 1987-05-11 | 1987-05-11 | Powder mixture containing zirconium oxide and boride and production of composite sintered body containing said powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62114156A JPS63282165A (en) | 1987-05-11 | 1987-05-11 | Powder mixture containing zirconium oxide and boride and production of composite sintered body containing said powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63282165A true JPS63282165A (en) | 1988-11-18 |
Family
ID=14630552
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62114156A Pending JPS63282165A (en) | 1987-05-11 | 1987-05-11 | Powder mixture containing zirconium oxide and boride and production of composite sintered body containing said powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63282165A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2006038406A1 (en) * | 2004-10-07 | 2008-05-15 | 日鉱金属株式会社 | High purity ZrB2 powder and method for producing the same |
-
1987
- 1987-05-11 JP JP62114156A patent/JPS63282165A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2006038406A1 (en) * | 2004-10-07 | 2008-05-15 | 日鉱金属株式会社 | High purity ZrB2 powder and method for producing the same |
| JP2011088819A (en) * | 2004-10-07 | 2011-05-06 | Jx Nippon Mining & Metals Corp | HIGH PURITY ZrB2 POWDER AND METHOD FOR PRODUCING THE SAME |
| JP4685023B2 (en) * | 2004-10-07 | 2011-05-18 | Ｊｘ日鉱日石金属株式会社 | High purity ZrB2 powder and method for producing the same |
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