JPH11323401A - Titanium boride-dispersed hard material - Google Patents
Titanium boride-dispersed hard materialInfo
- Publication number
- JPH11323401A JPH11323401A JP10146542A JP14654298A JPH11323401A JP H11323401 A JPH11323401 A JP H11323401A JP 10146542 A JP10146542 A JP 10146542A JP 14654298 A JP14654298 A JP 14654298A JP H11323401 A JPH11323401 A JP H11323401A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- tib2
- composite material
- tib
- 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.)
- Granted
Links
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 39
- 239000010936 titanium Substances 0.000 title claims description 33
- 239000000463 material Substances 0.000 title claims description 30
- 239000000843 powder Substances 0.000 claims abstract description 59
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 11
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 7
- 150000003624 transition metals Chemical class 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 238000005551 mechanical alloying Methods 0.000 abstract description 22
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052796 boron Inorganic materials 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 230000002706 hydrostatic effect Effects 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 229910033181 TiB2 Inorganic materials 0.000 abstract 5
- 239000002994 raw material Substances 0.000 abstract 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000003825 pressing Methods 0.000 description 6
- 230000002194 synthesizing effect Effects 0.000 description 6
- 238000011109 contamination Methods 0.000 description 5
- 229910052786 argon Inorganic materials 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
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910000669 Chrome steel Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、チタン硼化物分散
硬質材料およびその製造方法に関する。さらに詳しく
は、本発明は、チタン硼化物を分散した硬質材料を合成
する際に、チタン硼化物の一部をＴｉ粉末およびＢ粉末
に置換して、これを機械的合金化法により微細分散し、
焼結時にＴｉＢ2 相を合成することにより、緻密な硬質
材料を製造する方法およびその製品に関する。The present invention relates to a titanium boride-dispersed hard material and a method for producing the same. More specifically, in the present invention, when synthesizing a hard material in which titanium boride is dispersed, a part of the titanium boride is replaced with Ti powder and B powder, which are finely dispersed by a mechanical alloying method. ,
The present invention relates to a method for producing a dense hard material by synthesizing a TiB 2 phase during sintering, and a product thereof.
【０００２】[0002]
【従来の技術】チタン硼化物を硬質粒子とする複合材料
は焼結性が悪く、従来、鉄系材料を結合相とする緻密な
チタン硼化物分散硬質材料を作製することは困難であっ
た。また、該材料の焼結には大きな加圧力と高温での焼
結が必要となり、チタン硼化物の粗大化が生じ、成形体
の特性が低下するという問題があった。2. Description of the Related Art Composite materials containing titanium boride as hard particles have poor sinterability, and it has been conventionally difficult to prepare a dense titanium boride-dispersed hard material having an iron-based material as a binder phase. Further, sintering of the material requires a large pressing force and sintering at a high temperature, and there is a problem that the titanium boride is coarsened and the properties of the molded body are deteriorated.
【０００３】また、硬質粒子であるチタン硼化物と金属
粉末を機械的合金化処理すると、機械的合金化処理用の
容器や粉砕球からのコンタミネーションが多くなるとい
う問題もある。Further, when titanium boride, which is hard particles, and metal powder are subjected to mechanical alloying treatment, there is also a problem that contamination from a container for mechanical alloying treatment and grinding balls increases.
【０００４】[0004]
【発明が解決しようとする課題】本発明者らは、上記従
来技術の問題点を解決するために鋭意研究した結果、チ
タン硼化物を分散した硬質材料を合成する際に、チタン
硼化物の一部をチタン粉末とボロン粉末に置き換えて機
械的合金化処理を行い、焼結過程においてＴｉＢ2 を合
成することにより、焼結体の緻密さが向上すること、そ
して、低温で緻密な複合材料が作製できることを見出
し、本発明を完成した。本発明は、チタン硼化物を分散
した硬質材料を、チタン硼化物の一部を焼結過程におい
て合成することにより作製すること、それにより、低温
で緻密な高硬度材料を作製することを目的とするもので
ある。即ち、本発明は、チタン硼化物を含む複合材料を
低温で緻密に成形する方法を提供するためになされたも
のである。SUMMARY OF THE INVENTION The present inventors have made intensive studies to solve the above-mentioned problems of the prior art, and as a result, when synthesizing a hard material in which titanium boride is dispersed, one of titanium boride has been obtained. By replacing the parts with titanium powder and boron powder and performing mechanical alloying treatment, and synthesizing TiB 2 in the sintering process, the denseness of the sintered body is improved, and a dense composite material at low temperature They found that they could be made and completed the present invention. An object of the present invention is to produce a hard material in which titanium boride is dispersed by synthesizing a part of titanium boride in a sintering process, thereby producing a dense high-hardness material at a low temperature. Is what you do. That is, the present invention has been made to provide a method of forming a composite material containing titanium boride densely at a low temperature.
【０００５】[0005]
【課題を解決するための手段】上記課題を解決する本発
明は、以下の技術的手段からなる。 （１）５０重量％以上のＴｉＢ2 と残部が鉄あるいはニ
ッケル、コバルトなどの遷移金属より構成される複合材
料で、該ＴｉＢ2 の１０重量％〜５０重量％をＴｉ粉末
とＢ粉末で置き換え、機械的合金化処理した合金粉末。 （２）前記（１）で作製した合金粉末を加圧下で焼結す
ることにより成形したチタン硼化物を含む複合材料。 （３）前記（１）または（２）で作製した合金粉末また
は成形体を加熱熱処理し、必要により、その後急冷した
材料。 （４）ＴｉＢ2 の５重量％〜５０重量％をチタン炭化物
またはチタン窒化物粉末に置き換えた前記（１）記載の
合金粉末。 （５）前記（４）で作製した粉末を加圧下で焼結するこ
とにより成形したチタン硼化物を含む複合材料。 （６）５０重量％以上のＴｉＢ2 と残部が鉄あるいはニ
ッケル、コバルトなどの遷移金属より構成される複合材
料で、該ＴｉＢ2 の１０重量％〜５０重量％をＴｉ粉末
とＢ粉末で置き換え、機械的合金化処理した合金粉末を
加圧下で焼結することにより成形することからなるチタ
ン硼化物を含む複合材料の製造方法。The present invention for solving the above problems comprises the following technical means. (1) A composite material composed of 50% by weight or more of TiB 2 and the rest composed of a transition metal such as iron, nickel, or cobalt. 10% to 50% by weight of the TiB 2 is replaced with Ti powder and B powder; Alloy powder that has been mechanically alloyed. (2) A composite material containing titanium boride formed by sintering the alloy powder produced in (1) under pressure. (3) A material obtained by subjecting the alloy powder or the compact produced in the above (1) or (2) to heat treatment and, if necessary, quenching. (4) The alloy powder according to (1), wherein 5% to 50% by weight of TiB 2 is replaced with titanium carbide or titanium nitride powder. (5) A composite material containing titanium boride formed by sintering the powder produced in (4) under pressure. (6) A composite material composed of 50% by weight or more of TiB 2 and the remainder composed of a transition metal such as iron, nickel, or cobalt, and replacing 10% to 50% by weight of the TiB 2 with Ti powder and B powder; A method for producing a composite material containing titanium boride, comprising forming an alloy powder subjected to mechanical alloying by sintering under pressure.
【０００６】[0006]
【発明の実施の形態】次に、本発明をさらに詳細に説明
する。本発明は、従来、低温での緻密化が困難であった
チタン硼化物を分散した硬質材料をチタン硼化物の一部
を焼結時に合成することにより、その部分的な発熱現象
を利用して作製し、緻密な成形体を得るものである。本
発明に用いる材料としては、市販のＴｉＢ2 粉末、遷移
金属粉末（鉄、ニッケル、コバルトなど）、チタン粉末
およびボロン粉末が利用できる。この場合、ボロン粉末
としては、例えば、市販のボロン塊を粉砕機で粉砕した
もの、非晶質の粉末などが利用できる。粉末の粒度につ
いては特に指定しないが、一般的には数ミリ〜数ミクロ
ンの粉末が好適なものとして利用できる。Next, the present invention will be described in more detail. The present invention utilizes a partial heat generation phenomenon by synthesizing a part of titanium boride at the time of sintering a hard material in which titanium boride is dispersed, which has been difficult to densify at low temperatures. It is intended to obtain a dense compact. As the material used in the present invention, commercially available TiB 2 powder, transition metal powder (iron, nickel, cobalt, etc.), titanium powder and boron powder can be used. In this case, as the boron powder, for example, commercially available boron lump pulverized by a pulverizer, amorphous powder, or the like can be used. The particle size of the powder is not particularly specified, but generally a powder of several millimeters to several microns can be used as a suitable powder.
【０００７】硬質相となるＴｉＢ2 相の１０重量％〜５
０重量％をチタン粉末およびボロン粉末で置き換える。
この場合、チタン粉末とボロン粉末の混合量が１０重量
％未満では焼結が困難であり、また、５０重量％を越え
るとをＴｉＢ2 合成時の熱により他の硼化物の生成が促
進される。これらの粉末を機械的合金化法により処理す
る。上記ＴｉＢ2 をチタン粉末とボロン粉末に置き換え
る量を変化させることにより、緻密化温度をおよそ８０
０℃から１２００℃まで変化させることができる。[0007] 10% by weight to 5% of TiB 2 phase to be a hard phase
Replace 0% by weight with titanium powder and boron powder.
In this case, if the mixing amount of the titanium powder and the boron powder is less than 10% by weight, sintering is difficult, and if the mixing amount exceeds 50% by weight, the generation of other borides is promoted by heat during the synthesis of TiB 2. . These powders are processed by a mechanical alloying method. By changing the amount of replacing the TiB 2 with titanium powder and boron powder, the densification temperature can be increased to about 80%.
It can be varied from 0 ° C to 1200 ° C.
【０００８】硬質相にさらに高硬度のチタン炭化物やチ
タン窒化物を混合することも可能である。この場合は、
ＴｉＢ2 粉末の５重量％〜５０重量％をそれぞれの粉末
に置き換えればよい。５重量％未満の添加では、添加に
よる硬度の上昇が期待できず、また、５０重量％を越え
て添加すると焼結性が低下する。[0008] It is also possible to mix a titanium carbide or titanium nitride of higher hardness with the hard phase. in this case,
TiB 2 5 wt% to 50 wt% of the powder may be replaced with each of the powder. If the addition is less than 5% by weight, an increase in hardness due to the addition cannot be expected, and if the addition exceeds 50% by weight, the sinterability decreases.
【０００９】機械的合金化処理には、適宜の手段が使用
されるが、例えば、好適には、乾式の粉砕機が利用で
き、さらに、振動型ボールミル、遊星型ボールミル、転
動型ボールミル、アトライターなどが利用できる。機械
的合金化時の雰囲気は、粉末の酸化を防止するために、
不活性ガス雰囲気や減圧雰囲気が好ましい。For the mechanical alloying treatment, an appropriate means is used. For example, a dry pulverizer can be preferably used. Further, a vibration ball mill, a planetary ball mill, a rolling ball mill, Lighters are available. The atmosphere during mechanical alloying is to prevent powder oxidation.
An inert gas atmosphere or a reduced pressure atmosphere is preferable.
【００１０】機械的合金化に供する時間については特に
指定しないが、５０時間から２００時間が一般的であ
る。また、圧力伝達媒体としては、鋼球、セラミックス
球、超硬球など一般的な粉砕球が利用できる。Although the time for the mechanical alloying is not specified, it is generally 50 to 200 hours. In addition, as the pressure transmission medium, general pulverized balls such as steel balls, ceramic balls, and carbide balls can be used.
【００１１】機械的合金化法により合成された粉末は、
ＴｉＢ2 とサブミクロンサイズに微細化された鉄とチタ
ンとボロン粉末から構成される。なお、機械的合金化処
理時にはチタン粉末とボロン粉末からＴｉＢ2 相が合成
されておらず、機械的合金化時の容器やボールからの汚
染は５重量％以下である。得られた粉末は発火の危険性
があるため、容器からの取り出しは不活性ガス雰囲気中
あるいは真空中で行うことが好ましい。The powder synthesized by the mechanical alloying method is as follows:
It is composed of TiB 2 , iron, titanium, and boron powder refined to a submicron size. During the mechanical alloying process, the TiB 2 phase was not synthesized from the titanium powder and the boron powder, and the contamination from the container and the balls during the mechanical alloying was 5% by weight or less. Since the obtained powder has a risk of ignition, it is preferable to take out the powder from the container in an inert gas atmosphere or in a vacuum.
【００１２】次に、得られた合金粉末を焼結することに
より成形する。得られた粉末を成形するための焼結雰囲
気は、チタンの酸化を防止するために不活性ガス雰囲気
あるいは真空にする必要がある。焼結方法としては、加
圧下での加熱が好ましく、より好ましくは通電加熱によ
る焼結が好適なものとして例示される。通電加熱は、高
速な昇温が可能であるため、チタン硼化物の粒成長を抑
制できる。加圧は、焼結時のチタンとボロンの反応性を
よくするために必要であり、その加圧量は特に指定しな
いが、一般的には３０ＭＰａ以上である。Next, the obtained alloy powder is formed by sintering. The sintering atmosphere for molding the obtained powder needs to be an inert gas atmosphere or a vacuum in order to prevent oxidation of titanium. As the sintering method, heating under pressure is preferable, and sintering by electric heating is more preferable. The electric heating can raise the temperature at a high speed, so that the grain growth of titanium boride can be suppressed. Pressing is necessary to improve the reactivity between titanium and boron during sintering, and the amount of pressing is not particularly specified, but is generally 30 MPa or more.
【００１３】焼結温度は、遷移金属の量によって決定さ
れるが、その範囲は、８００℃から１２００℃が好まし
い。８００℃以下では焼結が不十分であり、１２００℃
以上ではチタン硼化物の結晶が大きく成長してしまう。[0013] The sintering temperature is determined by the amount of the transition metal, and the range is preferably from 800 ° C to 1200 ° C. If the temperature is lower than 800 ° C, sintering is insufficient.
Above, crystals of titanium boride grow large.
【００１４】得られた成形体は、静水圧雰囲気中で加熱
熱処理することにより、残留気孔を完全に除去すること
ができる。これにより、理論密度の９５％以上の密度を
有する緻密な成形体が得られる。また、加熱後に急冷す
ることにより硬質相以外の結晶粒径を微細化することが
できる。これにより、焼結体の硬度をおよそ１０％上昇
させた同じ組成の焼結体が得られる。The obtained molded body is subjected to a heat treatment in a hydrostatic pressure atmosphere, so that residual pores can be completely removed. Thereby, a dense molded body having a density of 95% or more of the theoretical density can be obtained. Further, by rapidly cooling after heating, the crystal grain size other than the hard phase can be refined. As a result, a sintered body having the same composition in which the hardness of the sintered body has been increased by about 10% is obtained.
【００１５】機械的合金化処理により合成された粉末を
加熱熱処理することにより、粉末形状のままＴｉＢ2 相
を生成させることができる。それにより、ＴｉＢ2 粒子
と金属が微細混合した複合粒子が得られ、金属相の展延
性を利用した粉末どうしの溶着が可能となる。この粉末
は、数ミクロン〜数十ミクロンの緻密な粉末であり、こ
のまま溶射用材料として利用が可能である。本発明によ
り、ＴｉＢ2 の熱的特性と高硬度を併せ持った複合材料
が提供される。また、本発明は、機械的合金化時のＴｉ
Ｂ2 をチタン粉末とボロン粉末に置き換える量を変化さ
せることにより、緻密化温度を変えることが可能であ
り、例えば、異種材料の接合、傾斜機能材料等の作製に
好適に応用することが可能である。By subjecting the powder synthesized by the mechanical alloying treatment to heat treatment, a TiB 2 phase can be generated in the powder form. As a result, composite particles in which the TiB 2 particles and the metal are finely mixed are obtained, and welding of the powders using the ductility of the metal phase becomes possible. This powder is a dense powder of several microns to several tens of microns, and can be used as it is as a material for thermal spraying. According to the present invention, a composite material having both the thermal properties of TiB 2 and high hardness is provided. In addition, the present invention provides a method for producing Ti
By the B 2 varying amounts to replace the titanium powder and boron powder, it is possible to vary the densification temperature, for example, bonding of dissimilar materials, can be suitably applied to the production of such FGM is there.
【００１６】[0016]
【実施例】以下、実施例に基づいて本発明をさらに具体
的に説明する。しかし、本発明は該実施例によって何ら
限定されるものではない。 実施例１ ＴｉＢ2 粉末（スタルク製）１８．４ｇに、チタン粉末
（和光純薬製試薬）１．８ｇ、ボロン粉末（和光純薬製
非晶質）０．８ｇ、鉄粉末（神戸製鋼製）９ｇを添加し
て、遊星型ボールミルによる１００時間の機械的合金化
処理を施した。機械的合金化の雰囲気は、減圧アルゴン
とし、粉末とボール重量比が約０．１になるようにし
た。容器と１０ｍｍ径の粉砕球にはクロム鋼を用いた。
得られた材料は、微細な粉末であり、容器やボールから
のコンタミネーションは１重量％以下であった。EXAMPLES The present invention will be described below more specifically based on examples. However, the present invention is not limited by the examples. Example 1 1.8 g of titanium powder (reagent made by Wako Pure Chemical), 0.8 g of boron powder (amorphous made by Wako Pure Chemical), iron powder (made by Kobe Steel) to 18.4 g of TiB 2 powder (made by Starck) 9 g was added, and a mechanical alloying treatment was performed for 100 hours by a planetary ball mill. The atmosphere for the mechanical alloying was argon under reduced pressure so that the weight ratio of the powder to the ball was about 0.1. Chromium steel was used for the container and the crushing balls having a diameter of 10 mm.
The obtained material was a fine powder, and contamination from a container or a ball was 1% by weight or less.
【００１７】得られた材料を直径１５ｍｍの黒鉛型に入
れ、１０-2Ｔｏｒｒの真空中で通電加熱を行って焼結し
た。焼結温度は１０００℃で３分間保持し、加圧力は３
５ＭＰａで成形した。得られた成形体は、割れなどはな
く、理論密度の９０％以上の密度を有する緻密な焼結体
であった。成形体は１０００Ｈｖ以上の硬度を示した。The obtained material was placed in a graphite mold having a diameter of 15 mm, and was heated and heated in a vacuum of 10 -2 Torr for sintering. The sintering temperature is maintained at 1000 ° C. for 3 minutes, and the pressing force is 3
It was molded at 5 MPa. The obtained molded body was a dense sintered body having no crack and having a density of 90% or more of the theoretical density. The molded body showed a hardness of 1000 Hv or more.
【００１８】実施例２ ＴｉＢ2 粉末（スタルク製）１０．５ｇに、チタン粉末
（和光純薬製試薬）７．２ｇ、ボロン粉末（和光純薬製
非晶質）３．３ｇ、鉄粉末（神戸製鋼製）９ｇを添加し
て、遊星型ボールミルによる２００時間の機械的合金化
処理を施した。機械的合金化の雰囲気は、減圧アルゴン
とし、粉末とボール重量比が約０．１になるようにし
た。容器と１０ｍｍ径の粉砕球にはクロム鋼を用いた。
得られた材料は、微細な粉末であり、容器やボールから
のコンタミネーションは１重量％以下であった。Example 2 To 10.5 g of TiB 2 powder (manufactured by Starck), 7.2 g of titanium powder (reagent made by Wako Pure Chemical), 3.3 g of boron powder (amorphous manufactured by Wako Pure Chemical), iron powder (Kobe) 9 g of steelmaking) and subjected to a mechanical alloying treatment with a planetary ball mill for 200 hours. The atmosphere for the mechanical alloying was argon under reduced pressure so that the weight ratio of the powder to the ball was about 0.1. Chromium steel was used for the container and the crushing balls having a diameter of 10 mm.
The obtained material was a fine powder, and contamination from a container or a ball was 1% by weight or less.
【００１９】得られた材料を内径１５ｍｍの黒鉛型に入
れ、１０-2Ｔｏｒｒの真空中で通電加熱を行って焼結し
た。焼結温度は１０００℃で３分間保持し、加圧力は３
５ＭＰａで成形した。得られた成形体は、割れなどがな
く、理論密度の９５％以上の密度を有する緻密な焼結体
であった。成形体は２１１１Ｈｖの硬度を示した。The obtained material was placed in a graphite mold having an inner diameter of 15 mm, and was heated and heated in a vacuum of 10 -2 Torr for sintering. The sintering temperature is maintained at 1000 ° C. for 3 minutes, and the pressing force is 3
It was molded at 5 MPa. The obtained molded body was a dense sintered body having no crack and a density of 95% or more of the theoretical density. The molded body showed a hardness of 2111 Hv.
【００２０】実施例３ ＴｉＢ2 粉末（スタルク製）１０．５ｇに、ＴｉＣ粉末
（スタルク製）２．１ｇ、チタン粉末（和光純薬製試
薬）７．２ｇ、ボロン粉末（和光純薬製）３．３ｇ、ニ
ッケル粉末（和光純薬製）９ｇを添加して、遊星型ボー
ルミルによる１００時間の機械的合金化処理を施した。
機械的合金化の雰囲気は、減圧アルゴンとし、粉末とボ
ール重量比が約０．１になるようにした。容器と１０ｍ
ｍ径の粉砕球にはクロム鋼を用いた。得られた材料は、
微細な粉末であり、容器やボールからのコンタミネーシ
ョンは２重量％以下であった。Example 3 To 10.5 g of TiB 2 powder (manufactured by Starck), 2.1 g of TiC powder (manufactured by Stark), 7.2 g of titanium powder (reagent manufactured by Wako Pure Chemical), and boron powder (manufactured by Wako Pure Chemical) 3 0.3 g and 9 g of nickel powder (manufactured by Wako Pure Chemical Industries, Ltd.) were added, and a mechanical alloying treatment was performed for 100 hours by a planetary ball mill.
The atmosphere for the mechanical alloying was argon under reduced pressure so that the weight ratio of the powder to the ball was about 0.1. Container and 10m
Chrome steel was used for the crushing balls having a diameter of m. The resulting material is
It was a fine powder, and the contamination from containers and balls was 2% by weight or less.
【００２１】得られた材料を内径１５ｍｍの黒鉛型に入
れ、１０-2Ｔｏｒｒの真空中で通電加熱を行って焼結し
た。焼結温度は１０００℃で３分間保持し、加圧力は３
５ＭＰａで成形した。得られた成形体は、割れなどは観
察されず、理論密度の９０％以上の比較的緻密な焼結体
が得られた。成形体をアルゴンガス雰囲気中で１０００
℃に加熱し、水中で急冷した。得られた材料は、NiTi相
を含んでおり、その硬度は１２００Ｈｖ以上であった。The obtained material was placed in a graphite mold having an inner diameter of 15 mm, and was heated and heated in a vacuum of 10 -2 Torr for sintering. The sintering temperature is maintained at 1000 ° C. for 3 minutes, and the pressing force is 3
It was molded at 5 MPa. No cracks were observed in the obtained molded body, and a relatively dense sintered body having a theoretical density of 90% or more was obtained. The molded body is placed in an argon gas atmosphere at 1000
C. and quenched in water. The obtained material contained a NiTi phase and had a hardness of 1200 Hv or more.
【００２２】[0022]
【発明の効果】本発明は、チタン硼化物を含む複合材料
を低温で緻密に成形する方法およびその製品に係り、本
発明によれば、遷移金属材料を結合相とする緻密なチタ
ン硼化物分散硬質材料を提供することができる。本発明
のチタン硼化物分散硬質材料の製造方法を用いて、チタ
ン硼化物を分散した硬質材料を合成する際に、焼結時に
ＴｉＢ2 を生成させることにより低温で緻密な高硬度材
料を作製することができる。特に、機械的合金化時のＴ
ｉＢ2 をチタン粉末とボロン粉末に置き換える量を変化
させることにより、緻密化温度を変えられることから、
異種材料の接合や傾斜機能材料の作製にも本技術が応用
できるものと期待される。本発明により、ＴｉＢ2 の熱
的特性と高硬度を併せ持った複合材料の開発に貢献でき
るものと考えられる。The present invention relates to a method for densely forming a composite material containing titanium boride at a low temperature and a product thereof. According to the present invention, a dense titanium boride dispersion containing a transition metal material as a binder phase is provided. A hard material can be provided. When the titanium boride-dispersed hard material production method of the present invention is used to synthesize a titanium boride-dispersed hard material, a dense high-hardness material is produced at a low temperature by generating TiB 2 during sintering. be able to. In particular, T at the time of mechanical alloying
By changing the amount of replacing iB 2 with titanium powder and boron powder, the densification temperature can be changed.
It is expected that this technology can be applied to the joining of different materials and the production of functionally graded materials. It is considered that the present invention can contribute to the development of a composite material having both the thermal characteristics and high hardness of TiB 2 .
─────────────────────────────────────────────────────
────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成１１年５月２４日[Submission date] May 24, 1999
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】発明の名称[Correction target item name] Name of invention
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【発明の名称】 チタン硼化物分散硬質材料 [Title of the Invention] Titanium boride dispersed hard material
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｃ２２Ｃ 38/00 ３０４ Ｃ２２Ｃ 38/00 ３０４ (72)発明者 尾崎 公洋 愛知県名古屋市名東区平和が丘１丁目70番 地 猪子石住宅６棟503号──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 6 Identification code FI C22C 38/00 304 C22C 38/00 304 (72) Inventor Kimihiro Ozaki 1-70 Heiwagaoka, Meito-ku, Nagoya City, Aichi Prefecture Inokoishi 6 houses, 503
Claims (5)
るいはニッケル、コバルトなどの遷移金属より構成され
る複合材料で、該ＴｉＢ2 の１０重量％〜５０重量％を
Ｔｉ粉末とＢ粉末で置き換え、機械的合金化処理した合
金粉末。1. A composite material comprising 50% by weight or more of TiB 2 and the balance being a transition metal such as iron or nickel or cobalt. 10% to 50% by weight of TiB 2 is composed of Ti powder and B powder. Replaced and mechanically alloyed alloy powder.
焼結することにより成形したチタン硼化物を含む複合材
料。2. A composite material containing titanium boride formed by sintering the alloy powder produced in claim 1 under pressure.
粉末または成形体を加熱熱処理し、必要により、その後
急冷した材料。3. A material obtained by subjecting the alloy powder or the compact produced in claim 1 or 2 to heat treatment and, if necessary, quenching.
ン炭化物またはチタン窒化物粉末に置き換えた請求項１
記載の合金粉末。4. The method of claim 1, wherein 5% to 50% by weight of TiB 2 is replaced by titanium carbide or titanium nitride powder.
The described alloy powder.
することにより成形したチタン硼化物を含む複合材料。5. A composite material containing titanium boride formed by sintering the powder produced in claim 4 under pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10146542A JP3032818B2 (en) | 1998-05-11 | 1998-05-11 | Titanium boride dispersed hard material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10146542A JP3032818B2 (en) | 1998-05-11 | 1998-05-11 | Titanium boride dispersed hard material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11323401A true JPH11323401A (en) | 1999-11-26 |
| JP3032818B2 JP3032818B2 (en) | 2000-04-17 |
Family
ID=15410017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10146542A Expired - Lifetime JP3032818B2 (en) | 1998-05-11 | 1998-05-11 | Titanium boride dispersed hard material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3032818B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005290530A (en) * | 2004-04-06 | 2005-10-20 | Kubota Corp | Metal boride-dispersed sintered compact |
| JP2012001755A (en) * | 2010-06-15 | 2012-01-05 | National Institute Of Advanced Industrial Science & Technology | High thermal conductivity hard material light in weight and excellent in oxidation resistance, and its manufacturing method |
| JP2017088972A (en) * | 2015-11-13 | 2017-05-25 | 新日本電工株式会社 | Titanium boride-containing powder and manufacturing method therefor and manufacturing method of sintered metal |
| EP3835443A4 (en) * | 2018-08-07 | 2022-07-20 | Hiroshima University | Fe-based sintered body, fe-based sintered body production method, and hot-pressing die |
-
1998
- 1998-05-11 JP JP10146542A patent/JP3032818B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005290530A (en) * | 2004-04-06 | 2005-10-20 | Kubota Corp | Metal boride-dispersed sintered compact |
| JP2012001755A (en) * | 2010-06-15 | 2012-01-05 | National Institute Of Advanced Industrial Science & Technology | High thermal conductivity hard material light in weight and excellent in oxidation resistance, and its manufacturing method |
| JP2017088972A (en) * | 2015-11-13 | 2017-05-25 | 新日本電工株式会社 | Titanium boride-containing powder and manufacturing method therefor and manufacturing method of sintered metal |
| EP3835443A4 (en) * | 2018-08-07 | 2022-07-20 | Hiroshima University | Fe-based sintered body, fe-based sintered body production method, and hot-pressing die |
| US11858045B2 (en) * | 2018-08-07 | 2024-01-02 | Hiroshima University | Fe-based sintered body, Fe-based sintered body production method, and hot-pressing die |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3032818B2 (en) | 2000-04-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4097275A (en) | Cemented carbide metal alloy containing auxiliary metal, and process for its manufacture | |
| Luo et al. | Recent advances in the design and fabrication of strong and ductile (tensile) titanium metal matrix composites | |
| JP2010236060A (en) | Nitride dispersion ti-al based target and method for producing the same | |
| US5640666A (en) | Composite silicide/silicon carbide mechanical alloy | |
| JPS6289803A (en) | Powdery particle for fine granular hard alloy and its production | |
| CN107056304A (en) | A kind of TiB2Based composite ceramic material and preparation method thereof | |
| JPH0578107A (en) | Nitride powder | |
| JPH02197535A (en) | Manufacture of intermetallic compound | |
| JP3032818B2 (en) | Titanium boride dispersed hard material | |
| EP0591305A1 (en) | Cermets based on transition metal borides, their production and use. | |
| JP3837332B2 (en) | In-situ powder metallurgy manufacturing method for wear-resistant composite materials | |
| JP3793813B2 (en) | High strength titanium alloy and method for producing the same | |
| US20030145685A1 (en) | Process for producing titanium carbide, titanium nitride, or tungsten carbide hardened materials | |
| JPH08120352A (en) | Method for reproducing cemented carbide composition and production of cemented carbide | |
| JP2005281769A (en) | High hardness high carbon nanocrystal iron alloy powder and bulk material and production method therefor | |
| Jõeleht | The influence of sintering temperature of reactive sintered (Ti, Mo) C-Ni cermets | |
| JP2877999B2 (en) | Method for producing TiAl-based composite intermetallic compound | |
| US4092156A (en) | Process for preparing titanium carbide base powder for cemented carbide alloys | |
| WO2012046773A1 (en) | Titanium-hydroxyapatite composite material having high strength and excellent biocompatibility | |
| Tarraste et al. | High Energy Milling of WС-FeСr Cemented Carbide | |
| JPH0252681B2 (en) | ||
| JPS6119593B2 (en) | ||
| JPH07188874A (en) | Ferrous alloy with high rigidity and its manufacture | |
| JP3413921B2 (en) | Method for producing Ti-Al based intermetallic compound sintered body | |
| JPH11172364A (en) | Production of sintered tool steel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term |