JP2003119504A - Method for sintering hard material - Google Patents
Method for sintering hard materialInfo
- Publication number
- JP2003119504A JP2003119504A JP2001315657A JP2001315657A JP2003119504A JP 2003119504 A JP2003119504 A JP 2003119504A JP 2001315657 A JP2001315657 A JP 2001315657A JP 2001315657 A JP2001315657 A JP 2001315657A JP 2003119504 A JP2003119504 A JP 2003119504A
- Authority
- JP
- Japan
- Prior art keywords
- sintering
- phase
- hard
- binder phase
- cooling
- 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.)
- Withdrawn
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、硬質相と鉄系金属
の１種以上からなる結合相と残部は不可避不純物からな
る硬質材料の焼結方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for sintering a hard material comprising a hard phase, a binder phase composed of at least one of iron-based metals, and the balance being inevitable impurities.
【０００２】[0002]
【従来の技術】金属等の切削加工には、超硬合金、サー
メット合金や被覆超硬合金の刃先交換型チップが広く市
場で用いられている。これらの超硬合金やサーメット合
金は、硬質相と金属結合相との２相で構成されている。
またこれらの表面に、ＴｉＣ，ＴｉＮ，Ａｌ２Ｏ３等を
単層または複層で被覆することで、実質的に靭性を維持
して耐摩耗性を増加させることも可能であり、広く一般
的に行はれている。2. Description of the Related Art For cutting metal and the like, exchangeable cutting edges of cemented carbide, cermet alloy and coated cemented carbide are widely used in the market. These cemented carbides and cermet alloys are composed of two phases, a hard phase and a metal binding phase.
Further, by coating these surfaces with TiC, TiN, Al 2 O 3 or the like in a single layer or multiple layers, it is possible to substantially maintain the toughness and increase the wear resistance. Have been to.
【０００３】[0003]
【発明が解決しようとする課題】超硬合金やサーメット
合金を焼結する際に、それらの表面を完全にまたは部分
的に覆う一般的に０．１μｍ以上の厚さの結合相の層が
よく発生する。超硬合金においては特にＣｏ勾配と言わ
れる焼結体最表面の下の面に豊富な結合相を有する超硬
合金、および結合相が均一分布する超硬合金において顕
著に発生する。サーメット合金の場合には、表面に硬質
相が豊富となった表面硬化型サーメットおよび結合相が
均一分布するサーメット合金において顕著に現れる。When sintering cemented carbides and cermet alloys, a layer of a binder phase having a thickness of 0.1 μm or more, which covers their surfaces completely or partially, is often used. Occur. Particularly in cemented carbide, it occurs remarkably in a cemented carbide having a rich binder phase on the surface below the outermost surface of the sintered body, which is called a Co gradient, and in a cemented carbide in which the binder phase is uniformly distributed. In the case of the cermet alloy, it appears remarkably in the surface hardening type cermet in which the hard phase is abundant on the surface and in the cermet alloy in which the binder phase is uniformly distributed.
【０００４】この結合相が豊富となっている層が形成さ
れる理由は現在解明されていない。しかしながら、この
層は、ＣＶＤ法、ＰＶＤ法による被覆層を形成する場
合、この被覆工程に悪影響をもたらし、品位の劣った特
性と不十分な接着力を持った被覆層となってしまう。The reason for the formation of this binder phase rich layer is not currently understood. However, when forming a coating layer by the CVD method or the PVD method, this layer adversely affects the coating step, resulting in a coating layer having poor quality properties and insufficient adhesive strength.
【０００５】また、この結合相が豊富となっている層は
被削材との化学的親和性にも富んでいるため、切削時に
被削材が刃先に溶着しやすくなり、さらには被削材の加
工面光沢に悪影響を及ぼす場合がある。そのため、こう
した結合相の層は、焼結体が被覆されるかされないかを
問わず除去された状態であることが望ましい。Further, since the layer rich in the binder phase has a high chemical affinity with the work material, the work material is apt to be welded to the cutting edge during cutting, and further the work material is May adversely affect the processed surface gloss. Therefore, it is desirable that such a binder phase layer is removed regardless of whether the sintered body is coated or not.
【０００６】このような結合相の層は、ブラスト等の噴
射加工で除去することができるが制御することが難し
い。この難しさは、必要な精度で噴射加工深さを確実に
制御できないことにあり、その事が加工後に被覆された
最終製品すなわち被覆インサートの特性を大きくばらつ
かせる原因となる。また、表面の硬質相構成材の粒子に
損傷が生じる。一方この欠点を補う方法として、スウェ
ーデン特許願書第９２０２１４２−７号には、微細な粒
子で噴射加工をすれば、硬質相構成材の粒子に損傷を与
えることなく結合相の層を除去できることが開示されて
いる。Such a binder phase layer can be removed by blasting or other blasting process, but is difficult to control. This difficulty lies in the inability to reliably control the blast depth with the required accuracy, which causes a large variation in the properties of the final product coated, ie the coated insert, after machining. Further, the particles of the hard phase constituent material on the surface are damaged. On the other hand, as a method of compensating for this drawback, Swedish Patent Application No. 9202142-7 discloses that a jetting process with fine particles can remove the binder phase layer without damaging the particles of the hard phase constituent material. Has been done.
【０００７】上記の機械的方法の代わりとして、化学的
方法または電解的方法を使用することができる。米国特
許第４，２８２，２８９号には、被覆工程の初期の段階
にＨＣｌを使用することによる気相中のエッチング法が
開示されている。ヨーロッパ特許Ａ−３３７６９６号に
は、硝酸、塩酸、フッ化水素酸、硫酸等での化学エッチ
ング法、または電気化学法が提案されている。また特開
昭６３−０６０２７９号公報にはアルカリ溶液すなわち
ＮａＯＨを使用することが示され、且つ特開昭６３−０
６０２８０号公報には酸溶液を使用することが示されて
いる。さらに特開昭６３−０５３２６９号公報にはダイ
ヤモンドの蒸着以前の硝酸エッチングが示されている。As an alternative to the mechanical methods described above, chemical or electrolytic methods can be used. U.S. Pat. No. 4,282,289 discloses a gas phase etching process by using HCl in the early stages of the coating process. European Patent A-337696 proposes a chemical etching method with nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid or the like, or an electrochemical method. Further, JP-A-63-060279 discloses the use of an alkaline solution, that is, NaOH, and JP-A-63-0.
JP 60280 discloses the use of an acid solution. Further, Japanese Patent Laid-Open No. 63-053269 discloses nitric acid etching before diamond vapor deposition.
【０００８】しかしこれらの方法には欠点がある。すな
わち、これらの方法では結合相の層のみを取り除くと言
うことができない。これらの方法では、特に、刃先に近
い領域が深く侵食される。エッチング剤は表面から結合
相を取り除くことができないばかりでなく、硬質相構成
材の粒子間に浸透し、結果として結合相が主成分で構成
された表面層がインサートの他の領域に部分的に残留す
るようになり、層と基材との間が同時に意図せずに多孔
的な状態となってしまう。However, these methods have drawbacks. That is, it cannot be said that these methods remove only the binder phase layer. In these methods, in particular, the region near the cutting edge is deeply eroded. Not only is the etchant unable to remove the binder phase from the surface, but it also penetrates between the particles of the hard phase constituent, resulting in a surface layer consisting mainly of the binder phase in other areas of the insert. It will remain and unintentionally become porous between the layer and the substrate at the same time.
【０００９】米国特許第５，３８０，４０８号には、硫
酸と燐酸の混合液中で実施される電解エッチング法が示
されている。この方法によると、深さ効果を生じさせず
に均一かつ完全に結合相の層を除去することができ、結
果として表面の結合相の含有率を零にすることができ
る。しかし場合によっては、被覆層の接着強度の観点か
ら表面の結合相の含有率を零にすることは望ましいこと
ではなく、むしろ公称含有率に近い結合相表面含有率が
望まれる。US Pat. No. 5,380,408 shows an electrolytic etching process carried out in a mixture of sulfuric acid and phosphoric acid. According to this method, the binder phase layer can be removed uniformly and completely without causing a depth effect, and as a result, the binder phase content on the surface can be reduced to zero. However, in some cases, it is not desirable from the viewpoint of the adhesive strength of the coating layer to make the content of the binder phase on the surface zero, but rather a binder phase surface content close to the nominal content is desired.
【００１０】その場合には、上記方法では、追加的な製
造工程が必要となり、そのため大きな寸法の製品の製造
には有効ではない。従って、焼結中に結合相が主成分で
構成された表面層が形成されないかまたはその冷却工程
中に除去できるような焼結方法が可能な場合には望まし
い方法ではない。In that case, the above method requires an additional manufacturing step and is therefore not effective for manufacturing a product having a large size. Therefore, it is not a desirable method if a surface layer having a binder phase as a main component is not formed during sintering or a sintering method that can be removed during the cooling step is possible.
【００１１】したがって本発明は、結合相が主成分で構
成された表面層は焼結処理の後に表面に存在しないが、
後述するような十分に規定されたＣｏ含有量を持つ表面
が存在するような超硬合金およびサーメット合金を焼結
する方法を提供することを目的としている。Therefore, according to the present invention, the surface layer having the binder phase as a main component does not exist on the surface after the sintering treatment.
It is an object of the present invention to provide a method for sintering a cemented carbide and a cermet alloy having a surface having a well-defined Co content as described below.
【００１２】[0012]
【課題を解決するための手段】本発明は、焼結時の加熱
工程と高温で保持する工程は従来の方法で実施し、冷却
工程を少なくとも１１００℃までの温度降下の範囲内で
は、０．０１〜４５Ｋpaの水素雰囲気中で、好ましくは
１〜１５Ｋｐａの水素雰囲気中で行うことにより、上記
の目的を達成する。０．０１Ｋｐａの圧力以下では結合
相が主成分で構成された表面層が生じてしまい、４５Ｋ
ｐａの圧力以上では超硬合金やサーメット合金に望まし
くない浸炭が発生してしまう。According to the present invention, the heating step during sintering and the step of holding at a high temperature are carried out by a conventional method, and the cooling step is performed within a temperature drop range of at least 1100 ° C. The above object is achieved by carrying out in a hydrogen atmosphere of 01 to 45 Kpa, preferably in a hydrogen atmosphere of 1 to 15 Kpa. At a pressure of 0.01 Kpa or less, a surface layer composed of a binder phase as a main component is produced,
Above a pressure of pa, undesired carburization will occur in the cemented carbide and cermet alloy.
【００１３】最適な圧力条件は、合金の組成、焼結条件
により異なり、またある程度までは使用する焼結装置の
設計にも依存している。結合相が主成分で構成された表
面層が生じず、かつ超硬合金やサーメット合金に望まし
くない浸炭が発生しない、より最適な水素圧力は当該業
者であれば容易に実験的に決定することができる。The optimum pressure conditions differ depending on the composition of the alloy and the sintering conditions, and to some extent also depend on the design of the sintering apparatus used. A person who is skilled in the art can easily experimentally determine a more optimal hydrogen pressure that does not generate a surface layer composed of a binder phase as a main component and does not cause undesirable carburization in cemented carbide or cermet alloy. it can.
【００１４】被覆層との接着強度を増し切削性能を向上
させるためには、合金の結合相含有量を配合体積分率で
表しそれを１とした場合に、焼結体表面では結合相の存
在する面積割合を０．３〜３、好ましくは０．５〜２に
する必要がある。具体的にはＷＣ−Ｃｏ１０wt％の超硬
合金の場合、混合則で比重を計算すると、ＷＣの原子量
を１９５．８、比重を１５．６とし、Ｃoの原子量を５
８．９、比重を８．９として理論比重は１４．５０８と
なり、ＷＣの配合体積分率は８３．７vol％、Ｃｏの配
合体積分率は１６．３vol％となる。従って、焼結体表
面でのＣoの存在する面積割合は、４．９〜４８．９
％、さらに望ましくは８．２〜３２．６％にする必要が
ある。In order to increase the adhesive strength with the coating layer and improve the cutting performance, when the binder phase content of the alloy is expressed as a blend volume fraction and it is set to 1, the presence of the binder phase on the surface of the sintered body. It is necessary to set the area ratio to be 0.3 to 3, preferably 0.5 to 2. Specifically, in the case of a cemented carbide of WC-Co10 wt%, when the specific gravity is calculated by the mixing rule, the atomic weight of WC is 195.8, the specific gravity is 15.6, and the atomic weight of Co is 5
8.9, the specific gravity is 8.9, the theoretical specific gravity is 14.508, the mixture volume fraction of WC is 83.7 vol%, and the mixture volume fraction of Co is 16.3 vol%. Therefore, the area ratio of Co on the surface of the sintered body is 4.9 to 48.9.
%, And more preferably 8.2 to 32.6%.
【００１５】表面のＣo含有量は、例えば、ＥＤＳ（エ
ネルギー分散分光計）を装備するＳＥＭ（走査型電子顕
微鏡）を使用し、未知の表面からのＣo強度を参照例と
比較する、すなわち、同一配合組成の試料の研磨した断
面のＣo強度と比較することによって決定することがで
きる。The Co content of the surface is compared, for example, with a SEM (scanning electron microscope) equipped with an EDS (energy dispersive spectrometer) to the Co intensity from an unknown surface, ie the same. It can be determined by comparing the Co strength of the polished cross section of the compounded composition sample.
【００１６】具体例としては、超硬合金の場合には焼結
体表面および研磨した断面をそれぞれ、ＳＥＭを使用し
て反射電子像（組成像）で観察して写真撮影し、その写
真をスキャナを用いてパーソナルコンピュータに取り込
み、画像解析ソフトを用いて白黒２階層化した上で白色
部と黒色部の面積比率（ピクセル数の総和の比率）を算
出し、これらを比較することによって決定することがで
きる。この方法はあくまで１例であり、他のどんな方法
を用いて白色部と黒色部の比率を決定してもよい。なお
ＳＥＭ反射電子像では白色部が硬質相で、黒色部がＣo
となる。勿論、ＥＰＭＡ分析や、湿式分析、オージェ分
析他、いかなる分析方法を用いてＣo量を同定しても構
わないのは言うまでもない。As a specific example, in the case of cemented carbide, the surface of the sintered body and the polished cross section are observed by backscattered electron images (composition images) using an SEM and photographed, and the photograph is taken by a scanner. To the personal computer using, and using image analysis software to create two layers of black and white, calculate the area ratio of white and black areas (the ratio of the total number of pixels), and determine by comparing these You can This method is merely an example, and any other method may be used to determine the ratio of the white portion and the black portion. In the SEM backscattered electron image, the white part is the hard phase and the black part is Co.
Becomes Needless to say, the amount of Co may be identified by using any analysis method such as EPMA analysis, wet analysis, Auger analysis and the like.
【００１７】本発明の方法は、すべての種類の超硬合金
およびサーメット合金に適用することができるが、次の
いずれかかが工業的に有意義であり好ましい。
（１） 超硬合金
硬質相：炭化タングステン
結合相：鉄系金属の１種以上で、含有量が３〜３０重量
％
残部：不可避不純物The method of the present invention can be applied to all kinds of cemented carbides and cermet alloys, but any of the following is industrially significant and preferred. (1) Cemented Carbide Hard Phase: Tungsten Carbide Bonding Phase: One or more types of iron-based metals with a content of 3 to 30 wt% Balance: Inevitable impurities
【００１８】（２）超硬合金
硬質相：炭化タングステン
周期律表IVa，Va，VIa、族遷移金属と炭素、窒素、酸
素および硼素から選択される１種以上との化合物または
固溶体相の、１種以上、含有量は０．１〜５０重量％
結合相：鉄系金属の１種以上で、含有量が３〜３０重量
％
残部：不可避不純物(2) Cemented Carbide Hard Phase: Tungsten Carbide Periodic Table IVa, Va, VIa, a compound or solid solution phase of a group transition metal and one or more selected from carbon, nitrogen, oxygen and boron, 1 Species or more, content is 0.1 to 50% by weight Binder phase: One or more kinds of iron-based metal, content is 3 to 30% by weight Remainder: unavoidable impurities
【００１９】（３）サーメット合金
硬質相：周期律表IVa，Va，VIa、族遷移金属と炭素、窒
素、酸素および硼素から選択される１種以上との化合物
または固溶体相の、１種以上、含有量は７０〜９７重量
％
結合相：鉄系金属の１種以上で、含有量が３〜３０重量
％
残部：不可避不純物(3) Cermet alloy hard phase: one or more of a compound or solid solution phase of a periodic table IVa, Va, VIa, a group transition metal and one or more selected from carbon, nitrogen, oxygen and boron, Content is 70 to 97% by weight Binder phase: One or more iron-based metals, content is 3 to 30% by weight Remainder: Inevitable impurities
【００２０】本発明方法によって製造される刃先交換型
切削チップは、焼結後に、当業界で既知のダイヤモンド
砥石による研削加工、ブラシなどによる刃先処理、およ
びチップ表面に単層若しくは複層の表面被覆層を形成し
ても本発明の効果は現れる。なお表面被覆層の形成方法
は、ＣＶＤ法、ＭＴＣＶＤ法、またはＰＶＤ法など、い
ずれの方法を用いてもよい。The cutting edge exchange type cutting tip manufactured by the method of the present invention is, after sintering, ground by a diamond grindstone known in the art, the cutting edge is processed by a brush, and the tip surface is coated with a single layer or multiple layers. Even if a layer is formed, the effect of the present invention will appear. The method of forming the surface coating layer may be any method such as the CVD method, the MTCVD method, or the PVD method.
【００２１】また焼結時の冷却工程において、水素分圧
が本発明の範囲内であれば、アルゴン等の希釈ガスを用
いて全圧を調整しても本発明の効果は現れる。希釈ガス
を用いるかどうかは、製造に使用する焼結炉の仕様によ
る。Further, in the cooling step at the time of sintering, if the hydrogen partial pressure is within the range of the present invention, the effect of the present invention will be exhibited even if the total pressure is adjusted by using a diluent gas such as argon. Whether to use a diluent gas depends on the specifications of the sintering furnace used for manufacturing.
【００２２】[0022]
【発明の実施の形態】（実施例１）原料粉末として、表
１に示した原料粉末を、同じく表１に示した組成で湿式
混合を１０Ｈｒ行った後、１ｔｏｎ／ｃｍ2の圧力にて
プレス成形し、真空中で４．０℃／ｍｉｎの昇温速度で
１４２０℃まで昇温し、真空中で１４２０℃の温度で６
０分間保持してから、水素１０Ｋｐａの雰囲気中で９０
０℃まで冷却をを行い、ＪＩＳ４１２１規定のＣＮＭＧ
１２０４０８形状の「本発明焼結体１」を製造した。比
較のために、冷却も真空中で行った同形状の「比較チッ
プＡ」を製造した。BEST MODE FOR CARRYING OUT THE INVENTION (Example 1) As raw material powders, the raw material powders shown in Table 1 were wet-mixed with the composition shown in Table 1 for 10 hours and then pressed at a pressure of 1 ton / cm 2 . Molded, heated to 1420 ° C. at a heating rate of 4.0 ° C./min in vacuum, and heated to 1420 ° C. in vacuum for 6
Hold for 0 minutes, and then in an atmosphere of hydrogen 10Kpa 90
After cooling to 0 ° C, CNMG specified in JIS4121
A 120408 shaped “inventive sintered body 1” was produced. For comparison, a “comparative chip A” of the same shape was also produced, which was cooled in a vacuum.
【００２３】[0023]
【表１】 [Table 1]
【００２４】ＳＥＭ反射電子像で観察した焼結体表面の
写真を、本発明チップ１は図１に、比較チップＡは図２
に示す。この写真で白く見えている部分はＷＣ結晶で、
黒く見えているところはＣｏである。これらの写真をコ
ンピュータを用いて白黒２階層に画像処理したものを、
それぞれ図３、図４に示す。A photograph of the surface of the sintered body observed by an SEM backscattered electron image is shown in FIG. 1 for the chip 1 of the present invention and FIG. 2 for the comparative chip A.
Shown in. The part that looks white in this photo is the WC crystal,
The part that looks black is Co. Image processing of these photographs into two layers of black and white using a computer,
They are shown in FIGS. 3 and 4, respectively.
【００２５】この画像処理写真の黒ピクセルと白ピクセ
ルの個数を集計したところ、本発明チップ１は黒部（Ｃ
ｏ部）は２９．０％で白部（ＷＣ部）が７１．０％であ
ったのに対し、比較チップＡは黒部が７２．２％、白部
が２７．８％と、かなり表面にＣｏが多い状態となって
いることが確認できた。When the numbers of black pixels and white pixels of this image-processed photograph were totaled, the chip 1 of the present invention showed that the black portion (C
o part) was 29.0% and the white part (WC part) was 71.0%, whereas the comparative chip A had a black part of 72.2% and a white part of 27.8%. It was confirmed that the Co content was high.
【００２６】さらに本発明チップ１および比較チップＡ
を、ダイヤモンド砥石で上下面のみ研削加工した後、公
知の化学蒸着法で表面に膜厚５μｍのＴｉＮ膜を被覆
し、下記条件で切削試験を行った。
連続切削試験
被削材：ＳＣＭ４３５（ＨＢ＝２４６） 丸棒
切削速度：１７０ｍ／ｍｉｎ
送り：０．２５ｍｍ／ｒｅｖ．
切り込み：２．０ｍｍ
切削時間：５分間
切削油：水溶性油
この結果、本発明チップの逃げ面摩耗量は０．０８３ｍ
ｍであり、被覆層の剥離は認められなかったのに対し、
比較チップＡは逃げ面摩耗量が０．１４８ｍｍであり、
焼結肌上に被覆層が被覆された側面部の被覆層の剥離が
認められた。Furthermore, the chip 1 of the present invention and the comparative chip A
After grinding only the upper and lower surfaces with a diamond grindstone, the surface was covered with a TiN film having a film thickness of 5 μm by a known chemical vapor deposition method, and a cutting test was performed under the following conditions. Continuous cutting test Work material: SCM435 (HB = 246) Round bar Cutting speed: 170 m / min Feed: 0.25 mm / rev. Cut: 2.0 mm Cutting time: 5 minutes Cutting oil: water-soluble oil As a result, the flank wear amount of the chip of the present invention is 0.083 m
m, and peeling of the coating layer was not observed, whereas
Comparative chip A has a flank wear amount of 0.148 mm,
Peeling of the coating layer on the side surface where the coating layer was coated on the sintered skin was observed.
【００２７】（実施例２）原料粉末として、表２に示し
た原料粉末を、同じく表２に示した組成で湿式混合を１
５Ｈｒ行った後、１ｔｏｎ／ｃｍ2の圧力にてプレス成
形し、真空中で４．０℃／ｍｉｎの昇温速度で１４４０
℃まで昇温し、真空中で１４４０℃の温度で６０分間保
持してから、水素２０Ｋｐａの雰囲気中で９５０℃まで
冷却をを行い、ＪＩＳ４１２１規定のＴＮＭＧ１６０３
０４形状の「本発明焼結体２」を製造した。比較のため
に、冷却も真空中で行った同形状の「比較チップＢ」を
製造した。(Example 2) As the raw material powder, the raw material powder shown in Table 2 was wet-mixed with the composition shown in Table 2 as well.
After 5 hours, press-molded at a pressure of 1 ton / cm 2 and 1440 at a temperature rising rate of 4.0 ° C./min in vacuum.
The temperature is raised to ℃, kept at 1440 ℃ in vacuum for 60 minutes, and then cooled to 950 ℃ in an atmosphere of hydrogen of 20 Kpa, and TNMG1603 specified in JIS4121.
A 04-shaped “inventive sintered body 2” was produced. For comparison, a “comparative chip B” of the same shape was also produced, which was cooled in a vacuum.
【００２８】[0028]
【表２】 [Table 2]
【００２９】本発明チップ２の焼結体表面をＳＥＭ反射
電子像で観察したところ、概ね表面の４１％の面積に結
合相が認められたのに対し、比較チップＢは表面全体、
即ち１００％の面積比率で表面に結合相が存在してい
た。When the surface of the sintered body of the chip 2 of the present invention was observed by an SEM backscattered electron image, a binder phase was observed in an area of approximately 41% of the surface, whereas in the comparative chip B, the entire surface,
That is, the binder phase was present on the surface at an area ratio of 100%.
【００３０】本発明チップ２および比較チップＢを、ダ
イヤモンド砥石で上下面のみ研削加工した後、下記条件
で切削試験評価を行った。
連続切削試験
被削材：ＳＣＭ４３５（ＨＢ＝２４６） 丸棒
切削速度：１５０ｍ／ｍｉｎ
送り：０．２１ｍｍ／ｒｅｖ．
切り込み：１．５ｍｍ
切削時間：１０分間
切削油：水溶性油
その結果、本発明チップの逃げ面摩耗量は０．０５６ｍ
ｍで刃先に被削材の溶着は認められず、被削材加工面の
光沢は非常に良好であった。一方、比較チップＢの逃げ
面摩耗量は０．０６２ｍｍであり、刃先部、特に焼結肌
である側面部への被削材の溶着は激しく、また被削材加
工面は明らかに白濁していた。The chip 2 of the present invention and the comparative chip B were grinded only on the upper and lower surfaces with a diamond grindstone, and then the cutting test was evaluated under the following conditions. Continuous cutting test Work material: SCM435 (HB = 246) Round bar Cutting speed: 150 m / min Feed: 0.21 mm / rev. Cut: 1.5 mm Cutting time: 10 minutes Cutting oil: Water-soluble oil As a result, the flank wear amount of the chip of the present invention is 0.056 m
At m, no welding of the work material was observed at the cutting edge, and the gloss of the work surface of the work material was very good. On the other hand, the flank wear amount of the comparative tip B was 0.062 mm, the welding of the work material to the cutting edge portion, particularly the side surface portion which is the sintered surface was severe, and the work surface of the work material was clearly clouded. It was
【００３１】（実施例３）原料粉末として、表３に示し
た原料粉末を、同じく表３に示した組成で湿式混合を８
Ｈｒ行った後、１ｔｏｎ／ｃｍ2の圧力にてプレス成形
し、真空中で５．０℃／ｍｉｎの昇温速度で１３９０℃
まで昇温し、真空中で１３９０℃の温度で６０分間保持
してから、水素１５Ｋｐａの雰囲気中で８００℃まで冷
却をを行い、ＪＩＳ４１２１規定のＳＮＭＡ１２０４１
２形状の「本発明焼結体３」を製造した。比較のため
に、冷却も真空中で行った同形状の「比較チップＣ」を
製造した。Example 3 As raw material powders, the raw material powders shown in Table 3 were wet-mixed with the same composition shown in Table 3 by 8 times.
After performing Hr, press molding was performed at a pressure of 1 ton / cm 2 , and the temperature was raised at 5.0 ° C./min in vacuum at 1390 ° C.
The temperature is raised to 1,390 ° C. in vacuum for 60 minutes, and then cooled to 800 ° C. in a hydrogen atmosphere of 15 Kpa.
Two-shaped "inventive sintered body 3" was produced. For comparison, a “comparative chip C” of the same shape was also produced, which was cooled in a vacuum.
【００３２】[0032]
【表３】 [Table 3]
【００３３】本発明チップ３の焼結体表面をＳＥＭ反射
電子像で観察したところ、概ね表面の３９％の面積に結
合相が認められたのに対し、比較チップＣは表面全体、
即ち１００％の面積比率で表面に結合相が存在してい
た。When the surface of the sintered body of the chip 3 of the present invention was observed by an SEM backscattered electron image, a binding phase was observed in an area of approximately 39% of the surface, whereas in the comparative chip C, the entire surface,
That is, the binder phase was present on the surface at an area ratio of 100%.
【００３４】本発明チップ３および比較チップＣを、ダ
イヤモンド砥石で上下面のみ研削加工し、さらに公知の
物理蒸着法でＴｉＮ膜を２μｍ形成した後、下記条件で
切削試験評価を行った。
連続切削試験
被削材：ＳＣＭ４３５（ＨＢ＝２４６） 丸棒
切削速度：１４０ｍ／ｍｉｎ
送り：０．２２ｍｍ／ｒｅｖ．
切り込み：２．０ｍｍ
切削時間：６分間
切削油：水溶性油
その結果、本発明チップの逃げ面摩耗量は０．０７２ｍ
ｍで刃先に被削材の溶着は認められず、また被削材加工
面の光沢は非常に良好であった。一方、比較チップＣの
逃げ面摩耗量は０．０９４ｍｍであり、刃先への被削材
の溶着、特に焼結肌である側面部での被覆膜の剥離およ
び被削材溶着は激しく、また被削材加工面は明らかに白
濁していた。The chip 3 of the present invention and the comparative chip C were ground by a diamond grindstone only on the upper and lower surfaces thereof, and a TiN film having a thickness of 2 μm was formed by a known physical vapor deposition method. Then, the cutting test was evaluated under the following conditions. Continuous cutting test Work material: SCM435 (HB = 246) Round bar Cutting speed: 140 m / min Feed: 0.22 mm / rev. Cut: 2.0 mm Cutting time: 6 minutes Cutting oil: Water-soluble oil As a result, the flank wear amount of the chip of the present invention is 0.072 m
At m, no welding of the work material was observed on the cutting edge, and the processed surface of the work material had very good gloss. On the other hand, the flank wear amount of the comparative tip C was 0.094 mm, and the welding of the work material to the cutting edge, especially the peeling of the coating film and the welding of the work material on the side surface, which is the sintered surface, was severe. The machined surface of the work material was clearly cloudy.
【００３５】[0035]
【発明の効果】以上説明したように、本発明の焼結方法
によれば、超硬合金やサーメット合金の焼結体表面の結
合相量を十分に規定された量に制御することができる。
従って、この様な表面を持った合金を使用して切削加工
を行うと、本発明の方法によらない合金に比べて耐溶着
性、耐摩耗性に優れるだけでなく、被削材加工面の光沢
性にも優れる。As described above, according to the sintering method of the present invention, the amount of binder phase on the surface of a sintered body of cemented carbide or cermet alloy can be controlled to a well-defined amount.
Therefore, when cutting is performed using an alloy having such a surface, not only is it superior in welding resistance and wear resistance as compared with an alloy not produced by the method of the present invention, Also excellent in gloss.
【００３６】また本発明の焼結方法により製造された合
金に、公知の方法により表面被覆層を形成した合金は、
本発明の焼結方法によらない合金に表面被覆層を形成し
た合金に比べて被覆層との間に十分な接着強度を持つ。
従って、この合金を使用して切削加工を行うと、被覆層
の耐剥離性に優れるだけでなく、耐摩耗性にも優れる。The alloy produced by the sintering method of the present invention and having a surface coating layer formed by a known method is
It has a sufficient adhesive strength with the coating layer as compared with the alloy in which the surface coating layer is formed on the alloy not based on the sintering method of the present invention.
Therefore, when cutting is performed using this alloy, not only the peel resistance of the coating layer is excellent, but also the wear resistance is excellent.
【図１】本発明チップ１の、ＳＥＭ反射電子像で観察し
た焼結体表面の写真。白く見えている部分はＷＣ結晶
で、黒く見えているところはＣｏである。FIG. 1 is a photograph of a surface of a sintered body of a chip 1 of the present invention observed by a SEM backscattered electron image. The part that looks white is WC crystal, and the part that looks black is Co.
【図２】比較チップＡの、ＳＥＭ反射電子像で観察した
焼結体表面の写真。白く見えている部分はＷＣ結晶で、
黒く見えているところはＣｏである。FIG. 2 is a photograph of the surface of a sintered body of Comparative Chip A observed by a SEM backscattered electron image. The part that looks white is WC crystal,
The part that looks black is Co.
【図３】本発明チップ１の、ＳＥＭ反射電子像で観察し
た焼結体表面の写真を、コンピュータを用いて白黒２階
層に画像処理したもの。FIG. 3 is a photograph of a surface of a sintered body of the chip 1 of the present invention observed by a SEM backscattered electron image, which is image-processed into two layers of black and white using a computer.
【図４】比較チップＡの、ＳＥＭ反射電子像で観察した
焼結体表面の写真を、コンピュータを用いて白黒２階層
に画像処理したもの。FIG. 4 is a photograph of a surface of a sintered body of a comparative chip A observed by an SEM backscattered electron image, which is image-processed into two layers of black and white using a computer.
Claims (3)
１種以上からなる結合相と、残部は不可避不純物からな
る硬質材料において、前記硬質相は炭化タングステンの
みからなる硬質材料の、焼結温度まで適切な雰囲気中で
加熱する工程と、冷却する工程とを含む焼結方法であっ
て、 前記冷却する工程を、焼結温度から 少なくとも１１０
０℃までは、０．０１〜４５Ｋｐａの圧力の水素雰囲気
中で行うことを特徴とする焼結方法。1. A hard material comprising a hard phase, a binder phase comprising 3 to 30% by weight of one or more iron-based metals, and the balance comprising inevitable impurities, wherein the hard phase comprises a hard material comprising only tungsten carbide. A method of sintering, comprising the steps of heating to a sintering temperature in an appropriate atmosphere and cooling, wherein the cooling step is performed at a temperature of at least 110 from the sintering temperature.
A sintering method, which is performed in a hydrogen atmosphere at a pressure of 0.01 to 45 Kpa up to 0 ° C.
１種以上からなる結合相と、残部は不可避不純物からな
る硬質材料において、前記硬質相は下記との材料か
ら構成される硬質材料の、焼結温度まで適切な雰囲気中
で加熱する工程と、冷却する工程とを含む焼結方法であ
って、 炭化タングステン 周期律表IVa，Va，VIa、族遷移金属と炭素、窒素、
酸素および硼素から選択される１種以上との化合物また
は固溶体相の、１種以上を、０．１〜５０重量％前記冷
却する工程を、焼結温度から少なくとも１１００℃まで
は、０．０１〜４５Ｋｐａの圧力の水素雰囲気中で行う
ことを特徴とする焼結方法。2. A hard material comprising a hard phase, a binder phase composed of 3 to 30% by weight of an iron-based metal, and the balance being inevitable impurities. The hard phase is composed of the following materials. What is claimed is: 1. A sintering method comprising heating a hard material to a sintering temperature in an appropriate atmosphere, and cooling the same, comprising: tungsten carbide, periodic table IVa, Va, VIa, group transition metal and carbon, nitrogen;
The step of cooling 0.1 to 50% by weight of one or more of the compound or solid solution phase with one or more selected from oxygen and boron, is 0.01 to A sintering method, which is performed in a hydrogen atmosphere at a pressure of 45 Kpa.
１種以上からなる結合相と、残部は不可避不純物からな
る硬質材料において、前記硬質相は下記の材料から構
成される硬質材料の、焼結温度まで適切な雰囲気中で加
熱する工程と、冷却する工程とを含む焼結方法であって
周期律表IVa，Va，VIa、族遷移金属と炭素、窒素、酸
素および硼素から選択される１種以上との化合物または
固溶体相の、１種以上前記冷却する工程を、焼結温度か
ら少なくとも１１００℃までは、０．０１〜４５Ｋｐａ
の圧力の水素雰囲気中で行うことを特徴とする焼結方
法。3. A hard material comprising a hard phase, a binder phase composed of 3 to 30% by weight of an iron-based metal, and the balance being inevitable impurities, wherein the hard phase is composed of the following materials: What is claimed is: 1. A sintering method comprising heating a material to a sintering temperature in an appropriate atmosphere, and cooling the material, comprising a periodic table IVa, Va, VIa, a group transition metal and carbon, nitrogen, oxygen and boron. The step of cooling one or more of the compound or solid solution phase with one or more selected is 0.01 to 45 Kpa from the sintering temperature to at least 1100 ° C.
A sintering method characterized in that the sintering is performed in a hydrogen atmosphere at a pressure of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001315657A JP2003119504A (en) | 2001-10-12 | 2001-10-12 | Method for sintering hard material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001315657A JP2003119504A (en) | 2001-10-12 | 2001-10-12 | Method for sintering hard material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003119504A true JP2003119504A (en) | 2003-04-23 |
Family
ID=19133785
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001315657A Withdrawn JP2003119504A (en) | 2001-10-12 | 2001-10-12 | Method for sintering hard material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2003119504A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110616357A (en) * | 2019-09-05 | 2019-12-27 | 长沙众鑫达工具有限公司 | Carbonitride-based cermet and preparation process thereof |
-
2001
- 2001-10-12 JP JP2001315657A patent/JP2003119504A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110616357A (en) * | 2019-09-05 | 2019-12-27 | 长沙众鑫达工具有限公司 | Carbonitride-based cermet and preparation process thereof |
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