JPS61127846A - High hardness sintered body and its manufacture - Google Patents
High hardness sintered body and its manufactureInfo
- Publication number
- JPS61127846A JPS61127846A JP24838384A JP24838384A JPS61127846A JP S61127846 A JPS61127846 A JP S61127846A JP 24838384 A JP24838384 A JP 24838384A JP 24838384 A JP24838384 A JP 24838384A JP S61127846 A JPS61127846 A JP S61127846A
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- particle size
- sintered body
- diamond particles
- powder
- 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
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- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は工具用高硬度焼結体およびその製造方法に関す
る。更に詳細には、本発明は、特にメッキ鋼線の如き高
硬度の鋼線の線引きダイスとして好適に使用される工具
用高硬度焼結体およびその製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a high hardness sintered body for tools and a method for manufacturing the same. More specifically, the present invention relates to a high-hardness sintered body for tools, which is particularly suitable for use as a drawing die for high-hardness steel wires such as plated steel wires, and a method for manufacturing the same.
従来の技術
現在、伸線用ダイスや非鉄金属、プラスチック、セラミ
ックの切削用に、ダイヤモンドが７０重量％を越した焼
結体が市販されている。これらの中でもダイヤモンド粒
度が細い焼結体は、特に銅線などの比較的軟かい線材を
伸線するダイスに使用した場合、伸線後の線表面は非常
になめらかで好評を博している。しかし、硬度の高いメ
ッキ鋼線、たとえば真鍮メッキ、亜鉛メッキ、銅メッキ
された高炭素鋼線の伸線では今のところ満足される性能
を有するダイヤモンド焼結体はない。BACKGROUND OF THE INVENTION Currently, sintered bodies containing more than 70% by weight of diamond are commercially available for wire drawing dies and for cutting nonferrous metals, plastics, and ceramics. Among these, sintered bodies with a fine diamond grain size have been well-received, especially when used in dies for drawing relatively soft wire materials such as copper wire, as the wire surface after drawing is extremely smooth. However, there is currently no diamond sintered body that has satisfactory performance in drawing highly hard plated steel wires, such as brass-plated, zinc-plated, and copper-plated high carbon steel wires.
発明の解決すべき問題点
まず、市販のダイヤモンド焼結体で高強度のメッキ鋼線
材を伸線した場合、満足した性能を示さない原因を調べ
るため、粒度３０〜６０μｍ、粒度２〜６μｍ及び特願
昭５３−２２３３３号公報に開示されている１μｍ以下
の３種のダイヤモンド焼結体を用いてダイスを作成し、
真鍮メッキされた鋼線を伸線した。Problems to be Solved by the Invention First, in order to investigate the reason why a high-strength plated steel wire rod drawn using a commercially available diamond sintered body does not exhibit satisfactory performance, A die was made using three types of diamond sintered bodies of 1 μm or less disclosed in Japanese Patent No. 53-22333,
Brass-plated steel wire was drawn.
ダイスが寿命となったときの線表面及びダイス内面を観
察した結果、どのダイスも内面に縦１が存在して荒れて
おり、伸線した線材表面にも、この傷が転写されていた
。傷の大きさは１〜３μｍ程度で非常に深い傷であった
。さらに、線材のメッキの付着量も減少していた。As a result of observing the wire surfaces and the inner surfaces of the dies when the dies reached the end of their lifespans, it was found that all the dies had vertical scratches on their inner surfaces and were rough, and these scratches were also transferred to the surface of the drawn wire. The size of the scratch was approximately 1 to 3 μm, and it was a very deep scratch. Furthermore, the amount of plating deposited on the wire rod was also reduced.
この問題を添付の図面を参照して詳細に説明する。第１
図は線引きダイスにより線材が引き抜かれる状態を示し
ており、ダイスＤの内面はつぎの４つの部分に分類でき
る。This problem will be explained in detail with reference to the attached drawings. 1st
The figure shows the state in which the wire is drawn by the wire drawing die, and the inner surface of the die D can be classified into the following four parts.
すなわち、線材Ｓが矢印Ｆの方向に引き抜かれてダイス
Ｄの内面に近接するときの最初の部分をアプローチ部１
といい、レダクション部２では線材Ｓがこの部分を通過
することによりその断面積減少が生じ、その後方の線材
Ｓが通過する部分をベアリング部３と称し、線材Ｓはバ
ックリリーフ部４でダイスＤの内面から離間する。That is, when the wire S is pulled out in the direction of the arrow F and comes close to the inner surface of the die D, the initial part is called the approach section 1.
In the reduction part 2, the cross-sectional area of the wire S is reduced as it passes through this part, and the part behind it through which the wire S passes is called the bearing part 3, and the wire S passes through the die D in the back relief part 4. separated from the inner surface of
まず、ダイス内面に上記したような傷が発生するのは、
次のように推定できる。用いたダイヤモンド焼結体は、
いずれもダイヤモンド粒子同士が強固に接合してダイヤ
モンドスケルトン（ダイヤモンド粒子相互の結合部分）
を形成しているものの、粒度３０〜６０μｍのダイヤモ
ンド焼結体は第１図に示しである線材とダイスが接触し
、その断面積減少ががおこなわれ大きな負荷が生ずるリ
ダクション部２でダイヤモンドスケルトン部やダイヤモ
ンド粒子のエッヂが破壊して、脱落し、それらの破損し
たダイヤモンド粒子がダイス内面を引かいて傷つけたも
のと考えられる。First of all, the scratches mentioned above occur on the inner surface of the die.
It can be estimated as follows. The diamond sintered body used was
In both cases, diamond particles are strongly bonded to each other to create a diamond skeleton (the bonding part between diamond particles).
However, the diamond sintered body with a particle size of 30 to 60 μm has a diamond skeleton part in the reduction part 2 where the wire rod and the die come into contact as shown in Figure 1, and the cross-sectional area is reduced and a large load is generated. It is thought that the edges of the diamond particles were broken and fell off, and these broken diamond particles scratched the inner surface of the die and caused damage.
また２〜６μｍのダイヤモンド焼結体では、ダイスのり
ダクション部２でダイヤモンドスケルトンが欠損するよ
りもむしろ２μｍ程度のダイヤモンド粒子が脱落して内
面を傷つけたものと思われる。Moreover, in the diamond sintered body with a diameter of 2 to 6 μm, it is thought that rather than the diamond skeleton being damaged at the die paste reduction portion 2, diamond particles of approximately 2 μm fell off and damaged the inner surface.
一方、１μｍ以下のダイヤモンド粒子より成る焼結体は
個々のダイヤモンド粒子の脱落と同時に数個のダイヤモ
ンド粒子のかたまりが脱落して、ダイス内面に微細な傷
とともに大きな傷をつけ、この傷により線材表面が引っ
かかれたものと考えられる。On the other hand, in the case of a sintered body made of diamond particles of 1 μm or less, a cluster of several diamond particles falls off at the same time as the individual diamond particles fall off, causing large scratches as well as minute scratches on the inner surface of the die. It is thought that it was scratched.
以上のように従来のダイヤモンド焼結体が使用できない
理由として、ダイヤモンドスケルトン部の欠損や、ダイ
ヤモンド粒子の脱落のため、ダイス内面に傷をつけ、こ
の傷が線材表面に転写されるからであることが判明した
が、ダイヤモンドスケルトン部の欠損やダイヤモンド粒
子の脱落が生じる原因について更に考察する。As mentioned above, the reason why conventional diamond sintered bodies cannot be used is that the diamond skeleton part is damaged or the diamond particles fall off, causing scratches on the inner surface of the die, and these scratches are transferred to the wire surface. However, we will further consider the causes of defects in the diamond skeleton and the falling off of diamond particles.
伸線時、ダイス内面には線材により垂直力と摩擦力が負
荷される。通常、固体接触面間に垂直力と摩擦力が作用
した場合にはせん断力や主応力が発生する。たとえば第
１図に示したダイス５の内面では、リダクション部２の
線材６とダイスの接触点で最大主応力が発生し、ベアリ
ング部３とバックＩＪ ＩＪ−フ部４の交点近傍で最大
せん断力が発生する。特に高強度の線材を伸線した場合
は、垂直力や摩擦力が増加し、最大主応力や最大せん断
力が大きくなる。一方、ダイヤモンド焼結体のダイヤモ
ンドスケルトン部は触媒金属等の不純物を含有するため
、焼結体の中で最も強度の低い部分である。この部分に
上記した主応力やせん断力が加わった場合、スケルトン
部の不純物を含んだ箇所に集中応力が負荷され破損しや
すい。During wire drawing, vertical force and frictional force are applied to the inner surface of the die by the wire rod. Normally, shear force and principal stress occur when normal force and frictional force act between solid contact surfaces. For example, on the inner surface of the die 5 shown in FIG. occurs. In particular, when a high-strength wire is drawn, the normal force and frictional force increase, and the maximum principal stress and maximum shearing force increase. On the other hand, the diamond skeleton portion of the diamond sintered body contains impurities such as catalytic metals, so it is the part with the lowest strength in the sintered body. If the above-mentioned principal stress or shear force is applied to this part, concentrated stress will be applied to the part of the skeleton part containing impurities, which will easily cause damage.
特にリダクション部２では線材との接触部が絶えず変動
するため繰返し応力が加わり、クラックが進展して破壊
するものと思われる。ダイヤモンド粒子が３０〜６０μ
ｍと大きい焼結体の場合には、前述した如く、リダクシ
ョン部２の表面近傍、特に表面下３μｍの部分に最大主
応力が発生するため、ダイヤモンド粒子周辺のスケルト
ン部は全て破壊されないが、表面層に近いスケルトン部
のみが先に破壊されて脱落する。ただし、大きなダイヤ
モンド粒子そのものは脱落し難い。Particularly in the reduction part 2, since the contact part with the wire constantly fluctuates, repeated stress is applied, and it is thought that cracks develop and break. Diamond particles are 30~60μ
In the case of a sintered body as large as m, as mentioned above, the maximum principal stress occurs near the surface of the reduction part 2, especially in the part 3 μm below the surface. Only the skeleton part close to the layer is destroyed first and falls off. However, large diamond particles themselves are difficult to fall off.
一方２〜６μｍのダイヤモンド焼結体は、ダイヤモンド
粒子が小さいため、スケルトン部も小さく、スケルトン
部が破壊されてダイヤモンド粒子が脱落する。１μｍ以
下のダイヤモンド焼結体はさらにスケルトン部が小さく
なるため、ダイヤモンド粒子数個が集団となって脱落す
ることがあり、これが内面に大きな傷をつけたものと思
われる。On the other hand, in a diamond sintered body having a diameter of 2 to 6 μm, since the diamond particles are small, the skeleton portion is also small, and the skeleton portion is destroyed and the diamond particles fall off. Since the skeleton portion of a diamond sintered body of 1 μm or less becomes even smaller, several diamond particles may fall off as a group, which is thought to have caused large scratches on the inner surface.
また線材のメッキ付着量が減少した原因としては次の如
く推定される。ダイスで伸線された線材は、バックリリ
ーフ部４で弾性回復して線径が太くなるが、このとき、
バックリリーフ部４の粗さが荒いと、この部分で線表面
が引っかかれて、メッキ層が削り取られる。前述した如
くリダクション部２で脱落したダイヤモンド粒子は、ベ
アリング部３のみならずバックＩＪ ＩＪ−フ部まで傷
をつけるのでダイス内面の傷が増せばメッキは付着量も
減少するものと考えられる。Furthermore, the reason for the decrease in the amount of plating on the wire is presumed to be as follows. The wire drawn with the die elastically recovers in the back relief part 4 and the wire diameter becomes thicker, but at this time,
If the back relief portion 4 is rough, the wire surface will be scratched at this portion and the plating layer will be scraped off. As mentioned above, the diamond particles falling off in the reduction part 2 damage not only the bearing part 3 but also the back IJ-IJ-F part, so it is thought that as the number of scratches on the inner surface of the die increases, the amount of plating deposited also decreases.
以上の如く、従来のダイヤモンド焼結体のダイスでは、
メッキ鋼線の如き高硬度の線材用に用いると、ダイスが
損傷し、この疵が線材表面に転写され、美麗な表面の線
材が得られないばかりか、ダイス寿命も短く、満足な性
能を提供できなかった。As mentioned above, in the conventional diamond sintered die,
If used for high hardness wire such as plated steel wire, the die will be damaged and the flaws will be transferred to the surface of the wire, making it impossible to obtain a wire with a beautiful surface, and the life of the die will be short, resulting in unsatisfactory performance. could not.
上記した実験の結果より本発明者は、従来のダイヤモン
ド焼結体の欠点を克服するには、微粒ダイヤモンド焼結
体の場合にはダイヤモンド粒子が集団となって脱落する
ことを防止し、また粗粒ダイヤモンド焼結体の場合には
ダイヤモンドスケルトン部で大きく欠損することを抑制
する必要があることを確δ忍した。Based on the results of the above experiments, the present inventor has determined that in order to overcome the drawbacks of conventional diamond sintered bodies, in the case of fine-grained diamond sintered bodies, it is necessary to prevent the diamond particles from falling off in groups, and to prevent the diamond particles from falling off as a group. It was confirmed that in the case of a grained diamond sintered body, it is necessary to suppress large defects in the diamond skeleton.
すなわち、本発明の目的は、耐摩耗性および強度に優れ
たダイヤモンド焼結体およびその製造方法を提供するこ
とにある。That is, an object of the present invention is to provide a diamond sintered body having excellent wear resistance and strength, and a method for manufacturing the same.
さらに詳細には本発明の目的は、メッキ鋼線の如き高硬
度の線材用の線引きダイスに好適に用いられるダイヤモ
ンド焼結体およびその製造方法を提供することにある。More specifically, an object of the present invention is to provide a diamond sintered body suitable for use in a wire drawing die for high-hardness wire such as plated steel wire, and a method for manufacturing the same.
問題点を解決する手段
本発明者等は、前記従来技術のダイヤモンド焼結体の欠
点を改良すべく鋭意研究を重ねた。Means for Solving the Problems The present inventors have conducted extensive research in order to improve the drawbacks of the diamond sintered bodies of the prior art.
まず、粗粒ダイヤモンド粒子を含む焼結体の場合のダイ
スの欠損を抑制するため、強度の高い粗粒ダイヤモンド
粉末を用いて、焼結ダイヤモンドダイスを作成し、真鍮
メッキされた鋼線を伸線したが、ダイヤモンド粒子の破
壊は抑制されなかった。次に１μｍ〜数μｍのダイヤモ
ンド焼結体の粒子の脱落防止のため、本発明者等のうち
の１人が発明者であり、本出願人による先願である特開
昭５７−４７７７１号公報に開示されている焼結ダイヤ
モンドからなるダイスを試作し、伸線テストを行ったと
ころ、焼結ダイヤモンドに高応力が負荷される場合は、
この焼結ダイヤモンドは含有される炭化物が多いため、
ダイヤモンド同士の結合力が十分でなく、１μｍ以上の
ダイヤモンド粒子の脱落は抑制できないことが判明した
。First, in order to suppress die breakage in the case of a sintered body containing coarse-grained diamond particles, a sintered diamond die was created using high-strength coarse-grained diamond powder, and a brass-plated steel wire was drawn. However, the destruction of diamond particles was not suppressed. Next, in order to prevent particles of 1 μm to several μm of the diamond sintered body from falling off, one of the inventors of the present invention is an earlier application filed by the present applicant, JP-A-57-47771. When we prototyped a die made of sintered diamond disclosed in 2003 and conducted a wire drawing test, we found that when high stress is applied to sintered diamond,
This sintered diamond contains many carbides, so
It was found that the bonding force between diamonds was not sufficient to prevent diamond particles of 1 μm or more from falling off.
これらの実験の後に本発明者等は、所定の粒度分布のダ
イヤモンド粉末を用いてダイヤモンド焼結体を製造する
ことによって、上記した如き問題が解決されることを見
出した。After these experiments, the present inventors discovered that the above-mentioned problems could be solved by manufacturing a diamond sintered body using diamond powder having a predetermined particle size distribution.
すなわち、本発明に従うと、８０〜９５容量％のダイヤ
モンド粒子と、０．５〜５容量％の１μｍ以下のＷＣま
たは（Ｍｏ、Ｗ）Ｃと、４．５〜１５容量％の鉄族金属
とを含み、該ダイヤモンド粒子の少なくとも９５容量％
以上は最大粒径が２μｍで且つ最小粒径が０．１μｍで
あり、残部が０．１μｍ以下の粒径のダイヤモンド粒子
であることを特徴とする工具用高硬度焼結体が提供され
る。That is, according to the present invention, 80-95% by volume of diamond particles, 0.5-5% by volume of WC or (Mo, W)C of 1 μm or less, and 4.5-15% by volume of iron group metal. comprising at least 95% by volume of the diamond particles.
The above provides a high-hardness sintered body for tools, characterized in that the maximum particle size is 2 μm, the minimum particle size is 0.1 μm, and the remainder is diamond particles with a particle size of 0.1 μm or less.
本発明に従うと、焼結体のダイヤモンド粒子において、
１〜２μｍの粒径のダイヤモンド粒子の容量と、０．１
〜１μｍの粒径のダイヤモンド粒子の容量との割合が４
〜１であることが好ましい。According to the present invention, in the diamond particles of the sintered body,
The capacity of diamond particles with a particle size of 1-2 μm and 0.1
The ratio of diamond particles with a particle size of ~1 μm to the volume is 4
It is preferable that it is 1.
更に本発明に従うと、最大粒径が２μｍで且つ最小粒径
が０．２μｍであるダイヤモンド粉末を調整し、該ダイ
ヤモンド粉末と、鉄族金属および１μｍ以下のＷＣまた
は（Ｍｏ、 Ｗ） Ｃ粉末とを、ダイヤモンド粉末が８
０〜９５容量％、ＷＣまたは（Ｍｏ、 Ｗ） Ｃ粉末が
０．５〜５５容量、鉄族金属が４．５〜１５容量％の割
合で混合し、得られた混合物を、超高圧高温装置を用い
てダイヤモンドが安定な高温、高圧下でホットプレスす
ることを特徴とする工具用高硬度焼結体の製造方法が提
供される。Furthermore, according to the present invention, a diamond powder having a maximum particle size of 2 μm and a minimum particle size of 0.2 μm is prepared, and the diamond powder is combined with an iron group metal and a WC or (Mo, W) C powder of 1 μm or less. , diamond powder is 8
0 to 95% by volume, 0.5 to 55% by volume of WC or (Mo, W)C powder, and 4.5 to 15% by volume of iron group metal, and the resulting mixture was heated in an ultra-high pressure and high temperature apparatus. Provided is a method for producing a high-hardness sintered body for tools, which is characterized by hot pressing under high temperature and high pressure in which diamond is stable.
更に、本発明の１態様に従うと、原料粉末の混合を、Ｗ
Ｃまたは（Ｍｏ、 Ｗ） Ｃを鉄族金属で結合したサー
メットで内張したポット及びボールを用いて行い、この
混合処理によりポット及びボールより１μｍ以下のＷＣ
もしくは（Ｍｏ、 Ｗ） Ｃの微粉末を混入させる。Furthermore, according to one aspect of the present invention, the raw material powder is mixed with W.
A pot and a ball lined with cermet bonded with C or (Mo, W) C are used. Through this mixing process, WC of 1 μm or less is removed from the pot and ball.
Alternatively, fine powder of (Mo, W) C is mixed.
さらに本発明に従うと、鉄族金属をダイヤモンド粉末の
焼結中に溶浸せしめてもよい。Further according to the invention, iron group metals may be infiltrated during sintering of the diamond powder.
発明の作用
上記した本発明のダイヤモンド焼結体が優れた性能を有
するのは次の如く考えられる。Effect of the Invention The reason why the diamond sintered body of the present invention described above has excellent performance is considered to be as follows.
本発明のダイヤモンド焼結体の特徴は、そのダイヤモン
ド粒子の粒度分布にある。０．２〜２μｍの粒度分布を
有するダイヤモンド粉末を出発原料として用いることに
より、１μｍ以下のダイヤモンド粒子の周りにい１μｍ
未満の微粒ダイヤモンド粒子が分散している焼結体構造
となるため、微粒ダイヤモンド粒子が集団塊となって脱
落することが防止されるとともに、また１μｍ以上のダ
イヤモンド粒子は、微粒ダイヤモンド粒子と強固に結合
して、これらの１μｍ以上の粒子の脱落が抑制されるか
らである。The diamond sintered body of the present invention is characterized by the particle size distribution of its diamond particles. By using diamond powder with a particle size distribution of 0.2 to 2 μm as a starting material, a particle size of 1 μm around diamond particles of 1 μm or less can be obtained.
Since the sintered body has a structure in which fine diamond particles with a diameter of less than 1 μm are dispersed, it is possible to prevent the fine diamond particles from forming clusters and falling off. This is because the bonding suppresses the falling off of these particles with a diameter of 1 μm or more.
換言すると、本発明のダイヤモンド焼結体中のダイヤモ
ンド粒子の少なくとも９５容量％は最大粒径が２μｍ１
最小粒径が０．１μｍである。ダイヤモンドの粒径が２
μｍを越すと、伸線中にこのようなダイヤモンド粒子が
脱落すれば、線材表面が引っかかれて線材およびダイス
表面が粗くなるとともに、メッキの付着量が低下する。In other words, at least 95% by volume of the diamond particles in the diamond sintered body of the present invention have a maximum particle size of 2 μm1.
The minimum particle size is 0.1 μm. Diamond particle size is 2
If the diameter exceeds μm, if such diamond particles fall off during wire drawing, the surface of the wire will be scratched, making the wire and die surfaces rough, and the amount of plating deposited will decrease.
一方、粒径が０．１μｍ未満のダイヤモンド粒子を多量
に、すなわち、含有されるダイヤモンド粒子の５容量％
以上含む場合には、微粒ダイヤモンド粒子が集団塊とな
りやすく、ダイヤモンドの焼結性が低下して容易に脱落
するので好ましくない。特に１〜２μｍの粒径のダイヤ
モンド粒子と、０．１〜１μｍのダイヤモンド粒子とが
４〜１の割合いで含有されるき、上述した如く、比較的
大きなダイヤモンド粒子の周りに比較的微細な粒子が分
散して、それらのダイヤモンド粒子全体が相互に強固に
保持しあう状態となり、ダイヤモンド粒子の脱落が非常
に少なく、優れた性能を示す。On the other hand, a large amount of diamond particles with a particle size of less than 0.1 μm, that is, 5% by volume of the diamond particles contained.
If the content is more than that, the fine diamond particles tend to form agglomerates, which deteriorates the sinterability of the diamond and makes it easy to fall off, which is not preferable. In particular, when diamond particles with a particle size of 1 to 2 μm and diamond particles with a particle size of 0.1 to 1 μm are contained in a ratio of 4 to 1, as described above, relatively fine particles are formed around relatively large diamond particles. is dispersed, and all of the diamond particles are firmly held together, resulting in very few diamond particles falling off and exhibiting excellent performance.
従って、焼結体中のダイヤモンド粒子全体の少なくとも
９５容量％以上は、最大粒径が２μｍで且つ最小粒径が
０．１μｍであり、残部が０，１μｍ以下の粒径のダイ
ヤモンド粒子であることが必要である。Therefore, at least 95% by volume of all the diamond particles in the sintered body must have a maximum particle size of 2 μm and a minimum particle size of 0.1 μm, with the remainder being diamond particles with a particle size of 0.1 μm or less. is necessary.
本発明に従うと、ダイヤモンド粒子の含有量は、８０〜
９５容量％である。ダイヤモンド粒子の含有量が８０容
量％未満であれば炭化物や鉄族金属の含有量が増し、ダ
イヤモンド同士の結合部が少なく、ダイヤモンド粒子の
保持力が弱く、耐摩耗性に劣る。一方、ダイヤモンド粒
子の含有量が９５容景％を越えると、結合材である鉄族
金属の量が減るためダイヤモンド粒子は脱落しやすくな
る。According to the invention, the content of diamond particles is between 80 and
It is 95% by volume. If the content of diamond particles is less than 80% by volume, the content of carbides and iron group metals will increase, there will be few bonding parts between diamonds, the holding power of diamond particles will be weak, and the wear resistance will be poor. On the other hand, when the content of diamond particles exceeds 95% by volume, the amount of iron group metal as a binder decreases, so that the diamond particles tend to fall off.
ＷＣまたは（Ｍｏ、 Ｗ） Ｃの含有量は０．５〜５容
量％である。これら炭化物の含有量が０．５％未満の場
合、微粒ダイヤモンド粒子の近傍に鉄族金属の異常集積
部が発生し、ダイヤモンド粒子の結合強度が低下する。The content of WC or (Mo, W)C is 0.5 to 5% by volume. When the content of these carbides is less than 0.5%, abnormal accumulations of iron group metals occur near the fine diamond particles, and the bonding strength of the diamond particles decreases.
一方、炭化物の含有量が５容量％を越すとダイヤモンド
粒子同士の結合部に介在する炭化物量が多くなるため、
ダイヤモンドスケルトン部の強度が低下しダイヤモンド
粒子が脱落しやすくなる。On the other hand, if the carbide content exceeds 5% by volume, the amount of carbides intervening in the joints between diamond particles increases.
The strength of the diamond skeleton portion decreases and the diamond particles tend to fall off.
本発明に従うと、結合材として含有する鉄族金属の含有
量は４．５〜１５容量％である。鉄族金属の含有量が４
．５容量％未満ではダイヤモンド粒子が脱落しやすくな
り、また、１５容量％を越えるとダイヤモンド粒子の含
有量が減るため耐摩耗性が低下する。According to the present invention, the content of iron group metal contained as a binder is 4.5 to 15% by volume. The content of iron group metals is 4
．． If it is less than 5% by volume, diamond particles tend to fall off, and if it exceeds 15% by volume, the content of diamond particles decreases, resulting in a decrease in wear resistance.
本発明の焼結体に使用するダイヤモンド原料粉末として
は、０．２μｍ〜２μｍのダイヤモンド粒子であれば、
合成ダイヤモンド、天然ダイヤモンドのいずれでもよい
。このようなダイヤモンド粉末とＷＣもしくは（Ｍｏ、
Ｗ） Ｃ粉末及びＦｅ、 Ｃｏ、Ｎｉの鉄族金属粉末
を均一にボールミル等の手段を用いて混合するのが好ま
しい。この鉄族金属は予め混合せずに焼結時に溶浸せし
めても良い。The diamond raw material powder used in the sintered body of the present invention may include diamond particles of 0.2 μm to 2 μm.
Either synthetic diamond or natural diamond may be used. Such diamond powder and WC or (Mo,
W) It is preferable to uniformly mix the C powder and the iron group metal powders of Fe, Co, and Ni using a means such as a ball mill. This iron group metal may be infiltrated during sintering without being mixed in advance.
また本出願人等の先願発明（特開昭５２−５１３８１号
）の如く、ＷＣもしくは（Ｍｏ、 Ｗ） Ｃと鉄族金属
の焼結体のライニングを有するポットとボールでダイヤ
モンド粉末をボールミル粉砕すると同時にポットとボー
ルからＷＣもしくは（Ｍｏ、Ｗ）Ｃと鉄族金属からなる
焼結体の微細粉末を混入せしめることも可能である。In addition, as in the prior invention of the present applicant (Japanese Patent Laid-Open No. 52-51381), diamond powder is ball-milled using a pot and ball lined with a sintered body of WC or (Mo, W)C and an iron group metal. At the same time, it is also possible to mix in fine powder of a sintered body made of WC or (Mo, W)C and an iron group metal from a pot and a ball.
混合した粉末、あるいはこの混合した粉末を１３００℃
以上の温度で加熱してダイヤモンドの一部を黒鉛化した
粉末を超高圧装置に入れ、ダイヤモンドが安定な条件下
で焼結する。このとき使用した鉄族金属と炭化物等の化
合物間に生じる共晶液相の出現温度以上で焼結する必要
がある。本発明のダイヤモンド焼結体は高強度の線材を
線引する場合、焼結ダイヤモンドダイス内面には高圧力
が発生するが、ダイヤモンド焼結体の外径が小さく肉厚
がうすくなる場合は、伸線中にダイヤモンド焼結体が縦
方向に割れることがある。このような場合はダイヤモン
ド焼結体の外周をＷＣまたは（Ｍｏ、 Ｗ） Ｃを鉄族
金属で焼結したサーメブト支持体で包囲してダイヤモン
ド焼結体の外周から予圧を加えることにより伸線中の縦
割れを防止することが可能である。本発明の焼結体をメ
ッキ鋼線伸線用のダイスとして使用する場合、その性能
を十分発揮させるには、ベアリング部からバックリリー
フ部に至る部分を滑らかに仕上る必要がある。Mixed powder or this mixed powder at 1300℃
The diamond powder, which has been partially graphitized by heating at above temperatures, is placed in an ultra-high pressure device and sintered under conditions where the diamond is stable. At this time, it is necessary to sinter at a temperature higher than the temperature at which a eutectic liquid phase appears between the iron group metal and the compound such as carbide used. When the diamond sintered body of the present invention is used to draw a high-strength wire, high pressure is generated on the inner surface of the sintered diamond die, but when the outer diameter of the diamond sintered body is small and the wall thickness is thin, The diamond sintered body may crack vertically during the wire. In such a case, the outer periphery of the diamond sintered body is surrounded by a thermbut support made of WC or (Mo, W)C sintered with an iron group metal, and preload is applied from the outer periphery of the diamond sintered body during wire drawing. It is possible to prevent vertical cracking. When the sintered body of the present invention is used as a die for drawing plated steel wire, in order to fully exhibit its performance, it is necessary to finish the part from the bearing part to the back relief part smoothly.
本発明の焼結体は微粒ダイヤモンド粒子より成るため、
強度が非常に高く、またダイヤモンド粒子同士の結合力
が高いため、耐摩耗性が優れたものである。したがって
、本発明の焼結体の用途としては、ダイスの他に切削工
具にも使用できる。Since the sintered body of the present invention is composed of fine diamond particles,
It has very high strength and high bonding strength between diamond particles, so it has excellent wear resistance. Therefore, the sintered body of the present invention can be used not only for dies but also for cutting tools.
特に本発明焼結体は微粒ダイヤモンド粒子同士が強固に
結合されているため切削工具として使用した場合、被削
面は非常に滑らかに仕上げることができ、また焼結体の
耐摩耗性が優れるととにも切゛ 削工具として使用する
場合、ダイヤモンド焼結体の靭性をさらに向上させるた
め、超硬合金等の支持体に超高圧焼結中に接合させるこ
とも可能である。In particular, the fine diamond particles of the sintered body of the present invention are strongly bonded to each other, so when used as a cutting tool, the cut surface can be finished very smoothly, and the sintered body has excellent wear resistance. In order to further improve the toughness of the diamond sintered body when used as a cutting tool, it is also possible to bond it to a support such as cemented carbide during ultra-high pressure sintering.
以下、実施例により本発明を具体的に説明するが、これ
らの実施例は本発明の単なる例示であり、本発明の技術
的範囲を何隻制限するものではない。EXAMPLES Hereinafter, the present invention will be specifically explained with reference to Examples, but these Examples are merely illustrative of the present invention and do not limit the technical scope of the present invention.
実施例１
粒径０．５〜１μｍと粒径１〜２μｍの合成ダイヤモン
ドを３ニアの割合で混合し、この粉末を（Ｍｏ’、 Ｗ
） Ｃ−Ｎｉ−Ｃｏ製のポットとボールを用いて１時間
ボールミルした。得られた粉末は、粒径０．２〜１μｍ
と粒径１〜２μｍの割合が３５：６５であるダイヤモン
ド粒子９５．５容量％、（Ｍｏ、 Ｗ） Ｃ３，３容量
％、Ｃｏ＋Ｎｉ １．２容量％であった。Example 1 Synthetic diamonds with a particle size of 0.5 to 1 μm and a particle size of 1 to 2 μm were mixed at a ratio of 3 nia, and this powder was mixed with (Mo', W
) Ball milling was carried out for 1 hour using a pot and ball made of C-Ni-Co. The obtained powder has a particle size of 0.2 to 1 μm.
95.5% by volume of diamond particles with a particle size ratio of 1 to 2 μm of 35:65, 3% by volume of (Mo, W)C, and 1.2% by volume of Co+Ni.
この混合粉末を予備処理した後、（Ｍｏ、 Ｗ）Ｃ−Ｎ
ｉ−Ｃｏの容器に詰め、超高圧装置を用いて先ず圧力５
５Ｋｂを加え、引き続いて１４００℃に加熱して、１５
分間保持した。焼結体を取り出して組織観察したところ
０．２〜２μｍのダイヤモンド粒子同士が強固に結合し
ていた。この焼結体を分析したところダイヤモンド粒子
が８８容量％、（Ｍｏ、Ｗ）Ｃが２．７容量％、Ｃｏ＋
Ｎｉが９．３容量％であった。この焼結体と市販の粒度
１μｍ以下の焼結ダイヤモンド、２〜６μｍの粒度の焼
結ダイヤモンド及び３０〜６０μｍの焼結ダイヤモンド
を加工して穴径０．２５０ｍｍのダイスに仕上げた。ダ
イスの加工に際してはバックＩＪ ＩＪ−７部も仕上げ
研摩した。これらのダイスを用いて、線速１０００ ｍ
／ｍｉｎで潤滑油中で真鍮メッキした鋼線を伸線した
。After pre-treating this mixed powder, (Mo, W)C-N
It is packed in an i-Co container and first heated to a pressure of 5% using an ultra-high pressure device.
5 Kb was added, followed by heating to 1400°C, and 15
Hold for minutes. When the sintered body was taken out and its structure was observed, it was found that diamond particles of 0.2 to 2 μm were firmly bonded to each other. Analysis of this sintered body revealed that diamond particles were 88% by volume, (Mo, W)C was 2.7% by volume, Co+
Ni was 9.3% by volume. This sintered body was processed with commercially available sintered diamonds having a particle size of 1 μm or less, sintered diamonds having a particle size of 2 to 6 μm, and sintered diamonds having a particle size of 30 to 60 μm to form a die with a hole diameter of 0.250 mm. When processing the die, the back IJ and IJ-7 portions were also finished and polished. Using these dies, linear speed of 1000 m
Brass-plated steel wire was drawn in lubricating oil at a speed of 1/min.
その結果、本発明のダイヤモンド焼結体のダイスでは５
．６ｔｏｎの線材を伸線できたのに対し、粒度１μｍ以
下の焼結ダイヤモンドダイスは２． Ｑｔｏｎ。As a result, in the die of the diamond sintered body of the present invention, 5
．． While it was possible to draw a 6 ton wire, a sintered diamond die with a grain size of 1 μm or less was only 2. Qton.
２〜６μｍの焼結ダイヤモンドダイスは２．１ｔｏｎ。The 2-6 μm sintered diamond die weighs 2.1 tons.
３０〜６０μｍの焼結ダイヤモンドダイスは１．５ｔｏ
ｎを伸線して寿命となった。30~60μm sintered diamond die is 1.5to
The life of the wire was reached when the wire was drawn.
実施例２
各種の粒度のダイヤモンド粉末をＷＣまたは（Ｍｏ、
Ｗ）Ｃ，およびＣｏまたは（Ｎｉ＋Ｃｏ）粉末と完全に
混合して、第１表に示す粒度および組成の完成粉末を作
成した。Example 2 Diamond powders of various particle sizes were mixed with WC or (Mo,
W) C, and Co or (Ni+Co) powders were thoroughly mixed to produce finished powders with particle sizes and compositions shown in Table 1.
この完成粉末を予備処理後、Ｔａ製の容器に充填し、実
施例１と同様にして焼結した後０．１７５ｍｍの穴径の
ダイスに仕上げた。これらのダイスを用いて線速１００
０ ｍ ／ｍ１ｎｔ、潤滑油中で真鍮メッキした鋼線を
伸線した。その結果を第１表に示す。After preliminary treatment, this finished powder was filled into a container made of Ta and sintered in the same manner as in Example 1, and then finished into a die with a hole diameter of 0.175 mm. Linear speed 100 using these dies
Brass-plated steel wire was drawn at 0 m/m1 nt in lubricating oil. The results are shown in Table 1.
実施例３
実施例２で作成した表ＩＣの焼結体を実施例１と同様に
して加工し穴径１．２ｍｍのダイスに仕上げた。これら
のダイスを用いて銅メッキされた鋼線を４００ｍ／ｍｉ
ｎ湿式で伸線した。比較のため粒度３０〜６０μｍの市
販のダイヤモンド焼結体及び超硬合金のダイスも作成し
テストした。Example 3 The sintered body shown in Table IC prepared in Example 2 was processed in the same manner as in Example 1 to form a die with a hole diameter of 1.2 mm. Using these dies, copper-plated steel wire can be cut at 400m/mi.
The wire was drawn using a wet method. For comparison, commercially available diamond sintered bodies and cemented carbide dies with particle sizes of 30 to 60 μm were also prepared and tested.
その結果本発明焼結体Ｃのダイスでは７０ｔｏｎの線材
を伸線可能であったのに対し、市販の焼結ダイヤモンド
ダイスは２Ｑｔｏｎの線材を、 超硬合金ダイスは８０
０ｋｇの線材を伸線した時点で寿命となった。As a result, the die of the sintered body C of the present invention was able to draw a wire rod of 70 tons, whereas the commercially available sintered diamond die could draw a wire rod of 2 Q tons, and the cemented carbide die could draw a wire rod of 80 tons.
The life span was reached when 0 kg of wire was drawn.
実施例４
実施例２で試作した表ＩＤの焼結体を研削して、切削加
工用のバイトを作成した。比較のため１０μｍ以下のダ
イヤモンド粒子より成る市販の焼結ダイヤモンドのバイ
トも作成した。これらのバイトを加工するのに要した時
間は本発明焼結体で１０分、市販の焼結ダイヤモンドで
２５分であった。これらのバイトを用いて、Ａｌ−２５
％Ｓｉを速度３００ｍ／ｍｉｎ、切込みＱ、 ２ｍｍ、
送り０．０５ｍｍ ／ ｒｅｖで６０分間切削し、工具
の逃げ面摩耗を測定した。本発明焼結体は、０、０４０
ｍｍであったのに対し、市販の焼結ダイヤモンドバイト
は０．０４３ｍｍであった。Example 4 The sintered body shown in Table ID produced as a prototype in Example 2 was ground to create a cutting tool. For comparison, a commercially available sintered diamond cutting tool consisting of diamond particles of 10 μm or less was also prepared. The time required to process these bits was 10 minutes for the sintered body of the present invention and 25 minutes for the commercially available sintered diamond. Using these bits, Al-25
%Si at a speed of 300 m/min, depth of cut Q, 2 mm,
Cutting was performed for 60 minutes at a feed rate of 0.05 mm/rev, and the flank wear of the tool was measured. The sintered body of the present invention has 0.040
mm, whereas the commercially available sintered diamond bite was 0.043 mm.
また、被削材の表面粗さ曲線を測定したところ本発明焼
結体はＲｍａｘで１μｍであったのに対し、比較材のそ
れは３μｍであった。Furthermore, when the surface roughness curve of the work material was measured, the Rmax of the sintered body of the present invention was 1 μm, whereas that of the comparative material was 3 μm.
発明の効果
上記に詳細に説明した如く、本発明は、所定の粒度分布
のダイヤモンド粉末を用いてダイヤモンド焼結体を製造
することによって、従来技術のダイヤモンド焼結体の問
題を解決したものである。Effects of the Invention As explained in detail above, the present invention solves the problems of the prior art diamond sintered bodies by manufacturing the diamond sintered bodies using diamond powder with a predetermined particle size distribution. .
すなわち、本発明は、最大粒径が２μｍで且つ最小粒径
が０．１μｍであり、好ましくは、１〜２μｍの粒径の
ダイヤモンド粒子の容量と、０．１〜１μｍの粒径のダ
イヤモンド粒子の容量との割合が４〜１であるダイヤモ
ンド粉末を焼結体とすることによって、比較的大きなダ
イヤモンド粒子の周りに比較的微細なダイヤモンド粒子
が分散して、それらのダイヤモンド粒子全体が相互に強
固に保持され、ダイヤモンド粒子の脱落が非常に少なく
、優れた性能を示すダイヤモンド焼結体を提供すること
に成功したものである。このような、粒度分布とするこ
とにより、微粒ダイヤモンド粒子が集団となって脱落す
ることが防止しされ、またダイヤモンド粒子相互がしっ
かりと結合してスケルトン部での欠損が抑制される。That is, the present invention has a maximum particle size of 2 μm and a minimum particle size of 0.1 μm, preferably a capacity of diamond particles with a particle size of 1 to 2 μm, and a capacity of diamond particles with a particle size of 0.1 to 1 μm. By making diamond powder into a sintered body with a ratio of 4 to 1, relatively fine diamond particles are dispersed around relatively large diamond particles, and the diamond particles as a whole are mutually strong. The present invention has succeeded in providing a diamond sintered body that exhibits excellent performance, with extremely low shedding of diamond particles. By having such a particle size distribution, fine diamond particles are prevented from falling off as a group, and the diamond particles are firmly bonded to each other, thereby suppressing defects in the skeleton portion.
従って、本発明のダイヤモンド焼結体は、耐摩耗性およ
び強度に優れ、特にメッキ鋼線の如き高硬度の線材用の
線引きダイスに好適に用いられ、高性能且つ長寿命の線
引きダイスを提供するものである。Therefore, the diamond sintered body of the present invention has excellent wear resistance and strength, and is particularly suitable for use in a wire drawing die for high-hardness wire such as plated steel wire, providing a wire drawing die with high performance and long life. It is something.
第１図は伸線中の線材のダイスの接触状態を示す概略図
である。
（主な参照番号）FIG. 1 is a schematic diagram showing the contact state of the die of the wire rod during wire drawing. (main reference number)
Claims (7)
〜５容量％の１μｍ以下のＷＣまたは（Ｍｏ、Ｗ）Ｃと
、４．５〜１５容量％の鉄族金属とを含み、該ダイヤモ
ンド粒子の少なくとも９５容量％以上は最大粒径が２μ
ｍで且つ最小粒径が０．１μｍであり、残部が０．１μ
ｍ以下の粒径のダイヤモンド粒子であることを特徴とす
る工具用高硬度焼結体。(1) 80-95% by volume of diamond particles and 0.5
~5% by volume of WC or (Mo,W)C of 1 μm or less and 4.5 to 15% by volume of iron group metal, and at least 95% by volume of the diamond particles have a maximum particle size of 2 μm.
m, and the minimum particle size is 0.1 μm, and the remainder is 0.1 μm.
A high-hardness sintered body for tools, characterized by comprising diamond particles having a particle size of less than m.
０．１〜１μｍの粒径のダイヤモンド粒子の容量との割
合が４〜１である特許請求の範囲第１項記載の工具用高
硬度焼結体。(2) the capacity of diamond particles with a particle size of 1 to 2 μm;
The high-hardness sintered body for tools according to claim 1, wherein the ratio of diamond particles having a particle size of 0.1 to 1 μm to the capacity is 4 to 1.
あるダイヤモンド粉末を調整し、該ダイヤモンド粉末と
、鉄族金属および１μｍ以下のＷＣまたは（Ｍｏ、Ｗ）
Ｃ粉末とを、ダイヤモンド粉末が８０〜９５容量％、Ｗ
Ｃまたは（Ｍｏ、Ｗ）Ｃ粉末が０．５〜５容量％、鉄族
金属が４．５〜１５容量％の割合で混合し、得られた混
合物を、超高圧高温装置を用いてダイヤモンドが安定な
高温、高圧下でホットプレスすることを特徴とする工具
用高硬度焼結体の製造方法。(3) Prepare diamond powder with a maximum particle size of 2 μm and a minimum particle size of 0.2 μm, and combine the diamond powder with an iron group metal and WC or (Mo, W) of 1 μm or less.
C powder, diamond powder at 80 to 95% by volume, W
C or (Mo, W)C powder is mixed at a ratio of 0.5 to 5% by volume and iron group metal is mixed at a ratio of 4.5 to 15% by volume, and the resulting mixture is heated using an ultra-high pressure and high temperature device to form diamonds. A method for producing a high-hardness sintered body for tools, which is characterized by hot pressing under stable high temperature and high pressure.
ｍの粒径のダイヤモンド粒子と０．１〜１μｍの粒径の
ダイヤモンド粒子の割合が４〜１であることを特徴とす
る特許請求の範囲第３項記載の工具用高硬度焼結体の製
造方法。(4) For the above mixed diamond powder, 1 to 2μ
Production of a high-hardness sintered body for a tool according to claim 3, characterized in that the ratio of diamond particles with a particle size of m and diamond particles with a particle size of 0.1 to 1 μm is 4 to 1. Method.
サーメットで内張したポット及びボールを用いて上記混
合を行い、この混合によりポット及びボールより１μｍ
以下のＷＣもしくは（Ｍｏ、Ｗ）Ｃの微粉末を混入させ
ることを特徴とする特許請求の範囲第３項または第４項
のいずれかに記載の工具用高硬度焼結体の製造方法。(5) The above mixing is carried out using a pot and ball lined with cermet made of WC or (Mo, W)C bonded with iron group metals, and this mixing causes a distance of 1 μm from the pot and ball.
A method for producing a high-hardness sintered body for tools according to claim 3 or 4, characterized in that the following fine powder of WC or (Mo, W)C is mixed.
あるダイヤモンド粉末を、ＷＣまたは（Ｍｏ、Ｗ）Ｃを
鉄族金属で結合したサーメットで内張したポット及びボ
ールを用いて粉砕処理し、該粉砕処理によりポット及び
ボールより１μｍ以下のＷＣもしくは（Ｍｏ、Ｗ）Ｃの
微粉末を混入させ、得られた混合粉末と、鉄族金属とを
、ダイヤモンド粉末が８０〜９５容量％、ＷＣまたは（
Ｍｏ、Ｗ）Ｃ粉末が０．５〜５容量％、鉄族金属が４．
５〜１５容量％の割合で、超高圧高温装置を用いてダイ
ヤモンドが安定な高温、高圧下でホットプレスすること
を特徴とする工具用高硬度焼結体の製造方法。(6) Grind diamond powder with a maximum particle size of 2 μm and a minimum particle size of 0.2 μm using a pot and ball lined with cermet made of WC or (Mo, W)C bonded with iron group metals. WC or (Mo, W)C fine powder of 1 μm or less is mixed in from the pot and ball through the pulverization process, and the resulting mixed powder and iron group metal are mixed to a diamond powder content of 80 to 95% by volume. , WC or (
Mo, W) C powder is 0.5 to 5% by volume, iron group metal is 4.
A method for producing a high-hardness sintered body for tools, characterized by hot pressing at a high temperature and pressure at which diamond is stable using an ultra-high pressure and high temperature device at a ratio of 5 to 15% by volume.
ｍの粒径のダイヤモンド粒子と０．１〜１μｍの粒径の
ダイヤモンド粒子の割合が４〜１であることを特徴とす
る特許請求の範囲第６項記載の工具用高硬度焼結体の製
造方法。(7) For the above mixed diamond powder, 1 to 2μ
Production of a high-hardness sintered body for tools according to claim 6, characterized in that the ratio of diamond particles with a particle size of m and diamond particles with a particle size of 0.1 to 1 μm is 4 to 1. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24838384A JPS61127846A (en) | 1984-11-24 | 1984-11-24 | High hardness sintered body and its manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24838384A JPS61127846A (en) | 1984-11-24 | 1984-11-24 | High hardness sintered body and its manufacture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61127846A true JPS61127846A (en) | 1986-06-16 |
Family
ID=17177285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24838384A Pending JPS61127846A (en) | 1984-11-24 | 1984-11-24 | High hardness sintered body and its manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61127846A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6324003A (en) * | 1986-07-16 | 1988-02-01 | Mitsubishi Metal Corp | Composite cutting tip |
| EP0583916A1 (en) * | 1992-08-05 | 1994-02-23 | De Beers Industrial Diamond Division (Proprietary) Limited | Abrasive product |
| EP0726330A1 (en) * | 1995-02-10 | 1996-08-14 | Fuji Die Co., Ltd. | Heat sinks and process for producing the same |
-
1984
- 1984-11-24 JP JP24838384A patent/JPS61127846A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6324003A (en) * | 1986-07-16 | 1988-02-01 | Mitsubishi Metal Corp | Composite cutting tip |
| EP0583916A1 (en) * | 1992-08-05 | 1994-02-23 | De Beers Industrial Diamond Division (Proprietary) Limited | Abrasive product |
| EP0726330A1 (en) * | 1995-02-10 | 1996-08-14 | Fuji Die Co., Ltd. | Heat sinks and process for producing the same |
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