JP2003055649A - Carbide coated diamond powder - Google Patents
Carbide coated diamond powderInfo
- Publication number
- JP2003055649A JP2003055649A JP2001251970A JP2001251970A JP2003055649A JP 2003055649 A JP2003055649 A JP 2003055649A JP 2001251970 A JP2001251970 A JP 2001251970A JP 2001251970 A JP2001251970 A JP 2001251970A JP 2003055649 A JP2003055649 A JP 2003055649A
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- Japan
- Prior art keywords
- diamond
- carbide
- diamond powder
- transition metal
- metal
- 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.)
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】 本発明は炭化物被覆ダイヤモン
ド粉末、特に表面が遷移金属の炭化物層で被覆され、ボ
ンド材との均一混合性並びにボンド材金属との接合強度
が向上したダイヤモンドの微粉末、及びかかるダイヤモ
ンド粉末の効果的な製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a carbide-coated diamond powder, and in particular, a fine diamond powder whose surface is coated with a carbide layer of a transition metal to improve the homogeneity of mixing with a bond material and the bonding strength with a bond metal. And an effective method for producing such a diamond powder.
【０００２】[0002]
【従来技術】 メタルボンドダイヤモンド工具の製作に
際して、化学的に表面が不活性なダイヤモンドをボンド
材金属で強固に保持するために、砥粒としてのダイヤモ
ンド粒子の表面を、チタン、クロム、またはシリコン
等、ある種の金属で被覆することが広く行われている。
被覆方法としては、蒸着、その他のＰＶＤによる手法
や、揮発性化合物の分解によるＣＶＤ等が用いられてい
る。これらの被覆金属はダイヤモンドとの接合部におい
て炭化物となり、ダイヤモンドとの間に強固な化学結合
を形成している。2. Description of the Related Art When manufacturing a metal bond diamond tool, in order to firmly hold a chemically inactive diamond with a bond material metal, the surface of diamond particles as abrasive grains is made of titanium, chromium, silicon or the like. It is widely practiced to coat with some kind of metal.
As the coating method, vapor deposition, another PVD method, CVD by decomposing a volatile compound, or the like is used. These coating metals become carbides at the joint with diamond and form a strong chemical bond with the diamond.
【０００３】これらの金属乃至金属炭化物は、ダイヤモ
ンドに比べるとボンド材金属への濡れが格段に良好であ
ることから、ダイヤモンド砥粒は、金属炭化物を介して
ボンド材金属に化学結合によって固定され、砥粒の脱落
阻止による工具の長寿命化が達成されている。Since these metals and metal carbides have much better wettability to the bond material metal than diamond, the diamond abrasive grains are fixed to the bond material metal through the metal carbide by chemical bonding, Longer tool life has been achieved by preventing the removal of abrasive grains.
【０００４】その上これらの被覆層はダイヤモンド表面
が酸素に触れることを防止する保護膜としても機能し、
ダイヤモンド工具製作の際の加熱時において、酸素との
接触によって促進されるダイヤモンドのグラファイト化
も阻止していることが知られている。Furthermore, these coating layers also function as a protective film for preventing the diamond surface from being exposed to oxygen,
It is known that during heating during diamond tool fabrication, diamond graphitization promoted by contact with oxygen is also prevented.
【０００５】精密加工技術の発展に伴って、切断、研
削、研磨に用いられるダイヤモンド工具も高機能化が進
み、従来遊離砥粒が用いられていた加工分野が、順次砥
石を用いた固定砥粒による加工に切り替わってきてい
る。そして砥石に用いられるダイヤモンドのサイズも細
かくなり、サブミクロンサイズのダイヤモンド粉末も砥
石中に固定可能となってきている。With the development of precision processing technology, diamond tools used for cutting, grinding, and polishing are also highly functionalized, and in the field of processing in which free abrasive grains have been used in the past, fixed abrasive grains using a grindstone have been successively used. It has been switched to processing by. The size of the diamond used for the grindstone has become finer, and even submicron size diamond powder can be fixed in the grindstone.
【０００６】上記のように細かなダイヤモンド砥粒をボ
ンド材中に固定する際に、ボンド材が金属系の場合、化
学結合による砥粒の固定効果を期待すると同時に、焼結
に先立って実施される原料の金属粉末とダイヤモンド粉
末との均一混合を可能にするために、ダイヤモンド粒子
の表面に金属または金属炭化物の被覆を予め形成してお
くことが望まれる。When the fine diamond abrasive grains are fixed in the bond material as described above, when the bond material is a metal-based material, the effect of fixing the abrasive particles by chemical bonding is expected, and at the same time, it is carried out prior to sintering. In order to enable uniform mixing of the raw material metal powder and diamond powder, it is desirable to previously form a coating of metal or metal carbide on the surface of the diamond particles.
【０００７】即ち、ダイヤモンド粒子の表面に吸着ない
し付着している酸素または酸素を含む官能基が原因とな
って、混合の際にはダイヤモンド粒子の凝集が生じ、ま
た焼結の際には主としてＣＯを含むガスが粒子表面から
放出され、この結果、ダイヤモンド粒子−ボンド材間の
接合強度が低下、即ちボンド材による粉末の保持力が低
下する。That is, due to oxygen or a functional group containing oxygen adsorbed on or adhering to the surface of the diamond particles, agglomeration of the diamond particles occurs during mixing, and mainly CO during sintering. The gas containing the is released from the particle surface, and as a result, the bonding strength between the diamond particles and the bond material is decreased, that is, the powder holding force by the bond material is decreased.
【０００８】そこで加熱によってダイヤモンド粒子表面
の酸素を除くと共に、遷移金属とダイヤモンドとの反応
によりダイヤモンド表面に金属炭化物膜を形成すること
によって、ダイヤモンド粒子表面を不活性化し、上記の
不具合を解消することが望ましい。同様の効果が樹脂系
のボンド材を用いる場合についても期待される。Therefore, the oxygen on the surface of the diamond particles is removed by heating, and the metal carbide film is formed on the surface of the diamond by the reaction between the transition metal and the diamond to inactivate the surface of the diamond particles and solve the above-mentioned problems. Is desirable. The same effect can be expected when a resin-based bond material is used.
【０００９】このようなボンド材との接合強度の向上
や、酸化防止効果を発揮するためには、既述のようにダ
イヤモンド粉末の全表面が金属または金属炭化物で覆わ
れていることが望ましい。しかし前記したＰＶＤやＣＶ
Ｄによる方法で、粉末の全表面を金属源に接触させるた
めには、混合・撹拌のために複雑な装置・操作を必要と
し、生産性が低い、という問題があった。In order to improve the bonding strength with such a bond material and to exert an antioxidant effect, it is desirable that the entire surface of the diamond powder is covered with a metal or a metal carbide as described above. However, PVD and CV mentioned above
In order to bring the entire surface of the powder into contact with the metal source by the method according to D, there is a problem that a complicated device and operation are required for mixing and stirring, and the productivity is low.
【００１０】[0010]
【発明が解決しようとする課題】 従って本発明の主な
目的は、金属系ボンド材との結合力が改善されたダイヤ
モンド砥粒、及びその効果的な製造法を提供することに
ある。SUMMARY OF THE INVENTION Therefore, a main object of the present invention is to provide a diamond abrasive grain having an improved bonding force with a metal-based bonding material, and an effective manufacturing method thereof.
【００１１】[0011]
【課題を解決するための手段】 本発明の要旨とすると
ころは、平均粒径40ミクロン以下のダイヤモンド粉末に
おいて、該粉末を構成するダイヤモンド粒子の表面を全
体的に遷移金属の炭化物で被覆した点にある。Means for Solving the Problems The gist of the present invention is that, in a diamond powder having an average particle size of 40 microns or less, the surfaces of the diamond particles constituting the powder are entirely covered with a transition metal carbide. It is in.
【００１２】本発明による炭化物被覆層の形成は上記の
ように平均(公称)粒径が40ミクロン以下のダイヤモンド
粉末に適用できるが、保持力の向上は粒径が細かいほど
顕著である。最も効果が発揮されるのは20ミクロン以
下、特に5ミクロン以下のダイヤモンド粉末においてで
ある。The formation of the carbide coating layer according to the present invention can be applied to the diamond powder having an average (nominal) particle size of 40 μm or less as described above, but the improvement of the holding power is more remarkable as the particle size is smaller. It is most effective in diamond powder of 20 microns or less, especially 5 microns or less.
【００１３】上記炭化物被覆層の量は、基体のダイヤモ
ンド粒子の粒径によってある程度変動するが、ダイヤモ
ンドに対する質量比において概ね0.5％以上かつ5％未満
とするのが適切である。この範囲より少ないと上記効果
が顕著でなく、一方過剰の被覆を施すと、結晶表面にお
ける炭化物形成のために移動する炭素原子の量が多くな
り、ダイヤモンド結晶内に多数の空格子点が形成されて
結晶自体の強度低下を招くことから好ましくない。The amount of the above-mentioned carbide coating layer varies to some extent depending on the particle size of the diamond particles of the substrate, but it is suitable that the mass ratio to diamond is generally 0.5% or more and less than 5%. If it is less than this range, the above effect is not remarkable, while if the coating is excessive, the amount of carbon atoms that move to form carbides on the crystal surface increases, and many vacancy points are formed in the diamond crystal. It is not preferable because the strength of the crystal itself is reduced.
【００１４】本発明において、炭化物被覆層を形成する
金属種は遷移金属が適切で、特にチタン、ジルコニウ
ム、クロム、モリブデン、タングステン、バナジウムか
ら選ばれる１種以上を含有する。しかして炭化物は、か
かる金属が、熱の影響下で基体のダイヤモンドと反応し
て形成されたものである。In the present invention, the metal species forming the carbide coating layer are suitably transition metals, and particularly contain at least one selected from titanium, zirconium, chromium, molybdenum, tungsten and vanadium. Carbides are then formed by the reaction of such metals with the diamond of the substrate under the influence of heat.
【００１５】上記の炭化物被覆ダイヤモンド粉末は、次
のようにして効果的に得ることができる。即ちダイヤモ
ンド粉末、好ましくは平均粒径40ミクロン以下のダイヤ
モンド粉末を、チタン、ジルコニウム、クロム、モリブ
デン、タングステン、バナジウムから選ばれる１種以上
のイオンを含有する溶融塩中に浸す。この際、溶融塩温
度を600℃以上に加熱保持して上記遷移金属イオンと充
分に接触させることにより、ダイヤモンド粒子表面に該
金属の炭化物層が形成される。The above-mentioned carbide-coated diamond powder can be effectively obtained as follows. That is, a diamond powder, preferably a diamond powder having an average particle size of 40 μm or less, is immersed in a molten salt containing one or more ions selected from titanium, zirconium, chromium, molybdenum, tungsten and vanadium. At this time, the molten salt temperature is kept at 600 ° C. or higher and is brought into sufficient contact with the above transition metal ions to form a carbide layer of the metal on the surface of the diamond particles.
【００１６】上記溶融塩としては、例えばＮaＣl−ＫＣ
l系の混合塩が利用可能である。この塩はチタンやジル
コニウムの溶融塩電解に用いられており、溶融塩中には
チタンやジルコニウムがイオンの形で少量溶解すること
が知られている。これらの金属イオンはダイヤモンド表
面の炭素原子と結合して炭化物を形成するので、溶融塩
中にダイヤモンド粉末を懸濁させることで、ダイヤモン
ド粒子表面を全体的に金属イオンと接触させて、炭化物
を形成させる条件が確保される。The molten salt may be, for example, NaCl-KC.
l-based mixed salts are available. This salt is used for molten salt electrolysis of titanium and zirconium, and it is known that a small amount of titanium and zirconium are dissolved in the molten salt in the form of ions. Since these metal ions combine with carbon atoms on the diamond surface to form carbides, suspending the diamond powder in the molten salt causes the entire diamond particle surface to come into contact with the metal ions and form carbides. The conditions to be ensured are secured.
【００１７】溶融塩に拠らない別の上記金属の炭化物層
形成法として、これらの金属のハロゲン化物蒸気による
方法も利用可能である。この手法では特に、金属のキャ
リアとして気相を用いることから、微細なダイヤモンド
粒子表面にも、炭化物層を効果的に形成することができ
る。As a method for forming a carbide layer of the above-mentioned metals which does not depend on the molten salt, a method using a halide vapor of these metals can also be used. In this method, in particular, since the vapor phase is used as the metal carrier, the carbide layer can be effectively formed even on the fine diamond particle surfaces.
【００１８】本発明によれば、第二の炭化物被覆層乃至
かかる被覆層を有するダイヤモンド粉末は次のように実
施される。According to the invention, the second carbide coating layer or diamond powder having such a coating layer is carried out as follows.
【００１９】(1)密閉容器内に(平均粒径40ミクロン以下
の)ダイヤモンド粉末並びにチタン、ジルコニウム、ク
ロム、モリブデン、タングステン、バナジウムから選ば
れる１種以上の遷移金属、及びハロゲン物質を充填した
後600℃以上に加熱し、(2)上記遷移金属とハロゲンとの
反応によって該金属のハロゲン化物を形成して上記ダイ
ヤモンド粒子の表面に到達せしめ、(3)ダイヤモンド表
面で上記ハロゲン化物を分解せしめる一方、該分解によ
って遊離した該遷移金属とダイヤモンドと反応せしめる
ことにより、ダイヤモンド表面に金属炭化物層を形成せ
しめる。(1) After filling a closed container with diamond powder (having an average particle size of 40 microns or less) and at least one transition metal selected from titanium, zirconium, chromium, molybdenum, tungsten and vanadium, and a halogen substance Heating to 600 ° C. or higher, (2) forming a halide of the transition metal with a halogen to reach the surface of the diamond particles, and (3) decomposing the halide on the diamond surface. By reacting the transition metal liberated by the decomposition with diamond, a metal carbide layer is formed on the diamond surface.
【００２０】上記においてハロゲンとしてはヨウ素が、
ハロゲン化物としては上記遷移金属のヨウ化物が利用可
能である。金属ヨウ化物蒸気は、微細なダイヤモンド粒
子間隙にも浸透できるので、ダイヤモンド粒子表面と全
体的に接触させることができるので、細かなダイヤモン
ド表面にも均一な被覆を施すことが可能となる。In the above, halogen is iodine,
As the halide, iodide of the above transition metal can be used. Since the metal iodide vapor can also penetrate fine diamond particle gaps, it can be brought into contact with the surface of the diamond particles as a whole, so that even a fine diamond surface can be uniformly coated.
【００２１】どちらの方法においても、炭化物中におけ
る炭素または金属原子の拡散速度は大きくないことか
ら、炭化物が生じた箇所では相互の反応速度は低下し、
見掛け上、炭素原子が露出している粒子表面での炭化物
形成反応が優先して進行する。この結果、本発明におい
ては、ダイヤモンド表面全体がほぼ均一な厚さの炭化物
の層で覆われるという特徴が得られる。従って溶融塩法
の場合には金属イオンの移動及びかかるイオンとの良好
な接触を確保するために、ダイヤモンド粉末は液相中に
懸濁していることが必須要件となる。In either method, since the diffusion rate of carbon or metal atoms in the carbide is not large, the mutual reaction rate decreases at the place where the carbide is generated,
Apparently, the carbide forming reaction preferentially proceeds on the surface of the particles where the carbon atoms are exposed. As a result, the present invention has the characteristic that the entire diamond surface is covered with a layer of carbide of substantially uniform thickness. Therefore, in the case of the molten salt method, it is an essential requirement that the diamond powder is suspended in the liquid phase in order to ensure the movement of metal ions and good contact with such ions.
【００２２】塩化物系の溶融塩は、組合わせを選ぶこと
によって共晶温度500℃以下の組成も可能であるが、炭
化物形成速度を確保する見地からは600℃以上が好まし
く、750℃以上がより好ましい。一方過度に処理温度を
高くすると、ダイヤモンド粒子内に微小なクラックが生
じ、砥粒としての強度が低下することから、処理温度の
上限は1000℃とすることが望ましい。The chloride-based molten salt may have a composition having a eutectic temperature of 500 ° C. or lower by selecting a combination, but 600 ° C. or higher is preferable, and 750 ° C. or higher is preferable from the viewpoint of ensuring the rate of carbide formation. More preferable. On the other hand, if the treatment temperature is excessively increased, minute cracks are generated in the diamond particles, and the strength of the abrasive grains is reduced. Therefore, the upper limit of the treatment temperature is preferably 1000 ° C.
【００２３】なおダイヤモンドの粒径の減少に伴って、
より高い処理温度を用いたり、共晶温度の低い組成の混
合塩を用いるのが好ましい。こうすることによって溶融
塩の粘度を低下させ、サブミクロン級のダイヤモンド粉
末にも、効果的に溶融塩を浸透させて、炭化物被覆を形
成することができる。As the diamond grain size decreases,
It is preferable to use a higher processing temperature or to use a mixed salt having a composition with a lower eutectic temperature. By doing so, the viscosity of the molten salt can be lowered, and the molten salt can be effectively permeated into the submicron grade diamond powder to form a carbide coating.
【００２４】なお溶融塩中に、フッ素化合物の形でフッ
素イオンを共存させるのも炭化物形成反応の促進に有効
である。Coexistence of a fluorine ion in the form of a fluorine compound in the molten salt is also effective in promoting the carbide forming reaction.
【００２５】一方ハロゲン化物蒸気処理による方法で
は、無水の金属フッ化物、塩化物も用い得るが、ダイヤ
モンドが金属ヨウ化物と反応して金属炭化物を形成し、
ヨウ素を分離する性質に基づいて、ヨウ素を金属のキャ
リアとして利用するヨウ化物法が、操作が容易になるの
で有利である。この場合、ダイヤモンド粒子間の間隙を
ヨウ化物蒸気で満たすことにより、粒子表面全体にわた
って炭化物を形成する条件が確立される。ダイヤモンド
表面で金属を分離したヨウ素は金属と接触して再び金属
ヨウ化物となるので、ダイヤモンド粒子表面が金属炭化
物で覆われて金属の移送速度が低下するまで、ヨウ素が
金属のキャリアとして働く。On the other hand, in the method using halide vapor treatment, anhydrous metal fluorides and chlorides can be used, but diamond reacts with metal iodides to form metal carbides,
Based on the property of separating iodine, the iodide method using iodine as a metal carrier is advantageous because it facilitates the operation. In this case, filling the gaps between the diamond grains with iodide vapor establishes the conditions for forming carbides over the grain surfaces. The iodine that has separated the metal on the diamond surface comes into contact with the metal again to become a metal iodide, so that the iodine acts as a carrier for the metal until the diamond particle surface is covered with the metal carbide and the metal transfer rate decreases.
【００２６】上記ヨウ化物法においても、炭化物形成速
度を確保する観点から処理温度は600℃以上、特に800℃
以上(ダイヤモンド表面における温度)とするのが好まし
い。Also in the above iodide method, the treatment temperature is 600 ° C. or higher, particularly 800 ° C., from the viewpoint of ensuring the carbide formation rate.
The above (temperature at the diamond surface) is preferable.
【００２７】このように本発明においては、ダイヤモン
ド粉末表面全部が、遷移金属を含む液相または蒸気相に
触れることから、粉末表面全部が液相または蒸気相から
析出した金属との反応で形成された炭化物で覆われるこ
ととなり、工具製作時のマトリックス金属への接着性の
向上、ならびに保護膜として加熱時におけるダイヤモン
ドの酸化・黒鉛化の防止効果が得られる。特に金属との
接着性の向上によって、例えば研削砥石中においては、
ダイヤモンドがボンド材金属に強固に保持される結果、
砥石寿命が増加すると同時に、ダイヤモンド砥粒の突き
出し高さが大きくなることによる研削抵抗の低下という
メリットも得られる。As described above, in the present invention, since the entire surface of the diamond powder comes into contact with the liquid phase or vapor phase containing the transition metal, the entire powder surface is formed by the reaction with the metal precipitated from the liquid phase or vapor phase. Since it is covered with the carbide, the adhesion to the matrix metal at the time of manufacturing the tool is improved, and as a protective film, the effect of preventing oxidation and graphitization of diamond during heating can be obtained. Especially by improving the adhesion with metal, for example, in a grinding wheel,
As a result of the diamond being held firmly in the bond metal,
At the same time as the life of the grindstone is increased, the protrusion height of the diamond abrasive grains is increased, resulting in a reduction in grinding resistance.
【００２８】また微粉(サブミクロン級)のダイヤモンド
においては、ダイヤモンド粒子同士の凝集の原因となっ
ているダイヤモンド表面の官能基が、金属炭化物で置換
されることにより、表面が不活性となって粉末の分散性
が向上し、粉末状のマトリックス原料との混合操作が容
易になった。このようなダイヤモンド表面状態の変化
は、赤外吸収分析によっても確かめられた。In the case of fine powder (submicron grade) diamond, the functional groups on the surface of the diamond, which are the cause of the aggregation of the diamond particles, are replaced with metal carbides, and the surface becomes inactive. The dispersibility was improved, and the mixing operation with the powdery matrix raw material was facilitated. Such changes in the diamond surface state were also confirmed by infrared absorption analysis.
【００２９】工具製作において、本発明のダイヤモンド
粉末をセラミックス系マトリックス材へ適用する場合に
は、炭化物で覆われたダイヤモンド粉末を窒素雰囲気中
で1000℃以上に加熱することによって、表面を炭窒化物
ないし窒化物に変え、マトリックス材への濡れ性及び接
着強度を上げることができる。When the diamond powder of the present invention is applied to a ceramic matrix material in tool fabrication, the surface of the carbonitride is covered by heating the diamond powder covered with carbide to 1000 ° C. or higher in a nitrogen atmosphere. Alternatively, it is possible to improve the wettability to the matrix material and the adhesive strength by changing to a nitride.
【００３０】上記窒化処理には次の方法が効果的であ
る。即ち、密閉容器内に炭化物被覆ダイヤモンドを入
れ、窒素雰囲気中で所定温度まで加熱する。加熱を保っ
た状態で容器内を排気し、窒素を充填する操作を反復す
るものである。この手法によりサブミクロン級のダイヤ
モンド粉末表面も窒化することが可能である。The following method is effective for the above nitriding treatment. That is, the carbide-coated diamond is placed in a closed container and heated to a predetermined temperature in a nitrogen atmosphere. The operation of evacuating the inside of the container while keeping the heating and filling with nitrogen is repeated. By this method, the surface of submicron diamond powder can be nitrided.
【００３１】[0031]
【実施例１】 平均粒径4ミクロンのダイヤモンド粉末5
0ｇと、2ｇのチタン粉末(粒径40μm)とを容量500mlのSU
Sビーカーへ入れ、モル比でＮaＣl:ＫＣl=1: 1の混合塩
(共晶温度約660℃) 約300ｇを加えた。このビーカーを
炉内で800℃に加熱し2時間保持した。Example 1 Diamond powder 5 having an average particle size of 4 microns
0g and 2g titanium powder (particle size 40μm) SU of 500ml capacity
Put into S beaker, mixed salt of NaCl: KCl = 1: 1 in molar ratio
(Eutectic temperature about 660 ° C.) About 300 g was added. The beaker was heated to 800 ° C. in the furnace and kept for 2 hours.
【００３２】放冷後、炉から取り出し、ビーカー中の塩
を水に溶かして除去し、次いで5倍に希釈した硫酸を加
えて1時間煮沸し、未反応チタンを溶解・除去した。得
られた粉末は黒色を呈しており、Ｘ線回折によって、ダ
イヤモンドと共にＴiＣの回折線が得られた。付着した
チタン量は、ダイヤモンドの質量増加から概略値として
求めることができるが、より正確な方法として、フッ硝
酸により被覆を溶解除去し、溶解前後の質量変化から決
定し、1.9％(質量％、以下同様)の値を得た。After allowing to cool, it was taken out of the furnace, the salt in the beaker was dissolved in water to be removed, and then sulfuric acid diluted 5 times was added and boiled for 1 hour to dissolve and remove unreacted titanium. The obtained powder had a black color, and TiC diffraction lines were obtained together with diamond by X-ray diffraction. The amount of titanium adhering can be obtained as an approximate value from the increase in mass of diamond, but as a more accurate method, the coating is dissolved and removed by hydrofluoric nitric acid, and the mass change before and after dissolution is determined, and 1.9% (mass%, The same applies hereinafter).
【００３３】[0033]
【実施例２】 実施例1と同じ仕込量及び処理条件でダ
イヤモンドにＴiＣの被覆を施した。処理原料として平
均粒径0.4ミクロンのダイヤモンド粉末を用い、溶融塩
の原料には、モル比でＮaＣl:ＫＣl:ＣaＣl2=5:3:2の混
合塩(共晶温度約600℃) を用いた。被覆チタン量をフッ
硝酸による溶解除去量から求めたところ、2.0％であっ
た。Example 2 Diamond was coated with TiC under the same amount and treatment conditions as in Example 1. Diamond powder having an average particle size of 0.4 micron was used as a processing raw material, and a mixed salt (eutectic temperature of about 600 ° C.) having a molar ratio of NaCl: KCl: CaCl 2 = 5: 3: 2 was used as a raw material of the molten salt. . The amount of coated titanium was 2.0% as determined from the amount of dissolved and removed hydrofluoric acid.
【００３４】[0034]
【実施例３】 内容積50ccのＳＵＳ製の密閉容器中へ、
平均粒径20μｍのダイヤモンド粉末10ｇ、平均粒径3μ
ｍのモリブデン粉末2ｇ、ヨウ素1ｇを入れ、容器内を排
気して密閉し、950℃に加熱して1時間保持した。取り出
したダイヤモンドは黒色を呈しており、Ｘ線回折によっ
てＭo2Cの生成を確認した。Example 3 Into a closed container made of SUS having an internal volume of 50 cc,
10 g of diamond powder with an average particle size of 20 μm, average particle size of 3 μ
2 g of molybdenum powder of m and 1 g of iodine were put therein, and the inside of the container was evacuated and sealed, heated to 950 ° C. and kept for 1 hour. The diamond taken out had a black color, and the formation of Mo 2 C was confirmed by X-ray diffraction.
【００３５】得られたモリブデン被覆ダイヤモンドを用
いてブロンズボンドの平面研削砥石を製作し、焼結アル
ミナ板の研削加工に用いた。砥石は外径150mm、厚さ8mm
のストレート砥石で、集中度は50とし、研削条件は周速
度1500ｍ/分、切込み3μｍとした。比較用として同時に
製作した被覆前のダイヤモンドを用いた研削砥石に比し
て、研削抵抗が15％小さく、砥石寿命が43％増しになる
結果が得られた。A bronze bond surface grinding wheel was produced using the obtained molybdenum-coated diamond and used for grinding a sintered alumina plate. The whetstone has an outer diameter of 150 mm and a thickness of 8 mm
With a straight grindstone, the concentration was 50, and the grinding conditions were a peripheral speed of 1500 m / min and a depth of cut of 3 μm. The grinding resistance was 15% smaller and the grinding wheel life was increased by 43% compared with the grinding wheel using uncoated diamond that was manufactured at the same time for comparison.
【００３６】[0036]
【実施例４】上記の方法をモリブデン粉末の代わりに、
平均粒径3μｍのタングステン粉末を用いて実施し、ダ
イヤモンド表面にＷＣの被覆層が形成され、ＳＥＭ観察
によって被覆層の厚さが約0.05μｍであることが認めら
れた。被覆量の定量には、フッ硝酸を用いて被覆を溶解
除去し、溶解前後の質量変化から求める方法を用い、約
3％の値を得た。Example 4 The method described above was used instead of molybdenum powder.
It was carried out using a tungsten powder having an average particle size of 3 μm, a WC coating layer was formed on the diamond surface, and it was confirmed by SEM observation that the coating layer had a thickness of about 0.05 μm. To quantify the coating amount, use a method in which the coating is dissolved and removed using hydrofluoric nitric acid and the mass change before and after dissolution is used.
A value of 3% was obtained.
【００３７】[0037]
【実施例５】実施例1で得られたTiCコートダイヤモンド
をアルミナ製るつぼに入れ、窒素雰囲気中で1100℃に加
熱し1時間保持する処理を実施した。得られた処理品は
褐色を呈しており、Ｘ線回折によってＴiＮに変化して
いることを確認した。[Example 5] The TiC-coated diamond obtained in Example 1 was placed in an alumina crucible and heated to 1100 ° C in a nitrogen atmosphere and held for 1 hour. The obtained treated product had a brown color, and it was confirmed that it was changed to TiN by X-ray diffraction.
【００３８】[0038]
【実施例６】次の表においてNo.１〜５に示すようなダ
イヤモンド粉末と被覆金属材・溶融塩組成、処理温度の
組合せを用いて処理を行い、被覆量の欄に示すとおりの
数値を得た。[Example 6] In the following table, treatment was carried out using a combination of diamond powder, coating metal material / molten salt composition, and treatment temperature as shown in Nos. 1 to 5, and the numerical values as shown in the column of coating amount were obtained. Obtained.
【表１】 [Table 1]
【００３９】[0039]
【発明の効果】１．周知のように、メタルボンド工具の
製作の際に、ダイヤモンド砥粒とボンド材の金属とはダ
イヤモンド表面に形成された炭化物被覆を介して化学結
合を形成するので、炭化物被覆を施した本発明のダイヤ
モンド粉末においてはボンド材による砥粒の保持強度が
向上し、砥粒の脱落阻止、有効利用による工具寿命の向
上が達成される。同時に工具表面における砥粒の突き出
し高さが大きく取れることから、加工に要するエネルギ
ーも低減できる。Effect of the Invention As is well known, during the production of a metal bond tool, the diamond abrasive grains and the metal of the bond material form a chemical bond through the carbide coating formed on the diamond surface. In the diamond powder, the holding strength of the abrasive grains by the bond material is improved, the abrasive grains are prevented from falling off, and the tool life is improved by effective utilization. At the same time, since the protrusion height of the abrasive grains on the tool surface can be made large, the energy required for processing can be reduced.
【００４０】２．微細なダイヤモンド粉末においても、
本発明の被覆を施すことにより、粉末凝集の原因である
粒子表面の官能基が炭化物で置換されて不活性化され
る。この結果、ダイヤモンド微粉含有工具あるいは耐摩
耗性硬質材料の製作において、マトリックス原料との混
合操作の際にダイヤモンドの分散性が向上し、微粉ダイ
ヤモンドを用いた材料内における組織の均一性が高ま
り、耐摩耗性能が向上する。2. Even in fine diamond powder,
By applying the coating of the present invention, the functional groups on the surface of the particles, which are the cause of powder agglomeration, are replaced with carbides to be inactivated. As a result, in the production of a tool containing diamond fine powder or a hard wear resistant material, the dispersibility of diamond is improved during the mixing operation with the matrix raw material, the uniformity of the structure in the material using fine diamond is increased, and Wear performance is improved.
Claims (11)
末において、該粉末を構成するダイヤモンド粒子の表面
が全体的に遷移金属の炭化物で被覆されているダイヤモ
ンド粉末。1. A diamond powder having an average particle size of 40 μm or less, in which the surfaces of the diamond particles constituting the powder are entirely covered with a transition metal carbide.
求項１に記載のダイヤモンド粉末。2. The diamond powder according to claim 1, wherein the average particle size is 20 microns or less.
求項１に記載のダイヤモンド粉末。3. The diamond powder according to claim 1, wherein the average particle size is 5 microns or less.
が、質量比において0.5％以上かつ5％未満である、請求
項１に記載のダイヤモンド粉末。4. The diamond powder according to claim 1, wherein the amount of carbide with respect to the diamond particles is 0.5% or more and less than 5% by mass ratio.
クロム、モリブデン、タングステン、バナジウムから選
ばれる１種以上を含有する、請求項１に記載のダイヤモ
ンド粉末。5. The transition metal is titanium, zirconium,
The diamond powder according to claim 1, containing at least one selected from chromium, molybdenum, tungsten, and vanadium.
ド粒子と、隣接配置された上記遷移金属との反応により
形成されたものである、請求項１に記載のダイヤモンド
粉末。6. The diamond powder according to claim 1, wherein the carbide is formed by a reaction between diamond particles constituting a substrate and the transition metal adjacently arranged.
ム、クロム、モリブデン、タングステン、バナジウムか
ら選ばれる１種以上の遷移金属のイオンを含有する溶融
塩中に浸し、600℃以上の溶融塩温度に保持して上記遷
移金属イオンと充分に接触させることによって、ダイヤ
モンド粒子表面に該金属の炭化物層を形成することを特
徴とする、炭化物被覆ダイヤモンド粉末の製造方法。7. A diamond powder is immersed in a molten salt containing ions of at least one transition metal selected from titanium, zirconium, chromium, molybdenum, tungsten and vanadium, and kept at a molten salt temperature of 600 ° C. or higher. A method of producing a carbide-coated diamond powder, which comprises forming a carbide layer of the metal on the surface of diamond particles by sufficiently contacting the transition metal ion with the transition metal ion.
ロン以下である、請求項７に記載の炭化物被覆ダイヤモ
ンド粉末の製造方法。8. The method for producing a carbide-coated diamond powder according to claim 7, wherein the diamond powder has an average particle size of 40 microns or less.
チタン、ジルコニウム、クロム、モリブデン、タングス
テン、バナジウムから選ばれる１種以上の遷移金属、及
びハロゲン物質を充填した後600℃以上に加熱し、 (2)上記遷移金属とハロゲンとの反応によって該金属の
ハロゲン化物を形成して上記ダイヤモンド粒子の表面に
到達せしめ、 (3)ダイヤモンド表面で上記ハロゲン化物を分解せしめ
る一方、該分解によって遊離した該遷移金属とダイヤモ
ンドとを反応せしめることにより、ダイヤモンド表面に
金属炭化物層を形成せしめることを特徴とする、炭化物
被覆ダイヤモンド粉末の製造方法。9. (1) Diamond powder and at least one transition metal selected from titanium, zirconium, chromium, molybdenum, tungsten, and vanadium, and a halogen substance are filled in a closed container and heated to 600 ° C. or higher, (2) by reacting the transition metal with a halogen to form a halide of the metal to reach the surface of the diamond particles, and (3) decompose the halide on the diamond surface, while releasing the decomposition by the decomposition. A method for producing a carbide-coated diamond powder, which comprises forming a metal carbide layer on a diamond surface by reacting a transition metal with diamond.
に記載の炭化物被覆ダイヤモンド粉末の製造方法。10. The method according to claim 9, wherein the halogen is iodine.
The method for producing a carbide-coated diamond powder according to [4].
クロン以下である、請求項９に記載の炭化物被覆ダイヤ
モンド粉末の製造方法。11. The method for producing a carbide-coated diamond powder according to claim 9, wherein the diamond powder has an average particle size of 40 microns or less.
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|---|---|---|---|
| JP2001251970A JP5081352B2 (en) | 2001-08-22 | 2001-08-22 | Method for producing carbide coated diamond powder |
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