JPH0761615B2 - Coated high hardness powder and method for producing the same - Google Patents
Coated high hardness powder and method for producing the sameInfo
- Publication number
- JPH0761615B2 JPH0761615B2 JP4257050A JP25705092A JPH0761615B2 JP H0761615 B2 JPH0761615 B2 JP H0761615B2 JP 4257050 A JP4257050 A JP 4257050A JP 25705092 A JP25705092 A JP 25705092A JP H0761615 B2 JPH0761615 B2 JP H0761615B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- coating
- grindstone
- coated
- diamond
- 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.)
- Expired - Lifetime
Links
- 239000000843 powder Substances 0.000 title claims description 74
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000000576 coating method Methods 0.000 claims description 49
- 239000011248 coating agent Substances 0.000 claims description 45
- 229910003460 diamond Inorganic materials 0.000 claims description 38
- 239000010432 diamond Substances 0.000 claims description 38
- 239000010936 titanium Substances 0.000 claims description 29
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 22
- FOZHTJJTSSSURD-UHFFFAOYSA-J titanium(4+);dicarbonate Chemical compound [Ti+4].[O-]C([O-])=O.[O-]C([O-])=O FOZHTJJTSSSURD-UHFFFAOYSA-J 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- -1 titanium halide Chemical class 0.000 claims description 6
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000012808 vapor phase Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 description 27
- 229910052760 oxygen Inorganic materials 0.000 description 23
- 239000010408 film Substances 0.000 description 15
- 239000011230 binding agent Substances 0.000 description 13
- 239000006061 abrasive grain Substances 0.000 description 10
- 238000010304 firing Methods 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000005388 borosilicate glass Substances 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000005355 lead glass Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Landscapes
- Polishing Bodies And Polishing Tools (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、被覆高硬質粉末及びそ
の製造方法に関し、さらに詳しくは、とくに、セラミッ
クスなどの硬脆材料の研削加工に好適な超砥粒となりう
る被覆高硬質粉末及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a coated high-hardness powder and a method for producing the same, and more particularly to a coated high-hardness powder capable of forming superabrasive grains suitable for grinding hard and brittle materials such as ceramics and the like. It relates to a manufacturing method.
【０００２】[0002]
【従来の技術】近年、セラミックス材料は各種分野にお
ける新素材として注目を集めており、例えば、工具材
料、ＩＣ基板用絶縁材料、人工骨、人工歯根などの医用
材料、あるいは自動車のエンジン部品などの各種機械材
料として、その重要性が高まっている。2. Description of the Related Art In recent years, ceramic materials have been attracting attention as new materials in various fields, for example, tool materials, insulating materials for IC substrates, medical materials such as artificial bones and artificial tooth roots, and automobile engine parts. As various machine materials, their importance is increasing.
【０００３】ところで、これらのセラミックス材料は硬
脆材料であるため、例えば高精度の研削加工を行う場
合、従来の工具を使用することができない場合が多い。By the way, since these ceramic materials are hard and brittle materials, it is often impossible to use a conventional tool when, for example, performing highly accurate grinding.
【０００４】そこで、セラミックス材料のような硬脆材
料の研削加工を行う場合は、ダイヤモンド粉末などの超
硬砥粒を含有する砥石を使用することが一般的である。
このような砥石は、該超硬砥粒をアルミナ（Ａｌ2 Ｏ3)
などの金属酸化物よりなる粒子とともに、樹脂またはガ
ラス質無機物などの結合剤と混合したものを成形、焼成
することにより製造される。このとき、結合剤として樹
脂を用いたものはレジノイドボンド砥石、また、ガラス
質無機物を用いたものはビトリファイドボンド砥石と称
される。Therefore, when grinding a hard and brittle material such as a ceramic material, it is common to use a grindstone containing cemented carbide grains such as diamond powder.
Such a grindstone is prepared by using the cemented carbide grains made of alumina (Al 2 O 3 ).
It is produced by molding and firing a mixture of particles made of a metal oxide such as the above with a binder such as a resin or a glassy inorganic substance. At this time, one using a resin as a binder is called a resinoid bond grindstone, and one using a glassy inorganic material is called a vitrified bond grindstone.
【０００５】ダイヤモンド粉末を主成分とするレジノイ
ドボンド砥石の場合、該粉末と結合剤である樹脂との結
合力を高めるために、通常、粉末表面にニッケル（Ｎ
ｉ）などの金属を被覆することが行われている。このよ
うにＮｉ被覆を施すことにより、ダイヤモンド粉末表面
に凹凸が形成されるため、樹脂との機械的結合力が高ま
り、結果として樹脂の粉末保持力が向上する。また、Ｎ
ｉは熱伝導性が低いため、砥石使用中に砥粒先端で発生
した熱により樹脂が劣化するのを防止するという利点が
ある。しかしながら、その反面、Ｎｉ被膜が砥石の目詰
まりを引起こすという問題が生ずる。また、ダイヤモン
ド粉末表面をＴｉ（Ｃ，Ｎ，Ｏ）で被覆してなる被覆ダ
イヤモンド粉末が特開昭５５−１６２４９９号公報に、
またＴｉＣで被覆してなる被覆ダイヤモンド粉末が特公
昭４７−１７９６４号公報に開示されている。しかし、
これら両公報に開示された被覆ダイヤモンド粉末も、被
膜の密着性という点においては未だ改良の余地を残すも
のであった。In the case of a resinoid bond grindstone containing diamond powder as a main component, nickel (N) is usually used on the surface of the powder in order to enhance the binding force between the powder and the resin as the binder.
Coating with a metal such as i) is performed. By applying the Ni coating in this manner, irregularities are formed on the surface of the diamond powder, so that the mechanical binding force with the resin is increased, and as a result, the powder holding force of the resin is improved. Also, N
Since i has low thermal conductivity, it has an advantage of preventing the resin from deteriorating due to the heat generated at the tip of the abrasive grains during use of the grindstone. However, on the other hand, the Ni coating causes a problem that the grindstone is clogged. Further, a coated diamond powder obtained by coating the surface of the diamond powder with Ti (C, N, O) is disclosed in JP-A-55-162499.
Further, a coated diamond powder coated with TiC is disclosed in Japanese Examined Patent Publication No. 47-17964. But,
The coated diamond powders disclosed in both of these publications still leave room for improvement in terms of coating adhesion.
【０００６】一方、同じくダイヤモンド粉末を主成分と
するビトリファイドボンド砥石は、高温焼成により製造
されるため、固相反応による砥粒と結合剤との結合力は
強い。しかしながら、その高温焼成工程においてダイヤ
モンドの熱腐食が生じ、製造が困難であるという問題を
有する。On the other hand, since the vitrified bond grindstone which also contains diamond powder as a main component is manufactured by high temperature firing, the bonding force between the abrasive grains and the binder due to the solid phase reaction is strong. However, there is a problem in that diamond is thermally corroded in the high temperature firing step, which makes production difficult.
【０００７】[0007]
【発明が解決しようとする課題】本発明は従来技術のこ
のような問題を解消し、砥石の砥粒として使用する被覆
高硬質粉末であって、結合剤が樹脂である場合は、該樹
脂との結合力が強く、かつ、被膜による砥石の目詰まり
が発生することなく、一方、結合剤がガラス質無機物の
場合は、焼成時に粉末自体の熱腐食が発生することのな
い被覆高硬質粉末及びその製造方法を提供することを目
的とする。DISCLOSURE OF THE INVENTION The present invention solves the above-mentioned problems of the prior art, and is a coated high-hardness powder used as abrasive grains of a grindstone, and when the binder is a resin, Has a strong binding force, and does not cause clogging of the grindstone due to the coating film, while the binder is a glassy inorganic material, a coating high-hard powder that does not cause thermal corrosion of the powder itself during firing and It is an object to provide a manufacturing method thereof.
【０００８】[0008]
【課題を解決するための手段】本発明者らは、上記目的
を達成するために鋭意研究を重ねた結果、ダイヤモンド
粉末及び／又は立方晶窒化ホウ素粉末表面に、従来のＮ
ｉ又はＴｉ（Ｃ，Ｎ，Ｏ）の被膜に代えて、炭化チタン
（ＴｉＣ）と炭酸化チタン（Ｔｉ（Ｃ，Ｏ））の被膜、
又は炭酸化チタンの被膜を被覆してなる被覆高硬質粉末
が超硬砥粒としての優れた性質を具備しており、かつ、
該粉末を主成分としてなる砥石が優れた研削性能を有す
ることを確認して、本発明を完成するに至った。DISCLOSURE OF THE INVENTION As a result of intensive studies to achieve the above-mentioned object, the inventors of the present invention have found that a conventional N powder is formed on the surface of diamond powder and / or cubic boron nitride powder.
Instead of i or Ti (C, N, O) coating, titanium carbide (TiC) and titanium carbonate (Ti (C, O)) coating,
Alternatively, a coated high-hardness powder formed by coating a coating film of titanium carbonate has excellent properties as a cemented carbide abrasive grain, and
The present invention has been completed by confirming that a grindstone containing the powder as a main component has excellent grinding performance.
【０００９】すなわち、本発明の被覆高硬質粉末は、ダ
イヤモンド粉末及び／又は立方晶窒化ホウ素粉末の表面
に、炭化チタンと炭酸化チタンを被覆、又は炭酸化チタ
ンを被覆してなることを特徴とし、その製造方法は、ハ
ロゲン化チタンと炭化水素ガスを反応ガスとする気相化
学成長法を適用して、ダイヤモンド粉末及び／又は立方
晶窒化ホウ素粉末の表面に、炭化チタンと炭酸化チタン
を被覆、又は炭酸化チタンを被覆する被覆高硬質粉末の
製造方法であって、該ハロゲン化チタンと炭化水素ガス
のモル比が１：３〜１：９、反応温度が８００〜１，１
００℃であることを特徴とする。That is, the coated high-hardness powder of the present invention is characterized in that the surface of the diamond powder and / or the cubic boron nitride powder is coated with titanium carbide and titanium carbonate, or with titanium carbonate. The production method is a vapor phase chemical growth method using titanium halide and a hydrocarbon gas as reaction gases to coat the surfaces of diamond powder and / or cubic boron nitride powder with titanium carbide and titanium carbonate. Or a method for producing a coated high hardness powder coating titanium carbonate, wherein the molar ratio of the titanium halide and the hydrocarbon gas is 1: 3 to 1: 9, and the reaction temperature is 800 to 1,1.
It is characterized in that it is 00 ° C.
【００１０】まず、本発明の被覆高硬質粉末において、
使用する粉末はダイヤモンド粉末または立方晶窒化ホウ
素（ＣＢＮ）粉末あるいはこれらの混合物である。使用
するダイヤモンド粉末の種類はとくに制限されるもので
はなく、天然、人工いずれのものであってもよい。ま
た、その形状等もとくに限定されないが、結晶軸に異方
性のあるもの、例えば、ＥＭＢＳ（＃３０／４０、ド・
ビアース社）あるいはＣＤＡ（＃８０／１００、ド・ビ
アース社）などは、通常の立方八面体型のものに比べて
熱膨張係数が小さいため、後述する工程で炭化チタン
（ＴｉＣ）と炭酸化チタン（Ｔｉ（Ｃ，Ｏ））の被覆、
又はＴｉ（Ｃ，Ｏ）の被覆を形成すると、該膜にクラッ
クが発生しにくいという点で好ましい。さらに、Ｎｉ、
Ｆｅ、Ｃｏなどの金属不純物が多く含まれているダイヤ
モンドは、ＴｉＣとＴｉ（Ｃ，Ｏ）の被膜、又はＴｉ
（Ｃ，Ｏ）被膜が付着強度を高めるので好ましい。砥石
として使用するダイヤモンド粉末又はＣＢＮ粉末の粒径
は、１０〜５０μm 程度であることが好ましい。First, in the coated high-hardness powder of the present invention,
The powder used is diamond powder or cubic boron nitride (CBN) powder or a mixture thereof. The type of diamond powder used is not particularly limited and may be natural or artificial. The shape and the like are not particularly limited, but those having an anisotropic crystal axis, such as EMBS (# 30/40,
Bias) or CDA (# 80/100, de Bias) has a smaller coefficient of thermal expansion than the ordinary cubic octahedron type, so titanium carbide (TiC) and titanium carbonate are used in the process described below. (Ti (C, O)) coating,
Alternatively, it is preferable to form a Ti (C, O) coating because cracks are less likely to occur in the film. In addition, Ni,
Diamond containing a large amount of metallic impurities such as Fe and Co is a film of TiC and Ti (C, O), or Ti.
A (C, O) coating is preferable because it enhances the adhesion strength. The particle size of diamond powder or CBN powder used as a grindstone is preferably about 10 to 50 μm.
【００１１】一方、該ダイヤモンド及び／又はＣＢＮ粉
末表面に形成される被膜はＴｉＣとＴｉ（Ｃ，Ｏ）、又
はＴｉ（Ｃ，Ｏ）よりなるものである。Ｔｉ（Ｃ，Ｏ）
は後述するＣＶＤ法を適用したＴｉＣコーティング工程
において、反応条件により酸素が混入して生成するもの
であるが、粉末表面への付着強度が高く、被膜として優
れた特性を有するものである。この場合、酸素の含有量
はできるだけ少ないことが望ましい。On the other hand, the film formed on the surface of the diamond and / or CBN powder is composed of TiC and Ti (C, O), or Ti (C, O). Ti (C, O)
In the TiC coating step using the CVD method described below, oxygen is mixed and generated depending on the reaction conditions, but it has high adhesion strength to the powder surface and has excellent properties as a coating. In this case, it is desirable that the oxygen content is as low as possible.
【００１２】これらＴｉＣとＴｉ（Ｃ，Ｏ）の被膜又は
Ｔｉ（Ｃ，Ｏ）被膜の層厚はとくに限定されるものでは
ないが、通常、０．１〜６μm 程度に設定することが好
ましい。The layer thickness of these TiC and Ti (C, O) coatings or Ti (C, O) coatings is not particularly limited, but it is usually preferable to set it to about 0.1 to 6 μm.
【００１３】ついで、本発明の被覆高硬質粉末の製造方
法について説明する。Next, a method for producing the coated high-hardness powder of the present invention will be described.
【００１４】本発明の被覆高硬質粉末は、前述したよう
に化学気相成長法（ＣＶＤ法）を適用してダイヤモンド
及び／又はＣＢＮ粉末表面をＴｉＣとＴｉ（Ｃ，Ｏ）の
被膜、又はＴｉ（Ｃ，Ｏ）の被膜によって被覆される。
この被覆工程には上記ＣＶＤ法の他にスパッタ法やイオ
ンプレーティング法などのＰＶＤ法による一般的な薄膜
形成法を適用することができるが、量産性および膜の付
着強度の２点を勘案すると、ＣＶＤ法を適用することが
最も好ましい。As described above, the coated high-hardness powder of the present invention is formed by applying the chemical vapor deposition method (CVD method) to the surface of diamond and / or CBN powder to form a film of TiC and Ti (C, O), or Ti. It is covered with a film of (C, O).
In addition to the above CVD method, a general thin film forming method using a PVD method such as a sputtering method or an ion plating method can be applied to this coating step, but in consideration of two points of mass productivity and film adhesion strength. It is most preferable to apply the CVD method.
【００１５】このＣＶＤ法を適用して行なわれる工程、
例えば、ＴｉＣ被覆は、次式：Steps performed by applying this CVD method,
For example, a TiC coating has the formula:
【化１】 で示される２つの反応により進められる。[Chemical 1] It is carried out by two reactions shown by.
【００１６】このような被覆工程における反応条件は、
ＴｉＣとＴｉ（Ｃ，Ｏ）の被膜又はＴｉ（Ｃ，Ｏ）被膜
の層厚等により適宜設定することが好ましいが、膜層の
成長速度及び密着性を勘案して、ハロゲン化チタンと炭
化水素ガスのモル比を１：３〜１：９に、また反応温度
を８００〜１，１００℃に設定する。さらにＣＨ4 など
の反応ガスの分圧を高めることが、付着強度の高い被膜
を得るうえで望ましい。このようにして得られた被膜は
微粒多結晶となり、極めて付着強度の高いものである。The reaction conditions in such a coating process are as follows:
It is preferable to set it appropriately according to the layer thickness of the TiC and Ti (C, O) coating or the Ti (C, O) coating, but in consideration of the growth rate and adhesion of the film layer, titanium halide and hydrocarbon The gas molar ratio is set to 1: 3 to 1: 9 and the reaction temperature is set to 800 to 1100 ° C. Further, it is desirable to increase the partial pressure of the reaction gas such as CH 4 in order to obtain a film having high adhesion strength. The coating film obtained in this way becomes fine-grained polycrystals and has extremely high adhesion strength.
【００１７】さらに、ダイヤモンド粉末を使用する場合
は、この被覆工程に先立って、ダイヤモンド粉末に真空
中、９００〜１，３００℃において熱処理を施すと、被
膜の付着強度がさらに向上するので、好ましい。これ
は、このような熱処理工程において、ダイヤモンド粉末
表面にＮｉなどの内部不純物が析出し、このようなダイ
ヤモンド粉末に被覆すると、被膜がウィスカー状とな
り、付着強度が向上するものと考えられる。なお、この
被覆工程において、諸条件を調節することにより、ダイ
ヤモンド粉末表面にまずＴｉＣx(０＜ｘ＜１）よりなる
層を形成し、そののちＴｉ（Ｃ，Ｏ）で被覆することに
より、炭素の割合が連続的に変化する被膜を形成する
と、被膜の密着性を向上させるうえで、さらに有利であ
る。Further, in the case of using diamond powder, it is preferable to heat-treat the diamond powder in vacuum at 900 to 1,300 ° C. prior to this coating step because the adhesion strength of the coating is further improved. It is considered that internal impurities such as Ni are deposited on the surface of the diamond powder in such a heat treatment step, and when the diamond powder is coated with such impurities, the coating becomes whiskers and the adhesion strength is improved. In this coating step, by adjusting various conditions, a layer made of TiC x (0 <x <1) is first formed on the surface of the diamond powder, and then the layer is coated with Ti (C, O). Forming a coating film in which the proportion of carbon changes continuously is more advantageous in improving the adhesion of the coating film.
【００１８】ついで、本発明の被覆高硬質粉末を砥石に
適用する場合について説明する。Next, the case of applying the coated high-hardness powder of the present invention to a grindstone will be described.
【００１９】該砥石は、前述のように、砥粒主成分とし
て、被覆高硬質粉末（ＴｉＣとＴｉ（Ｃ，Ｏ）の被膜又
はＴｉ（Ｃ，Ｏ）の被膜で被覆したダイヤモンド及び／
又はＣＢＮ粉末）を使用し、これと、結合剤および添加
剤を含むものである。結合剤は、砥粒その他の成分を結
合せしめ、担持するための成分であり、特に制限される
ものではないが、主として、樹脂とガラス質無機物の２
種類に分けられる。結合剤として熱硬化性樹脂、例え
ば、フェノール樹脂、エポキシ樹脂、ポリイミド樹脂な
どを使用した砥石をレジノイドボンド砥石、結合剤とし
てホウケイ酸ガラス、鉛ガラス、ナトリウムガラスなど
のガラス質無機物を使用した砥石をビトリファイドボン
ド砥石と称する。As described above, the grindstone is a diamond and / or diamond coated with a coating of high-hardness powder (TiC and Ti (C, O) coating or Ti (C, O) coating as the main abrasive grain.
Or CBN powder), which contains a binder and an additive. The binder is a component for binding and supporting the abrasive grains and other components, and is not particularly limited, but is mainly composed of the resin and the glassy inorganic substance.
It is divided into types. Thermosetting resin as a binder, for example, a grindstone using a phenol resin, an epoxy resin, a polyimide resin, a resinoid bond grindstone, a borosilicate glass as a binder, lead glass, a grindstone using a glassy inorganic material such as sodium glass It is called a vitrified bond grindstone.
【００２０】本発明の被覆高硬質粉末を砥石に適用する
場合には、このほかに、添加剤として、中空カーボン、
カーボン、Ａｌ2 Ｏ3 、ＺｒＯ2 、ＳｉＣ、ＢａＣ、ク
リオライト、ＦｅＳなどの充填剤（中でも、Ａｌ2 Ｏ
3 、ＺｒＯ2 、ＳｉＣ、ＢａＣを含有すると、ドレッシ
ングが容易になって目詰まりが起こりにくい点で好まし
い）；フルフラール、水ガラスなどの湿潤剤；生石灰な
どの吸水剤の１種又は２種以上を含有する。When the coated high-hardness powder of the present invention is applied to a grindstone, in addition to this, as an additive, hollow carbon,
Fillers such as carbon, Al 2 O 3 , ZrO 2 , SiC, BaC, cryolite, FeS (among others, Al 2 O
3 , ZrO 2 , SiC, and BaC are preferable in that dressing is easy and clogging is less likely to occur); wetting agents such as furfural and water glass; water absorbing agents such as quick lime; contains.
【００２１】一方、本発明の被覆高硬質粉末を砥石に適
用する場合、砥石はある程度の気孔を含有していること
が好ましい。気孔は研削時に生ずる切屑を排出し、か
つ、研削時に発生する熱を放散させる機能を有するため
である。この気孔の含有量、すなわち、気孔率は２０〜
３５％程度であることが好ましい。On the other hand, when the coated high-hardness powder of the present invention is applied to a grindstone, the grindstone preferably contains some pores. This is because the pores have a function of discharging chips generated during grinding and dissipating heat generated during grinding. The content of the pores, that is, the porosity is 20 to
It is preferably about 35%.
【００２２】このような砥石は、次のようにして製造さ
れる。すなわち、まず、上述の各成分を所定の配合比で
混合する。そののち、ホットプレス法、真空焼成法、不
活性ガス雰囲気焼成法など、通常の方法を適用して、所
定の形状に成形する。ついで、この成形体を焼成して目
的とする砥石を得る。この場合の焼成温度は、レジノイ
ドボンド砥石の場合は１６０〜２５０℃が好ましく、ビ
トリファイドボンド砥石の場合は結合剤の軟化点に合せ
て決定することが必要であり、例えばホウケイ酸ガラス
では８００℃程度、高鉛ガラスでは５００℃程度に設定
することが好ましい。Such a grindstone is manufactured as follows. That is, first, the above-mentioned components are mixed in a predetermined mixing ratio. After that, a normal method such as a hot pressing method, a vacuum firing method, an inert gas atmosphere firing method, or the like is applied to form the material into a predetermined shape. Then, the formed body is fired to obtain a target grindstone. In this case, the firing temperature is preferably 160 to 250 ° C in the case of resinoid bond grindstone, and it is necessary to determine it in accordance with the softening point of the binder in the case of vitrified bond grindstone, for example, about 800 ° C in borosilicate glass. For high lead glass, it is preferable to set the temperature to about 500 ° C.
【００２３】[0023]
実施例１ ダイヤモンド粉末としてＣＤＡ＃１４０／１７０（ド・
ビアース社）を使用し、この粉末にＣＶＤ法を適用して
被覆ダイヤモンド粉末を作製した。被覆方法は、大気圧
下の炉内でダイヤモンド粉末を揺動させ、９５％のＨ2
と５％のＣＨ4(９９．９％純度）の組成を有するガスを
流入させながら、１，０７０℃まで昇温した後、ガスの
流入を停止し、真空ポンプを用いて炉内を減圧とした。
ついで、表１に示す炉内圧力、Ｈ2 、ＴｉＣｌ4 とＣＨ
4 の炉内ガス組成及び保持時間により、ダイヤモンド粉
末の表面に被膜を形成した。Example 1 As a diamond powder, CDA # 140/170 (
Coated diamond powder was produced by applying a CVD method to this powder using a BEARTH company. The coating method was rocking the diamond powder in a furnace under atmospheric pressure to obtain 95% H 2
And a gas having a composition of 5% CH 4 (99.9% purity) were flowed in, the temperature was raised to 1,070 ° C., the gas flow was stopped, and the pressure inside the furnace was reduced using a vacuum pump. did.
Then, the pressure in the furnace shown in Table 1, H 2 , TiCl 4 and CH
A film was formed on the surface of the diamond powder according to the gas composition in the furnace and the holding time of 4 .
【００２４】こうして得た被覆ダイヤモンド粉末の被膜
の組成及び厚さを測定した。その結果を表２に示す。The composition and thickness of the coating of the coated diamond powder thus obtained were measured. The results are shown in Table 2.
【００２５】[0025]
【表１】 [Table 1]
【００２６】[0026]
【表２】 [Table 2]
【００２７】これらの被覆ダイヤモンド粉末を砥粒の主
成分とし、表３に示す組成を有するビトリファイドボン
ド砥石を作製した。A vitrified bond grindstone having the composition shown in Table 3 was prepared by using these coated diamond powders as a main component of abrasive grains.
【００２８】[0028]
【表３】 [Table 3]
【００２９】まず、秤量した砥粒に水ガラスをスポイト
で少量加え、砥粒全体を湿潤させた後、結合剤を加えて
充分に混合した。ついで、所定形状の金型を使用し、適
度に湿潤した原料を入れ、加圧成形した。このとき、成
形圧力は２kgf/mm2 とし、保持時間は３分間とした。し
かるのち、水素雰囲気中で、得られた成形体を昇温速度
２９０℃／h 、８００℃において約１時間焼成し、２０
mm×５０mm×５mmの砥石を得た。なお、通常のビトリフ
ァイドボンド砥石の焼成温度は１，２００〜１，３００
℃であるが、本実施例ではダイヤモンド粉末の熱腐食を
防ぐために、上記の８００℃という低温で焼成を行っ
た。このようにして得られたビトリファイドボンド砥石
の気孔率は約３０％、曲げ強度は１．７kgf/mm2 であっ
た。First, a small amount of water glass was added to the weighed abrasive grains with a dropper to wet the entire abrasive grains, and then a binder was added and thoroughly mixed. Then, a mold having a predetermined shape was used, an appropriately moistened raw material was charged, and pressure molding was performed. At this time, the molding pressure was 2 kgf / mm 2 , and the holding time was 3 minutes. After that, the obtained molded body is fired in a hydrogen atmosphere at a temperature rising rate of 290 ° C./h and 800 ° C. for about 1 hour, and
A grindstone of mm × 50 mm × 5 mm was obtained. The firing temperature of a normal vitrified bond grindstone is 1,200 to 1,300.
However, in this example, in order to prevent thermal corrosion of the diamond powder, the firing was carried out at the low temperature of 800 ° C. mentioned above. The vitrified bond grindstone thus obtained had a porosity of about 30% and a bending strength of 1.7 kgf / mm 2 .
【００３０】このようなビトリファイドボンド砥石を使
用して、以下に示す耐久性試験を行った。その結果を図
１に示す。The following durability test was conducted using such a vitrified bond grindstone. The result is shown in FIG.
【００３１】耐久性試験 被加工体に１００mm×１５mm×１０mmのＳｉ3 Ｎ4 基焼
結体を使用し、切込み量を２０μm ／回として、片道ご
とに切込みを入れ、５，０００μm まで切込んだ。この
とき、切込み１，０００μm ごとに、砥石外周部の摩耗
量を電気マイクロメーターで測定し、研削距離と砥石摩
耗量との関係を求めた。なお、被膜の被覆されていない
ダイヤモンド粉末を用いた砥石を作製し、比較品２とし
て耐久性試験を行った。その結果を併せて図１に示す。Durability Test A 100 mm × 15 mm × 10 mm Si 3 N 4 based sintered body was used as a work piece, and the cut amount was 20 μm / time, and a cut was made for each way to cut up to 5,000 μm. . At this time, the wear amount of the outer peripheral portion of the grindstone was measured with an electric micrometer for every 1,000 μm of cut, and the relationship between the grinding distance and the grindstone wear amount was obtained. In addition, a grindstone using diamond powder not coated with a coating was prepared, and a durability test was performed as Comparative Product 2. The results are also shown in FIG.
【００３２】実施例２ 実施例１のダイヤモンド粉末に代えて、ＣＢＮ粉末（昭
和電工社製ＳＢＮ−Ｔ＃１４０／１７０）を使用し、実
施例１の本発明品１及び４と同様にしてＣＢＮ粉末の表
面に被膜を被覆して、本発明品５及び６を作製した。ま
た、比較として実施例１の比較品１と同様にしてＣＢＮ
粉末の表面にＴｉＣ被膜を被覆し、比較品３を作製し
た。Example 2 CBN powder (SBN-T # 140/170 manufactured by Showa Denko KK) was used in place of the diamond powder of Example 1, and CBN was used in the same manner as in the invention products 1 and 4 of Example 1. Inventive products 5 and 6 were prepared by coating the surface of the powder with a coating. Further, as a comparison, the CBN was prepared in the same manner as the comparative product 1 of Example 1.
Comparative product 3 was prepared by coating the surface of the powder with a TiC film.
【００３３】こうして得た本発明品５、６及び比較品３
を用いて、実施例１と同様にしてビトリファイドボンド
砥石を作製し、実施例１と同一の条件で耐久性試験を行
ったところ、本発明品５、６は、いずれも実施例１の本
発明品１、４とほとんど同様の傾向を示し、比較品３は
比較品１とほとんど同様の傾向を示した。The invention products 5, 6 and comparative product 3 thus obtained
A vitrified bond grindstone was produced in the same manner as in Example 1 and a durability test was conducted under the same conditions as in Example 1. The products 1 and 4 showed almost the same tendency, and the comparison product 3 showed almost the same tendency as the comparison product 1.
【００３４】[0034]
【発明の効果】以上の説明から明らかなように、本発明
の被覆高硬質粉末は、レジノイドボンドおよびビトリフ
ァイドボンドのいずれのタイプの砥石の砥粒として用い
た場合も、優れた研削性能を有するとともに、耐久性に
も優れた砥石が得られることが確認された。これは本発
明のＴｉＣとＴｉ（Ｃ，Ｏ）の被膜又はＴｉ（Ｃ，Ｏ）
被膜による被覆ダイヤモンド及び／又はＣＢＮ粉末と結
合剤との結合力が極めて高いことによるものである。ま
た、本発明の被覆高硬質粉末にあっては、ＴｉＣとＴｉ
（Ｃ，Ｏ）の被膜又はＴｉ（Ｃ，Ｏ）被膜の付着強度が
従来のＮｉ、ＴｉＣ又はＴｉ（Ｃ，Ｎ，Ｏ）よりなる被
膜の付着強度に比べて高いため、被膜の剥離による砥石
の目詰まりなどの発生が全くない。As is clear from the above description, the coated high-hardness powder of the present invention has excellent grinding performance when used as an abrasive grain of any type of grindstone of resinoid bond and vitrified bond. It was confirmed that a grindstone excellent in durability was obtained. This is a coating of TiC and Ti (C, O) or Ti (C, O) of the present invention.
This is because the bond strength between the coating diamond and / or CBN powder and the binder is extremely high. Further, in the coated high-hardness powder of the present invention, TiC and Ti
Since the adhesion strength of the (C, O) coating or the Ti (C, O) coating is higher than the adhesion strength of the conventional Ni, TiC or Ti (C, N, O) coating, the grindstone by peeling the coating There is no occurrence of clogging.
【００３５】さらに、該被覆粉末を使用したビトリファ
イドボンド砥石の場合、８００〜９００℃の低温で焼成
できるため、ダイヤモンドの熱腐食の発生が防止され
る。したがって、その工業的価値は極めて大きい。Further, in the case of a vitrified bond grindstone using the coating powder, since it can be fired at a low temperature of 800 to 900 ° C., thermal corrosion of diamond is prevented. Therefore, its industrial value is extremely large.
【図１】実施例１の耐久性試験における研削距離と砥石
摩耗量との関係を示すグラフである。FIG. 1 is a graph showing a relationship between a grinding distance and a grindstone wear amount in a durability test of Example 1.
１ 本発明品１ ２ 本発明品２ ３ 本発明品３ ４ 本発明品４ ５ 比較品１ ６ 比較品２ 1 Inventive product 1 2 Inventive product 2 3 Inventive product 3 4 Inventive product 4 5 Comparative product 1 6 Comparative product 2
Claims (2)
ホウ素粉末の表面に、炭化チタンと炭酸化チタンを被
覆、又は炭酸化チタンを被覆してなることを特徴とする
被覆高硬質粉末。1. A coated high-hardness powder characterized in that the surface of diamond powder and / or cubic boron nitride powder is coated with titanium carbide and titanium carbonate, or with titanium carbonate.
ガスとする気相化学成長法を適用して、ダイヤモンド粉
末及び／又は立方晶窒化ホウ素粉末の表面に、炭化チタ
ンと炭酸化チタンを被覆、又は炭酸化チタンを被覆する
被覆高硬質粉末の製造方法であって、 該ハロゲン化チタンと炭化水素ガスのモル比が１：３〜
１：９、反応温度が８００〜１，１００℃であることを
特徴とする被覆高硬質粉末の製造方法。2. The surface of diamond powder and / or cubic boron nitride powder is coated with titanium carbide and titanium carbonate by applying a vapor phase chemical growth method using titanium halide and hydrocarbon gas as reaction gases. Alternatively, a method for producing a coated high-hardness powder coating titanium carbonate, wherein the molar ratio of the titanium halide to the hydrocarbon gas is 1: 3 to.
1: 9, The reaction temperature is 800-1,100 degreeC, The manufacturing method of the coating high hardness powder characterized by the above-mentioned.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4257050A JPH0761615B2 (en) | 1992-09-28 | 1992-09-28 | Coated high hardness powder and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4257050A JPH0761615B2 (en) | 1992-09-28 | 1992-09-28 | Coated high hardness powder and method for producing the same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13914285A Division JPS61297079A (en) | 1985-06-27 | 1985-06-27 | Covered highly hard powder and manufacture thereof and grindstone made of said powder as main component |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05220668A JPH05220668A (en) | 1993-08-31 |
| JPH0761615B2 true JPH0761615B2 (en) | 1995-07-05 |
Family
ID=17301045
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4257050A Expired - Lifetime JPH0761615B2 (en) | 1992-09-28 | 1992-09-28 | Coated high hardness powder and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0761615B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2005213530A1 (en) * | 2004-01-15 | 2005-08-25 | Element Six Limited | Coated abrasives |
| CN108447507B (en) * | 2013-09-28 | 2020-07-28 | Hoya株式会社 | Method for manufacturing glass substrate for magnetic disk, method for manufacturing magnetic disk, and grinding tool |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5531563A (en) * | 1978-08-29 | 1980-03-05 | Tatsuro Kuratomi | Built-up diamond tool and its manufacturing method |
-
1992
- 1992-09-28 JP JP4257050A patent/JPH0761615B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05220668A (en) | 1993-08-31 |
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