JPH08267644A - Diamond composite member and its manufacture - Google Patents

Abstract

PURPOSE: To provide a diamond composite member which can strongly bond a diamond-like film and a substrate film and a method for manufacturing it. CONSTITUTION: A substrate film 3 consisting of at least one of metals, plastics and ceramics is formed on a recessed part side of a diamond-like film 1 consisting of at least one of diamond and diamond-like carbon prepd. by means of a vapor phase synthetic method on the surface of which a recessed part 2 is formed. In addition, a diamond-like film 1 consisting of at least one of diamond and diamond-like carbon is formed on the surface of a base sheet by means of the vapor phase synthetic method and the recessed part 2 is formed on this diamond-like film 1 and a substrate film 3 consisting of at least one among metals, plastics and ceramics is formed on the face of the recessed part side of the diamond-like film and then, the base sheet is removed to form a diamond composite member.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a diamond composite member and a method for manufacturing the same, and more particularly to industrial cutting tools such as machining cutting tools, drills, end mills and slitter knives, various sliding parts, yarn paths, The present invention relates to wear resistant members such as guide bushes, parts for various measuring instruments, precision processing blades, medical instruments, various electronic elements, heat dissipation plates for electronic parts, and the like, and a manufacturing method thereof.

[0002]

2. Description of the Related Art Ultra-hard materials such as diamond have hitherto been produced by a large-scale ultra-high pressure press machine. However, according to the vapor phase synthesis method (CVD), these materials can be obtained by a simple method, and therefore, ultra-hard materials such as diamond produced by the vapor phase synthesis method are expected to have a wide range of applications in the future ( See JP-A-60-54995).

However, the ultra-hard film such as diamond formed by CVD has a problem that the adhesion to the base material is insufficient and peeling easily occurs. Therefore, as a countermeasure against this, it has been proposed to form a diamond film on a silicon substrate, then remove the silicon substrate, cut out the diamond film and braze it to a base material made of a cemented carbide tool.

[0004]

However, in the method of directly brazing the diamond film to the base material, the wettability between the diamond and the brazing material (for example, Ag, Au-Sn, etc.) is low, so that the diamond film There is a problem that the bonding strength between the base material and the base material is low and, for example, the diamond film falls off from the base material in a short time. Further, in this method, since it is necessary to coat diamond thickly, there is a problem in that there are variations in the size of the crystal grains and there is a large variation in performance.

Moreover, since it is necessary to form a thick diamond film, the cost for forming a thick diamond film (for example, electric power cost, equipment cost, time required for manufacturing) increases, and as a whole, it is conventional. No superiority to the artificial diamond by the ultra-high pressure synthesis method was observed.

Therefore, at present, tools in which an ultra-hard film such as diamond is formed have not yet become widespread.

[0007]

The present inventor has developed a method of forming a porous diamond film, filling voids between the diamond crystal grains with tungsten or the like, and applying the method previously. . However, in this method, especially in the case of a diamond film coated on a large area, the size and crystal state of the diamond particles in the diamond film may vary, and it has been found that the filling property of tungsten or the like tends to vary. did. Therefore, the inventors have found a method of forming a recess by a certain means irrespective of the material of the produced diamond-like film and filling the recess with a metal or the like, and arrived at the present invention.

That is, the diamond composite member of the present invention is
Consists of at least one of diamond and diamond-like carbon produced by the vapor phase synthesis method, and at least one of metal, plastic and ceramics on the concave-side surface of the diamond film having concaves formed on the surface thereof. It is formed by forming a support film.

Further, the diamond composite member of the present invention is
A diamond film made of at least one of diamond and diamond-like carbon is formed on the surface of the substrate by a vapor phase synthesis method, a recess is formed in the diamond film, and a metal is formed on the recess-side surface of the diamond film. This is a method of removing the substrate after forming a support film made of at least one of plastic and ceramics.

The diamond-like carbon in the present invention means
It means carbon which is very dense and has high hardness, no grain boundaries are observed, and a structure different from that of crystalline diamond having a regular crystal structure. These can be formed on a substrate made of silicon, molybdenum or the like by a known method such as microwave CVD.

The porosity of the concave portion of the diamond film is 5 to 8
From the viewpoint of improving the adhesion of the diamond film to the support film, it is preferably 35 to 65%. The porosity of the concave portion of the diamond film is the area ratio of the concave portion of the diamond film to other areas, and is expressed as the ratio of the area occupied by the concave portion to the total area. This porosity is calculated by measuring the areas of the concave portions and the other convex portions with an image analyzer.

The recesses are formed in a dot shape as shown in FIG. 3 by using a laser or a diamond grindstone, or as shown in FIG.
As shown in FIG. The concave portion may be formed in a curved shape. Also, in an atmosphere containing oxygen, 500 to 750
The depressions can be formed by heat treatment at 0.5 ° C. for 0.5 to 4 hours or by etching in plasma containing oxygen.

Of these, the case of using a laser is excellent in forming the recesses from various points. Although the type of laser can be arbitrarily selected, a YAG laser is generally effectively used. The excimer laser is particularly effective when fine processing is required.

Although the desired thickness of the diamond film can be used, it is generally 1 to 500 μm, preferably 5 to 200 μm in consideration of wear resistance and economy. Although the depth and width of the recess can be set arbitrarily, generally, the depth of the recess is one-half or less of that of the diamond film, and the width of the recess is about the same as or less than the depth of the recess, and the anchor effect is obtained. Is desirable. However, for special applications such as electronic devices, a through hole is formed in the diamond film as a recess, and the above metal, plastic, and ceramics are filled in the through hole,
It is also possible to prepare a composite member in which diamonds having a desired shape are dispersed between filling materials.

The shape of the concave portion can be set arbitrarily, but if the shape is planar (when the width of the concave portion is wide), the adhesiveness is low, so that it is desirable to be dot-like or linear (the width of the concave portion is narrow). In the case of a linear shape, the corners of the diamond tend to be chipped at the intersections of the lines, so make the depth of the recess deep at the intersections of the lines,
It is better to prevent chipping.

The material of the support film can be arbitrarily selected according to the application. As the metal used for the support film material, Al, M
o, Zr, W, Ti, Ni, Ta, Nb, Co, Fe,
It is made of at least one kind of metal selected from Cr, Cu and the like, and W and Mo are particularly preferable in that the coefficient of thermal expansion is close to that of diamond. In addition, Ni, Co, and Cu are desirable in terms of easy plating. The thickness of the support film made of metal is preferably 0.05 to 3.0 mm, and particularly preferably 0.1 to 1.0 mm from the viewpoint of manufacturing cost. The support film is formed by a physical vapor phase method such as a vacuum deposition method, a sputtering method, an ion plating method (PV
D), thermal CVD, plasma CVD, photo CVD, chemical jet method (CVD) such as plasma jet method, but when filling metal such as Cu, Ni, Cr, electroless plating, electroplating, etc. It is effective to manufacture by the method of. Diamond is not conductive, so Ni, Co,
Electroless plating of Cu is preferably used. PVD, CV
After imparting conductivity with D or electroless plating, a thick metal may be formed by electroplating or electroforming.

When the supporting film material is plastic, the supporting film is formed by filling the recesses with the plastic having plasticity. In this case, it is effective to pressurize the plastic or reduce the atmosphere to facilitate permeation.

When the support film material is at least one of metallic tungsten and tungsten carbide or ceramic, the CVD method is effective. Examples of tungsten carbide include WC and W ₂ C.

When ceramics is used as the support film material, at least one selected from the group consisting of metal carbides, nitrides, borides, oxides, and silicides,
Considering economy and practicality, T is used as the ceramic layer.
At least one carbide or nitride selected from i, Zr, Cr, Mo, W, Al and Si is preferable.

Among these, aluminum nitride,
Silicon nitride and silicon carbide can be used favorably. The thickness of the support film made of ceramics is preferably 0.05 to 3 mm from the viewpoint of cost. Considering severe usage conditions and cost, 0.1 to 1.0 mm is particularly desirable.
A known CVD method can be used to form the support film of ceramics. However, for silicon carbide, silicon nitride, etc., it is necessary to devise to lower the temperature during CVD to about 1000 ° C. or lower. As a composite material of metal and ceramics, there are cemented carbide and cermet materials.

The production of the diamond composite member of the present invention is
A diamond film made of at least one of diamond and diamond-like carbon is formed on the surface of a substrate made of silicon or the like by a CVD method, and a recess is formed in the diamond film by, for example, a laser, and A diamond composite member is formed by filling at least one of metal, plastic, and ceramics, and stacking the same material as the filling material of the recess on the surface of the diamond film on the recess side to form a support film. A material different from the filling material for the recess may be laminated as the support film. Further, the supporting film may be formed of a gradually changing graded material.

The diamond composite member thus formed is brazed to the base material if desired, and then the substrate of silicon or the like is removed, or the diamond composite member is removed after the substrate of silicon or the like is removed. It is brazed to the base metal.

[0023]

According to the diamond composite member of the present invention, a concave portion is formed in a diamond film by a laser or the like, and the concave portion is filled with at least one of metal, plastic and ceramics, and the concave surface is, for example, Since the supporting film is formed by laminating the same material as the filling material, the supporting film made of metal, plastic or ceramics and the diamond film can be firmly bonded.

If the recess is formed by laser,
Not affected by the size and shape of diamond crystal particles,
It is possible to firmly bond the metal, plastic, ceramics and the diamond film in a stable state.

[0025]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The diamond composite member of the present invention and its manufacturing method will be described in detail with reference to the drawings.

FIG. 1 shows a diamond composite member of the present invention. Reference numeral 1 is a diamond film, and a recess 2 is formed in the diamond film 1, and a recess 2 is formed.
A support film 3 is formed on the surface of the diamond-like film 1 on which is formed.

In such a diamond composite member, first, as shown in FIG. 2A, a diamond film 1 is formed on a substrate 8 made of a known material by a CVD method. At this time, the substrate 8 on which the film 1 is formed is, for example, silicon,
It is formed from a metal such as molybdenum or titanium, or a ceramic such as silicon nitride or silicon carbide, or carbon, and can be arbitrarily selected. However, it can be selected from silicon because of the ease of nucleation in the initial stage of film formation and the ease of removal in later steps. A substrate 8 consisting of is suitable.

For forming the diamond film 1, known methods such as microwave plasma CVD, hot filament CVD, ECR plasma CVD and plasma jet method are used. The diamond film is, for example, ECR plasma CV
In the D method, a Si substrate is installed in the device and the maximum strength is 2KG.
The magnetic field of 3 to 5 kW,
Substrate temperature 700 ° C or less, pressure inside the device 0.05 to 0.5T
It can be obtained by forming a film under the condition of orr. It should be noted that CH ₄ , CO ₂ , and H ₂ are used as the reaction gas, and the concentration of methane can be 5% or less.

Next, as shown in FIG. 2B, a recess 2 is formed in the diamond film 1 by laser. Recess 2
Are formed in a dot shape or a lattice shape as shown in FIGS. 3 and 4. A known method can be used for laser processing, but a YAG laser or an excimer laser is preferable. Y
Since heat is generated in the AG laser, it is necessary to allow a cooling time during processing so that the diamond is not overheated. The excimer laser is easy to perform fine processing and is preferably used, but it has a drawback that the device is expensive.

Then, as shown in FIG. 2C, a support film made of at least one of metal, plastic and lamix is formed on the diamond film having the recesses 2 formed therein. When forming this support film, metal is
It will be filled with plastic and ceramics.
The support film is formed by a known method. In the case of plating, the electroless plating method is preferably used because diamond has no conductivity.

After that, the substrate made of silicon or the like is mechanically peeled off. It may be removed by dissolution with an acid or the like. This allows
A diamond composite member as shown in FIG. 1 is obtained.
Next, this is cut into a predetermined shape with a laser or the like, and then, if necessary, the diamond composite member is fixed to a desired component by a method such as brazing. The substrate such as silicon may be removed after brazing the diamond composite member to the base material.

In order to confirm the effect of the present invention, the inventor
By changing the thickness of the diamond film, the width and depth of the recess, the occupancy of the recess, the method of processing the recess, the material of the support film (the same as the filling material for the recess) and the forming method thereof, Was tested for adhesion.

The occupancy rate of the concave portions was calculated by measuring the area ratio between the concave portions and the convex portions by an image analyzer.

Regarding the adhesion between the diamond film and the support film, as shown in FIG.
The jigs 11 were adhered to the support film 3 and the supporting film 3, respectively, and these jigs were pulled, and it was judged from the degree of peeling. That is, when peeling from the interface between the diamond film and the supporting film, there is no adhesion, and when peeling from a part of the interface, Δ,
When peeled off at a place other than the interface, it was marked with ◯. Table 1 shows the results.
Shown in

[0035]

[Table 1]

From Table 1, it is understood that the diamond composite member of the present invention has excellent adhesion between the diamond film and the support film.

Sample No. 8 has spot-shaped recesses with a diameter of 20 μm as shown in FIG.
3 formed dot-shaped recesses having a diameter of 100 μm as shown in FIG. Further, except for Nos. 8, 12, and 13, the lattice-shaped concave portions as shown in FIG. 4 were formed, and in the sample No. 21, the portions where the concave portions intersect each other have the same groove depth as the other portions. However, except for the sample No. 21, the concave portions were formed deeper (about twice the depth) at the portions where the concave portions intersect each other than the other portions.

In the present invention, a dense film made of at least one of diamond and diamond-like carbon may be formed on the surface of the diamond film on the side opposite to the support film to a thickness of 0.2 μm or more. In this case, wear resistance and heat conductivity can be improved. The thickness of the dense film is
The thickness is preferably 2 to 10 μm for improving wear resistance, and 10 to 100 μm for improving thermal conductivity.

[0039]

As described in detail above, in the diamond composite member of the present invention, for example, a recess is formed in the diamond film by laser, and a metal, plastic,
Along with filling at least one of the ceramics, since the support film was formed on the concave side surface of the diamond film, it is possible to firmly bond the diamond film and the support film, such a diamond composite member, Machine parts, cutting tools for metalworking, industrial tools such as drills, end mills, slitter knives, various sliding parts, abrasion resistant members such as yarn paths and guide bushes, and various measurements by brazing to the base material. Machine parts, precision cutting tools, medical instruments, etc. can be manufactured.

Further, since the formation of the concave portion is performed in a step different from the diamond film formation, for example, by a laser, a stable bonding force can be imparted regardless of the size and shape of the diamond crystal particles. The peeling of the quality film is less likely to occur, and the performance of various products can be stabilized.

Furthermore, since the diamond film and the metal are firmly adhered to each other, even when used in a heat sink for electronic parts,
There is little decrease in the thermal conductivity at the joint surface between the diamond and the heat sink material made of Cu or Al. Furthermore, since fine processing is possible, it is suitable for manufacturing various electronic devices.

[Brief description of drawings]

FIG. 1 is a vertical sectional view showing a diamond composite member of the present invention.

FIG. 2 is an explanatory view showing a method for manufacturing a diamond composite member of the present invention.

3A and 3B are diagrams showing a diamond film having recesses, in which FIG. 3A is a plan view and FIG. 3B is a longitudinal sectional view thereof.

4A and 4B show a diamond film in which a concave portion is formed, in which FIG. 4A is a plan view and FIG. 4B is a longitudinal sectional view thereof.

FIG. 5 is an explanatory diagram illustrating a test method of adhesion between a diamond film and a support film.

[Explanation of symbols]

 1 ... Diamond film 2 ... Recessed portion 3 ... Supporting film 8 ... Substrate

Claims (2)

[Claims] 1. A diamond film made of at least one of diamond and diamond-like carbon produced by a vapor phase synthesis method, and having a recess formed on the surface thereof, the surface of the diamond film facing the recess is made of metal, plastic or ceramics. A diamond composite member formed by forming a support film of at least one of them. 2. A diamond film made of at least one of diamond and diamond-like carbon is formed on the surface of a substrate by a vapor phase synthesis method, and a concave portion is formed in the diamond film, and the concave portion side of the diamond film is formed. A method for manufacturing a diamond composite member, comprising forming a support film made of at least one of metal, plastic, and ceramics on the surface and then removing the substrate.