WO1992014689A1

WO1992014689A1 - Diamond-clad hard material, throwaway tip, and method of making said material and tip

Info

Publication number: WO1992014689A1
Application number: PCT/JP1991/001542
Authority: WO
Inventors: Naoya Omori; Toshio Nomura
Original assignee: Sumitomo Electric Industries, Ltd.
Priority date: 1991-02-18
Filing date: 1991-11-11
Publication date: 1992-09-03
Also published as: CA2074482C; CA2074482A1

Abstract

A diamond-clad hard material having a high adhesion strength to the base material and a diamond-clad throwaway tip capable of cutting various kinds of light metals such as Al-Si alloy at high speed for a long period of time, wherein said diamond-clad hard material is composed of a material to be sintered which is constituted mainly of Si3N4, sintered at at least a part of the skin thereof, and clad with diamond on at least said sintered skin, and said throwaway tip composed of a base material constituted mainly of Si3N4 and clad with a layer in thickness of 0.1-200 νm of diamond or/and diamond-like carbon separated from vapor phase is characterized by being clad partly or entirely on the sintered skin of the surface of the base material with a layer of diamond or/and diamond-like carbon, thereby enabling the object to be effectively achieved.

Description

叨叨

Diamond hardened u-materials, slow way chips and methods of manufacturing

Technical field

The present invention provides a diamond coated hard material having high adhesion strength to a high base material and various light alloys such as A1-si alloy which can be cut at a high speed for a long time. It is intended to be applied to the throw-away tip.

Technology

Diamonds are extremely hard, chemically stable, and have many excellent properties, including high thermal conductivity and sonic velocity. The following materials are widely used in the Yang River, for example, as a hard U material that takes advantage of its characteristics, or as a diamond or a diamond-coated coal-coated S-hardened material. .

(1) Since it hardly reacts with A-Cu and the ultra-light gold ^ or the alloys supplied to the real river, these alloys are cut at a high speed and only very good. Finished diamond, sintered diamond or diamond-coated cutting tools, such as slow way chips, drills, etc. Cutting tools such as micro drills and end mills.

(2) Various damping tools, such as bonding tools, that have high dimensional accuracy due to their high resistance to chalk wear.

③ Various mechanical parts such as heat radiation ②. 各 Various diaphragms including speakers.

各種 Various electronic components.

Among the methods for producing artificial diamond, the methods for forming a diamond coating layer from the gas phase include wave plasma CVD, RF-plasma CVD, and EA. — CVD, induced magnetic field / z-wave plasma CVD, RF thermal plasma CVD, DC plasma CVD, DC plasma CVD, filament thermal CVD, combustion A number of methods are known, and are an effective method for producing diamond coated hard U materials. -As a surface coating tool, carbides, nitrides, carbonitrides and oxides of A1 oxides of Ti, I, Zr are formed on the surface of cemented carbide-based neo by PVD or CVD. A metabolic slope that forms a stratum or an exorcism is widely available to the public.

As mentioned earlier, diamond is extremely hard and chemically stable, so it hardly reacts with Al, Cu or practically used alloys of gold. . For this reason, when adapted to cutting tools, the diamond is used as a tool.) T1 or something like this: When cutting metal, or these alloys at high speed, Due to the extremely good finish of the work material, ill crystals, sintered diamond cutting tools or diamond coated cutting tools are widely used for actual ffl.

However, most of the diamond coated tools are steel and die. Since the adhesion strength of the diamond coating layer is insufficient, the service life is often extended due to the separation of the diamond-shaped IS. The reason for this is

1) Diamond is an extremely stable substance, does not form any substance and compound, and the diamond coating calendar and the base material are bonded by intermolecular attraction. Conceivable. The molecular IH1 attraction has a lower adhesion strength to the substrate than a coating layer that is bonded by forming a chemical compound. ,

2) The coefficient of thermal expansion between the diamond and the base material is significantly different, and residual stress is generated in the diamond coating layer. Therefore, adhesion strength is low.

There are two possibilities.

At the boundary between the base material and the diamond coating layer, the larger the contact capacity between the two, the stronger the molecular attraction, and the higher the adhesion strength of the diamond coating layer to the base material. It becomes bad. In addition, the higher the nucleation density of the diamond on the surface of the substrate, the greater the contact between the substrate and the diamond coating layer.

So, what is the diamond surface on the surface? A method of removing gold bending, which has an adverse effect on the formation of S-foot, by etching to increase the density of metanuclear nuclei (see Japanese Patent Application Laid-Open No. In addition, the surface of the cemented carbide is etched with an acid solution to remove the Co (gold) i component, thereby preventing the diamond nuclei from being graphitized.)閗 Showa 6 1 — 1 2 4 5 7 3 In the report, diamond abrasive grains or grinding stones are used to damage the surface of the base material to improve the nucleation density of diamond on the surface of the base material.) However, at present, its adhesion strength is insufficient.

In addition, as a base material having a thermal expansion coefficient almost the same as that of diamond, Japanese Patent Application Laid-Open No. 61-214943 discloses a sintered material containing Si ₃ N ₄ as a main component. It proposes a sintering bath consisting mainly of body and SiC. By using these, the separation phenomenon of the diamond coating layer due to thermal residual stress was not seen, but there was still PrH S of surface treatment, and At present, there is no diamond covering calendar with sufficient adhesion strength to the base metal.

Disclosure of the birthplace

Therefore, in researching and questioning diamond coating layers and substrates with excellent release resistance, the inventors of the present invention, based on the above-mentioned theory, found that the metabolism of the substrate As a result of repeated research focusing on the deformation, the base material was molded and sintered using a mixed powder containing Si ₃ N <as the main component. It was found that the film had a high adhesion strength when the yam coating layer was formed, and reached the present invention.

In addition, the present inventors conducted a heat treatment again on the base material once ground after sintering, so that the surface state became a sintered surface before grinding (hereinafter referred to as a heat-treated surface). Even when the diamond coating layer is formed, high adhesion strength is maintained as before. I saw the thing.

That is, the tree Hatsu叨is (1) S i, of Shoyuikyu mainly composed of N _4, least for the even 1- parts are tempered - and Yuihada, the portion of the該焼Yuihada also small instrument A diamond-coated hard material coated with a diamond and (2) a metamaterial of a slow-way base material mainly composed of Si ₃ N ₄ The diamond or the diamond-like carbon which has been exposed to the gas phase has a thickness of 0.1 to 200 // m. In the lower chip, the diamond is placed on the surface of a part of the base material, or the whole surface, of the lower surface base material whose surface is made of sintered surface. The present invention provides a diamond-coated slow-exposure characterized by having a coating layer of a diamond or diamond-like carbon.

Illustration of the metaphor

FIG. 1 is a conceptual diagram schematically showing the state of the covering layer of the wood invention and the substrate.

FIG. 2 is a conceptual diagram schematically showing the state of the coating layer-substrate interface of the present invention.

FIG. 3 is an explanatory diagram nj] in which the state shown in FIG. 2 is simulated as a straight line.

Figures 4 and 4 are conceptual diagrams showing an example of the cutting edge processing performed in the embodiment.

BEST MODE FOR CARRYING OUT THE INVENTION

The present inventor further proposes that a mechanical or chemical The base material is formed on the surface of the substrate, and a diamond coating layer is formed on the surface of the base material. It has been discovered that the adhesion strength between the diamond coating layer and the base material is very high when the state penetrates the diamond coating layer. This is due to the fact that the contact area between the diamond coating layer and the base material has been increased, the projections have an effect of anchoring the diamond coating layer, and the diamond coating layer has a negative effect. It is thought that it became difficult to be.

The irregularities described here are not microscopic irregularities formed by (I) a diamond grinding wheel, (2) a scratching process using diamond abrasive grains, or the like, but rather microscopic irregularities. R5I is a concave-convex shape.In the diamond coating layer, the base length is a minute section, such as 10 μm, in the base material. It is. The present inventors have found that a beam having various concave and convex states has at least one or more convex portions within a reference length of 10 m and at least one convex portion within a standard length of 10 m. In this case, the ratio of the total length B of the convex portions to the total length A of the concave portions is 0.05 ≤ AZB20, and the convex portions correspond to the width of the diamond coating layer. It was discovered that the state of penetration of 0.2 mm or more increased the adhesion strength. This was calculated by wrapping the cross section of the base after diamond coating, observing and photographing, and modeling the state of the diamond coating layer and substrate.

Diamond and Z or Diamond Fig. 1 schematically shows the state of a single carbon substrate layer. In this case, the sum A of the lengths of the protrusions, that is, the sum B of the lengths of the recesses and the sum B of the lengths of the recesses, that is, the ratio of ら B must be 0.05 ∑ A / B ≤ 20. It is preferable that the intrusion length of the projection is 0.2 μm or more. For example, 1 AZ ∑ B = 19 when there is one in a 0.5 m convex force of 10 m.

In any case, the projections formed in this way have a reference length at the interface between the diamond and / or the diamond-like carbon coating. Is set to 10 m, there are at least one or more locations within this reference length, and the ratio of the total length B of the convex portions to the total length A of the concave portions is 0.05. In this case, if it is necessary to be in the range BH of 20 or less, and the convex must penetrate into the diamond coating layer, the penetration length is 0.2. It is preferably at least u.m. If the ratio of the total length B of the convex portions to the total length A of the concave portions deviates from the range of 0.05 ≤ A / B ≤ 20, no improvement in adhesion strength is observed.

In addition, as a result of the creation of various irregularities, the authors found that within a reference length of 50 / m, the meta-roughness at the boundary was 1 at R max. It was discovered that the contact strength was higher in the state between 5 and 30 µm. This metaphysical value can be determined by observing the cross section of the substrate after the diamond coating after rubbing, photographing, and taking an image of the interface between the diamond coating layer and the substrate. of The boundary is defined as the metaphysical value (R max) of the coated substrate.

FIG. 2 schematically shows the state of the diamond and / or diamond-like carbon coating layer-substrate interface according to the present invention. That is, although macroscopic undulation is recognized in the field, Rmax is calculated by regarding this as a pseudo straight line as shown in FIG.

In any case, the convex portion formed in the earthenware pots good This is die algicidal down de and _/ / or die algicidal down de, in Fushimi carbon coating曆one substrate boundaries Thus, the reference length a When 50 u rn is used, it is necessary that within this reference length, the degree of filtration at the interface of the base material is 1.0 to 30 zm at R max. It is preferable that the protrusion penetrates into the diamond coating layer with a penetration length of 0.2〃rn or more. When the roughness at the substrate interface was less than 1.0 in R max, no improvement in adhesion strength was observed, and when it exceeded 30 m, a decrease in adhesion strength was observed. As a specific method of making unevenness in the material,

① Method of extruding columnar crystals and Z or needles on the substrate surface

(2) How to remove binders that are likely to be etched by etching

(3) Base 1 = A method of applying a mask to a young person, etching, and then removing the mask.

方法 Method by physical processing with laser etc. Select an appropriate method according to the key.

In method (1), the base material is subjected to some kind of heat treatment, and columnar or acicular crystals are freely grown on the surface, depending on the base material components, and / or secondary crystals. The method (2) is effective for the material that is formed by the addition of corrosive hard fouling to acids and alkalis and the ffl, and the method (3) is effective. This is a method in which a mask is provided on an arbitrary pattern using a photomask, and then the mask is removed by etching.

Here, the reason why the hard material whose main component is Si ₃ N <was selected as the base material is as follows: (1) The thermal expansion coefficient of Si ₃ N ₄ is close to that of a diamond. (2) Furthermore, it is produced by molding and sintering a mixed powder mainly composed of Si ₃ N <. Since the columnar crystal structure of Si ₃ N <grows on the surface of the base material, coarse columnar crystals are present, and the state where the base surface is uneven by the method (1) described above. Because it can be easily made. The following two effects can be considered as the effects of the presence of the self-grown columnar structure.1) Coarse columnar structure due to the free growth of the metamorphic Si ₃ N 4 columnar crystal structure It becomes a crystal. For this reason, the surface has irregularities as compared to the ground surface, and the contact between the base material and the diamond coating phase increases.

2) The tying of the knots is a singular point, and the nucleation of diamonds is likely to occur.

In the ground surface, the columnar structure of freely grown Si ₃ N ₄ The presence of sapphire is not seen at all, the surface of the sintered body is not uneven, and the grain boundaries of the crystal grains are not clear.

Here, in the early stage of the coating, a general diamond diamond grinding process is used to promote the generation of diamond nuclei during the entire chip display. Is desirable. At this time, in the method of physically pressing and scratching the abrasive grains, there is a possibility that the formed protrusions may be broken or broken, so the base material and the diamond abrasive grains may be washed with water. It is desirable that the solution is injected into a solvent such as ethyl alcohol or acetone and the solution is subjected to ultrasonic vibration to perform a damaging treatment. — As a result of this scratching treatment, diamond nuclei are evenly generated on the convex and non-convex portions of the substrate surface. As a result, it was possible to create a state in which the protrusions penetrated the diamond coating layer.

Also, as the specific composition of the substrate, α - Si ₃ N ₄ was used as a main component Si ₃ N ₄ powder containing 50% or _{_{more, A 1 2 0 3, Y}} 2 0 3, MgO A1N, Si0 ₂ or we selected one or more even and rather low sintering aid剂. meter 1 ~ 5 0 t¾ also of the desired by sintering mixed powder containing arbitrariness. First, if more than 50% of one Sis is sintered under any conditions, the cast crystal structure of Si ₃ N ₄ will be insufficient, and the base material itself This is because both the strength and the paddy properties decrease. Also, Si ₃ N ₄ is a covalently bonded substance and is known to have poor sinterability. However, as a sintering aid

_{_{_{Al 2 0 3, Y 2 0}}} 3, one MgO, AIN, Si0 ₂ Urn Chi least for the even From the above, it was found that when a total of 1 to 50 was mixed, good sinterability was exhibited, and that the formation of 5-Si ₃ N in the form of a filament was promoted.

If the total amount of addition is 50 wt% or more, the strength of the sintering itself will be reduced, so that 50 wt% or less is desirable. In addition, as other components other than the sintering aid, a hardened material such as Ti carbides, nitrides, various compounds such as nitrides, borohydrides, and the like, or It goes without saying that additives that improve high-temperature properties such as ZrO ₂ and HfO ₂ can be added. In 1 6 0 0 Hand below for the sintering temperature, grain Ri growth inadequate, and the strength is low down rather then remarkable in Shoyuikyu, at or 2 0 0 0 Hand above, S i ₃ N ₄ Since the decomposition of this starts, the value is set to 160 to 200. Atmosphere (For gaseous gas, for gaseous gases, Si decomposes except for N ₂ gas. At 1 atm or less, Si ₃ N ₄ decomposes and 3000 atm Since it is difficult to commercialize the above, it is desirable to use a N ₂ gas atmosphere of 300 atm.

Also, regarding the firing time, if the time is less than 30 minutes, the densification of the crystal grains is insufficient, and if the time is more than 5 hours, the crystal grains become coarse and the strength is reduced. Min ~ 5 o'clock GH of R51 is good.

When this base material was sintered under the above sintering conditions, the existence of columnar crystals of Si ₃ N ₄ was recognized in the base material.

Coating on the sintered surface is, from an economic point of view, a grinding process. In addition, there is also an advantage that the manufacturing cost / 11 can be reduced by the amount of processing cost. The diamond-coated hard material obtained in this way can be used as a slow-through, micro-drill, micro-drill, end-roll, end-roll, or It can cover a wide range of mechanical parts such as reamers, shochu tools, bonding tools, whetstones, dressers and printer heads. .

For chips with complicated shapes, such as chips, or chips that require high dimensional accuracy, some or all of the chips that have been sintered once the grinding, if necessary were New ₂ gas or in the temperature range of the scan b over a c d b Chi Tsu Bed that facilities the edge preparation in 1 3 0 0-2 0 0 0 Ζ and Heat treatment was performed in an inert gas atmosphere. The gas pressure range was 1 to 300 atm. As a result, the entire surface of the chip was heat treated. As the conditions of the heat treatment, when the temperature is below 1300'C, changes in tissue Ken βΐί skin was not observed, or, exceeds in _{2 0 0 0, Si 3 Ν} 4 of decomposition reaction Ji live Therefore, the temperature range was limited to 130 to 2000. Kiri ΒΗ outs Si ₃ N <of the decomposition reaction is to Seki was Ν ₂ gas or to the scan species other than your good beauty inert gas Ζ raw Jill.

On the ground surface of the base material, the presence of a Si ₃ N ₄ puffed product was not recognized, but the heat treatment of the throw-away chip under the above heat treatment conditions The presence of columnar crystals of Si ₃ N ₄ was observed on the heat-treated skin of the substrate surface, similar to the sintered skin. Was.

In addition, if necessary for dimensional accuracy, a part of the throw-away chip, which had been entirely heat treated, was ground.

Even if IMI is applied to the heat-treated skin, when the diamond coating is formed, the strength is much higher than that of the ground skin, and the adhesion strength is equivalent to that of the sintered skin. showed that. This is because the same columnar crystal structure as that of the sintered skin exists in the heat-treated skin.

In addition, if the average major axis of the columnar crystals is 1.5 or less, and if there is no casting with a major axis of more than 2 inches, the improvement of the diamond membrane adhesion is not improved. I can't stop it.

In the present invention, it was possible to form a diamond coating calendar with high adhesion strength and no thermal residual stress, so that it exceeded the thickness of the commonly used hard coating layer. It is now possible to set a calendar thickness of m or more.

Regarding the layer thickness, when the thickness is 0.1 μm or less, no improvement in the abrasion resistance due to the coating layer is observed, and when the coating layer has a thickness of 200 fm or more. No significant improvement in abrasion is observed anymore, so it is not suitable for hard material or as a slender tip. M of 0 um is good.

Up to this point, the discussion has focused on the case where the coating layer is a diamond, but the diamond coating is not included in the diamond coating layer. Including diamonds with carbon-like carbon and other crystalline structures, and those composed of more than one of these calendars or multilayers The same effect can be obtained when the effect is recognized and the diamond coating or the diamond-like carbon coating layer contains different kinds of atoms such as boron and nitrogen.

In the present application, the upper surface of the slider is a rake surface, and the lower surface is a surface facing the upper surface.

Hereinafter, the embodiment will be described in detail.

[Example 1] ''

Next, the hard surface member of the present invention will be specifically described with reference to examples.

As a base material, composition Si _₃ N <S i ₃ in Serra Mi click (specifically the base N * - 4 wt% A 1 2 03 - 4 wt% Z r 0 2 - 3 wt% Y 2 0 ₃ ) Sinter the mixed powder for 1 lir in an atmosphere of N 2 gas at 1800 T; at 5 atm to form a SPG422 shaped lower way chip on the material surface. A columnar crystal structure of Si ₃ N _{4 having} an average minor axis of 2 / m and an average major axis of 4 nm was observed.

First, the following base metal chips were prepared in order to compare the sintered surface with the ground surface. Fig. 4 shows a schematic diagram of the tip processing of the chip. Here, a is the negative land, 3 is the escape, ¾ is the negative land width, and cr is 25 °, respectively; 3 is 11 ° and 0.05 mm. I. 2.

3. As an edge treatment, NL processing of 0.05 x 25 ° is applied, and the other parts are chips with the same sintered surface.

4. A chip that has been subjected to upper and lower surface grinding and the above-mentioned edge treatment, and has a sintered surface

5. Chips with flank grinding and the above-mentioned edge treatment, with upper and lower surfaces with sintered surfaces

Furthermore, in order to confirm the effectiveness of the heat-treated skin, the above-mentioned chip was subjected to up-and-down movement and escape, and the above-mentioned 0.05 x 25 was used. A chip was prepared with the NL cutting edge treatment. At this time, it was confirmed that no columnar crystal structure was present on the surface of the ground surface of the throw-away chip. This switch-up the 1700 'C ;, 5 atm N ₂ gas Kiri 1 in four gas-hr, was One row of the heat treatment,

6. 7.Tip with heat treated skin

8. A chip with only the edge treatment (hereinafter referred to as NL surface) ground and heat treated skin for both the escape and rake surfaces

9. Chips with upper and lower surfaces and NL surface ground and only flank surface treated with heat treatment

10. A chip with the escaped surface and the NL surface ground, and only the upper and lower surfaces heat treated.

II. A chip in which the escape and upper and lower surfaces are ground and only N L is heat treated.

12. Grind the escapement and heat treat only the upper and lower surfaces, NL fl / L chips

1 3. Chip with upper and lower surfaces ground and heat-treated skin on flank and NL only

In this ripening treatment, the ground surface of the throw-away chip, in which no columnar grain structure was observed before heat treatment, showed a Si with an average minor axis of 1.5 nm and an average major axis of 3 fim. ₃ pillars Fushimi crystal structure of N ₄ was observed.

These cutting chips were heated to 100 ° C using a 2.45 GHz microwave plasma CVD apparatus, and hydrogen-metal 2 was heated to a total pressure of 80 Torr. % For 4 to 100 hours, forming a diamond coating layer on the entire upper surface of the chip, near the flank cutting edge, and on the NL. As a result, the diamond-coated slow-way tips 1 to 13 shown in Table 1 were produced.

In addition, for comparison, a comparative chip 1 having the same shape and the same composition, ground on the upper and lower surfaces and the relief, and having been subjected to the above-mentioned edge treatment, and a diamond coating layer were applied thereto. The prepared comparison chip 2 was prepared.

In this test, the coating calendar deposited on the surface of the substrate was analyzed by Raman spectroscopy to determine the characteristics of the diamond and / or diamond-1 carbon coating layer. It was confirmed that a peak was observed at 133 3 cnr '. 1

Stream these cutting tips

Machining U A 1 — 24 wt% Si alloy Cutting speed 300 m / min.

0.1 mm / re \ ^r . Cutting: 0.2 mm

Intermittent cutting was performed under the following conditions, and the amount of relief, wear of the cutting edge, and welded state of the work material were observed after 2 minutes and 10 minutes. Table 2 shows the results of these tests.

From the results shown in Table 2, it can be seen that all of the diamond-attached slotted blades 1 to 11 of the present invention have a good separation from the conventional cutting tips 1 to 2. It is understood that it has abrasion property and shochu abrasion property.

According to the results, when the NL surface and / or the escape surface was used as the grinding surface, minute separation was recognized. From this, it can be seen that the adhesion strength of the diamond coating layer to the base material is considerably high when the escape surface and the N1 surface are sintered surfaces.

Also, when comparing the diamond-coated α-away tips 1 to 5 and 6 to 10 of the present invention, it was found that there was no difference between the HO of the sintered skin and the HO of the heat treatment. That is.

Table 2

2 minutes later 10 minutes later Escape TS Kirimm mm Wear condition mm m

Welding of the participant:!

(删)

1 0.07 Normal Separation, no welding

2 0.05 Normal wear, separation, no welding Wood 3 0.10 Slightly 11 on NL surface

4 0.12 Minute separation on NL surface

5 0.21 Escape 1S, slight separation in NL® Light 6 Total friction 4 《0.08 Normal friction because not seen ½ No separation. No welding

7 Measurement ¾τ, ability 0.05 Normal wear.

8 0.11 Slight separation on NL surface

'SO 9 0.12 Slight peeling on NL surface

10 0.20 Slight clearance on flank and NL

11 0.18 Escape t ® has slight peeling

12 0.16 Escape There is a small moment in IB

13 0.09 Normal friction ½ '剝 separation No welding Specific flux 1 0.45 Normal separation, large welding

寿命 2 min. (Example 2)

As a base material, silicon nitride group: a cell La Mi click (rest thereof include A composition: S i ₃ N 4 one _{4 wt% A 1 2 03 -} 4 wt% Z r 02 - 3 t% Y 2 03 B composition: S i ₃ N 4 - was prepared 5 wt% Y ₂ 0 ₃₎ in the form of SPG 422 scan B over-away Chi Tsu Bed _{_{- 2 t% AI 2 0 3}} . This chip was heat-treated under the conditions shown in Table 3. Table 3 also shows the state of the columnar crystals generated at that time. Here, chips 9 and 10 of the present invention are out of the range CH of the present invention. These chips were put into ethyl alcohol together with 2 g of diamond abrasive grains having a diameter of 8 to 16 m, and were subjected to ultrasonic vibration for 15 minutes. The thus-prepared chip base material was heated to 100 0 using a 2.45 GHz microwave plasma CVD device, and hydrogen was heated to a total pressure of 80 Torr. — Hold in a 2% methane mixed plasma for 4 to 20 hours.] As shown in Table 3, the diamond coated cutting tool of the present invention having a layer thickness of 4 to 20 m was used. Tips 14 to 23 were prepared. In addition, for comparison, a heat treatment was not performed with the same shape and the same composition, so that a chip having no diamond nitride cast crystal on its surface was provided with a diamond coating layer. 3 was prepared. These are also shown in Table 3. (No ultrasonic treatment was applied to the comparison chip) Table 3

(Note) * is data after 30 minutes, il! I is data after 10 minutes In this test, the coating layer deposited on the surface of the base material showed a peak at 133,3 cm- ', which is a characteristic of diamond, by Raman spectroscopy. -Confirmed to be present.

These cutting fiij tips;

Work material: A1-2-4 wt% Si alloy (block material)

Cutting speed: 400 m Z min

Sent: O. lmmmrev.

Depth of cut: 0.5 mm

Table 3 shows the results of observations of the amount of escape wear, the wear of the cutting edge, and the welded state of the work material after 3 and 10 minutes. It was shown to.

After cutting and wrapping the chip after the cutting test, the interface between the base material and the diamond coating was observed with an optical microscope and a laser microscope. In tips 14 to 21, columnar crystals of silicon nitride penetrate the diamond coating layer at a maximum depth of 1 to 5 m, and within a reference length of 1 m, 3 to Five convex parts are present, AB is in the range of 0.1 to 10 or the reference length is 50 «m at the interface between the diamond coating layer and the base. Then, it was confirmed that R max was 1 to 8 / m. In addition, it was confirmed that both of the present invention chips 22 and 23 were out of the scope of the present invention. In the comparative chip, the base material-diamond coating layer No columnar crystals were present, and no penetration of the substrate into the diamond coating calendar was observed.

Industrial applicability

The present invention can be applied not only to the throw-away tool but also to various cutting tools and TAB tools such as drill drills, micro-driners, end-minoles, rimmers, and knives. It can be applied to wear-resistant tools such as casters, cabriolets, various grinding wheels, and mechanical parts.

Claims

The scope of the claims

. Si ₃ sintered body New ₄ as main components, 1 part also least for A and Shoyuihada, ing to cover the die algicidal down de the least for the portion of the well該焼Yuihada die A hard material coated with yam.

In the case of a coated hard material in which a diamond coating layer is formed on the surface of a hard material mainly composed of Si ₃ N ₄ ,

(1) There are microscopic irregularities on the substrate surface,

(2) When the reference length is set at 10 m at the diamond coating layer-base boundary, at least one or more protrusions exist within the reference length. ,-

(3) Within the reference length at the interface, the ratio of the saturation B of the length of the convex portion to the sum A of the length of the concave portion is 0.055 ≤ A / B ≤ 20.

(4) And the convex part has penetrated into the diamond coating layer,

A diamond-coated hard material characterized by this.

In the case of a coated hard material in which a diamond and / or a diamond-like carbon coating layer is formed on the surface of a hard material mainly containing Si and N ₄ ,

(1) There are microscopic irregularities on the surface of the base material,

(2) When the reference length is 50 μm at the interface between the diamond coating layer and the base material, the surface roughness within the reference length is 1.0 at R max. ~ 30 m

Diamond or diamond shape characterized by this Carbon coated hard material.

Diamond cover © iG face 2-3, characterized in that at least 0.2 μm of protrusion is invaded in the width of the diamond Diamond-shaped carbon-coated hard material.

The die according to any one of claims 4 to 4, wherein the protrusion is a silicon nitride crystal and / or a crystal containing silicon nitride or a sialo. Hard material coated with yam. ,

Diamond or diamond and diamond deposited from the vapor phase on the surface of a silicon substrate whose main component is Si ₃ N ₄ . Slow wire with surface texture of sintered skin in a throw-away type with a cover carbon thickness of 0.1 to 200 / m It is characterized in that it has a coating layer of diamond or diamond and carbon on part or all of the surface of the chip base material. Diamond coated slider ゥヱ chip.

Grind only the upper and lower surfaces of the sintered lower way chip base material, or the rake face, and leave the flank face with the sintered surface at least. Coating layer of diamond or Z and diamond-like carbon on part or all of the rake face, flank face of the chip Claim 6 characterized by having a diamond Insulated through-way tips.

. Sintered die-cut base material is treated with a cutting edge, and only the upper and lower surfaces or the rake face are ground. Diamond or Z and diamond on a part or all of the surface of the chip 7. The diamond coated throw-away chip according to claim 6, wherein a coating layer of a diamond-like carbon is formed. ,

Sintered Slope Die tip base material is subjected to edge milling, and only upper and lower surfaces or rake face are ground, and flank is the surface of sintered skin The diamond or Z and die surfaces are partially or entirely formed on the rake face of the chip, the treated face of the tip, and the relief face, respectively. 7. The diamond-coated throw-away chip according to claim 6, wherein a coating layer of a diamond-like carbon is formed.

. Slow-through tips with some or all surfaces of the sintered through-chip base material ground and, if necessary, treated with cutting edges The base metal is heat-treated, and the entire surface of the chip is heat-treated, and the rake face of the chip, and a part of each of the edge-treated surface and the flank surface, or Claims characterized in that a coating layer of diamond or Z and a diamond-like carbon is formed on the entire surface. 黻 6 4 記黻黻 6 被覆被覆 — — — — — — — 4

11. Grind a part or all of the surface of the sintered slender chip base metal or the whole surface, apply cutting edge treatment if necessary, and re-use After heat-treating the base material of the chip and making the entire surface a heat-treated skin, grinding some or all of the chip surface and then cutting the chip A diamond or Z and diamond-like carbon coating layer is formed on a part or all of the surface, the edge-treated surface, and the relief surface. The scope of the claim, characterized by the following: 6. A diamond-coated, throw-away chip from Shun.

12. Die algicidal down Dochi-up on the base metal surface of freely grown Si ₃ range 1 to claims columnar crystal structure of N ₄ is characterized that you present 1 1, wherein the die algicidal emissions de-coated hard Material or diamond coating sigma-a-way chip.

13. Si, Ν ₄ columnar crystals are average major axis average minor ί St ratio 1. was or die algicidal down de coated hard materials according to the range 1 2 according to have a 5 die algicidal down de coated scan B -A way chip.

14. The diamond-coated hard material or diamond according to claim 12, wherein at least a part of the columnar crystal of Si 34 has a major axis of 2 μm or more. End coated slow way tip.

15. Si ₃ N ₄ powder containing 50% or more of Si ₃ N ₄ as base material The mainly _{_{_{Naru夯, A1 2 0 3, Y 2}}} 0 3, MgO, A IN, Si0 2 or al least the sintering剂selected rather with one or more than a total of 1 ~ 5 0 wt% content the mixed powder, 1 in 6 0 0-2 0 0 0 'temperature range of C, 1 to ~ 3 0 0 0 atm hands 3 0 minutes to 5 hours sintering N ₂ gas atmosphere, rather small The flank is a sintered surface or a heat-treated surface, and at least the flank is coated with a diamond. The method of manufacturing the chip.

16. After heat-treated surface is ground after silicon nitride sintering

行う δ ΠΗ Ι5, characterized in that it is carried out in an atmosphere of l to 3 OOO atm 0 N ₂ gas or Z and an inert gas at a temperature range of 4 000 ^e C Manufacturing method of diamond-coated coated lower way chip.