JP4275896B2 - Polycrystalline diamond and method for producing the same - Google Patents

Polycrystalline diamond and method for producing the same Download PDF

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JP4275896B2
JP4275896B2 JP2002098180A JP2002098180A JP4275896B2 JP 4275896 B2 JP4275896 B2 JP 4275896B2 JP 2002098180 A JP2002098180 A JP 2002098180A JP 2002098180 A JP2002098180 A JP 2002098180A JP 4275896 B2 JP4275896 B2 JP 4275896B2
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diamond
polycrystal
pressure
heating
graphite
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JP2003292397A (en
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徹男 入舩
均 角谷
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住友電気工業株式会社
株式会社テクノネットワーク四国
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[0001]
BACKGROUND OF THE INVENTION
The present invention relates to diamond and a method for producing the same, and more particularly to a high-purity diamond polycrystal having high strength and excellent thermal characteristics used for a cutting tool, a drill bit, and the like, and a method for producing the same.
[0002]
[Prior art]
Diamond polycrystals used for conventional cutting tools and drill bits use iron group metals such as Co, Ni and Fe, and ceramics such as SiC as sintering aids or binders. In addition, those using carbonate as a sintering aid are known (Japanese Patent Laid-Open Nos. 4-74766 and 4-114966). These can be obtained by sintering diamond powder together with a sintering aid and a binder under high pressure and high temperature conditions (usually pressure 5-8 GPa, temperature 1300-2200 ° C.) under which the diamond is thermodynamically stable. On the other hand, naturally-occurring diamond polycrystals (carbonados and ballasts) are also known, and some of them are used as drilling bits. However, they are widely used industrially due to large variations in material and low output. Not.
[0003]
[Problems to be solved by the invention]
The polycrystalline diamond using an iron-based metal such as Co as a sintering aid contains an iron-based metal such as Co, which acts as a catalyst for promoting the graphitization of diamond, and therefore has poor heat resistance. That is, diamond is graphitized at about 700 degrees even in an inert gas atmosphere. Further, due to the difference in thermal expansion between the catalytic metal and diamond, fine cracks are likely to occur in the polycrystalline body. Further, since a metal such as Co exists as a continuous layer between the diamond particles, the mechanical properties such as hardness and strength of the polycrystalline body are lowered. It is also known that the metal at the grain boundary is removed in order to increase the heat resistance. This improves the heat resistance temperature to about 1200 ° C, but the polycrystalline body becomes porous, so the strength is further greatly reduced. To do. A diamond sintered body using SiC as a bonded body is excellent in heat resistance, but the diamond grains are not bonded to each other, so that the strength is low. In addition, a diamond sintered body using carbonate as a sintering aid is superior in heat resistance compared to a sintered body using a Co binder, but has sufficient mechanical properties due to the presence of a carbonate substance at the grain boundary. That's not true.
[0004]
On the other hand, as a diamond manufacturing method, non-diamond carbon such as graphite, glassy carbon, and amorphous carbon can be directly converted to diamond without a catalyst or a solvent under an ultra-high pressure and high temperature. A single-phase polycrystalline diamond can be obtained by direct conversion from non-diamond phase to diamond phase and sintering. For example, J.Chem.Phys., 38 (1963) 631-643 [FPBundy], Japan.J.Appl.Phys., 11 (1972) 578-590 [M.Wakatsuki, K.Ichinose, T.Aoki], In Nature 259 (1976) 38 [S. Naka, K. Horii, Y. Takeda, T. Hanawa], a polycrystalline diamond is obtained by direct conversion at 14-18 GPa or more under high pressure and high temperature of 3000-18 K or more using graphite as a starting material. Is disclosed. However, since all are based on the direct current heating method in which a current is directly applied to conductive non-diamond carbon such as graphite, unconverted graphite remains, the diamond particle size is uneven, or partially Sintering is insufficient. For this reason, mechanical properties such as hardness and strength are insufficient, and only a piece-like polycrystal is obtained. Therefore, it cannot be applied to cutting tools and bits, and has not been put into practical use. For example, JP 2002-66302 A discloses a method of synthesizing fine diamond by heating a carbon nanotube to 10 GPa or more and 1600 ° C. or more. However, the raw material carbon nanotubes are extremely expensive, and there is a big problem in manufacturing cost. Moreover, since the disclosed method pressurizes carbon nanotubes with a diamond anvil and condenses and heats them with a carbon dioxide laser, it is impossible to produce a homogeneous diamond polycrystal having a size applicable to a cutting tool.
[0005]
The present invention has been made in order to solve the above-mentioned problems of the prior art, and is a dense and homogeneous diamond single-phase polycrystal having sufficient strength, hardness and heat resistance as a cutting tool or a drill bit. The purpose is to provide.
[0006]
[Means for Solving the Problems]
In order to solve the above-mentioned problems, the present inventors, when heating non-diamond carbon under ultra-high pressure and directly converting it to diamond, do not directly heat non-diamond carbon, but indirectly heat stably. As a result of developing and carrying out a method that can be used, it has been found that a fine and tough polycrystalline body made of diamond of 99% or more can be obtained from a carbon material having a normal graphite layer structure. The obtained polycrystalline diamond has a dense structure composed of fine diamond particles having an average particle diameter of 100 nm or less, and often 20 nm or less, hardly contains inclusions, and has a hardness of 70 GPa or more, which is equivalent to that of a single crystal. It has been found that it has an unprecedented characteristic that it exhibits hardness and does not deteriorate to 1600 ° C. in an inert gas. Further, since it was conventionally produced with a belt-type or girdle-type uniaxial compressible ultra-high pressure apparatus, the polycrystalline diamond has anisotropy, and in particular, has a strong tendency to be (111) -oriented in the compression direction, resulting in layered cleavage Although there was a tendency for cracking to occur, the present invention adopts a highly isostatically compressible pressure chamber called a multi-anvil and isotropic because it has a highly isostatic pressure. It was found that this polycrystal has high strength against compression and pulling from any direction.
[0007]
That is, the feature of the present invention is that a non-diamond carbon material is placed in a pressure cell equipped with a means for indirectly heating, and heating and pressurizing are performed, so that diamond can be directly converted without adding a sintering aid or a catalyst. It is to produce a polycrystal. As the heating means, it is advantageous for stable and effective indirect heating that a current is passed through a heater made of a refractory metal to generate heat. An insulator layer may be provided between the non-diamond carbon material and the means for indirectly heating, and an alkali halide material may be provided on at least a part of the insulator layer. It is desirable to use graphite having a purity of 99% or more as the non-diamond carbon material. As conditions for the heating temperature T and the pressure P to be applied, heating at 1800 ° C. or higher and pressurization at 20 GPa or higher, or heating at 2300 ° C. or higher and pressurization at 12 GPa or higher is preferable. More generally, a high-quality diamond polycrystal can be obtained by satisfying the relationship of the following formula.
T> 5P 2 -241P + 4909
Where T: temperature (° C.), P: pressure (GPa)
[0008]
Further, the polycrystalline diamond according to the present invention is not limited to a novel manufacturing method, and the polycrystalline diamond itself is novel and has the following characteristics. That is, it is a polycrystalline body made of diamond obtained by converting and sintering a carbon material having a graphite-type layered structure under an ultra-high pressure and high temperature without adding a sintering aid or a catalyst, and the average particle diameter of diamond is 100 nm or less, purity Is a polycrystalline diamond having 99% or more. In many cases, the average particle diameter is 20 nm or less, the hardness is 70 GPa or more, and the (111) diffraction intensity of the (220) diffraction intensity (I (220) ) of X-ray diffraction in any direction of the polycrystalline body. (I (111)) ratio I (220) / I (111 ) is 0.1 or more.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
An embodiment of a method for producing a polycrystalline body according to the present invention will be described with reference to an example shown in FIG. FIG. 1 shows a cross section of a high-temperature high-pressure cell used in the method for producing a polycrystalline body according to the present invention. The outside is a container made of lanthanum chromite (LaCrO 3 ), and the sample 1 is stored inside. In this example, two samples can be set in the high temperature and high pressure cell. This sample 1 is obtained by forming non-diamond carbon as a raw material of diamond, such as graphite, into a predetermined shape. The shape of the sample 1 is almost the same as that of the synthesized polycrystalline body. Here, graphite is formed in a cylindrical shape, and FIG. 1 shows a cross section cut in half along the axis of the cylinder. Around the sample 1, a powder 2 of sodium chloride, which is an alkali halide substance, is disposed, and the periphery is wrapped with magnesium oxide 3 (MgO). Further, a heater 4 made of rhenium (Re) is provided outside the layer of magnesium oxide 3, and a heat insulating material 5 made of zirconia (ZrO 2 ) is provided outside the heater 4. By causing a current to flow through a heater made of a refractory metal such as rhenium to generate heat, the sample 1 is effectively and stably heated while being indirectly heated. Further, between the sample 1 and the heater 4, the sodium chloride powder 2, which is an alkali halide material that is stable even at high temperatures, is disposed, so that the sample 1 or the produced polycrystalline diamond is insulated from the heater 4. At the same time, the surface is protected even during pressurization. There are electrodes 6 made of molybdenum (Mo) above and below the high-temperature high-pressure cell, and power for heating the heater is supplied from the outside. A pressure medium 7 of magnesium oxide or cobalt oxide is provided around the heat insulating material 5, and a pressure medium 8 of lanthanum chromite (LaCrO 3 ) is provided above and below the electrode 6, respectively. A tungsten-rhenium thermocouple for measuring the temperature of the sample is provided almost at the center of the high-temperature and high-pressure cell.
[0010]
When a sample and various pressure media are loaded as shown in FIG. 1, the high-temperature and high-pressure cell is put into a multi-anvil pressurizing device and pressurized. The load from the pressurizing device is applied to the sample as almost hydrostatic pressure through the pressure medium of the high-temperature and high-pressure cell. At the same time, power is supplied to the heater 4 through the electrode 6 to heat the sample 1. The pressure applied to the sample can be obtained from the load of the pressurizer output from the load cell or the like and the angle / area of the pressurization surface, and the temperature of the sample 1 can be grasped by the thermocouple 9 provided nearby. Sample 1 is synthesized into a polycrystal by holding at a predetermined temperature and pressure for a certain period of time. For example, if the pressure is reduced after synthesis, for example, at about 600 ° C., it is particularly effective to obtain a high-quality sintered body.
[0011]
【Example】
Next, an example in which the present invention is applied to the synthesis of a polycrystalline diamond will be described. In this example, graphite having a purity of 99.9995% was used as the sample 1 in the high-temperature and high-pressure cell shown in FIG. The shape of the sample 1 is a cylinder having a diameter of 1.5 mm and a height of 1 mm. Heat and pressurize to a predetermined temperature and pressure, hold that state for about 10 minutes, then rapidly cool and reduce the pressure to atmospheric pressure over several hours. The test was repeated with varying temperature and pressure. As a result, it was found that when the pressure was 12 GPa (about 120,000 atm), a transparent cubic diamond polycrystal was obtained at a temperature of 2300 ° C. or higher. It was also found that when the pressure was 20 GPa, the same diamond polycrystal was obtained at a temperature of 1800 ° C. or higher. Further, the graph shown in FIG. 2 shows the results of tests conducted by changing the temperature and pressure. The vertical axis represents temperature and the horizontal axis represents pressure, and the points shown in the figure indicate test data performed. Among these test data, a transparent cubic diamond polycrystal was obtained at the points indicated by circles. Next, in terms of the squares, a white turbid cubic polycrystalline diamond was obtained. Moreover, the hexagonal diamond was mixed in the point represented by the triangle. From these results, the temperature and pressure are expressed by the following formula T> 5P 2 -241P + 4909.
Where T: temperature (° C.), P: pressure (GPa)
It has been found that a transparent cubic polycrystalline diamond can be obtained when The temperature is preferably 3000 ° C. or lower in order not to dissolve the high temperature / high pressure cell.
[0012]
The polycrystalline diamond obtained under the conditions indicated by the circles in this example was found to be pure cubic diamond by X-ray diffraction and Raman spectroscopic analysis. Further, it is a polycrystalline sintered body that is extremely well sintered by X-ray diffraction, scanning electron microscope observation and optical observation, and optically colorless and transparent like single crystal diamond. Since it is polycrystalline, it does not have the cleavage property of single crystal diamond, and has stable strength and hardness against load in any direction. The polycrystalline diamond obtained by the manufacturing method of this example can be used for parts and cutting tools of research ultra-high pressure generators. In addition, since the shape of the sample is the shape of a polycrystalline body that is synthesized almost as it is, any shape other than the cylindrical shape of this example can be formed in accordance with the use form. Graphite is easier to process into the desired shape than diamond. Furthermore, a polycrystalline body of an arbitrary size can be obtained by changing the size of the sample, and a diamond polycrystalline body of about 10 mm can be manufactured by using a large sample by enlarging the high-temperature and high-pressure cell.
[0013]
The properties of the polycrystalline diamond obtained by the production method of this example will be described in detail based on test data.
[0014]
In order to investigate the microstructure of the obtained polycrystalline diamond, it was observed with a transmission electron microscope (TEM). As a result, under the conditions indicated by the circles in FIG. 2, fine diamonds having a particle size of 100 nm or less, and most often 10-20 nm or less, are closely bonded, and impurities and inclusions are not observed at the particle interface. I found it impossible. FIG. 3 shows a typical transmission electron micrograph thereof.
[0015]
It was found from the X-ray diffraction experiment that the polycrystalline diamond obtained by the present invention is highly isotropic. That is, the ratio I (220) / I (111) of (220) diffraction intensity (I (220) ) to (111) diffraction intensity (I (111) ) of X-ray diffraction in any direction of the polycrystalline diamond is It was 0.1 or more, and many were in the range of 0.2 to 0.25. On the other hand, the polycrystalline diamond produced by the belt-type uniaxial compressible ultra-high pressure apparatus has some {111} orientation parallel to the direction of uniaxial compression, and depending on the measurement direction of the X-ray diffraction line, The ratio I (220) / I (111) was less than 0.1.
[0016]
Next, the hardness of the obtained polycrystalline diamond was measured. The surface of the sample was polished to a mirror surface with a diamond electrodeposition grindstone to obtain a measurement surface. Using a micro hardness meter, the hardness was measured with a micro Knoop indenter under a load of 500 g. For comparison, the Knoop hardness in the <100> orientation on the (100) plane of a high-purity diamond single crystal having an impurity of 0.1 ppm or less was measured under the same conditions. Table 1 shows the results. All showed hardness exceeding 70 GPa and depending on conditions, it exceeded 110 GPa and showed a value almost equivalent to the hardness of a single crystal.
[Table 1]
[0017]
【The invention's effect】
As described above, the method for producing a polycrystal according to the present invention synthesizes a polycrystal having a high purity from a raw material having a high purity without adding a catalyst or a sintering aid. There is an effect that the body can be obtained. It is an extremely well-sintered polycrystalline sintered body that has no cleaving property like single crystal diamond, and has stable strength and hardness against loads in any direction. A suitable material is obtained.
[Brief description of the drawings]
FIG. 1 is a cross-sectional view showing an example of a high-temperature and high-pressure cell used in a method for producing a polycrystalline body of the present invention.
FIG. 2 is a graph showing examples and comparative examples of the present invention.
FIG. 3 is a transmission electron micrograph of the polycrystalline body of the present invention.
[Explanation of symbols]
1. Sample 2. 2. Sodium chloride 3. Magnesium oxide 4. Heater Insulation material6. Electrodes 7,8. Pressure medium 9. thermocouple

Claims (7)

  1. A cubic diamond polycrystal obtained by direct conversion and sintering from graphite under an ultrahigh pressure and high temperature without addition of a sintering aid or a catalyst, wherein the diamond has an average particle diameter of 100 nm or less and a purity of 99 % Diamond polycrystal having a hardness of 110 GPa or more.
  2. The diamond polycrystal according to claim 1, wherein the diamond has an average particle diameter of 20 nm or less.
  3. The ratio I (220) / I (111) of (220) diffraction intensity (I (220) ) to (111) diffraction intensity (I (111) ) of X-ray diffraction in any direction of the polycrystal is 0.1 or more. The diamond polycrystal according to claim 1 or 2, wherein
  4. By placing graphite in a pressure cell equipped with a means for indirect heating of the sample by passing an electric current through a heater made of a refractory metal, heating and pressurizing can be performed directly without adding a sintering aid or catalyst. A diamond characterized in that it is converted and sintered to a polycrystalline diamond crystal, the pressure is applied by a multi-anvil apparatus, and the heating temperature T and the applied pressure P satisfy the following relationship: A method for producing a polycrystal.
    T> 5P 2 -241P + 4909
    Where T: temperature (° C.), P: pressure (GPa)
  5. The method for producing a polycrystalline diamond according to claim 4, wherein the graphite is graphite having a purity of 99% or more.
  6. By placing graphite in a pressure cell equipped with a means for indirect heating of the sample by passing an electric current through a heater made of a refractory metal, heating and pressurizing can be performed directly without adding a sintering aid or catalyst. A diamond characterized in that it is converted into a crystalline diamond polycrystal and is pressed by a multi-anvil apparatus , heated at 1800 ° C. or higher, and pressed at 20 GPa or higher. A method for producing a polycrystal.
  7. By placing graphite in a pressure cell equipped with a means for indirect heating of the sample by passing an electric current through a heater made of a refractory metal, heating and pressurizing can be performed directly without adding a sintering aid or catalyst. A diamond characterized in that it is converted into a crystalline diamond polycrystal and is pressed by a multi-anvil apparatus , heated at 2300 ° C. or higher, and pressed at 12 GPa or higher. A method for producing a polycrystal.
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