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WO2021199260A1 - Carbure cémenté et outil de coupe comprenant du carbure cémenté - Google Patents

Carbure cémenté et outil de coupe comprenant du carbure cémenté Download PDF

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Publication number
WO2021199260A1
WO2021199260A1 PCT/JP2020/014778 JP2020014778W WO2021199260A1 WO 2021199260 A1 WO2021199260 A1 WO 2021199260A1 JP 2020014778 W JP2020014778 W JP 2020014778W WO 2021199260 A1 WO2021199260 A1 WO 2021199260A1
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WIPO (PCT)
Prior art keywords
less
range
tungsten carbide
cemented carbide
carbide particles
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.)
Ceased
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PCT/JP2020/014778
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English (en)
Japanese (ja)
Inventor
広瀬　和弘
隆洋 山川
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Sumitomo Electric Hardmetal Corp
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Sumitomo Electric Hardmetal Corp
Priority date (The priority date 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 date listed.)
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Publication date
Application filed by Sumitomo Electric Hardmetal Corp filed Critical Sumitomo Electric Hardmetal Corp
Priority to JP2020548827A priority Critical patent/JP6912033B1/ja
Priority to CN202080002969.6A priority patent/CN113748222A/zh
Priority to PCT/JP2020/014778 priority patent/WO2021199260A1/fr
Priority to TW109134615A priority patent/TWI748676B/zh
Priority to JP2021044526A priority patent/JP2021161539A/ja
Publication of WO2021199260A1 publication Critical patent/WO2021199260A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B41/00—Boring or drilling machines or devices specially adapted for particular work; Accessories specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B51/00—Tools for drilling machines
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide

Definitions

  • This disclosure relates to cemented carbide and cutting tools equipped with it.
  • JP-A-2007-92090 Japanese Unexamined Patent Publication No. 2012-52237 Japanese Unexamined Patent Publication No. 2012-117100
  • the cemented carbide of the present disclosure is a cemented carbide including a first phase composed of a plurality of tungsten carbide particles and a second phase containing cobalt.
  • the equivalent circle diameter of each of the tungsten carbide particles is calculated by performing image processing on the image of the cemented carbide taken with a scanning electron microscope, the equivalent circle diameter is 0.3 ⁇ m or more and 1.0 ⁇ m.
  • the ratio based on the number of the tungsten carbide particles below is 50% or more.
  • the distribution of the equivalent circle diameter of the tungsten carbide particles is represented by a histogram with the frequency as the vertical axis and the class as the horizontal axis,
  • the frequency is the number of the tungsten carbide particles, and is In the class, the equivalent circle diameter is divided in ascending order at intervals of 0.1 ⁇ m.
  • On the horizontal axis a range of more than 0.3 ⁇ m and 0.6 ⁇ m or less is defined as the first range, and a range of more than 0.6 ⁇ m and 1.0 ⁇ m or less is defined as the second range.
  • the first range and the second range each have at least one maximum frequency.
  • the ratio of the largest first maximum power to the total number of the tungsten carbide particles is 10% or more. It is a cemented carbide in which the ratio of the largest second maximum power to the total number of the tungsten carbide particles among the maximum powers existing in the second range is 10% or more.
  • the cutting tool of the present disclosure is a cutting tool having a cutting edge made of the above-mentioned cemented carbide.
  • FIG. 1 is an example of an image of the cemented carbide of the present disclosure taken by a scanning electron microscope.
  • FIG. 2 is an image obtained by performing image processing on the captured image of FIG.
  • FIG. 3 is a diagram showing an example of the distribution of the equivalent circle diameters of the tungsten carbide particles in the cemented carbide of the present disclosure.
  • FIG. 4 is a diagram showing another example of the distribution of the equivalent circle diameters of the tungsten carbide particles in the cemented carbide of the present disclosure.
  • FIG. 5 is a diagram showing another example of the distribution of the equivalent circle diameters of the tungsten carbide particles in the cemented carbide of the present disclosure.
  • FIG. 6 is a diagram showing another example of the distribution of the equivalent circle diameters of the tungsten carbide particles in the cemented carbide of the present disclosure.
  • an object of the present disclosure is to provide a cemented carbide capable of extending the life of a tool when used as a tool material, particularly even in microfabrication of a printed circuit board, and a cutting tool provided with the cemented carbide. ..
  • the cemented carbide of the present disclosure enables a long life of a tool, especially in microfabrication of a printed circuit board.
  • the cemented carbide of the present disclosure is a cemented carbide including a first phase composed of a plurality of tungsten carbide particles and a second phase containing cobalt.
  • the equivalent circle diameter of each of the tungsten carbide particles is calculated by performing image processing on the image of the cemented carbide taken with a scanning electron microscope, the equivalent circle diameter is 0.3 ⁇ m or more and 1.0 ⁇ m.
  • the ratio based on the number of the tungsten carbide particles below is 50% or more.
  • the distribution of the equivalent circle diameter of the tungsten carbide particles is represented by a histogram with the frequency as the vertical axis and the class as the horizontal axis,
  • the frequency is the number of the tungsten carbide particles, and is In the class, the equivalent circle diameter is divided in ascending order at intervals of 0.1 ⁇ m.
  • On the horizontal axis a range of more than 0.3 ⁇ m and 0.6 ⁇ m or less is defined as the first range, and a range of more than 0.6 ⁇ m and 1.0 ⁇ m or less is defined as the second range.
  • the first range and the second range each have at least one maximum frequency.
  • the ratio of the largest first maximum power to the total number of the tungsten carbide particles is 10% or more. It is a cemented carbide in which the ratio of the largest second maximum power to the total number of the tungsten carbide particles among the maximum powers existing in the second range is 10% or more.
  • the cemented carbide of the present disclosure makes it possible to extend the life of the tool, especially in the microfabrication of printed circuit boards.
  • the cemented carbide contains 75 area% or more and less than 100 area% of the first phase and more than 0% by volume and 20 area% or less of the second phase in an image taken by a scanning electron microscope. Is preferable. According to this, the tool life is further improved.
  • the cemented carbide preferably contains the second phase in an amount of 5 area% or more and 12 area% or less in an image taken with a scanning electron microscope. According to this, the tool life is further improved.
  • the cemented carbide contains chromium and contains chromium.
  • the mass-based ratio of the chromium to the cobalt is preferably 5% or more and 10% or less. According to this, the breakage resistance of the cemented carbide is improved, and the tool life is further improved.
  • the mass-based content of the vanadium in the cemented carbide is preferably less than 100 ppm. According to this, the strength of the cemented carbide is improved.
  • the ratio based on the number of the tungsten carbide particles having the equivalent circle diameter of less than 0.3 ⁇ m is preferably 7% or less. According to this, the tool life is further improved.
  • the ratio of the second maximum frequency to the first maximum frequency is preferably 0.8 or more and 1.2 or less. According to this, the tool life is further improved.
  • the third range has the first maximal frequency and the fourth range preferably has the second maximum frequency. According to this, the tool life is further improved.
  • the cutting tool of the present disclosure is a cutting tool provided with a cutting edge made of the above-mentioned cemented carbide.
  • the cutting tools of the present disclosure have a long tool life.
  • the cutting tool is preferably a rotary tool for processing a printed circuit board.
  • the cutting tool of the present disclosure is suitable for microfabrication of a printed circuit board.
  • the notation in the form of "A to B” means the upper and lower limits of the range (that is, A or more and B or less) unless otherwise defined, and the unit is not described in A and the unit is described only in B. If so, the unit of A and the unit of B are the same.
  • a compound or the like when represented by a chemical formula in the present specification, it shall include all conventionally known atomic ratios when the atomic ratio is not particularly limited, and should not necessarily be limited to those in the stoichiometric range.
  • the ratio of the number of atoms constituting the WC includes any conventionally known atomic ratio.
  • a glass epoxy substrate in which a glass woven cloth in which glass fibers are woven into a cloth shape is impregnated with an epoxy resin, a glass polyimide substrate in which a glass woven cloth is impregnated with a polyimide resin, or the like is used. ing.
  • the cemented carbide of the present disclosure is a cemented carbide including a first phase composed of a plurality of tungsten carbide particles and a second phase containing cobalt.
  • the equivalent circle diameter of each of the tungsten carbide particles is calculated by performing image processing on the image of the cemented carbide taken with a scanning electron microscope, the equivalent circle diameter is 0.3 ⁇ m or more and 1.0 ⁇ m or less.
  • the ratio based on the number of tungsten carbide particles is 50% or more, and when the distribution of the equivalent circle diameter of the tungsten carbide particles is represented by a histogram with the frequency as the vertical axis and the class as the horizontal axis, the frequency is the tungsten carbide particles.
  • the equivalent circle diameter is divided in ascending order at 0.1 ⁇ m intervals, and the range of more than 0.3 ⁇ m and 0.6 ⁇ m or less is defined as the first range on the horizontal axis, and is 0.6 ⁇ m.
  • the range of super 1.0 ⁇ m or less is defined as the second range, and the first range and the second range each have at least one maximum frequency, and the first maximum frequency existing in the first range is the largest.
  • the ratio of the maximum frequency to the total number of tungsten carbide particles is 10% or more, and the ratio of the maximum second maximum frequency to the total number of tungsten carbide particles existing in the second range is 10% or more. It is a cemented carbide.
  • the cemented carbide of the present disclosure makes it possible to extend the life of the tool, especially in the microfabrication of printed circuit boards. The reason for this is not clear, but it is presumed to be as shown in (i) and (ii) below.
  • the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less is 50% or more. According to this, the cemented carbide structure becomes homogeneous, it is possible to suppress a decrease in the accuracy of microfabrication due to use, and the tool life is extended.
  • the distribution of the equivalent circle diameter of the WC particles is in the range of the particle size of more than 0.3 ⁇ m and not more than 0.6 ⁇ m (first range) and the range of more than 0.6 ⁇ m and not more than 1.0 ⁇ m (the first range).
  • Each of the second range) has at least one maximum frequency.
  • the maximum maximum power in the first range (first maximum power) and the maximum maximum power in the second range (second maximum power) are each 10% of the total number of tungsten carbide particles in the cemented carbide. That is all.
  • the cemented carbide has a structure in which WC particles having a large circle-equivalent diameter form a skeleton, and WC particles having a small circle-equivalent diameter fill a gap between the WC particles. Since the WC particles are bonded to each other in the cemented carbide, the wear resistance is improved by suppressing the WC particles from falling off. Further, by suppressing wear, an increase in cutting resistance is suppressed and breakage resistance is improved. Therefore, the tool life is extended.
  • the amount of cobalt exposed on the tool surface during machining is reduced as compared with the conventional fine-grained cemented carbide. Therefore, the cobalt is less likely to be worn during processing, the WC particles can be suppressed from falling off, and the tool life is extended.
  • the first phase consists of tungsten carbide particles.
  • tungsten carbide includes not only "pure WC (WC containing no impurity elements, WC in which impurity elements are below the detection limit)", but also "as long as the effects of the present disclosure are not impaired.”"WC” in which other impurity elements are intentionally or unavoidably contained is also included.
  • the concentration of impurities contained in tungsten carbide (when two or more kinds of elements constituting the impurities are the total concentration thereof) is less than 0.1% by mass with respect to the total amount of the tungsten carbide and the impurities. ..
  • the content of impurity elements in the first phase is measured by ICP emission spectrometry (Inductively Coupled Plasma) Emission Spectroscopy (measuring apparatus: Shimadzu Corporation "ICPS-8100" (trademark)).
  • the ratio of the number-based number of tungsten carbide particles having a circle-equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less is 50% or more. According to this, the cemented carbide structure becomes homogeneous, it is possible to suppress a decrease in the accuracy of microfabrication due to use, and the tool life is extended.
  • the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less is 50% or more, preferably 70% or more, from the viewpoint of improving the homogeneity of the cemented carbide structure.
  • the upper limit of the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less is not particularly limited, but may be, for example, 100% or less, 90% or less, or 80% or less.
  • the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less can be 50% or more and 100% or less, 60% or more and 90% or less, and 70% or more and 80% or less.
  • the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of less than 0.3 ⁇ m is preferably 7% or less.
  • Tungsten carbide particles having a circle-equivalent diameter of less than 0.3 ⁇ m have a small contribution to improving the strength of cemented carbide and reducing the amount of cobalt exposed on the tool surface during machining. Therefore, by reducing the ratio based on the number of tungsten carbide particles having a circle-equivalent diameter of less than 0.3 ⁇ m, the tool life is further extended.
  • the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of less than 0.3 ⁇ m is preferably 0% or more and 7% or less, and more preferably 0% or more and 5% or less. Further, the ratio based on the number of tungsten carbide particles having a circle equivalent diameter of less than 0.2 ⁇ m is preferably 0% or more and 3% or less.
  • the equivalent circle diameter of the tungsten carbide particles is measured by the following procedures (A1) to (C1).
  • (A1) Mirror finish any surface or any cross section of cemented carbide. Examples of the mirror surface processing method include a method of polishing with diamond paste, a method of using a focused ion beam device (FIB device), a method of using a cross section polisher device (CP device), and a method of combining these.
  • FIB device focused ion beam device
  • CP device cross section polisher device
  • FIG. 1 shows an example of an image of the cemented carbide of the present disclosure taken with a scanning electron microscope. On the lower right scale of FIG. 1, one scale indicates 1 ⁇ m.
  • (C1) The captured image obtained in (B1) above is taken into a computer, image processing is performed using image analysis software (ImageJ: https://imagej.nih.gov/ij/), and a circle of tungsten carbide particles.
  • the equivalent diameter (Heywood diameter: equivalent area circle equivalent diameter) is calculated.
  • the first phase composed of tungsten carbide particles and the second phase containing cobalt can be distinguished by the shade of color in the photographed image.
  • An image obtained by performing image processing on the captured image of FIG. 1 is shown in FIG. In FIG. 2, the black region is the first phase and the white region is the second phase. White lines indicate grain boundaries. On the lower right scale of FIG. 2, one scale indicates 1 ⁇ m.
  • the ratio based on the number of tungsten carbide particles having a circle-equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less in the cemented carbide is calculated by the following procedures (D1) and (E1).
  • D1) The image processing of the above (C1) is performed in three measurement fields of view.
  • the size of one measurement field of view is a rectangle having a length of 25.3 ⁇ m and a width of 17.6 ⁇ m.
  • the ratio of the number-based number of tungsten carbide particles having a circle equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less in the cemented carbide is selected as the measurement field. It was confirmed that even if the measurement results were changed multiple times, the variation in the measurement results was small, and even if the measurement field was set arbitrarily, it would not be arbitrary.
  • the distribution of the equivalent circle diameter of the tungsten carbide particles contained in the cemented carbide of the present disclosure satisfies the following (a). Further, when the distribution of the equivalent circle diameters of the tungsten carbide particles contained in the cemented carbide of the present disclosure is represented by a histogram having the frequency as the vertical axis and the class as the horizontal axis, the following (b) and (c) are satisfied.
  • the frequency is the number of tungsten carbide particles
  • the class is divided by 0.1 ⁇ m intervals in ascending order of the equivalent circle diameters.
  • the ratio based on the number of tungsten carbide particles having a circle-equivalent diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less is 50% or more.
  • the ratio of the largest first maximum power to the total number of tungsten carbide particles is 10% or more, which is the largest among the maximum powers existing in the second range.
  • the ratio to the total number of tungsten carbide particles having the second maximum frequency is 10% or more.
  • the histogram is prepared by the following procedures (A2) and (B2).
  • the equivalent circle diameter of the tungsten carbide particles is calculated by the procedure (A1) to (C1) described in the above method for measuring the equivalent circle diameter of the tungsten carbide particles.
  • the measurement of the equivalent circle diameter of the tungsten carbide particles is performed in three measurement fields.
  • the maximum frequency is the frequency of a class whose frequency is one lower than the class to which the frequency belongs (the side having a smaller equivalent circle diameter), and the frequency of the class to which the frequency belongs (one higher than the class to which the frequency belongs (). It means that it is larger than any of the frequencies of the class (on the side with the larger equivalent diameter of the circle).
  • the class one level below the class to which the maximum frequency belongs and the class one level above the class to which the maximum frequency belongs may be a class outside the first range or a class outside the second range.
  • the class to which the maximum frequency belongs in the first range is more than 0.3 ⁇ m and 0.4 ⁇ m or less
  • the next lower class is more than 0.2 ⁇ m and 0.3 ⁇ m or less outside the first range.
  • the class to which the maximum frequency belongs in the second range is more than 0.9 ⁇ m and 1.0 ⁇ m or less
  • the class one level higher is more than 1.0 ⁇ m and 1.1 ⁇ m or less outside the second range.
  • FIGS. 3 to 6 are examples of diagrams showing the distribution of the equivalent circle diameters of the tungsten carbide particles in the cemented carbide of the present disclosure, respectively.
  • the horizontal axis shows the class in which the equivalent circle diameter is divided in ascending order at intervals of 0.1 ⁇ m
  • the vertical axis shows the ratio (%) of the number of tungsten particles belonging to each class to all the tungsten particles. ..
  • the notation in the form of "C to D” means C super D or less.
  • the notation “0 to 0.1” on the horizontal axis of FIGS. 3 to 6 means more than 0 ⁇ m and 0.1 ⁇ m or less
  • the notation “0.1 to 0.2” means 0. It means more than 1 ⁇ m and 0.2 ⁇ m or less.
  • FIGS. 3 to 6 can be regarded as the shape of the histogram when the rules of the class on the horizontal axis are the same and the frequency on the vertical axis is the number of tungsten carbide particles. Therefore, the above (a) to (c) can be described using the shapes of FIGS. 3 to 6.
  • the vertical axis shows the ratio (%) of the number of tungsten particles belonging to each class to the total tungsten particles.
  • the axis may be referred to as frequency.
  • the frequency in the class having a circle equivalent diameter of more than 0.4 ⁇ m and 0.5 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the circle equivalent diameter is more than 0.3 ⁇ m and 0.4 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs (the equivalent circle diameter is more than 0.5 ⁇ m and 0.6 ⁇ m or less). That is, in FIG. 3, the first range (the equivalent circle diameter is more than 0.3 ⁇ m and 0.6 ⁇ m or less) has one maximum frequency.
  • the frequency in the class having a circle equivalent diameter of more than 0.7 ⁇ m and 0.8 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the circle equivalent diameter is more than 0.6 ⁇ m and 0.7 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs (the equivalent circle diameter is more than 0.8 ⁇ m and 0.9 ⁇ m or less). That is, in FIG. 3, the second range (the equivalent circle diameter is more than 0.6 ⁇ m and 1.0 ⁇ m or less) has one maximum frequency.
  • the first maximum frequency which is the largest maximum frequency existing in the first range, is a frequency in a class having a circle equivalent diameter of more than 0.4 ⁇ m and 0.5 ⁇ m or less.
  • the ratio of the first maximum power to the total number of tungsten carbide particles is 10% or more (about 14.3%).
  • the second maximum frequency which is the largest maximum frequency existing in the second range, is a frequency in a class having a circle equivalent diameter of more than 0.7 ⁇ m and 0.8 ⁇ m or less.
  • the ratio of the second maximum power to the total number of tungsten carbide particles is 10% or more (about 12.6%).
  • the frequency in the class having a circle equivalent diameter of more than 0.5 ⁇ m and 0.6 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the circle equivalent diameter is more than 0.4 ⁇ m and 0.5 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs (the equivalent circle diameter is more than 0.6 ⁇ m and 0.7 ⁇ m or less). That is, in FIG. 4, the first range (the equivalent circle diameter is more than 0.3 ⁇ m and 0.6 ⁇ m or less) has one maximum frequency.
  • the frequency in the class having a circle equivalent diameter of more than 0.7 ⁇ m and 0.8 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the circle equivalent diameter is more than 0.6 ⁇ m and 0.7 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs is more than 0.8 ⁇ m and 0.9 ⁇ m or less.
  • the frequency in the class having a circle equivalent diameter of more than 0.9 ⁇ m and 1.0 ⁇ m or less is one class lower than the class to which the frequency belongs (the circle equivalent diameter is more than 0.8 ⁇ m and 0.9 ⁇ m or less).
  • the equivalent circle diameter is more than 1.0 ⁇ m and 1.1 ⁇ m or less. That is, in FIG. 4, the second range (the equivalent circle diameter is more than 0.6 ⁇ m and 1.0 ⁇ m or less) has two maximum frequencies.
  • the first maximum frequency which is the largest maximum frequency existing in the first range, is a frequency in a class having a circle equivalent diameter of more than 0.5 ⁇ m and 0.6 ⁇ m or less.
  • the ratio of the first maximum power to the total number of tungsten carbide particles is 10% or more (about 13.4%).
  • the second maximum frequency which is the largest maximum frequency existing in the second range, is a frequency in a class having a circle equivalent diameter of more than 0.7 ⁇ m and 0.8 ⁇ m or less.
  • the ratio of the second maximum power to the total number of tungsten carbide particles is 10% or more (about 12.7%).
  • the frequency in the class having the equivalent circle diameter of more than 0.3 ⁇ m and 0.4 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the equivalent circle diameter is more than 0.2 ⁇ m and 0.3 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs (the equivalent circle diameter is more than 0.4 ⁇ m and 0.5 ⁇ m or less). That is, in FIG. 5, the first range (the equivalent circle diameter is more than 0.3 ⁇ m and 0.6 ⁇ m or less) has one maximum frequency.
  • the frequency in the class having a circle equivalent diameter of more than 0.7 ⁇ m and 0.8 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the circle equivalent diameter is more than 0.6 ⁇ m and 0.7 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs is more than 0.8 ⁇ m and 0.9 ⁇ m or less.
  • the frequency in the class having a circle equivalent diameter of more than 0.9 ⁇ m and 1.0 ⁇ m or less is one class lower than the class to which the frequency belongs (the circle equivalent diameter is more than 0.8 ⁇ m and 0.9 ⁇ m or less).
  • the equivalent circle diameter is more than 1.0 ⁇ m and 1.1 ⁇ m or less. That is, in FIG. 5, the second range (the equivalent circle diameter is more than 0.6 ⁇ m and 1.0 ⁇ m or less) has two maximum frequencies.
  • the first maximum frequency which is the largest maximum frequency existing in the first range, is a frequency in a class having a circle equivalent diameter of more than 0.3 ⁇ m and 0.4 ⁇ m or less.
  • the ratio of the first maximum power to the total number of tungsten carbide particles is 10% or more (about 11.8%).
  • the second maximum frequency which is the largest maximum frequency existing in the second range, is a frequency in a class having a circle equivalent diameter of more than 0.7 ⁇ m and 0.8 ⁇ m or less.
  • the ratio of the second maximum power to the total number of tungsten carbide particles is 10% or more (about 12.2%).
  • the frequency in the class having the equivalent circle diameter of more than 0.4 ⁇ m and 0.5 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the equivalent circle diameter is more than 0.3 ⁇ m and 0.4 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs (the equivalent circle diameter is more than 0.5 ⁇ m and 0.6 ⁇ m or less). That is, in FIG. 6, the first range (the equivalent circle diameter is more than 0.3 ⁇ m and 0.6 ⁇ m or less) has one maximum frequency.
  • the frequency in the class having a circle equivalent diameter of more than 0.6 ⁇ m and 0.7 ⁇ m or less is the frequency of the class one below the class to which the frequency belongs (the circle equivalent diameter is more than 0.5 ⁇ m and 0.6 ⁇ m or less).
  • the frequency of the class one level higher than the class to which the frequency belongs (the equivalent circle diameter is more than 0.7 ⁇ m and 0.8 ⁇ m or less). That is, in FIG. 6, the second range (the equivalent circle diameter is more than 0.6 ⁇ m and 1.0 ⁇ m or less) has one maximum frequency.
  • the first maximum frequency which is the largest maximum frequency existing in the first range, is a frequency in a class having a circle equivalent diameter of more than 0.4 ⁇ m and 0.5 ⁇ m or less.
  • the ratio of the first maximum power to the total number of tungsten carbide particles is 10% or more (about 14.2%).
  • the second maximum frequency which is the largest maximum frequency existing in the second range, is a frequency in a class having a circle equivalent diameter of more than 0.6 ⁇ m and 0.7 ⁇ m or less.
  • the ratio of the second maximum power to the total number of tungsten carbide particles is 10% or more (about 12.4%).
  • the range of more than 0.4 ⁇ m and less than 0.6 ⁇ m is defined as the third range, and the range of more than 0.6 ⁇ m and less than 0.8 ⁇ m is defined as the third range.
  • the third range has a first maximum frequency and the fourth range has a second maximum frequency. According to this, the tool life is further improved.
  • the ratio of the second maximum frequency to the first maximum frequency is preferably 0.8 or more and 1.2 or less. According to this, the tool life is further improved. The reason for this is that the bonding by contact between the tungsten carbide particles is important, and when the difference between the maximum power existing in the first range and the maximum power existing in the second range becomes large, the tungsten carbide in the cemented carbide eventually becomes large. It is presumed that this is because the contact between particles is reduced.
  • the second phase contains cobalt.
  • the second phase is a bonding phase in which the tungsten carbide particles constituting the first phase are bonded to each other.
  • the second phase contains cobalt (Co)
  • the main component of the second phase is Co.
  • the main component of the second phase is Co means that the mass ratio of cobalt in the second phase is 90% by mass or more and 100% by mass or less.
  • the mass ratio of cobalt in the second phase can be measured by ICP emission spectroscopic analysis (equipment used: "ICPS-8100” (trademark) manufactured by Shimadzu Corporation).
  • the second phase can contain iron group elements such as nickel and dissolved substances (Cr, W, etc.) in the alloy in addition to cobalt.
  • iron group elements such as nickel and dissolved substances (Cr, W, etc.) in the alloy in addition to cobalt.
  • the cemented carbide includes a first phase composed of a plurality of tungsten carbide particles and a second phase containing cobalt.
  • the cemented carbide preferably contains 75 area% or more and less than 100 area% of the first phase and 0 area% or more and 20 area% or less of the second phase in the image taken by the scanning electron microscope.
  • the ratio of the second phase in the cemented carbide is 20 area% or less, it is possible to suppress the dissolution of fine tungsten carbide particles having a circle equivalent diameter of 0.6 ⁇ m or less in the cobalt of the second phase. It is possible to suppress the decrease of tungsten carbide particles having a circle-equivalent diameter of more than 0.3 ⁇ m and 0.6 ⁇ m or less. In addition, the amount of cobalt exposed on the tool surface during machining is further reduced. Therefore, the tool life is further improved.
  • the cemented carbide preferably contains the second phase in an amount of 5 area% or more and 12 area% or less in the image taken by the scanning electron microscope. According to this, the hardness and wear resistance required for processing the printed circuit board can be exhibited, and the occurrence of variation in tool life can be suppressed.
  • the lower limit of the ratio of the first phase in the cemented carbide can be 75 area% or more and 85 area% or more.
  • the upper limit of the ratio of the first phase in the cemented carbide can be less than 100 area% and 95 area% or less.
  • the ratio of the first phase in the cemented carbide can be 75 area% or more and less than 100 area%, and 85 area% or more and 95 area% or less.
  • the lower limit of the ratio of the second phase in the cemented carbide can be more than 0 area% and 5 area% or more.
  • the upper limit of the ratio of the second phase in the cemented carbide can be 20 area% or less and 12 area% or less.
  • the ratio of the second phase in the cemented carbide can be more than 0 area% and 20 area% or less, 5 area% or more and 12 area% or less.
  • the area ratio of each of the first phase and the second phase in the cemented carbide is measured by the following procedures (A3) to (C3).
  • (C3) Perform the image processing of (B3) above in five measurement fields of view.
  • the average of the area ratios of the first phase obtained in the five measurement fields is taken as the area ratio of the first phase in the cemented carbide.
  • the average of the area ratios of the second phase obtained in the five measurement fields is taken as the area ratio of the second phase in the cemented carbide.
  • the cemented carbide contains chromium (Cr), and the mass-based ratio of chromium to cobalt is preferably 5% or more and 10% or less. Chromium has a grain growth inhibitory effect on tungsten carbide particles. Further, by solid-solving in cobalt, the generation of lattice strain of cobalt is promoted. Therefore, when the cemented carbide contains chromium in the above ratio, the breakage resistance is further improved.
  • chromium may precipitate as carbide and become the starting point of damage.
  • mass-based ratio of chromium to cobalt is 5% or more and 10% or less, precipitation of chromium carbide is unlikely to occur, and the effect of improving breakage resistance can be obtained.
  • the mass-based ratio of chromium to cobalt is 10% or less, the degree of grain growth inhibitory action becomes appropriate, and the amount of tungsten carbide particles having a circle equivalent diameter of more than 1.0 ⁇ m in the cemented carbide becomes excessive. It can be suppressed.
  • the lower limit of the mass-based ratio of chromium to cobalt is preferably 5% or more, more preferably 7% or more.
  • the mass-based ratio of chromium to cobalt is preferably 10% or less, more preferably 9% or less.
  • the mass standard of chromium with respect to cobalt can be 5% or more and 10% or less, and 7% or more and 9% or less.
  • the content of cobalt and chromium in cemented carbide is measured by ICP emission spectroscopy.
  • the mass-based content of vanadium in the cemented carbide is preferably less than 100 ppm.
  • vanadium Since vanadium has a grain growth inhibitory effect, it has been used in the production of conventional ultrafine cemented carbide. If vanadium is present during the grain growth of the tungsten carbide particles, vanadium is precipitated on the surface of the tungsten carbide particles, or vanadium intervenes in the growth surface of the tungsten carbide particles in a short period of time, so that the tungsten carbide particles grow. It is thought to be suppressed.
  • the content of vanadium in the cemented carbide is preferably 100 ppm or less, more preferably 10 ppm or less. Since the smaller the content of vanadium in the cemented carbide is, the more preferable it is, the lower limit thereof is preferably 0 ppm. In addition, vanadium of several ppm may be unintentionally detected in the manufacturing process.
  • the content of vanadium in the cemented carbide can be 0 ppm or more and 100 ppm or less, and 0 ppm or more and 10 ppm or less.
  • the content of vanadium in cemented carbide is measured by ICP emission spectroscopy.
  • the cemented carbide of the present embodiment can be typically produced by performing a raw material powder preparation step, a mixing step, a molding step, a sintering step, and a cooling step in the above order. Hereinafter, each step will be described.
  • the preparation step is a step of preparing all the raw material powders of the materials constituting the cemented carbide.
  • the raw material powder include tungsten carbide powder, which is a raw material for the first phase, and cobalt (Co) powder, which is a raw material for the second phase, as essential raw material powders.
  • chromium carbide (Cr 3 C 2 ) powder can be prepared as a grain growth inhibitor.
  • Vanadium carbide (VC) powder can also be prepared as long as the effects of the present disclosure are exhibited.
  • As the tungsten carbide powder, cobalt powder, chromium carbide powder, and vanadium carbide powder commercially available ones can be used.
  • the tungsten carbide powder includes (a) tungsten carbide powder having an average particle size of 0.4 ⁇ m or more and 1.2 ⁇ m or less (hereinafter, also referred to as “first tungsten carbide powder”), and (b) an average particle size of 0.8 ⁇ m or more and 1.2 ⁇ m or more.
  • Tungsten carbide powder of ⁇ m or less (hereinafter, also referred to as “second tungsten carbide powder”) is prepared.
  • the first tungsten carbide powder having an average particle size smaller than the average particle size of the second tungsten carbide powder is prepared.
  • the average particle size of the raw material powder means a median diameter d50 having a diameter equivalent to a circle.
  • the average particle size is measured using a particle size distribution measuring device (trade name: MT3300EX) manufactured by Microtrac.
  • the average particle size of the cobalt powder can be 0.8 ⁇ m or more and 1.2 ⁇ m or less.
  • the average particle size of the chromium carbide powder can be 1.0 ⁇ m or more and 2.0 ⁇ m or less.
  • the average particle size of the vanadium carbide powder can be 0.5 ⁇ m or more and 1.0 ⁇ m or less.
  • the mixing process is a step of mixing each raw material powder prepared in the preparation step. By the mixing step, a mixed powder in which each raw material powder is mixed is obtained.
  • the ratio of the first tungsten carbide powder in the mixed powder can be, for example, 30% by mass or more and 94.6% by mass or less.
  • the ratio of the second tungsten carbide powder in the mixed powder can be, for example, 30% by mass or more and 64.6% by mass or less.
  • the ratio of the cobalt powder in the mixed powder can be, for example, 2.8% by mass or more and 10% by mass or less.
  • the ratio of chromium carbide powder in the mixed powder can be, for example, 0.2% by mass or more and 1.2% by mass or less.
  • the ratio of vanadium carbide powder in the mixed powder can be, for example, 0% by mass or more and 0.2% by mass or less.
  • the mixing time can be 20 hours or more and 48 hours or less.
  • the mixed powder may be granulated as needed.
  • a known granulation method can be applied to the granulation, and for example, a commercially available granulator such as a spray dryer can be used.
  • the molding step is a step of molding the mixed powder obtained in the mixing step into a predetermined shape to obtain a molded product.
  • a predetermined shape include a cutting tool shape (for example, the shape of a small-diameter drill).
  • the sintering step is a step of sintering the molded product obtained in the molding step to obtain a cemented carbide.
  • the sintering temperature can be a general cemented carbide sintering temperature (1350 to 1500 ° C.).
  • Cemented carbide is generally sintered at 1350 to 1500 ° C., but fine tungsten carbide particles have a large surface area and are easily dissolved in cobalt, so that an abnormal structure is likely to occur due to dissolution and reprecipitation. Therefore, in the sintering of fine tungsten carbide particles, in order to suppress dissolution and reprecipitation, sintering is performed in a low temperature region of 1350 to 1380 ° C., which has a low solid solution limit of tungsten carbide with cobalt. However, in the cemented carbide obtained by sintering in a low temperature region, the tungsten carbide particles do not grow, so the surface of the tungsten carbide particles remains crushed by crushing or mixing in the previous process. It has become. Therefore, the bonding force between the tungsten carbide particles and cobalt and the interface between the tungsten carbide particles is low, and the wear resistance and breakage resistance tend to decrease.
  • the generation of fragments of ultrafine tungsten carbide particles generated by crushing or mixing raw materials is suppressed, and the effect of suppressing grain growth by chromium is maximized. Furthermore, it has been found that abnormal grain growth can be suppressed even in a temperature range where grain growth normally occurs by providing a distribution of coarse particles and fine particles having peaks having similar particle sizes in the fine structure. .. Therefore, in the method for producing cemented carbide of the present disclosure, even if the tungsten carbide particles are sintered at a higher temperature than before, the generation of abnormal structure can be suppressed, and the interface between the tungsten carbide particles and cobalt can be suppressed. Further, by improving the bonding force at the interface between the tungsten carbide particles, it is possible to improve the wear resistance and the breaking resistance of the cemented carbide. This was newly discovered by the present inventors as a result of diligent studies.
  • the cooling step is a step of cooling the cemented carbide after the sintering is completed.
  • the cooling condition general conditions may be adopted, and there is no particular limitation.
  • the cutting tool of the present disclosure includes a cutting edge made of the above cemented carbide.
  • the cutting edge means a portion involved in cutting, and in cemented carbide, the distance between the cutting edge ridge line and the cutting edge ridge line from the cutting edge ridge line to the cemented carbide side along the perpendicular line of the tangent line of the cutting edge ridge line is 2 mm. It means a virtual surface that is and an area surrounded by.
  • the cutting tool examples include a cutting tool, a drill, an end mill, a cutting tip with a replaceable cutting edge for milling, a cutting tip with a replaceable cutting edge for turning, a metal saw, a gear cutting tool, a reamer or a tap, and the like.
  • the cutting tool of the present disclosure can exert an excellent effect in the case of a small-diameter drill for processing a printed circuit board.
  • the cemented carbide of the present embodiment may constitute the whole of these tools, or may constitute a part of them.
  • “partially constituting” indicates an embodiment in which the cemented carbide of the present embodiment is brazed to a predetermined position of an arbitrary base material to form a cutting edge portion.
  • the cutting tool according to the present embodiment may further include a hard film that covers at least a part of the surface of a base material made of cemented carbide.
  • a hard film for example, diamond-like carbon or diamond can be used.
  • Example 1 cemented carbides of Samples 1 to 24 were prepared by changing the type and compounding ratio of the raw material powder. A small-diameter drill having a cutting edge made of the cemented carbide was produced and evaluated.
  • ⁇ Preparation of sample ⁇ As the raw material powder, a powder having the composition shown in the “raw material” column of Table 1 was prepared. A plurality of tungsten carbide (WC) powders having different average particle sizes were prepared. The average particle size of the carbonized WC powder is as shown in the "Average particle size ( ⁇ m)" column of the "first WC powder” in Table 1.
  • WC tungsten carbide
  • the average particle size of cobalt (Co) powder is 1 [mu] m
  • an average particle diameter of the vanadium carbide (VC) powder was 0.8 [mu] m
  • an average particle size of chromium carbide (Cr 3 C 2) powder is 1 [mu] m.
  • Co powder, VC powder and Cr 3 C 2 powder are commercially available products.
  • the average particle size of the raw material powder is a value measured using a particle size distribution measuring device (trade name: MT3300EX) manufactured by Microtrac.
  • the distribution of the equivalent circle diameter of the tungsten carbide particles was measured, and the ratio based on the number of tungsten carbide particles having the equivalent circle diameter of 0.3 ⁇ m or more and 1.0 ⁇ m or less, and the existence of the first maximum frequency.
  • the class to be used the ratio of the first maximum frequency to the total number of tungsten carbide particles, the class in which the second maximum frequency exists, the ratio of the second maximum frequency to the total number of tungsten carbide particles, and the ratio of the second maximum frequency to the first maximum frequency. Calculated. Since the specific measurement method and calculation method are described in the first embodiment, the description thereof will not be repeated.
  • the maximum frequency does not exist within the first range (more than 0.3 ⁇ m and less than 0.6 ⁇ m) or the second range (more than 0.6 ⁇ m and less than 1.0 ⁇ m), it is indicated as “-”. If the maximum frequency is outside the first range (more than 0.3 ⁇ m and 0.6 ⁇ m or less) or outside the second range (more than 0.6 ⁇ m and 1.0 ⁇ m or less), the class of the maximum frequency is shown in parentheses. Shown in parentheses.
  • Samples 1, 4 and 12 do not have a maximum frequency (second maximum frequency) within the second range, and correspond to a comparative example.
  • the maximum frequency was present in the class of more than 1.0 ⁇ m and 1.1 ⁇ m or less.
  • Samples 2, 10 and 11 do not have a maximum frequency (first maximum frequency) within the first range, and correspond to a comparative example.
  • Sample 2 had a maximum frequency in a class of more than 0.2 ⁇ m and 0.3 ⁇ m or less, and the ratio of the number standard of this maximum frequency was 10.1%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Powder Metallurgy (AREA)
  • Drilling Tools (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Drilling And Boring (AREA)

Abstract

Un carbure cémenté comprend : une première phase comprenant une pluralité de particules de carbure de tungstène ; et une seconde phase contenant du cobalt, lorsque le diamètre circulaire équivalent de chaque particule de carbure de tungstène est calculé au moyen d'un traitement d'image sur une image du carbure cémenté capturée à l'aide d'un microscope électronique à balayage, la proportion de particules de carbure de tungstène ayant un diamètre circulaire équivalent de 0,3 à 1,0 µm est d'au moins 50 % en nombre de particules, et lorsque la distribution des diamètres circulaires équivalents des particules de carbure de tungstène est représentée par un histogramme dans lequel l'axe vertical indique le compte et l'axe horizontal indique des niveaux, ledit compte représente le nombre de particules de carbure de tungstène, et les niveaux sont formés par délimitation du diamètre circulaire équivalent dans un ordre croissant à intervalle de 0,1 µm, et, sur l'axe horizontal, une plage supérieure à 0,3 µm mais inférieure ou égale à 0,6 µm est désignée comme première plage et une plage supérieure à 0,6 µm mais inférieure ou égale à 1,0 µm est désignée comme seconde plage, et la première plage et la seconde plage ayant chacune au moins un compte maximum local, et, des comptes maximaux locaux dans la première plage, la proportion de particules de carbure de tungstène conduisant à un premier compte maximal local qui est la plus important que le nombre total de particules de carbure de tungstène est supérieure ou égale à 10 %, et, des comptes maximaux locaux dans la seconde plage, la proportion de particules de carbure de tungstène conduisant à un second compte maximal local qui est la plus important que le nombre total de particules de carbure de tungstène est supérieure ou égale à 10 %.
PCT/JP2020/014778 2020-03-31 2020-03-31 Carbure cémenté et outil de coupe comprenant du carbure cémenté Ceased WO2021199260A1 (fr)

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