WO2010113555A1 - Céramique composite à base de nitrure de silicium et son procédé de production - Google Patents

Céramique composite à base de nitrure de silicium et son procédé de production Download PDF

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WO2010113555A1
WO2010113555A1 PCT/JP2010/052417 JP2010052417W WO2010113555A1 WO 2010113555 A1 WO2010113555 A1 WO 2010113555A1 JP 2010052417 W JP2010052417 W JP 2010052417W WO 2010113555 A1 WO2010113555 A1 WO 2010113555A1
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composite ceramic
phase
raw material
boron nitride
composite
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PCT/JP2010/052417
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English (en)
Japanese (ja)
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井筒　靖久
英紀 北
秀樹 日向
近藤　直樹
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三井金属鉱業株式会社
独立行政法人産業技術総合研究所
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Priority to CN201080001148.7A priority Critical patent/CN101959831B/zh
Publication of WO2010113555A1 publication Critical patent/WO2010113555A1/fr

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Definitions

  • the present invention relates to a silicon nitride-based composite ceramic suitable as a cast member made of aluminum, magnesium or the like and a method for producing the same.
  • Silicon nitride ceramics are applied in many industrial fields because of their high strength, high hardness, heat resistance, and corrosion resistance.
  • a composite with boron nitride has been attempted.
  • boron nitride has poor wettability with the silicon nitride glass component, when a large amount of boron nitride is added, the sinterability is lowered, and it is difficult to obtain a dense material having high strength.
  • normal hexagonal boron nitride h-BN
  • h-BN normal hexagonal boron nitride
  • a mixture of silicon nitride powder and boron nitride powder is added and mixed with ⁇ sialon powder, aluminum nitride powder and rare earth element oxide powder as sintering aids, respectively.
  • a method for producing a composite ceramic to be sintered has been proposed (see Patent Document 1).
  • silicon nitride powder and boron nitride powder are mixed in a weight ratio of 90:10 to 70:30.
  • urea and boric acid are used at the time of production, and hydrogen treatment is required, so the process becomes complicated. Moreover, not only are facilities limited, but they can be dangerous. Further, the document discloses that the content ratio of hexagonal boron nitride is 1 to 25 vol. %, The lower limit of the ratio described as a specific example is 5 vol. %, And 5 vol. No specific effect has been confirmed in the case of less than%. Moreover, although the document describes the effect on thermal shock resistance, the effect is not specifically illustrated.
  • an object of the present invention is to provide a silicon nitride-based composite ceramic that can eliminate the various drawbacks of the above-described prior art.
  • the present invention uses a silicon nitride-based ceramic as a parent phase, and boron nitride is 2.5 vol. % Or more, 10 vol. % As a dispersed phase at a ratio of
  • the four-point bending strength at 25 ° C. according to JIS R1601 is ⁇ i
  • the present invention provides a suitable method for producing the above composite ceramics, Including mixing and forming a silicon nitride-based ceramic raw material powder forming a parent phase and a boron nitride raw material powder forming a dispersed phase, followed by firing.
  • the present invention provides a method for producing a composite ceramic, characterized by using a crystallite size defined by rad) of 40 nm or more and less than 48 nm.
  • the composite ceramic of the present invention is made of a silicon nitride-based ceramic as a parent phase.
  • This matrix is generally composed of ⁇ -silicon nitride.
  • boron nitride is compounded as a dispersed phase.
  • Boron nitride which is a dispersed phase, is 2.5 vol. % Or more, 10 vol. % Or less in a generally uniform and fine state.
  • the ratio of boron nitride is 2.5 vol. If it is less than%, boron nitride is not uniformly dispersed throughout the composite ceramic, and the thermal shock resistance is not improved. Conversely, 10 vol. If it exceeds 50%, the sinterability of silicon nitride decreases and the fracture strength decreases.
  • the ratio of boron nitride to the entire composite ceramic is 2.5 vol. % Or more, 5 vol. % Or less is preferable.
  • the proportion of boron nitride in the composite ceramic can be measured by X-ray diffraction, wavelength dispersion elemental analysis, or the like.
  • the composite ceramic of the present invention has high strength and excellent thermal shock resistance.
  • the strength of a ceramic material is evaluated by a four-point bending strength in accordance with JIS R1601, and the composite ceramic of the present invention has a four-point bending strength ⁇ i of 400 MPa or more at room temperature, for example, 25 ° C., Preferably, it exhibits a very high value of 500 MPa or more and 900 MPa or less, more preferably 600 MPa or more and 900 MPa or less.
  • the thermal shock resistance when it is assumed that the four-point bending strength ⁇ f conforms to JIS R1601 after applying a thermal shock by quenching by dropping into water of 800 ° C.
  • the composite ceramic of the present invention has a small decrease in strength after applying a thermal shock.
  • a composite ceramic exhibiting high strength and high thermal shock resistance is particularly suitably used as a material for a member used for casting aluminum or magnesium, for example.
  • the ratio of ⁇ f and ⁇ i is the above-mentioned value.
  • the composite ceramic of the present invention is preferably 400 MPa or more and 900 MPa or less, more preferably 500 MPa or more and 800 MPa or less. Shows a high value.
  • the composite ceramic of the present invention has high strength even at high temperatures.
  • the composite ceramic of the present invention has a four-point bending strength ⁇ h in accordance with JIS R1604-1995, preferably at 400 ° C. or higher at high temperature, for example, 1200 ° C., more preferably 500 MPa or higher, 900 MPa or lower, More preferably, it shows a very high value of 600 MPa or more and 900 MPa or less.
  • the composite ceramic of the present invention exhibits high strength at both room temperature and high temperature.
  • the ratio ⁇ h / ⁇ i between the four-point bending strength ⁇ h at a high temperature and the four-point bending strength ⁇ i at room temperature is preferably 0.85 or more, more preferably 0.9 or more, A close value.
  • the value of the four-point bending strength ⁇ h according to JIS R1604-1995 is measured by the following method.
  • a test piece of JIS R1601 is prepared, and the temperature of the test piece is increased to 1200 ° C. in the atmosphere at a temperature increase rate of 200 ° C./h.
  • a load is applied to the load point of the test piece by four-point bending at a crosshead speed of 0.5 mm / min. Measure the maximum breaking load until the specimen breaks, and let that value be ⁇ h .
  • the composite ceramic of the present invention also has high oxidation resistance.
  • the oxidation resistance can be expressed as a measure of the rate of weight increase after the composite ceramic of the present invention is oxidized. Specifically, by subtracting the weight before the oxidation treatment from the weight of the composite ceramic after the oxidation treatment at 1300 ° C. or 1400 ° C. for 100 hours in the atmosphere, dividing the result by the weight before the oxidation treatment, and multiplying by 100 The ratio of weight increase due to oxidation treatment (hereinafter, this ratio is referred to as “weight-based weight increase rate”) is calculated. A smaller increase rate means higher oxidation resistance.
  • this increase rate is preferably a small value of 0.01 to 0.10%, more preferably 0.01 to 0.08%.
  • the range of the weight-based weight increase rate is preferably satisfied when the oxidation treatment temperature is 1300 ° C., and more preferably satisfied when the oxidation treatment temperature is 1400 ° C. in addition to the oxidation treatment temperature 1300 ° C.
  • the rate of weight increase due to the oxidation treatment may depend on the surface area of the composite ceramic to be measured. This is because the greater the surface area, the higher the probability of oxidation. Therefore, the ratio of weight increase calculated by subtracting the weight before oxidation treatment from the weight of the composite ceramic after oxidation treatment at 1300 ° C or 1400 ° C for 100 hours in the atmosphere and dividing it by the surface area before oxidation treatment (Hereinafter, this ratio is referred to as “surface area-based weight increase rate”) can also be used as a measure of oxidation resistance. A smaller increase rate means higher oxidation resistance.
  • this increasing rate is preferably a small value of 0.01 to 0.29 g / cm 2 , more preferably 0.01 to 0.15 g / cm 2 .
  • the range of the surface area-based weight increase rate is preferably satisfied when the oxidation treatment temperature is 1300 ° C., and is more preferably satisfied when the oxidation treatment temperature is 1400 ° C. in addition to the oxidation treatment temperature 1300 ° C.
  • the weight-based weight increase rate and the surface area-based weight increase rate are measured by the following methods.
  • This measurement method conforms to JIS R1609-1990.
  • a test piece of JIS R1601 is prepared, and the weight and surface area at 25 ° C. are measured.
  • a test piece is installed in the center soaking
  • composite ceramics are used.
  • the ratio of boron nitride to the whole needs to be within the above-mentioned range, and the silicate or oxynitride phase containing Y, Yb or Lu element is confirmed by X-ray diffraction, and the diffraction peak is the main.
  • a relative integral strength of 0.01 to 0.6 with respect to the crystal phase is preferable from the viewpoint of further improving the thermal shock resistance of the composite ceramic.
  • the present inventors consider that the inclusion of such a crystal phase in the composite ceramic increases the thermal conductivity of the composite ceramic and improves the thermal shock resistance of the composite ceramic.
  • the composite ceramic of the present invention As a grain boundary phase of ordinary silicon nitride ceramics, it is known that a low melting point oxide glass phase added as an auxiliary agent precipitates.
  • the high-temperature stability of the composite ceramic is ensured by precipitation of a silicate or oxynitride phase crystal phase containing a Y, Yb or Lu element which is a high melting point compound, It can be a composite ceramic having excellent heat conduction.
  • Y, Yb and Lu may be at least one of them, and it is particularly preferable to use an element having a small ionic radius among these from the viewpoint of further improving the high-temperature stability of the composite ceramic.
  • the thermal conductivity of the composite ceramic is further improved by the precipitation of the oxynitride phase out of the silicate phase and the oxynitride phase.
  • a silicate or oxynitride phase crystal phase containing Y, Yb or Lu elements for example, yttrium oxide, ytterbium oxide, lutetium oxide, silicon oxide, or the like is used as a raw material when producing a composite ceramic. Good.
  • Examples of the silicate phase containing Y, Yb, or Lu element include Y 2 Si 2 O 7 , Yb 2 Si 2 O 7, and Lu 2 Si 2 O 7 .
  • examples of the oxynitride phase containing Y, Yb, or Lu element include Y 2 Si 3 O 3 N 4 , Yb 4 Si 2 O 7 N 2, and Lu 4 Si 2 O 7 N 2 .
  • One or more kinds of crystal phases composed of these phases can be present in the composite ceramic. Whether a silicate phase or an oxynitride phase occurs in the composite ceramic depends on the ratio of each raw material used when manufacturing the composite ceramic, the firing temperature, the nitrogen partial pressure at the time of firing, and the like.
  • the crystal phase of the silicate phase or oxynitride phase containing the above elements has a diffraction peak with a relative integrated intensity of 0.01 to 0.6, particularly 0.3, relative to the main crystal phase, that is, the silicon nitride matrix. Preferably it is present to be .about.0.5. Thereby, the heat conduction of the composite ceramic can be further improved.
  • a method of manufacturing a composite ceramic by adding raw materials such as yttrium oxide, ytterbium oxide, or lutetium oxide in an element ratio of a target crystal phase may be employed.
  • the relative integrated intensity can be obtained by calculating the following equation using an X-ray diffraction pattern.
  • the integrated intensity of the X-ray diffraction pattern is for the main peak.
  • the main peak of silicon nitride is about 36 degrees.
  • the main peak of the oxynitride phase of Yb is about 29 degrees.
  • Relative integrated strength integrated strength of silicate phase or oxynitride phase / integrated strength of silicon nitride matrix
  • the silicate phase or oxynitride crystal phase containing the above elements is preferably present in the grain boundary phase of the silicon nitride-based ceramic matrix from the viewpoint of increasing the thermal conductivity of the composite ceramic and thus improving the thermal shock resistance. .
  • the presence of this crystalline phase at the grain boundary of the silicon nitride-based ceramic matrix makes the oxidation protective coating formed on the surface of the composite ceramic dense and prevents oxidation from proceeding inside the ceramic. Thus, a composite ceramic with high oxidation resistance can be obtained.
  • the presence of this crystal phase at the grain boundary of the parent phase can be confirmed by observation with a scanning electron microscope (SEM).
  • each raw material is mixed and molded so as to be uniformly dispersed and fired in a nitrogen atmosphere at 1700 ° C. or higher. .
  • the above-described silicate phase and oxynitride phase are preferably used, and combinations of Y 2 O 3 and Al 2 O 3 , combinations of Y 2 O 3 , MgO and TiO 2 are used. You can also. These auxiliaries contribute to improving the strength of the composite ceramic by liquid phase sintering.
  • the composite ceramic does not contain an Al element.
  • the source material containing Al element include the above-described Al 2 O 3 and AlN.
  • Such a substance has a function of greatly reducing the thermal conductivity by being dissolved in silicon nitride and scattering phonons, which is the main heat conduction mechanism of composite ceramics. This contributes to lowering the thermal shock resistance of the composite ceramic.
  • the composite ceramic does not contain an Al element.
  • the presence or absence of Al element in the composite ceramics can be confirmed by elemental analysis such as fluorescent X-ray analysis or ion emission spectroscopic analysis.
  • elemental analysis such as fluorescent X-ray analysis or ion emission spectroscopic analysis.
  • the composite ceramic of the present invention does not contain any Al element.
  • the content is a very small amount of 500 ppm or less in terms of Al atom, the Al element is inevitably mixed. .
  • the composite ceramic of the present invention may have fine pores.
  • pore sizes pore diameter
  • pores having a diameter of 1 to 10 ⁇ m are 1.5 vol. % Or less, especially 1.1 vol. % Or less, especially 0.7 vol.
  • pore content this value is referred to as “pore content”
  • ceramics having a large number of pores having a large pore diameter tend to decrease in strength.
  • a boron nitride raw material powder used in the production of composite ceramics may be of an appropriate size.
  • the distribution of the pore diameter and the pore content are measured by image analysis or the like from a microstructural photograph obtained by SEM observation of the mirror-polished surface of the composite ceramic.
  • the shape of the pores described above affects the performance of the composite ceramic. Further, as a result of the examination by the present inventors, the shape of the pores varies depending on the kind of the raw material powder of boron nitride which is a dispersed phase. More specifically, when t-BN is used as the raw material powder of boron nitride, substantially circular pores with low isotropicity are generated, whereas when h-BN is used as the raw material powder of boron nitride, the anisotropy is large. An elongated pore is formed. The composite ceramics having substantially circular pores improve the strength and thermal shock resistance of the composite ceramics compared to the composite ceramics having elongated pores.
  • the composite ceramic of the present invention has a good thermal conductivity, and its thermal conductivity is preferably 50 W / mK or more, particularly preferably 60 W / mK or more.
  • This thermal conductivity is a value measured by a laser flash method in accordance with JIS R1611.
  • a dispersed phase of boron nitride which is a material with good thermal conductivity, is present, or a silicate phase or an oxynitride phase containing Y, Yb or Lu element.
  • a crystal phase may be present in the grain boundary phase.
  • This manufacturing method includes a step of mixing, forming, and firing a silicon nitride-based ceramic raw material powder forming a parent phase and a boron nitride raw material powder forming a dispersed phase.
  • a silicon nitride-based ceramic raw material powder it is preferable to use a powder having an average particle size of about 0.2 to 1 ⁇ m measured using a laser diffraction type particle size distribution analyzer.
  • sintering aids such as yttrium oxide, ytterbium oxide, and lutetium oxide.
  • the ratio of the silicon nitride-based ceramic raw material powder to the boron nitride raw material powder in the raw material is preferably set to 92: 8 to 99: 1, particularly 96: 4 to 98: 2, expressed as a weight ratio.
  • These raw material powders are mixed to obtain a mixed powder, and this mixed powder is formed into a predetermined shape, for example, a plate shape or a rod shape.
  • a mixing system For example, the wet mixing using media, such as alcohol and water, is employable.
  • a ball mill or the like can be employed as the mixing device.
  • the molding apparatus for example, a uniaxial press molding machine, an isotropic pressure press (CIP) apparatus, a casting molding apparatus, or the like can be adopted.
  • the molded body formed into a predetermined shape is subjected to a firing process. Firing is generally performed in a nitrogen atmosphere. In this case, the nitrogen pressure is preferably about 4 to 10 atm.
  • the firing temperature is preferably about 1700 to 2000 ° C., particularly about 1750 to 1950 ° C.
  • the firing time at the maximum temperature is preferably about 2 to 30 hours, particularly about 6 to 12 hours.
  • the boron nitride raw material powder has a small crystallite size, specifically 40 nm or more and 48 nm or less, particularly 40 nm or more and 42 nm or less. Use of such boron nitride is preferable because boron nitride is more easily dispersed in the composite ceramic.
  • t-BN having a turbulent layer structure that can be confirmed by an X-ray diffraction method is preferably used as the above-mentioned boron nitride raw material powder. Since such t-BN has little shape anisotropy, boron nitride is easily dispersed uniformly in the composite ceramic. Such t-BN is also advantageous in that it promotes sintering. On the other hand, hexagonal boron nitride (h-BN) that has been conventionally used generally has a plate-like shape and therefore tends to hinder sintering. As a result, it is not easy to increase the strength of the composite ceramic.
  • h-BN hexagonal boron nitride
  • t-BN having the crystallite size described above is commercially available and is a commercially available material.
  • the composite ceramics produced by the above method utilizing the characteristics of high strength and excellent thermal shock resistance at room temperature, for example, cast members such as aluminum and magnesium, rotor members for stirring molten metal, protective tubes for heaters, etc. It is suitably used for applications.
  • Example 1 The raw material powder shown in Table 1 was mixed, and 150 wt% ethanol was blended with the mixed powder to form a slurry.
  • the average particle size of each raw material powder was in the range of 0.1 to 3 ⁇ m.
  • the obtained slurry was filled in a ball mill and mixed. After the mixing was completed, ethanol was removed by an evaporator and the mixed powder was dried. After forming the mixed powder by applying a pressure of 2 MPa using a uniaxial molding machine, a plate of 45 ⁇ 45 ⁇ 7 tmm was produced by CIP molding of 200 MPa. This plate was put in a baking furnace, heated to a maximum of 1850 ° C. in a 9 atmosphere nitrogen atmosphere (100% nitrogen gas), and held for 8 hours for baking. In this way, the intended silicon nitride based composite ceramic was obtained.
  • Example 2 The amount of Yb 2 O 3 raw material powder used in Example 1 was increased to 25 parts, and the amount of Si 3 N 4 raw material powder was reduced to 70 parts. Except for this, a composite ceramic was obtained in the same manner as in Example 1.
  • Example 3 The amount of Yb 2 O 3 raw material powder used in Example 1 was increased to 15 parts, and the amount of Si 3 N 4 raw material powder was reduced to 80 parts. Except for this, a composite ceramic was obtained in the same manner as in Example 1.
  • Example 4 The amount of the t-BN raw material powder used in Example 1 was increased to 5 parts. Except for this, a composite ceramic was obtained in the same manner as in Example 1.
  • Example 5 The amount of t-BN raw material powder used in Example 1 was increased to 10 parts. Except for this, a composite ceramic was obtained in the same manner as in Example 1.
  • Example 6 The t-BN raw material powder used in Example 3 had a crystallite size of 47.3 nm. Except for this, a composite ceramic was obtained in the same manner as in Example 3.
  • Example 7 Instead of the t-BN raw material powder used in Example 1, h-BN raw material powder (crystallite size 48.7 nm) was used. Except for this, a composite ceramic was obtained in the same manner as in Example 1.
  • Example 8 Instead of the t-BN raw material powder used in Example 2, h-BN raw material powder (crystallite size 48.7 nm) was used. Except for this, a composite ceramic was obtained in the same manner as in Example 2.
  • Example 9 A composite ceramic was obtained in the same manner as in Example 1 except that the raw material powder shown in Table 1 was used.
  • Example 10 The amount of the Si 3 N 4 raw material powder used in Example 9 was reduced to 85 parts, and the amount of the t-BN raw material powder was increased to 7 parts. Except for this, a composite ceramic was obtained in the same manner as in Example 9.
  • Example 1 The amount of t-BN raw material powder used in Example 3 was reduced to 1 part. Except for this, a composite ceramic was obtained in the same manner as in Example 3.
  • Comparative Example 2 The amount of the t-BN raw material powder used in Comparative Example 1 was increased to 10 parts, and the amount of the Yb 2 O 3 raw material powder was decreased to 10 parts. Except for this, a composite ceramic was obtained in the same manner as in Comparative Example 1.
  • Example 3 A composite ceramic was obtained in the same manner as in Example 1 except that the raw material powder shown in Table 1 was used.
  • Example 4 instead of the t-BN raw material powder used in Example 9, h-BN raw material powder (crystallite size 48.7 nm) was used. Except for this, a composite ceramic was obtained in the same manner as in Example 9.
  • Comparative Example 5 The amount of h-BN raw material powder used in Comparative Example 4 was increased to 5 parts. Except for this, a composite ceramic was obtained in the same manner as in Comparative Example 4.
  • a silicon nitride-based composite ceramic having high strength at both room temperature and high temperature and excellent in thermal shock resistance and oxidation resistance.

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Abstract

Cette invention concerne une céramique composite qui comprend une céramique à base de nitrure de silicium à titre de phase matricielle et, combinée à celle-ci, du nitrure de bore à titre de phase dispersée, la proportion du nitrure de bore étant de 2,5 à 10 % en vol. Quand la résistance à la flexion quatre points mesurée à 25°C selon JIS R1601 est exprimée par σi et que la résistance à la flexion quatre points mesurée après application d'un choc thermique par brusque refroidissement depuis 800°C ou plus par versage goutte-à-goutte dans une eau à 25°C par le procédé de versage goutte-à-goutte dans l'eau selon JIS R1615 est exprimée par σf, alors la valeur de σi est de 400 MPa ou plus et le rapport σf/oi est de 0,85 ou plus.
PCT/JP2010/052417 2009-03-31 2010-02-18 Céramique composite à base de nitrure de silicium et son procédé de production WO2010113555A1 (fr)

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CN105683129B (zh) * 2013-10-23 2018-03-06 株式会社东芝 氮化硅基板及使用其的氮化硅电路基板
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CN108002841B (zh) * 2017-03-30 2021-01-08 中国科学院金属研究所 六方氮化硼-镱硅氧氮陶瓷基复合材料及其原位制备方法
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