WO2006038489A1 - 導電性窒化ケイ素材料とその製造方法 - Google Patents
導電性窒化ケイ素材料とその製造方法 Download PDFInfo
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- WO2006038489A1 WO2006038489A1 PCT/JP2005/017701 JP2005017701W WO2006038489A1 WO 2006038489 A1 WO2006038489 A1 WO 2006038489A1 JP 2005017701 W JP2005017701 W JP 2005017701W WO 2006038489 A1 WO2006038489 A1 WO 2006038489A1
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- nitride
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/963—Surface properties, e.g. surface roughness
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
Definitions
- the present invention relates to a sintered carbon nitride body including a carbon nanotube (hereinafter referred to as “CNT”) having a conductive sintered body mainly composed of nitride nitride and a method for producing the same. .
- This silicon nitride sintered body can be applied to wear-resistant members and resistors.
- Cyanide nitride has attracted attention as an engineering ceramic because it has excellent characteristics such as heat resistance, high strength, wear resistance, and thermal shock resistance.
- various roll materials for bearing members, rolling, etc. It has been put to practical use in compressor vanes, turbo rotors and cutting tools.
- this silicon nitride is a hard-to-sinter material
- various additives mainly sintering aids, are used in the production of sintered bodies.
- a silicon nitride rare earth oxide acid-aluminum system a silicon nitride rare earth oxide acid aluminum, a oxalic acid titanium system, and the like are known.
- sintering aids such as rare earth oxides have strong grain boundary phases (glass phases) such as Si—R—Al—O—N compounds (R represents rare earth elements) during sintering. This is a component for increasing the strength by densifying the sintered body.
- TiB titanium diboride
- ZrB zirconium diboride
- Non-patent Document 1 There are also examples of adding carbon fibers (CNT) to the nitride nitride-rare earth oxide-acid-aluminum system, but densification is more difficult than using carbon powder (non-patent Reference 2, patent reference 1).
- CNT carbon fibers
- Patent Document 2 the addition of titanium oxide, hafnium oxide, zirconium oxide, etc. to the silicon nitride / rare earth oxide / monooxide / aluminum system improves wear resistance, and if necessary, aluminum nitride can be added. It is known that when added, the sinterability is significantly improved (Patent Document 2).
- Patent Document 1 US Published Patent 20040029706
- Patent Document 2 JP 2004-2067
- Non-patent literature 1 Cs. Balazsi et al., Manufacture ana examination of C / Si3N4 nanoco mposites ", Journal of the European Ceramic Society 2004, vol. 24, p3287-3294
- Non-patent literature 2 Material Science and Engineering C23 (2003 ) 1133-1137
- An object of the present invention is to provide a silicon nitride sintered body having conductivity and denseness. That is, carbon nitride as a conductor in a nitride-rare earth oxide-acid-aluminum system, a nitride-rare earth oxide magnesia system, or a nitride-rare earth oxide magnesia acid aluminum system.
- a dense nitrided nitride sintered body is provided by adding nanotubes to provide conductivity.
- CNTs carbon nanotubes
- the present inventors promoted densification by adding titanium oxide and the like, and by further adding aluminum nitride to further promote densification, even if CNT is added to this system, It has been found that densification can be achieved more easily, and a nitrided silicon sintered body having conductivity and excellent mechanical properties (bending strength, toughness, wear resistance, etc.) can be obtained.
- the present invention provides a titanium nitride / rare earth acid / monoacid / aluminum system or a silicon nitride / rare earth acid / ceramic / magnesia system. ⁇ Hafnium
- nitrided silicon-based sintered body here consists of nitrided nitride crystal grains (with some Al and O in solid solution) and a grain boundary phase. In other words, in addition to the above-mentioned manufacturing method, anything that can be such a structure is allowed.
- CNT reacts with contacted or nearby silicon nitride, etc., depending on the firing time at high temperature to produce carbide (SiC).
- SiC carbide
- carbon carbide is produced along with the nanotubes, so that it can function sufficiently as a conductor excellent in heat resistance and corrosion resistance.
- the present invention provides (1) 0.5 to 10% by weight of the rare earth compound in terms of oxide, (2) 0.1 to 5% by weight of aluminum oxide or a precursor thereof, and (3) Aluminum nitride is 0 to 5% by weight, and (4 1) Titanium group element oxide or titanium group element compound that becomes a nitride of titanium group element by firing is 0.1 mol in terms of equimolar titanium nitride.
- the silicon nitride sintered body comprises 0.2 to 5% by weight of titanium group nitride particles having an average particle size of 1.0 ⁇ m or less, Si—R—Al—O. — 2 to 20% by weight of grain boundary phase mainly containing N compound (R represents rare earth element), the remaining amount of nitride nitride, and 0.3 to 12% by weight of CNT as an outer shell.
- a nitrided silicon sintered body containing 0.3 to 12% by weight of CNT as an outer shell.
- the present invention relates to (1) 0.5 to 10% by weight of the rare earth compound in terms of oxide, (2) 0.1 to 5% by weight of aluminum oxide or a precursor thereof, and (3) Aluminum nitride is 0 to 5% by weight, and (4 1) Titanium group element compound that becomes an oxide of titanium group element with an average particle size of 1.0 m or less or becomes nitride of titanium group element by firing.
- a mixture comprising a nitrided nitride powder having a content of 1.7% by weight or less, an ⁇ -phase type nitride nitride of 90% by weight or more and an average particle size of 1.0 m or less, further comprising (6) CNT
- a method for producing a nitrided nitride sintered body comprising a step of forming a mixture containing 0.3 to 12% by weight into a desired shape by decoating and degreasing, and a step of sintering the formed body at 1600 to 1900 ° C. .
- the silicon nitride sintered body of the present invention is conductive because it contains CNTs, and has a high density because denseness is ensured despite the inclusion of CNTs. Therefore, the wear-resistant member made of such a nitrided silicon sintered body is electrically conductive, so it does not generate static electricity during use and does not adhere fine powder, and has high wear resistance. Can have the following characteristics:
- the silicon nitride sintered body of the present invention comprises (1) 0.5 to 10% by weight of the rare earth compound in terms of oxide, (2) 0.1 to 5% by weight of oxalic aluminum or its precursor, and ( 3) Aluminum nitride is 0 to 5% by weight, and (4 1) Titanium element oxide or titanium group element compound that becomes nitride of titanium element by firing is equimolar in terms of titanium nitride. 1 to 5% by weight, or (4 2) magnesium oxide 0.1 to 5% by weight, the balance being (5) oxygen content 1. a mixture of 7% by weight or less of a-phase type nitride nitride and 90% by weight or more of an average particle size of 1. O / zm or less of nitrided nitride powder, and (6) CNT coating And is formed by sintering a mixture containing 0.3 to 12% by weight.
- the raw material nitride nitride includes an ⁇ -phase type and a j8-phase type, and either may be used, but an ⁇ -phase content of 45% or more is suitable.
- the silicon nitride raw material powder preferably has an average particle size of 1.0 m or less and an oxygen content of 1.7% by weight or less.
- the average particle diameter of the silicon nitride raw material powder is more preferably in the range of 0.4 to 0.8 m.
- the oxygen content is more preferably in the range of 0.5 to 1.5% by weight.
- the content of silicon nitride in the sintered body obtained using such a raw material is usually 75 to 97% by weight, preferably 80 to 95% by weight.
- the amount of sintering aid increases with respect to the silicon nitride, and the properties of the sintered body, such as bending strength, fracture toughness, and wear characteristics, tend to decrease.
- the content of the nitride nitride is large, the amount of the sintering aid is relatively small, so that the densification is insufficient.
- the rare earth compound is not particularly limited, but yttrium, lanthanum (La), cerium (Ce), samarium (Sm), neodymium (Nd), dysprosium (Dy), erbium (Er), etc. Of these, at least one of the following oxides, nitrides, borides, carbides and silicas is preferred.
- Si—R—Al—O—N compound (R represents a rare earth compound), Si—R—Mg—A1 O—N compound, or Si—R—Mg—O—N compound (R Represents a rare earth compound.)
- an oxide such as Y, Ce, Sm, Nd, and Er.
- the aluminum oxide precursors thereof, such as transition alumina or carbonate, may be used. These aluminum compounds easily form a Si—R—Al—O—N compound (R represents a rare earth compound) during sintering.
- a grain boundary phase mainly composed of Si—R—Al—O—N compound (R represents a rare earth compound) is easily formed.
- a grain boundary phase mainly composed of Si—R—Mg—Al—O—N compound (R represents a rare earth compound) is easily formed. Is done.
- the amount of rare earth compound and aluminum compound (including aluminum oxide and aluminum nitride) added to the Si—R—Al—O—N compound (R is The rare earth compound is not particularly limited as long as the amount of the grain boundary phase mainly composed of) is in the range of 2 to 20% by weight, but the rare earth compound is converted to an oxide of 0.5 to 10%.
- the aluminum compound is preferably added in the range of 0.1% by weight to 0.1% by weight.
- the amount of aluminum nitride added is preferably 7% by weight or less, more preferably 0 to 5% by weight, and still more preferably 0.5 to 5% by weight.
- the amount of added force of acid aluminum is 0.1 to 5% by weight.
- a grain boundary phase composed of a Si—R—Al—O—N compound (R represents a rare earth element) is easily formed.
- acid-aluminum and / or aluminum nitride may be used if necessary.
- Si-R-Mg-Al-O-N compounds Or, a grain boundary phase composed of a Si-R-Mg-O-N compound (R represents a rare earth element) is easily formed.
- the silicon nitride sintered body of the present invention includes Si—R—A1—0—N compound (R represents a rare earth element), Si—R—Mg—O—N compound, or Si— It contains 2 to 20% by weight, preferably 5 to 15% by weight, of a grain boundary phase mainly containing an R—Mg—Al-0—N compound (R represents a rare earth element). If the content of the grain boundary phase is less than 2% by weight, the sintered silicon nitride will not be sufficiently densified, and the porosity will increase and the bending strength and fracture toughness will decrease.
- the content of the grain boundary phase exceeds 20% by weight, the bending strength, fracture toughness of the silicon nitride sintered body, rolling life when used for sliding members, and the like are reduced due to excessive grain boundary phase.
- the grain boundary phase can be measured with an X-ray microanalyzer (EPMA). The amount is converted to cross-sectional area force.
- Titanium, hafnium, and zirconium are listed as titanium group elements. These may be used as oxides or as carbonates or nitrates that change to acid during the firing process. These enhance the sinterability and do not reduce the properties of the nitrided silicon sintered body. These become nitrides of titanium group elements by firing.
- titanium oxide particularly promotes densification during the sintering process, and finally changes to titanium nitride, which precipitates as spherical particles at the grain boundaries and improves the sliding characteristics.
- TiO may be in the form of rutile or anatase, but if it is strong,
- the effect is larger in the tase type.
- a fine powder having an average particle size of 1.0 m or less.
- the amount of loading of titanium element acid is about 0.1% depending on the amount of CNT loading and purpose of use.
- the silicon nitride sintered body of the present invention may contain components other than those described above.
- an oxide such as tungsten (W), nitride, boride, silicide or silica may be included for further densification of the nitrided silicon sintered body.
- the total content of these compounds is preferably in the range of 0.1 to 5% by weight.
- CNT carbon nanotubes
- US Patent No. 4663230 US Patent No. 4663230, US Patent No. 5165909, US Patent No. 5171560, US Patent No. 5578543, US Patent No.
- This is a carbon-based fiber with a hollow structure described in No. etc. and having few branches.
- the size of the CNT is usually 0.4 to 200 nm in diameter and 1 to long axis: L000 ⁇ m, preferably 20 nm in diameter and 100 to 500 ⁇ m in long axis.
- the added amount is 0.3 to 12% by weight, preferably 1.2 to 4.2% by weight (ie, based on the weight of the silicon nitride sintered body containing no CNT).
- the conductivity can be controlled according to the amount. If the amount of CNTs is small, the sinterability is good. The conductivity is as low as 10 _1 ⁇ _ 1 m _ 1 or less. On the other hand, if the amount of CNTs is large, the sinterability decreases.
- Baked Conductivity of the sintered body by adjusting the content of CNT depending on the application, for example, can be set in the range of 10- 1 ⁇ 10 4 ⁇ one 1 m _1.
- the manufacturing method is not particularly limited, but is usually based on the following process.
- the composition is Si N (85-97 weight 0 /.) -YO (0.5-10 weight 0 /.)— Al 2 O (0.1
- the molded body produced as described above is degreased to produce a degreased molded body.
- the degreased compact is sintered at 1600 to 1900 ° C, preferably 1750 to 1850 ° C to obtain a nitrided silicon sintered body. If this temperature is low, densification is difficult to proceed, and if it is too high, decomposition of the nitride nitride tends to occur.
- Hot isostatic press hot isostatic press
- Various sintering methods such as sintering can be applied.
- the obtained nitrided silicon sintered body is 30 MPa or more. It is preferable to perform a hot isostatic pressing (HIP) treatment at 1600 to 1850 ° C in a non-acidic atmosphere.
- HIP hot isostatic pressing
- CNT exists mainly in the vicinity of the grain boundary, its aspect ratio is 500 to 10,000, and its content is in the range of 0.3 to 12% by mass.
- This silicon nitride sintered body has a porosity of 1.5% by mass or less and a maximum pore diameter of 2 m or less.
- the three-point bending strength of this silicon nitride sintered body is 600 MPa or more, and the fracture toughness value is 5 MPa'm 1/2 or more.
- Y O (yttrium oxide) powder manufactured by Shin-Etsu Chemical Co., Ltd. with an average particle size of 0.
- O / z m was weighed on an external weight of 5% by weight.
- 1.8 wt% of CNTs were weighed with these outer coats. These were wet-mixed for 96 hours in ethyl alcohol using silicon nitride balls and then dried to prepare a raw material mixture.
- a predetermined amount of an organic binder was added to the obtained raw material mixture to prepare a blended granulated powder, which was then press-molded at a molding pressure of 50MPa, and a sample for measuring bending strength was 15mm in diameter x 5mm in thickness and 25mm in diameter A number of disk shaped products with a thickness of 5 mm were produced.
- the compact was subjected to degreasing, heat treatment (holding treatment), sintering, and HIP treatment under the same conditions as above to obtain a dense sintered body.
- the sintered body after the HIP treatment is ground into a ball with a diameter of 9.52 mm and a surface roughness force a of 0.01 ⁇ m, which is used as a bearing ball.
- a member was prepared.
- the surface roughness (Ra) was 0.004 / z m. Ra is the average roughness of the center line obtained by measuring the equator of the ball with a stylus type surface roughness tester.
- a raw material mixture was prepared by blending so as to have the composition ratio shown in the following table (Table 1), and a nitrided silicon sintered body was produced in the same manner as in Example 1. Detailed firing conditions are noted in the table notes.
- Example 1 a nitrided nitride sintered body was produced under the same conditions as in Example 1 except that CNT was used as V, and a nitrided nitride ball was similarly produced.
- Example 2 a sintered nitride nitride was produced under the same conditions as in Example 1 except that 13% by weight of CNT was added.
- Example 3 a sintered silicon nitride body was produced under the same conditions as in Example 1 except that titanium oxide and aluminum nitride were not added.
- Table 1 shows the compositions and properties of the respective nitrided silicon sintered bodies according to the examples and comparative examples thus obtained.
- Example 1 92 5 (Y 2 0 3 ) 3 5 (Ti0 2 ) 5 1, 8 1 99.7 1100 6.2 15
- Example 2 92 5 (Y 2 0 3 ) 3 5 (Ti0 2 ) 5 1.8 2 98.5 950 5.9
- Example 3 92 5 CY 2 0 3 ) 3 5 (Ti0 2 ) 5 1,0 1 99.8 1070 6.3 5
- Example 4 92 5 (Y 2 0 3 ) 3 5 (Ti0 2 ) 5 1,0 2 98.8 980 6.3 3
- Example 6 91 6 CY 2 0 3 ) 3 5 (Ti0 2 ) 5 5.0 3 99.8 1150 6.3 11
- Example 7 91 6 (Y z 0 3 ) 3 5 (Ti0 2 ) 5 8.0 4
- R represents a rare earth element
- R ' represents a titanium group element
- R'0 and AIN represents the weight of Si N R 0 and Al 0 with respect to the total weight of 100, C
- the amount of NT represents the weight based on the total weight of Si N R 0 Al 0 R′O and AIN of 100.
- composition contains lwt% of MgO.
- Comparative Example 2 showed electrical conductivity, but it was insufficiently densified, had low fracture toughness and bending strength, and was unable to obtain the desired wear resistance.
- Fig. 3 shows a scanning electron micrograph of the sintered silicon nitride obtained in Comparative Example 1. It can be seen that CNT disappears.
- Example 1 the nitride nitride balls obtained in Example 1 and Comparative Example 2 were used as a counterpart material in accordance with JIS G-4805 using a thrust type rolling S wear test device.
- load is 5.9 GPa at maximum contact stress per ball
- rotation speed is 1 200 rpm
- turbine nitride ball surface is peeled off under oil bath lubrication conditions of turbine oil
- the rolling life (time) until it was measured was measured.
- the conductivity was 10 Q _1 m _ 1 (Example 1) and l X 10 _4 Q _1 m _ 1 or less (Comparative Example 1), respectively.
- the grain boundary phase is based on Si—R—Al—O—N compound (R is a rare earth compound), and some other additives are used. When added, the presence of corresponding compounds was observed. For example, when a compound containing titanium or hafnium is added, after sintering, TiO ⁇ TiN, HfO ⁇ HfN (0 solid solution) or HfO (Si, Y solid solution).
- Sue (Ube Industries, Ltd. 10—10) 92% by weight with an average particle size of 0.9 111 as a sintering aid
- the grain boundary phase in this sintered silicon nitride was observed with an X-ray microanalyzer (manufactured by Enomoto Electronics Co., Ltd.).
- the Si—Y—Mg—A1—O—N compound was the main component and its proportion was about 13% by weight.
- Raw material nitride nitride powder used in Example 19 magnesium oxide powder, Al 2 O powder, A
- R represents a rare earth element
- the amount of A1N and MgO represents the weight with respect to the total weight 100 of Si N, RO and Al O
- the amount of CNT is the total weight of Si N, RO, Al O, MgO and A1N.
- the silicon nitride sintered body of the present invention has excellent conductivity.
- a scanning electron micrograph (JEOL Co., Ltd. TSM-5200, secondary electron image) of the silicon nitride sintered body obtained in Example 19, the CNTs were surrounded by the grain boundary phase. It is recognized that it exists.
- a nitrided nitride sintered body was produced under the same conditions as in Example 19 except that CNT was not used, and similarly a nitrided nitride ball was produced.
- CNT was not used
- a nitrided nitride ball was produced.
- FIG. 1 is a view showing a scanning electron micrograph of a sintered silicon nitride (Example 1).
- FIG. 2 The same diagram as FIG. Arrow indicates CNT.
- FIG. 3 is a view showing a scanning electron micrograph of a sintered silicon nitride (Comparative Example 1).
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EP2323959A1 (en) * | 2008-08-29 | 2011-05-25 | Aktiebolaget SKF | Large ceramic component and method of manufacture |
US8741797B2 (en) * | 2011-09-30 | 2014-06-03 | Saint-Gobain Ceramics & Plastics, Inc. | Composite body including a nitride material, a carbide material, and an amorphous phase material |
EP2869666B1 (en) * | 2012-06-29 | 2017-03-29 | Kyocera Corporation | Heater and glow plug equipped with same |
US9440887B2 (en) * | 2012-10-30 | 2016-09-13 | Kabushiki Kaisha Toshiba | Silicon nitride sintered body and wear resistant member using the same |
WO2014200014A1 (ja) * | 2013-06-13 | 2014-12-18 | 株式会社東芝 | 窒化珪素製耐摩耗性部材および窒化珪素焼結体の製造方法 |
KR102243956B1 (ko) | 2014-01-31 | 2021-04-22 | 어플라이드 머티어리얼스, 인코포레이티드 | 챔버 코팅들 |
US10059595B1 (en) * | 2014-09-17 | 2018-08-28 | Neil Farbstein | Ultra high strength nanomaterials and methods of manufacture |
RU2610744C1 (ru) * | 2015-12-22 | 2017-02-15 | Открытое акционерное общество "Композит" (ОАО "Композит") | Шихта на основе нитрида кремния и способ изготовления изделий из нее |
CN113461425A (zh) * | 2021-07-28 | 2021-10-01 | 福建臻璟新材料科技有限公司 | 一种高导热高强度氮化物陶瓷基板的制作方法 |
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