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    • 21. 发明授权
    • High-strength porous silicon nitride body and process for producing the
same
    • 高强度多孔氮化硅体及其制造方法
    • US5780374A
    • 1998-07-14
    • US774612
    • 1996-12-30
    • Chihiro KawaiTakahiro MatsuuraAkira Yamakawa
    • Chihiro KawaiTakahiro MatsuuraAkira Yamakawa
    • C04B35/584C04B38/00C04B38/06
    • C04B38/00C04B38/06
    • A high-porosity and high-strength porous silicon nitride body comprises columnar silicon nitride grains and an oxide bond phase containing 2 to 15 wt. %, in terms of oxide based on silicon nitride, of at least one rare earth element, and has an SiO.sub.2 /(SiO.sub.2 +rare earth element oxide) weight ratio of 0.012 to 0.65 and an average pore size of at most 3.5 .mu.m. The porous silicon nitride body is produced by compacting comprising a silicon nitride powder, 2 to 15 wt. %, in terms of oxide based on silicon nitride, of at least one rare earth element, and an organic binder while controlling the oxygen content and carbon content of said compact; and sintering said compact in an atmosphere comprising nitrogen at 1,650.degree. to 2,200.degree. C. to obtain a porous body having a three-dimensionally entangled structure made up of columnar silicon nitride grains and an oxide bond phase, and having an SiO.sub.2 /(SiO.sub.2 +rare earth element oxide) weight ratio of 0.012 to 0.65.
    • 高孔隙率和高强度多孔氮化硅体包括柱状氮化硅颗粒和含有2至15wt。 至少一种稀土元素为基于氮化硅的氧化物的%,SiO 2 /(SiO 2 +稀土元素氧化物)的重量比为0.012〜0.65,平均孔径为3.5μm以下。 多孔氮化硅体通过压制而制成,其包含氮化硅粉末,2〜15重量% %,基于氮化硅的氧化物,至少一种稀土元素和有机粘合剂,同时控制所述成型体的氧含量和碳含量; 并在包含氮气的气氛中在1650℃-2200℃下烧结所述成型体,得到由柱状氮化硅晶粒和氧化物结合相构成的三维缠结结构的多孔体,并具有SiO 2 /(SiO 2 + 稀土元素氧化物)重量比为0.012〜0.65。
    • 22. 发明授权
    • Sintered body of silicon nitride and method of producing the same
    • 氮化硅烧结体及其制造方法
    • US5756411A
    • 1998-05-26
    • US696823
    • 1996-08-20
    • Seiji NakahataAkira YamakawaHisao Takeuchi
    • Seiji NakahataAkira YamakawaHisao Takeuchi
    • C04B35/591
    • C04B35/591
    • The invention reduces the time required for nitriding in the process of reaction sintering for production of a sintered body of silicon nitride, thereby improving productivity, and provides a sintered body of silicon nitride having sufficient compactness and high strength which can be produced by reaction sintering. The sintered body is Si.sub.3 N.sub.4 having an unpaired electron density of 10.sup.15 /cm.sup.3 to 10.sup.21 /cm.sup.3. The sintered body is produced through reaction sintering by using a Si powder having an unpaired electron density of 10.sup.15 -10.sup.20 /cm.sup.3, which is obtained by annealing a commercially available Si powder at temperatures of 300.degree. to 800.degree. C. in other than nitrogen atmosphere for 3-5 hours. In particular, the sintered body is produced by adding to the so obtained Si powder, together with a sintering assistant, an element having a valence of, particularly, from +1 to +3, the element having a covalent bond radius RM which bears such a relation with the covalent bond radius RSi of Si that (RM - RSi)/RSi
    • PCT No.PCT / JP95 / 02679 Sec。 371日期1996年8月20日 102(e)日期1996年8月20日PCT 1995年12月26日PCT公布。 WO96 / 20144 PCT出版物 日本1996年7月4日本发明减少了在制造氮化硅烧结体的反应烧结过程中氮化所需的时间,从而提高了生产率,并提供了具有足够的致密性和高强度的氮化硅烧结体,其可以是 通过反应烧结制备。 烧结体是不成对电子密度为1015 / cm 3至1021 / cm 3的Si 3 N 4。 通过使用不成对电子密度为1015〜1020 / cm 3的Si粉末,通过反应烧结制造烧结体,其通过在氮气气氛以外的温度下在300℃〜800℃下退火市售的Si粉末而得到 持续3-5小时。 特别地,通过将​​如此获得的Si粉末与烧结助剂一起加入具有共价键半径RM的元素(特别是从+1至+3的价数)特别是这样的元素制备烧结体 与RS的共价键半径RSi(RM-RSi)/ RSi <0.5的关系,或作为氮气发生剂的元素的化合物,并使所得复合材料进行反应烧结。
    • 23. 发明授权
    • Silicon nitride based sintered body
    • 氮化硅基烧结体
    • US5622905A
    • 1997-04-22
    • US269021
    • 1994-06-30
    • Takashi MatsuuraAkira YamakawaMasaya Miyake
    • Takashi MatsuuraAkira YamakawaMasaya Miyake
    • C04B35/584C04B35/64C04B35/587C04B35/599
    • C04B35/64C04B35/584
    • Discloses a silicon nitride based sintered body composed only of uniform, fine crystal grains, and improved in both strength and fracture toughness in the middle and low temperature ranges. A crystalline silicon nitride powder composed of crystal grains whose longer-axis diameter is not more than 200 nm or an amorphous silicon nitride powder is used as material powder. The silicon nitride powder is sintered at a temperature of 1200.degree. C. to 1400.degree. C. or sintered with a product of sintering temperature (.degree. C.) and sintering time (sec) below 600000 (.degree. C..multidot.sec) at a temperature of 1400.degree. C. to 1900.degree. C. Thus, a silicon nitride based sintered body in which the longer-axis diameter of silicon nitride and/or sialon crystals is not more than 200 nm is obtained.
    • 公开了仅由均匀的细晶粒组成的氮化硅基烧结体,并且在中低温范围内提高了强度和断裂韧性。 使用由长轴径不大于200nm的晶粒构成的结晶氮化硅粉末或非晶氮化硅粉末作为原料粉末。 氮化硅粉末在1200℃至1400℃的温度下烧结,或烧结温度(℃)和烧结时间(秒)低于600000℃(℃)的产物在温度为 1400℃〜1900℃。因此,得到氮化硅和/或赛隆晶体的长径比不大于200nm的氮化硅系烧结体。
    • 24. 发明授权
    • Aluminum nitride sintered body and method of producing the same
    • 氮化铝烧结体及其制造方法
    • US5482905A
    • 1996-01-09
    • US178642
    • 1994-01-05
    • Seiji NakahataTakahiro MatsuuraKouichi SogabeAkira Yamakawa
    • Seiji NakahataTakahiro MatsuuraKouichi SogabeAkira Yamakawa
    • C04B35/581C04B35/58
    • C04B35/581
    • An aluminum nitride sintered body comprising aluminum nitride crystals belonging to a Wurtzite hexagonal crystal system wherein the 3 axes a, b and c of the unit lattice of the crystal are defined such that the ratio b/a of the lengths of the axes b and a is 1.000 near the center of the crystal grain and lies within the range 0.997-1.003 in the vicinity of the grain boundary phase. Aluminum nitride sintered body is produced by sintering a molded body of a raw material powder having aluminum and nitrogen as its principal components at a temperature of 1700.degree.-1900.degree. C. in a non-oxidizing atmosphere having a partial pressure of carbon monoxide or carbon of not more than 200 ppm and then cooling the sintered body to 1500.degree. C. or a lower temperature at a rate of 5.degree. C./min or less. The aluminum nitride sintered body has a greatly improved thermal conductivity and, therefore, is suitable for heat slingers, substrates or the like for semiconductor devices.
    • 一种氮化铝烧结体,其包含属于纤锌矿六方晶系的氮化铝晶体,其中晶体的单位晶格的3轴a,b和c被定义为使得轴b和a的长度的比率b / a 在晶粒中心附近为1.000,位于晶界相附近的0.997-1.003范围内。 氮化铝烧结体通过在具有一氧化碳或碳分压的非氧化性气氛中,在1700〜1900℃的温度下烧结以铝和氮为主要成分的原料粉末的成型体 不超过200ppm,然后以5℃/分钟以下的速度将烧结体冷却至1500℃或更低温度。 氮化铝烧结体具有大大提高的导热性,因此适用于半导体器件的热引脚,基板等。
    • 25. 发明授权
    • Silicon nitride composite sintered body and process for producing the
same
    • 氮化硅复合烧结体及其制造方法
    • US5384292A
    • 1995-01-24
    • US220457
    • 1994-03-31
    • Jin-Joo MatsuiOsamu KomuraAkira YamakawaMasaya Miyake
    • Jin-Joo MatsuiOsamu KomuraAkira YamakawaMasaya Miyake
    • C04B35/584C04B35/58
    • C04B35/584
    • A silicon nitride composite sintered which comprises crystal grains of silicon nitride and/or sialon having an average minor axis length of 0.05 to 3 .mu.m and an aspect ratio of 10 or less and foreign particles dispersed in the crystal grains and/or the grain boundary phase, said particles having a thermal expansion coefficient of 5.times.10.sup.-6 /.degree.C. or more and an average particle size of 1 to 500 nm. The sintered body is produced by wet mixing silicon nitride powder, at least two sintering aids selected from among Y.sub.2 O.sub.3, Al.sub.2 O.sub.3, AlN and MgO and at least one compound selected from among the oxides, nitrides, carbides and silicides of the elements, excluding Si and C, of the groups IIa, IIIa, IVa, Va, VIa, IIb, IIIb and IVb of the Periodic Table to form a molding; and heat treating under the specified conditions. The sintered body can also be obtained by coating the surfaces of silicon nitride crystal grains with an organometallic compound convertible to the above foreign particles, heat treating and sintering with the sintering aid.
    • 一种氮化硅复合材料,其包含平均短轴长度为0.05〜3μm,长径比为10以下的氮化硅和/或赛隆的晶粒和分散在晶粒和/或晶界中的异物的氮化硅复合体 所述颗粒的热膨胀系数为5×10 -6 /℃以上,平均粒径为1〜500nm。 烧结体通过湿式混合氮化硅粉末,至少两种选自Y 2 O 3,Al 2 O 3,AlN和MgO的烧结助剂和选自元素的氧化物,氮化物,碳化物和硅化物中的至少一种化合物,除Si和 C,元素周期表IIa,IIIa,IVa,Va,VIa,IIb,IIIb和IVb族中的一种,形成一个成型体; 并在规定条件下进行热处理。 烧结体也可以通过用可转化为上述外来颗粒的有机金属化合物涂覆氮化硅晶粒表面,用烧结助剂进行热处理和烧结来获得。
    • 27. 发明授权
    • Silicon nitride sintered body and process for producing the same
    • 氮化硅烧结体及其制造方法
    • US5369065A
    • 1994-11-29
    • US118023
    • 1993-09-08
    • Masashi YoshimuraJin-Joo MatsuiTakehisa YamamotoAkira Yamakawa
    • Masashi YoshimuraJin-Joo MatsuiTakehisa YamamotoAkira Yamakawa
    • C04B35/584C04B35/593C04B35/58
    • C04B35/5935
    • A silicon sintered body comprising a matrix phase consisting of silicon nitride and a grain boundary phase in which the silicon nitride consists of 66 to 99% by volume of .beta.-Si.sub.3 N.sub.4 and/or .beta.'-sialon with the balance being .alpha.-Si.sub.3 N.sub.4 and/or .alpha.'-sialon, the .beta.-Si.sub.3 N.sub.4 and/or .beta.'-sialon consisting of hexagonal rod-like grains having a diameter of 500 nm or less in the minor axis and an aspect ratio 5 to 25, the .alpha.-Si.sub.3 N.sub.4 and/or .alpha.'-sialon consisting of equi-axed grains having an average diameter of 300 nm or less, and titanium compounds are contained within the grains of the matrix phase and in the grain boundary phase. The sintered body is produced by mixing (1) 100 parts by weight of .alpha.-Si.sub.3 N.sub.4 powder, (2) 0.1 to 10 parts by weight of titanium oxide having an average particle size of 100 nm or less and (3) 2 to 15 parts by weight, in total, of specified sintering aids; molding the resultant powder mixture into a green compact; subjecting the green compact to primary sintering and secondary sintering under the prescribed conditions.
    • 一种硅烧结体,包括由氮化硅和晶界相组成的基质相,其中氮化硅由66-99体积%的β-Si 3 N 4和/或β' - 赛隆组成,余量为α-Si 3 N 4和/ 或α' - 塞隆,β-Si 3 N 4和/或β'-Sialon由短轴具有500nm或更小直径的六角棒状晶粒和5至25的长宽比组成,α-Si 3 N 4和/ 或由平均直径为300nm以下的等轴晶粒组成的α'-Sialon,并且钛化合物包含在基质相的晶粒内和晶界相中。 烧结体通过混合(1)100重量份的α-Si 3 N 4粉末,(2)0.1〜10重量份的平均粒径为100nm以下的氧化钛和(3)2〜15重量份 总共为指定的烧结助剂; 将所得粉末混合物成型为生坯; 在规定的条件下对生坯进行一次烧结和二次烧结。
    • 29. 发明授权
    • Method of machining silicon nitride ceramics and silicon nitride
ceramics products
    • 氮化硅陶瓷和氮化硅陶瓷制品的加工方法
    • US5297365A
    • 1994-03-29
    • US921255
    • 1992-07-29
    • Takao NishiokaKenji MatsunumaAkira Yamakawa
    • Takao NishiokaKenji MatsunumaAkira Yamakawa
    • B24B1/00B24B7/22B24B19/22B24D3/00C04B35/584
    • B24B19/22B24B1/00
    • An industrially feasible method of grinding silicon nitride ceramics, is disclosed and provides a sufficiently smooth surface. Namely, the surface has a maximum height-roughness Rmax of 0.1 microns or less and a ten-point mean roughness Rz of 0.05 microns. Further, with this method, surface damage can be repaired while grinding. The vertical cutting feed rate of a grinding wheel into a workpiece should be within the range of 0.005-0.1 micron for each rotation of the working surface of the wheel and change linearly or stepwise. The cutting speed of the grinding wheel in a horizontal (rotational) direction should be within the range of 25 to 75 m/sec. With this arrangement, the contact pressure and grinding heat that is generated between the workpiece and the hard abrasive grains during grinding are combined. In other words, mechanical and thermal actions are combined.
    • 公开了一种工业上可行的研磨氮化硅陶瓷的方法,并提供了足够光滑的表面。 即,表面的最大高度粗糙度Rmax为0.1微米以下,十点平均粗糙度Rz为0.05微米。 此外,通过该方法,可以在磨削时修复表面损伤。 砂轮进入工件的垂直切削进给速率应在车轮工作表面的每次旋转时在0.005-0.1微米的范围内,并且线性或逐步改变。 砂轮在水平(旋转)方向上的切割速度应在25至75米/秒的范围内。 通过这种布置,在磨削期间在工件和硬磨粒之间产生的接触压力和磨削热被组合。 换句话说,组合了机械和热动作。