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XRD Results of Ca(NH2)2 (Calcium Amide) Patent Application Publication Sep

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XRD Results of Ca(NH2)2 (Calcium Amide) Patent Application Publication Sep US 20120225005Al (19) United States (12) Patent Application Publication (10) Pub. No.: US 2012/0225005 A1 Suzuki et al. (43) Pub. Date: Sep. 6, 2012 (54) METHOD FOR PRODUCING ALKALI METAL (30) Foreign Application Priority Data NITRIDE OR ALKALINE EARTH METAL NITRIDE Nov. 12, 2009 (JP) ............................... .. 2009-258801 Feb. 8,2010 2010-025135 __ _ _ Feb. 8, 2010 2010-025152 (75) Inventors: Shop Suzuki, Sakura-sh1 (JP); ' Apt 28’ 2010 2010403334 Kaluhiko T0k0y0da,Sakura-sh1 Aug. 24, 2010 2010-187114 (JP); Tsutomu Suzuki, Sakura-shi Aug. 24, 2010 (JP) ............................... .. 2010-187115 (JP) Publication Classi?cation (73) Asslgnee.- . TAIHEIYO CEMENT ( 51) Int. Cl. CORPORATION’ Tokyo (JP) C01B 21/06 (2006.01) (52) US. Cl. ...................................................... .. 423/409 (21) Appl. No.: 13/509,457 (57) ABSTRACT There is provided a method for e?iciently producing a high (22) PCT Filed; Nov, 11, 2010 purity alkali metal nitride or alkaline earth metal nitride by simple processes. (86) PCT No.: PCT/JP2010/070113 Speci?cally provided is a method for producing an alkali metal nitride, an alkaline earth metal nitride, or a composite § 371 (0X1), thereof, the method including thermally decomposing one or (2), (4) Date: May 11, 2012 more alkali metal amides or alkaline earth metal amides. Star’nng materlal (Ca(NHg)g) 40000 35000 30000 25000 I"\ m 5“ v 20000 4.5 5 l 5000 l 0000 5000 0 10 20 30 40 50 60 2 5 (” CuK Cf) XRD results of Ca(NH2)2 (calcium amide) Patent Application Publication Sep. 6, 2012 Sheet 1 0f 11 US 2012/0225005 A1 Figure 1 Starting material (cam-0);) T 40000 35000 { 30000 (cps) 25000 ' 20000 ' lnt 15000 7, 10000 5000 A‘ ‘I v 77L, 7 ,, 0‘, 10 20 a0 40 50 so 29 (” CuKa') XRD results of Ca(NH2)2 (calcium amide) Patent Application Publication Sep. 6, 2012 Sheet 2 0f 11 US 2012/0225005 A1 Figure 2 30000 25000 20000 (cps)Int. 15000 ' 10000 ‘ I ; 5000 30 40 29 km CuKll') Patent Application Publication Sep. 6, 2012 Sheet 3 0f 11 US 2012/0225005 A1 Figure 3 Boone-4"‘ snot-15h 00000 25000 20000 "M E ~55 3 15000 i 2 10000 5000 0 10 20 a0 40 50 so 29;‘ 00M) 29(' GuKu) goose-‘h 900'0-1 611 00000 25000 20000 '2 t; 15000 E 10000 1 ‘ 0000 o 26 ' 00K ) ( a 2 9 (' CuK?) r_ 100003-411 1300°C (only rising temperature) 40000 W I y . r , 55000 0083012, 60000 00000 50000 A 25000 A I‘ 1 g 3 40000 ' 1 320000 e l3 L‘ 00000 15000 ( 10000 ‘ 20000 5000 10000 D 0 10 20 so 40 50 00 w 20 30 w 50 60 29C Gum) 29c“ CuKt!) 1000”0—4h Ar gas (nus)Int 28 (' CuKcl) Patent Application Publication Sep. 6, 2012 Sheet 4 0f 11 US 2012/0225005 A1 Figure 4 0.05 "0.05 - —0.1 - ~0.15 - Weightreduction(%)rate | o N | 50 100 1 50 200 250 300 350 400 450 Temperature (°C) Patent Application Publication Sep. 6, 2012 Sheet 5 0f 11 US 2012/0225005 A1 Figure 5 0 0 Li3N (cps)Int. 1o 20 3o 40 50 60 29 (° CuKa') Patent Application Publication Sep. 6, 2012 Sheet 6 0f 11 US 2012/0225005 A1 Figure 6 lnt.(cps) 1O 20 30 40 2 6 (° CuKOl) Patent Application Publication Sep. 6, 2012 Sheet 7 0f 11 US 2012/0225005 A1 Figure '7 70000 60000 50000 (cps)Int. 40000 30000 20000 10000 10 20 30 40 50 60 2 9 (° CuK 0! ) Patent Application Publication Sep. 6, 2012 Sheet 8 0f 11 US 2012/0225005 A1 Figure 8 , 0Li3N la _ O. 3 +3 .5. _ _ Q 0 O W L_L_i l \ A 7 M" J 10 20 30 40 50 60 26(° CuKO!) Patent Application Publication Sep. 6, 2012 Sheet 9 0f 11 US 2012/0225005 A1 Figure 9 E 5 ‘ L' 2' ‘IO 30 50 10 20 30 40 5O 80 26 (' sum) 29 (‘ CuKG) Calcium amide Calcium nitride (cps)Int. (cps)Int. i0 20 no *0 m 30 _ 50 20 (' cm) 29( CuKa) Strontium amide Strontium nitride O lBa(NH2k [El MW . i . g a I r” - j ‘0 I O I C. 10 30 50 I0 3U 50 2M‘ CuKOt) 2H‘ cuux) Barium amide Barium nitride Patent Application Publication Sep. 6, 2012 Sheet 10 0f 11 US 2012/0225005 A1 Figure 10 1O 20 30 4O 5O 00 29 (‘ Cum!) XRD analysis results of CaSr amide Calcium nitn'de lni. Strontium nitride OaSrN 10 2D 3D 40 50 6D 28 (' GuKa) XRD analysis results of CaSrN Patent Application Publication Sep. 6, 2012 Sheet 11 0f 11 US 2012/0225005 A1 Figure 11 (cps)Int. 1o 20 30 4o 50 so 2 9 (' CuKO'.) XRD analysis results of BaSr amide Strontium g nitride Barium nitride BaSrN 10 20 3o 40 50 e0 2 9 (' cuKa) XRD analysis results of BaSrN US 2012/0225005 A1 Sep. 6, 2012 METHOD FOR PRODUCING ALKALI METAL [0011] [Non Patent Literature 4] “Muki Kagoubutsu NITRIDE OR ALKALINE EARTH METAL Sakutai Jiten (Dictionary of Inorganic Compounds and Com NITRIDE plexes)”, Masayoshi Nakahara, Kodansha Ltd., p. 476, 1997 SUMMARY OF INVENTION TECHNICAL FIELD Problem to be Solved by the Invention [0001] The present invention relates to a method for pro [0012] It is an object of the present invention to provide a ducing an alkali metal nitride and an alkaline earth metal method for simply producing a high-purity alkali metal nitride. nitride and alkaline earth metal nitride With good yield With out causing the above-mentioned problems. BACKGROUND ART Means for Solving the Problem [0002] In recent years, attention has been directed to an [0013] The present inventors have carried out diligent stud alkali metal nitride or an alkaline earth metal nitride as a ies in vieW of the above-mentioned circumstances. As a material such as a raW material of aluminum nitride used for result, the inventors have found that an easily available alkali a semiconductor device, a metal sliding member, an electrode metal amide or alkaline earth metal amide is used as a raW construction material and the like. A high-purity product is material, and the amide can merely be thermally decomposed required for the metal nitride used for the applications. to obtain a high-purity metal nitride With good yield, and [0003] Examples of a conventional method for producing completed the present invention. an alkali metal nitride and an alkaline earth metal nitride [0014] That is, the present invention provides a method for producing an alkali metal nitride, an alkaline earth metal include a method for heating alkaline earth metals such as nitride, or a composite thereof, the method including ther calcium in a nitrogen gas stream (Non Patent Literatures 1 mally decomposing one or more alkali metal amides or alka and 2). line earth metal amides. [0004] HoWever, this method nitrides only the surfaces of these metals, and has dif?culty in nitriding the inside thereof. Advantageous Effect of Invention Therefore, the metal nitride obtained by the method cannot be used for the above-mentioned application requiring a high [0015] The present invention can simply produce a high purity product. purity alkali metal nitride, alkaline earth metal nitride, and composite thereof With good yield. [0005] Another method is a method for heating calcium With ammonia, a problem of Which method is production of BRIEF DESCRIPTION OF DRAWINGS calcium hydride as a by-product (Non Patent Literature 3). Furthermore, yet another method is a method for heating [0016] FIG. 1 shoWs the XRD results of a starting material. tricalcium tetranitride to 250° C., problems of Which are [0017] FIG. 2 shoWs the XRD results of an alkaline earth explosiveness and toxicity (Non Patent Literature 4). metal nitride. [0006] Furthermore, there is disclosed a method for react [0018] FIG. 3 shoWs the XRD results of alkaline earth ing a molten Zinc-calcium alloy With a heated and pressurized metal nitrides obtained by various reaction conditions of nitrogen jet to synthesiZe calcium nitride (Patent Literature Example 1. 1). HoWever, this method requires a special device, and thus it [0019] FIG. 4 shoWs the TG/DTA measurement results of is di?icult to say that the method is an industrially advanta lithium amide. geous method. [0020] FIG. 5 shoWs the XRD results of lithium nitride obtained in Example 3. [0021] FIG. 6 shoWs the XRD results of lithium amide. PRIOR ART LITERATURE [0022] FIG. 7 shoWs the XRD results of lithium nitride obtained in Example 4. Patent Literature [0023] FIG. 8 shoWs the XRD results of lithium nitride obtained in Example 5. [0007] [Patent Literature 1] JP-A-2005-531483 [0024] FIG. 9 shoWs the XRD results of alkaline earth metal amides and alkaline earth metal nitrides obtained in Non Patent Literature Examples 6 to 8. [0025] FIG. 10 shoWs the XRD results of an alkaline earth [0008] [Non Patent Literature 1] “Kagaku Daijiten (Ency metal amide and an alkaline earth metal nitride obtained in clopedic Dictionary of Chemistry)”, ?rst edition, edited by Example 9. Michinori Oki et al., Tokyo Kagaku Dojin, ?rst edition, p. [0026] FIG. 11 shoWs the XRD results of an alkaline earth 1413, 1989 metal amide and an alkaline earth metal nitride obtained in [0009] [Non Patent Literature 2] “Shin Jikken Kagaku Example 10. KoZa 8, Muki Kagoubutsu no Gosei (I) (New Experimental Chemistry Course 8, Synthesis of Inorganic Compounds (I)) MODES FOR CARRYING OUT THE INVENTION ”, edited by the Chemical Society of Japan, MaruZen Co., [0027] RaW materials used for the present invention are one Ltd., p. 414, 1976, or more selected from alkali metal amides and alkaline earth [0010] [Non Patent Literature 3] “Kagaku Daijiten 5 (En metal amides.
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