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 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.

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Figure 1

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Figure 10

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Figure 11

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XRD analysis results of BaSr amide

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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 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 , 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. For example, (Li, Na, K)3N, (Be, Mg, Ca, Sr, cyclopaedia Chimica 5)”, miniature edition, Kyoritsu Shup Ba)3N2, and (Be, Mg, Ca, Sr, Ba)2N are preferable as alkali pan Co., Ltd., p. 880, 1987 metal nitrides and alkaline earth metal nitrides obtained. Of US 2012/0225005 A1 Sep. 6, 2012

these, one or more selected from Li3N, Ca3N2, Sr3N2, Ba3N2, in vieWs of a reactor and economical e?iciency. Therefore, Ca2N, Sr2N, and Ba2N are preferable. As a composite thereof, the temperature for thermally decomposing the metal amides a composite of tWo or more of the metal nitrides is a combi is preferably from 100 to 1500° C., and more preferably from nation of tWo or more of the above-mentioned alkali metal 300 to 1300° C. nitrides and alkaline earth metal nitrides. A combination of [0034] Particularly, the temperature for thermally decom tWo or more metals may be suitably determined for any pur posing the alkali metal amide in the present invention is pose. Examples of the combination include combinations of preferably 100° C. or more, more preferably 200° C. or more, calcium-strontium, calcium-barium, and strontium-barium. and still more preferably 300° C. or more. The upper limit of A content ratio of the tWo or more metals may be also suitably the temperature is preferably a temperature at Which the alkali determined for any purpose. For example, a molar ratio of the metal nitride is not decomposed. The loWer limit thereof is tWo metals is preferably from 1:99 to 99:1, more preferably preferably a temperature at Which lithium nitride is com from 1:20 to 20:1, and still more preferably 1:10 to 10:1. pletely produced. Therefore, the temperature for thermally [0028] An alkali metal amide as a raW material of the decomposing the alkali metal amide is preferably from 100 to present invention is a knoWn compound. The alkali metal 700° C., more preferably from 200 to 700° C., and particu amide can be produced by a knoWn method, for example, a larly preferably from 300 to 700° C. method for making ammonia act on an alkali metal at a high [0035] Furthermore, in the present invention, the tempera temperature (“Kagaku Daijiten (Encyclopaedia Chimica)”, ture for thermally decomposing the alkaline earth metal miniature edition, Kyoritsu Shuppan Co., Ltd., the para amide is preferably 510° C. or more, more preferably 800° C. graphs of sodium amide and potassium amide), and the like. or more, and still more preferably 1000° C. or more. The [0029] An alkaline earth metal amide as a raW material of upper limit of the temperature is a temperature at Which the the present invention is a knoWn compound used for a hydro alkaline earth metal nitride is not decomposed. HoWever, the gen storage material and the like. The alkaline earth metal upper limit is preferably 1500° C. or less in vieWs of a reactor amide can be produced by a knoWn method. Examples and economical e?iciency. Therefore, the temperature for thereof include a method for producing hexaammine calcium thermally decomposing the alkaline earth metal amide is (0) from a calcium metal and ammonia, and decomposing the preferably from 5 10 to 1500° C., more preferably from 800 to hexaammine calcium in the presence of a catalyst (“Kagaku 1300° C., and particularly preferably from 1000 to 1200° C. Daijiten (Encyclopaedia Chimica)”, miniature edition, [0036] Because the metal amide as a starting material is Kyoritsu Shuppan Co., Ltd., the paragraph of calcium amide), easily oxidiZed in the air, a reaction is preferably performed and a method for reacting a metal hydride With ammonia under vacuum, or under an inert gas such as nitrogen gas, (JP-A-2006-8440). helium gas, or argon gas. Particularly, the reaction is prefer [0030] The alkali metal amide or the alkaline earth metal ably performed under an inert gas such as nitrogen gas, amide used in the present invention can also be obtained by helium gas, or argon gas. When the reaction is performed the above-mentioned method. HoWever, means for reacting under a gas atmosphere, a pressure thereof is not particularly an alkali metal or alkaline earth metal amide With ammonia to limited. HoWever, the reaction is preferably performed at a form a liquid phase thereof, thereby obtaining the amide is normal as being economical. The reaction may be performed particularly preferably employed in vieW of producing a high in a batch or continuous system. In the case of mass produc purity alkali metal nitride or alkaline earth metal nitride. tion, the reaction is advantageously performed in the continu [0031] The amount of ammonia used is preferably 2 mol or ous system. more based on 1 mol of the alkali metal or the alkaline earth [0037] The reaction time may be suitably determined metal. Because ammonia is used also as a solvent, the more depending on the device, the reaction temperature, and the ammonia is more preferred. The reaction temperature of the amount of a raW material. Usually, the reaction time is pref alkali metal or the alkaline earth metal and ammonia may be erably from 10 minutes to 48 hours, more preferably from 1 suitably determined depending on the kind of the alkali metal hour to 24 hours, and particularly preferably from 3 hours to or the alkaline earth metal. The reaction temperature is pref 12 hours. erably from —77 to 300° C., more preferably from 20 to 200° [0038] The reaction device may be a device capable of C., and still more preferably from 50 to 100° C. Because the Withstanding a high temperature. For example, a tubular fur alkali metal or the alkaline earth metal and ammonia form a nace, an electric fumace, a batch kiln, and a rotary kiln may be liquid phase, a uniform alkali metal amide or alkaline earth used. metal amide is produced. Therefore, a reaction time is the [0039] Because only the target metal nitride or the compos time required to form a liquid phase. Usually, the reaction ite thereof remains in a poWdery state in the reaction device in time is preferably from 1 minute to 72 hours, and more the case of the batch system, for example, after completing preferably from about 1 hour to about 3 hours. the reaction, the metal nitride or the composite is extremely [0032] When the alkali metal amide or the alkaline earth easily collected. metal amide is produced by the method in the case Where the [0040] On the other hand, When the rotary kiln ?lled With, composite of tWo or more alkali metal nitrides or alkaline for example, N2, He, and Ar is used in the case of the con earth metal nitrides is obtained, the mixture of the raW mate tinuous system, the target metal nitride is easily and continu rials forrns a liquid phase. Thereby, the obtained composite ously collected. also becomes uniform. [0041] The alkali metal nitride and the alkaline earth metal [0033] In the present invention, a temperature for thermally nitride obtained by the method of the present invention have decomposing the alkali metal amide or the alkaline earth high purity because the thermal decomposition reaction eas metal amide is preferably 100° C. or more, and more prefer ily undergoes a reaction to the inside thereof. ably 300° C. or more. The upper limit of the temperature is a [0042] Because the alkali metal nitrides and alkaline earth temperature at Which the target metal nitride is not decom metal nitrides are uniformly dispersed in the various alkali posed. HoWever, the upper limit is preferably 1500° C. or less metal nitride composites and alkaline earth metal nitride US 2012/0225005 A1 Sep. 6, 2012

composites thus obtained, to produce little maldistribution, sis of the obtained compound Was performed, resulting that various applications can be expected. A solid solution of the the Whole of the phase Was Li3N (see FIG. 7). various alkali metal nitrides and alkaline earth metal nitrides may be formed depending on the combination of the alkaline Example 5 earth metals. NeW applications for the solid solution are expected. [0051] The same operation as that of Example 3 Was per formed using 3 g of lithium amide. A temperature Was 700° EXAMPLES C., and a reaction time Was 4 hours. The poWder XRD analy sis of the obtained compound Was performed, resulting that [0043] Hereinafter, the present invention Will be further the Whole of the phase Was Li3N (see FIG. 8). described in detail With reference to Examples. However, the present invention is not limited to these Examples. Example 6 Example 1 [0052] After 2.00 g of metal calcium Was placed in a 200 cc reaction container, and the reaction container Was ?lled With [0044] A producing test of an alkaline earth metal nitride 40 g of ammonia, the metal calcium is reacted With the ammo Was performed under conditions of a temperature and a time nia at 100° C. for 2 hours. The structure of product collected (h) as shoWn in FIG. 3. That is, 3 g of calcium amide Was after the reaction Was analyZed by XRD, resulting that the placed in a fumace core tube (an inner diameter of 50 mm and structure Was a single phase of calcium amide (FIG. 9). The a length of 600 mm) and the fumace core tube Was sealed With Weight of the collected calcium amide Was 3.58 g, and the a silicon cap in a glove box. The furnace core tube taken out yield thereof Was 99.6%. from the glove box Was set in a tubular furnace, and Was [0053] 2.00 g of the obtained calcium amide compound Was heated in a nitrogen atmosphere. Under the same conditions heated in a nitrogen atmosphere at 1000° C. for 4 hours. The as above except that 3 g of strontium amide Was placed in a structure of the reaction product Was analyZed by XRD, furnace core tube inplace of 3 g of calcium amide, the furnace resulting that the structure Was a single phase of calcium core tube Was heated. A temperature under an Ar gas atmo nitride (FIG. 9). The Weight of the obtained calcium nitride sphere Was 900° C., and a reaction time Was 6 hours. Was 1.37 g, and the yield thereofWas 99.8%. [0045] PoWder XRD analysis of the obtained compound Was performed. The results are shoWn in FIG. 3. For refer Example 7 ence, the XRD of the calcium amide as a raW material is shoWn in FIG. 1. The XRD of Ca3N2 is shoWn in FIG. 2. [0054] When 2.00 g of metal strontium Was used as a start [0046] The XRD results shoW that a target high-purity alka ing material in the same manner as Example 6, the structure of line earth metal nitride is produced at high yield by heating an amide compound after the reaction of the metal strontium from 500 to 1500° C. The XRD results also shoW that the and ammonia Was a single phase of strontium amide. The higher a reaction temperature is, the shorter the reaction time yield thereof Was 99.2% (FIG. 9). The product after the ther is. mal decomposition of the obtained strontium amide Was a single phase of strontium nitride. The yield thereof Was Example 2 99.5% (FIG. 9). [0047] The thermal decomposition temperature of lithium Example 8 amide Was measured using a thermogravimetric/ differential thermal analyZer (TG/DTA). The measurement Was per [0055] Furthermore, When 2.00 g of metal barium Was used formed under a nitrogen gas ?oW from room temperature to as a starting material in the same manner as Example 6, the 450° C. after a sample pan Was ?lled With 10 mg of lithium structure of an amide compound after the reaction of the metal amide. As shoWn in FIG. 4, the thermal decomposition start barium and ammonia Was a single phase of barium amide. temperature of the lithium amide Was 250° C. The yield thereof Was 99.7% (FIG. 9). The product after the thermal decomposition of the obtained barium amide Was a Example 3 single phase of barium nitride. The yield thereof Was 99.3% (FIG. 9). [0048] 3 g of lithium amide Was placed in a furnace core tube (an inner diameter of 50 mm and a length of 600 mm) and Example 9 the furnace core tube Was sealed With a silicon cap in a glove box. The fumace core tube taken out from the glove box Was [0056] 1.04 g of metal calcium and 2.23 g of metal stron set in a tubular furnace, and Was heated in a helium atmo tium Were Weighed, and Were placed in a pressure vessel (200 sphere. mL). The pressure vessel Was vacuumiZed. Then, 40 g of [0049] A temperature Was 300° C., and a reaction time Was ammonia Was placed therein, and the reaction Was performed 24 hours. The poWder XRD analysis of the obtained com at 100° C. for 2 hours. The mineral phase of the obtained pound Was performed, resulting that the Whole of the phase product after the reaction Was con?rmed by XRD, resulting Was lithium nitride (Li3N) (see FIG. 5). For reference, the that the mineral phase Was a mixed phase of calcium amide XRD of the lithium amide is shoWn in FIG. 6. and strontium amide (upper side in FIG. 10). The thermal decomposition reaction of the obtained product Was per Example 4 formed in a nitrogen atmosphere at 1000° C. for 4 hours. The mineral phase of the product thus obtained Was con?rmed [0050] The same operation as that of Example 3 Was per using XRD, and it Was con?rmed that the mineral phase Was formed using 3 g of lithium amide. A temperature Was 400° a single phase of the product. It Was con?rmed that a peak C., and a reaction time Was 5 hours. The poWder XRD analy position Was in the middle of calcium nitride and strontium US 2012/0225005 A1 Sep. 6, 2012

nitride (lower side in FIG. 10). This is presumed to be a solid amide is obtained by reacting at least one of an alkali metal solution of nitrides of calcium and strontium. and an alkaline earth metal With ammonia to form a liquid phase thereof. Example 10 7. The method according to claim 1, Wherein an alkali metal amide is thermally decomposed to form an alkali metal [0057] 0.68 g of metal strontium and 2.60 g of metal barium nitride. Were Weighed, and Were placed in a pressure Vessel (200 mL). 8. The method according to claim 7, Wherein the alkali The pressure Vessel Was VacuumiZed. Then, 40 g of ammonia metal amide is decomposed as a raW material. Was placed therein, and the reaction Was performed at 100° C. 9. The method according to claim 1, Wherein an alkaline for 2 hours. The mineral phase of the obtained product after earth metal amide is thermally decomposed to form an alka the reaction Was con?rmed by XRD, resulting that the min line earth metal nitride. eral phase Was a mixed phase of strontium amide and barium 10. The method according to claim 9, Wherein the alkaline amide (upper side in FIG. 11). The thermal decomposition earth metal amide is thermally decomposed as a raW material. reaction of the obtained product Was performed in a nitrogen 11. The method according to claim 2, Wherein a thermal atmosphere at 900° C. for 4 hours. The mineral phase of the decomposition temperature is from 100 to 15000 C. product thus obtained Was con?rmed using XRD, and it Was 12. The method according to claim 3, Wherein a thermal con?rmed that the mineral phase Was a single phase of the decomposition temperature is from 100 to 15000 C. product. It Was con?rmed that a peak position Was in the 13. The method according to claim 2, Wherein the thermal middle of strontium nitride and barium nitride (loWer side in decomposition occurs under Vacuum, or under nitrogen gas or FIG. 11). It is presumed that a solid solution of nitrides of an inert gas. strontium and barium Was produced. 14. The method according to claim 3, Wherein the thermal decomposition occurs under Vacuum, or under nitrogen gas or 1. A method for producing a metal nitride, the method an inert gas. comprising thermally decomposing at least one of an alkali 15. The method according to claim 2, Wherein the at least metal amide and an alkaline earth metal amide to form a metal one of the alkali metal amide and the alkaline earth metal nitride. amide is obtained by reacting at least one of an alkali metal 2. The method according to claim 1, Wherein the at least and an alkaline earth metal With ammonia to form a liquid one of the alkali metal amide and the alkaline earth metal phase thereof. amide is decomposed as a raW material. 16. The method according to claim 3, Wherein the at least 3. The method according to claim 1, Wherein at least tWo of one of the alkali metal amide and the alkaline earth metal the alkali metal amide and the alkaline earth metal amide are amide is obtained by reacting at least one of an alkali metal thermally decomposed, as raW materials, to form a composite and an alkaline earth metal With ammonia to form a liquid comprising at least tWo of an alkali metal nitride, an alkaline phase thereof. earth metal nitride, or a mixture thereof. 17. The method according to claim 7, Wherein the alkali 4. The method according to claim 1, Wherein a thermal metal amide is obtained by reacting an alkali metal With decomposition temperature is from 100 to 15000 C. ammonia to form a liquid phase thereof. 5. The method according to claim 1, Wherein the thermal 18. The method according to claim 9, Wherein the alkaline decomposition occurs under Vacuum, or under nitrogen gas or earth metal amide is obtained by reacting an alkaline earth an inert gas. metal With ammonia to form a liquid phase thereof. 6. The method according to claim 1, Wherein the at least one of the alkali metal amide and the alkaline earth metal * * * * *