TWI471266B - Method for manufacturing carbide fine particles - Google Patents
Method for manufacturing carbide fine particles Download PDFInfo
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- TWI471266B TWI471266B TW99131463A TW99131463A TWI471266B TW I471266 B TWI471266 B TW I471266B TW 99131463 A TW99131463 A TW 99131463A TW 99131463 A TW99131463 A TW 99131463A TW I471266 B TWI471266 B TW I471266B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
Description
本發明係有關一種奈米尺寸之碳化物微粒子之製造方法，特別是於原料中使用金屬氧化物，製造奈米尺寸之碳化物微粒子的方法。The present invention relates to a method for producing a nano-sized carbide fine particle, and more particularly to a method of producing a nano-sized carbide fine particle by using a metal oxide in a raw material.
現在，氧化物微粒子、氮化物微粒子、碳化物微粒子等之微粒子係被使用於製造半導體基板、印刷基板、各種電性絕緣零件等之電性絕緣材料、切削工具、塑模、軸承等之高硬度高精度之機械工作材料、粒界電容器、濕度感應器等之機能性材料、精密燒結成形材料等之燒結體、製造引擎閥等之要求高溫耐摩擦性材料等之溶射零件，以及燃料電池之電極、電解質材料及各種觸媒等領域。藉由使用該微粒子，可提高燒結體及照射零件等之不同種陶瓷間或不同種金屬間之接合強度及緻密性與機能性。At present, fine particles such as oxide fine particles, nitride fine particles, and carbide fine particles are used for manufacturing high hardness such as electrical insulating materials such as semiconductor substrates, printed boards, and various electrical insulating parts, cutting tools, molds, and bearings. High-precision mechanical working materials, functional materials such as grain boundary capacitors and humidity sensors, sintered bodies such as precision sintered molding materials, and molten parts requiring high-temperature and friction-resistant materials such as engine valves, and electrodes of fuel cells , electrolyte materials and various catalysts and other fields. By using the fine particles, it is possible to improve the joint strength, compactness, and functionality between the different kinds of ceramics such as the sintered body and the irradiated parts or between different kinds of metals.
製造該微粒子的方法之一，為氣相法。氣相法係有使各種氣體等在高溫下進行化學反應的化學方法，與照射電子束或雷射等之束，使物質分解‧蒸發以生成微粒子的物理方法。One of the methods for producing the fine particles is a gas phase method. The gas phase method includes a chemical method in which various gases and the like are chemically reacted at a high temperature, and a physical method in which a beam of electron beams or a laser is irradiated to decompose the material and evaporate to generate fine particles.
上述氣相法中之一種為熱電漿法。熱電漿法係在熱電漿中使原材料瞬間蒸發後，予以急冷凝固，製造微粒子的方法，另外，為於純化時生產性高，在高溫下熱容量大時，高熔點材料亦可對應，與其他的氣相法相比時，大多數具有較為容易複合化的優點。因此，熱電漿法可積極利用作為製造微粒子的方法。One of the above vapor phase methods is a thermoelectric plasma method. The pyroelectric method is a method in which a raw material is instantaneously evaporated in a thermo-plasma, and is rapidly solidified to produce fine particles. In addition, the product has high productivity in purification, and when the heat capacity is high at a high temperature, the high-melting material can also correspond, and other materials. Most of them have the advantage of being easier to composite when compared with the gas phase method. Therefore, the pyroelectric method can be actively utilized as a method of manufacturing fine particles.
使用習知的熱電漿法之微粒子的製造方法，係藉由使原材料物質形成粉末狀，且使該經粉末狀的原材料(粉末原材料、粉體)與載負氣體等同時被分散，直接投入熱電漿中，製造微粒子。In the method for producing fine particles by a conventional thermo-plasma method, the raw material is formed into a powder, and the powdery raw material (powder material, powder) and the carrier gas are simultaneously dispersed, and the thermoelectric power is directly input. In the slurry, fine particles are produced.
而且，於專利文獻1中記載，藉由於可燃性材料中分散有微粒子製造用材料之漿料、或使用微粒子製造用材料與分散媒與可燃性材料之漿料予以液滴化，導入熱電漿焰中，形成氣相狀態之混合物，且使氣相狀態之混合物急冷，生成微粒子之微粒子的製造方法。Further, Patent Document 1 discloses that a slurry of a material for producing fine particles is dispersed in a combustible material, or a slurry of a material for producing fine particles and a slurry of a dispersing medium and a combustible material is dropletized, and a pyroelectric flame is introduced. In the middle, a mixture of gas phase states is formed, and a mixture of the gas phase states is rapidly cooled to produce a microparticle fine particle.
[習知技術文獻][Practical Technical Literature]
[專利文獻][Patent Literature]
[專利文獻1]日本特開2006-102737號公報[Patent Document 1] Japanese Patent Laid-Open Publication No. 2006-102737
然而，於專利文獻1中沒有具體地揭示有關碳化物微粒子之製造方法。由於碳化物之硬度高，不易使該物粉碎，製造碳化物微粒子。而且，由於氮化物之熔點高，大多數超過3000K，故以氣相法製造碳化物微粒子時，無法使用碳化物作為原料。However, Patent Document 1 does not specifically disclose a method of manufacturing a carbide fine particle. Since the hardness of the carbide is high, it is difficult to pulverize the material to produce carbide fine particles. Further, since the melting point of the nitride is high and most of them exceed 3000 K, when carbide fine particles are produced by a vapor phase method, carbide cannot be used as a raw material.
使用金屬製造碳化物微粒子等之微粒子時，為更為促進蒸發時，在金屬原料中使用微粒者，視物質而定會有爆發的可能性，有處理上的問題。When a fine particle such as a carbide fine particle is produced by using a metal, in order to promote the evaporation more, when a fine particle is used in the metal raw material, there is a possibility that the material may be erupted depending on the substance, and there is a problem in handling.
而且，亦有進行檢討使用溶液原料之金屬烷氧化物，惟就原料高價、不安定而言，於工業上使用時會有處理上的問題。Further, there has been a review of metal alkoxides using a raw material of a solution, but there are problems in handling when industrially used, because of high price and instability.
此外，揭示有使用甲烷等之氣體作為碳化處理時之碳源的方法、或在金屬中混合碳粒子者作為原料的方法，惟皆沒有進行檢討在原料中使用氧化物。Further, a method of using a gas such as methane as a carbon source in the carbonization treatment or a method of mixing carbon particles in a metal as a raw material has been disclosed, but the use of an oxide in a raw material has not been examined.
目前有關由氧化物製造碳化物微粒子之製造方法，沒有具體的方法。There is currently no specific method for producing a method for producing carbide fine particles from an oxide.
本發明之目的，係以上述習知技術為基準，解決問題且提供在原料中使用金屬氧化物，製造奈米尺寸之碳化物微粒子的製造方法。An object of the present invention is to provide a method for producing a nano-sized carbide fine particle by using a metal oxide in a raw material based on the above-mentioned conventional techniques.
為達成上述目的時，本發明提供一種碳化物微粒子之製造方法，其係使用金屬氧化物製造碳化物微粒子的製造方法，其特徵為使上述金屬氧化物之粉末分散於含碳之液體狀物質中，形成漿料，且使該漿料液滴化，供應給不含氧之熱電漿焰。In order to achieve the above object, the present invention provides a method for producing carbide fine particles, which is a method for producing carbide fine particles using a metal oxide, characterized in that a powder of the above metal oxide is dispersed in a liquid substance containing carbon. A slurry is formed and the slurry is dropletized and supplied to a hot plasma flame containing no oxygen.
於本發明中，上述金屬氧化物例如TiO2 、ZrO2 、V2 O5 、Nb2 O5 、SiO2 或WO3 。In the present invention, the above metal oxide is, for example, TiO 2 , ZrO 2 , V 2 O 5 , Nb 2 O 5 , SiO 2 or WO 3 .
而且，於本發明中，上述含碳之液體狀物質為醇、酮、煤油、辛烷或汽油。Further, in the present invention, the above carbon-containing liquid material is an alcohol, a ketone, kerosene, octane or gasoline.
此外，於本發明中，上述熱電漿焰係來自氫氣、氦氣及氬氣中至少一種的氣體。Further, in the invention, the pyroelectric flame is a gas derived from at least one of hydrogen, helium and argon.
[發明效果][Effect of the invention]
藉由本發明，可以金屬氧化物作為原料，以高生產性製造奈米尺寸之碳化物微粒子。According to the present invention, a metal oxide can be used as a raw material to produce nanosized carbide fine particles with high productivity.
[為實施發明之形態][In order to implement the invention]
於下述中，以附加的圖面所示之較佳實施形態為基準，詳細說明本發明之碳化物微粒子的製造方法。Hereinafter, a method of producing the carbide fine particles of the present invention will be described in detail based on preferred embodiments shown in the additional drawings.
第1圖係表示為實施本發明之實施形態的碳化物微粒子之製造方法時的微粒子製造裝置之全體構成的模式圖。第2圖係表示第1圖中電漿炬12附近的部分擴大圖。第3圖係表示擴大第1圖中所示之反應室16的天板17及該天板17所具備的氣體射出口28a及氣體射出口28b附近之剖面圖。另外，第4圖係表示擴大旋風分離機19之剖面圖。Fig. 1 is a schematic view showing the overall configuration of a fine particle production apparatus in the method of producing a carbide fine particle according to an embodiment of the present invention. Fig. 2 is a partially enlarged view showing the vicinity of the plasma torch 12 in Fig. 1. Fig. 3 is a cross-sectional view showing the vicinity of the gas injection port 28a and the gas injection port 28b provided in the sky plate 17 and the sky plate 17 of the reaction chamber 16 shown in Fig. 1 . In addition, Fig. 4 is a cross-sectional view showing the expanded cyclone separator 19.
第1圖所示之微粒子製造裝置10，係含有產生熱電漿之電漿炬12、使金屬氧化物之粉末如下所述形成漿料狀，供應給電漿炬12內之材料供應裝置14、具有為生成微粒子(一次微粒子)15時之作為冷卻槽的機能之反應室16、自生成的一次微粒子15除去具有任意規定的粒徑以上之粒徑的粗大粒子之旋風分離機19，與回收藉由旋風分離機19所分級的具有企求粒徑的碳化物微粒子(二次微粒子)18之回收部20所構成。The fine particle production apparatus 10 shown in Fig. 1 includes a plasma torch 12 that generates a thermo-plasma, and a powder of a metal oxide is formed into a slurry as described below, and is supplied to the material supply device 14 in the plasma torch 12, and has In the reaction chamber 16 which is a function of the cooling tank when the fine particles (primary fine particles) 15 are formed, the cyclone separator 19 which removes coarse particles having a particle diameter of a predetermined particle diameter or more from the generated primary fine particles 15 is recovered by the cyclone The collecting unit 20 having the carbide fine particles (secondary fine particles) 18 having a predetermined particle size classified by the separator 19 is constituted.
於本實施形態中，使金屬氧化物之粉末(以下亦稱為金屬氧化物原料)分散於含碳之液體狀物質(以下亦稱為分散媒)，形成漿料狀，使用該漿料，藉由微粒子製造裝置10製造奈米尺寸之碳化物微粒子。In the present embodiment, a powder of a metal oxide (hereinafter also referred to as a metal oxide raw material) is dispersed in a liquid substance containing carbon (hereinafter also referred to as a dispersion medium) to form a slurry, and the slurry is used. Nanoparticle-sized carbide fine particles are produced by the microparticle manufacturing apparatus 10.
第2圖所示之漿料炬12，係以石英管12a與捲取其外側之高頻率發振用線圈12b所構成。在電漿炬12之上部上，其中央部設置為使金屬氧化物之粉末與噴霧氣體供應給電漿炬12內時之下述供應管14f，其周邊部(同一圓周上)形成電漿氣體供應口12c。The slurry torch 12 shown in Fig. 2 is composed of a quartz tube 12a and a high frequency oscillation coil 12b wound around the outside. On the upper portion of the plasma torch 12, the central portion thereof is disposed such that the metal oxide powder and the spray gas are supplied to the plasma torch 12 in the following supply tube 14f, and the peripheral portion (on the same circumference) forms a plasma gas supply. Port 12c.
電漿氣體係自電漿氣體供應源22送入電漿氣體供應口12c(參照第2圖)。The plasma gas system is supplied from the plasma gas supply source 22 to the plasma gas supply port 12c (see Fig. 2).
於本實施形態中，為於下述之熱電漿焰24中、在沒有使含碳之液體狀物質(分散媒)被燃燒下進行分解而產生碳時，電漿氣體係使用不含氧氣者。該電漿氣體例如氫氣、氦氣、氬氣等。電漿氣體不受限於單體，可如氫氣與氬氣、氦氣與氬氣，組合此等電漿氣體使用。In the present embodiment, in the pyroelectric flame 24 described below, when carbon is generated by decomposing without burning a carbon-containing liquid material (dispersion medium), the plasma gas system uses oxygen-free gas. The plasma gas is, for example, hydrogen, helium, argon or the like. The plasma gas is not limited to a monomer, and may be used in combination with such a plasma gas as hydrogen and argon, helium and argon.
電漿氣體供應源22，例如準備氫氣與氬氣等2種類之電漿氣體。電漿氣體係自電漿氣體供應源22，經由第2圖所示之圓環狀電漿氣體供應給12c，如箭頭P所示送入電漿炬12內。然後，對高頻率發振用線圈12b施加高頻率電壓，產生不含氧之熱電漿焰24。The plasma gas supply source 22 is, for example, prepared two types of plasma gases such as hydrogen gas and argon gas. The plasma gas system is supplied from the plasma gas supply source 22 to the 12c via the annular plasma gas shown in Fig. 2, and is fed into the plasma torch 12 as indicated by the arrow P. Then, a high frequency voltage is applied to the high frequency oscillation coil 12b, and a hot plasma flame 24 containing no oxygen is generated.
而且，石英管12a之外側，以形成同心圓狀之管(途中沒有表示)圍住，在該管與石英管12a之間，使冷卻水循環且使石英管12a水冷，以防止因電漿炬12內產生的熱電漿焰24導致石英管12a變得過於高溫。Further, the outer side of the quartz tube 12a is surrounded by a tube forming a concentric shape (not shown), and between the tube and the quartz tube 12a, the cooling water is circulated and the quartz tube 12a is water-cooled to prevent the plasma torch 12 from being cooled. The pyroelectric flame 24 generated inside causes the quartz tube 12a to become too hot.
如第1圖所示，材料供應裝置14係經由管26與供應管14f，連接於電漿炬12之上方，使金屬氧化物原料混於分散媒中所調製的漿料14a，自材料供應裝置14均勻地供應給電漿炬12內。As shown in Fig. 1, the material supply device 14 is connected to the upper portion of the plasma torch 12 via the tube 26 and the supply tube 14f, and the metal oxide raw material is mixed with the slurry 14a prepared in the dispersion medium. 14 is uniformly supplied into the plasma torch 12.
材料供應裝置14，係加入漿料14a之容器14b、使容器14b中之漿料14a進行攪拌的攪拌機14c、為經由供應管14f、對漿料14a施加高壓、供應給電漿炬12內時之幫浦14d、為使漿料14a噴霧於電漿炬12內時之供應噴霧氣體之噴霧氣體供應源14e，及使漿料14a液滴化，供應給電漿炬12內之供應管14f所構成。The material supply device 14 is a mixer 14c to which the slurry 14a is added, a stirrer 14c for stirring the slurry 14a in the container 14b, and a high pressure for supplying the slurry 14a to the slurry torch 12 via the supply pipe 14f. The pump 14d is configured to supply the spray gas supply source 14e for the spray gas when the slurry 14a is sprayed into the plasma torch 12, and to dropletize the slurry 14a, and supply it to the supply tube 14f in the plasma torch 12.
施加押出壓力的噴霧氣體，與自噴霧氣體供應源14e之漿料14a，如第2圖中同時經由箭頭G所示之供應管14f，供應給電漿炬12內之熱電漿焰24。供應管14f具有使電漿噴霧於電漿炬內之熱電漿焰24中且進行液滴化時之二流體噴嘴機構，藉此使漿料14a噴霧於電漿炬12內之熱電漿焰24中。換言之，可使漿料14a液滴化。噴霧氣體例如單獨或適當組合氬氣、氦氣、氫氣等使用。而且，只要是可使漿料14a液滴化即可，不一定必須供應噴霧氣體。The spray gas to which the pressure is applied is supplied to the slurry 14a of the self-spraying gas supply source 14e, as shown in Fig. 2 via the supply pipe 14f shown by the arrow G, to the hot plasma flame 24 in the plasma torch 12. The supply tube 14f has a two-fluid nozzle mechanism for spraying the plasma into the hot plasma flame 24 in the plasma torch and performing dropletization, whereby the slurry 14a is sprayed into the hot plasma flame 24 in the plasma torch 12. . In other words, the slurry 14a can be dropletized. The spray gas is used, for example, argon gas, helium gas, hydrogen gas or the like alone or in a suitable combination. Further, as long as the slurry 14a can be dropletized, it is not always necessary to supply the spray gas.
該二流體噴嘴機構，係使用可對漿料施加高壓，藉由氣體之噴霧氣體以噴霧漿料，作為使漿料液滴化時之一種方法。例如，使用內徑1mm者作為噴嘴時，使供應壓力為0.2～0.3MPa，以每分鐘20ml流入漿料，以每分鐘10～20L使噴霧氣體噴霧時，可得約5～10μm之液滴。The two-fluid nozzle mechanism is a method in which a high pressure is applied to the slurry and a spray slurry of the gas is used as a spray slurry as a method of dropletizing the slurry. For example, when a nozzle having an inner diameter of 1 mm is used as the nozzle, the supply pressure is 0.2 to 0.3 MPa, the slurry is allowed to flow into the slurry at 20 ml per minute, and when the spray gas is sprayed at 10 to 20 L per minute, droplets of about 5 to 10 μm can be obtained.
而且，於本實施形態中使用二流體噴嘴機構，惟亦可使用一流體噴嘴機構。另外，其他的方法例如在回轉的圓板上，使漿料以一定速度落下，藉由離心力予以液滴化(形成液滴)的方法，在漿料表面上施加高電壓予以液滴化(產生液滴)的方法等。Further, in the present embodiment, a two-fluid nozzle mechanism is used, but a fluid nozzle mechanism can also be used. In addition, other methods, for example, on a rotating circular plate, the slurry is dropped at a certain speed, and a method of dropletizing (formation of droplets) by centrifugal force is applied to the surface of the slurry to apply a high voltage to be dropletized (produced). Method of droplets, etc.
另外，如第1圖所示，反應室16鄰接於電漿炬12之下方予以設置。電漿炬12內之熱電漿焰24中所噴霧的漿料14a中之分散媒，在沒有以熱電漿焰24燃燒下，藉由分解產生的碳，使金屬氧化物原料還原。此外，經還原的金屬材料原料與碳反應，形成碳化物。然後，形成該碳化物之碳化物微粒子，在反應室16內被急冷，生成一次微粒子(碳化物微粒子)15。如此反應室16具有作為冷卻槽之機能。Further, as shown in Fig. 1, the reaction chamber 16 is disposed adjacent to the lower side of the plasma torch 12. The dispersing medium in the slurry 14a sprayed in the pyroelectric flame 24 in the electric torch 12 reduces the metal oxide raw material by decomposing the generated carbon without burning the pyroelectric flame 24. In addition, the reduced raw material of the metallic material reacts with carbon to form a carbide. Then, the carbide fine particles of the carbide are formed and quenched in the reaction chamber 16 to form primary fine particles (carbide fine particles) 15. Thus, the reaction chamber 16 has a function as a cooling tank.
而且，此處為更有效地製造碳化物微粒子的方法之一，具備為使所生成的碳化物微粒子急冷時之氣體供應裝置28。於下述中，說明有關該氣體供應裝置28。Further, here, one of the methods for producing carbide fine particles more efficiently, is provided with a gas supply device 28 for rapidly cooling the generated carbide fine particles. The gas supply device 28 will be described below.
第1圖、第3圖所示之氣體供應裝置28，係由朝向熱電漿焰24之尾部(與電漿氣體供應口12c相反側之熱電漿焰端、即熱電漿焰之終端部)，以所定的角度射出氣體之氣體射出口28a，沿著反應室16之側壁、自上方朝向下方射出氣體之氣體射出口28b，對供應給反應室16內的氣體施加押出壓力之壓縮機28c，供應給反應室16內的上述氣體之供應源28d，與連接此等之管28e所構成。而且，壓縮機28c亦可為送風機。The gas supply device 28 shown in Fig. 1 and Fig. 3 is directed to the tail portion of the pyroelectric flame 24 (the hot plasma flame end opposite to the plasma gas supply port 12c, that is, the end portion of the pyroelectric flame). The gas injection port 28a that emits the gas at a predetermined angle, and the gas injection port 28b that emits gas from the upper side toward the lower side of the reaction chamber 16 and the compressor 28c that applies the extrusion pressure to the gas supplied to the reaction chamber 16 is supplied to The supply source 28d of the gas in the reaction chamber 16 is constituted by a tube 28e connected thereto. Moreover, the compressor 28c may also be a blower.
而且，自上述氣體射出口28a射出的氣體，除如下詳述使在反應室16內所生成的一次微粒子15急冷之作用外，具有賦予自氣體射出口28b射出的氣體，與旋風分離機19之一次微粒子15分級等之加成作用。Further, the gas emitted from the gas injection port 28a has a function of quenching the primary fine particles 15 generated in the reaction chamber 16 as described below, and a gas which is supplied from the gas injection port 28b, and the cyclone separator 19 The addition of a microparticle 15 fraction or the like.
上述之壓縮機28c與氣體供應源28d，經由管28e，連接於反應室16之天板17。The compressor 28c and the gas supply source 28d described above are connected to the top plate 17 of the reaction chamber 16 via a pipe 28e.
此處，上述氣體射出口28b，係在氣體供應裝置28之外側部天板零件17b內所形成的隙縫，以可防止所生成的一次微粒子15附著於反應室16之內壁部，同時可賦予以一次微粒子15以下游的旋風分離機19、以任意的分級點進行分級之流速的量之氣體射出較佳。自上述氣體射出口28b，沿著反應室16之內壁，由上方朝向下方射出氣體。Here, the gas injection port 28b is a slit formed in the outer side plate member 17b of the gas supply device 28 to prevent the generated primary fine particles 15 from adhering to the inner wall portion of the reaction chamber 16, and at the same time It is preferable that the primary neutrons 15 emit gas at a flow rate of the downstream cyclone separator 19 at an arbitrary classification point. From the gas ejection port 28b, a gas is emitted from the upper side toward the lower side along the inner wall of the reaction chamber 16.
自氣體供應源28d(參照第1圖及第3圖)，經由以箭頭S所示之管28e，供應給天板17(詳言之，外側部天板零件17b及上部外側部天板零件17c)之氣體，係經由設置於此處之通氣路，自氣體射出口28b(下述中亦可為氣體射出口28a)被射出。The gas supply source 28d (see FIGS. 1 and 3) is supplied to the ceiling 17 via a tube 28e indicated by an arrow S (in detail, the outer portion of the sky plate member 17b and the upper outer portion of the sky plate member 17c) The gas is emitted from the gas injection port 28b (hereinafter also referred to as the gas injection port 28a) via the air passage provided therein.
自材料供應裝置14被射出於電漿炬12內(經液滴化)的漿料，在熱電漿焰24中，如下所述在沒有被燃燒下，形成金屬氧化物原料被還原及碳化的碳化物。然後，該碳化物藉由自上述氣體射出口28a被射出(參照箭頭Q)的氣體，在反應室16內被急冷，生成由碳化物所成的一次微粒子15。此時，藉由自氣體射出口28b所射出的(參照箭頭R)氣體，防止一次微粒子15附著於反應室16之內壁。The material supply device 14 is injected into the slurry in the plasma torch 12 (dropped), and in the hot plasma flame 24, carbonization of the metal oxide raw material is reduced and carbonized without being burned as described below. Things. Then, the carbide is rapidly cooled in the reaction chamber 16 by a gas which is emitted from the gas injection port 28a (see the arrow Q) to generate primary fine particles 15 made of carbide. At this time, the primary fine particles 15 are prevented from adhering to the inner wall of the reaction chamber 16 by the gas (refer to the arrow R) emitted from the gas ejection port 28b.
如第1圖所示，在反應室16之側方下部，設置為使所生成的一次微粒子15以企求的粒徑分級時之旋風分離機19。該旋風分離機19，如第4圖所示，具備自反應室16供應一次微粒子15之入口管19a，連接於該入口管19a、位於旋風分離機19之上方的圓筒形狀之外筒19b，自該外筒19b下方朝向下側連接，且使內徑漸減的圓錐台部19c，使連接於該圓錐台部19c下側之具有上述企求的粒徑以上之粒徑的粗大粒子回收的粗大粒子回收反應室19d，與連接於如下詳述的回收部20、突設於外筒19b之內管19e。As shown in Fig. 1, a cyclone separator 19 is provided in a lower portion of the reaction chamber 16 so that the generated primary fine particles 15 are classified by a desired particle size. As shown in Fig. 4, the cyclone separator 19 includes an inlet pipe 19a for supplying the primary particles 15 from the reaction chamber 16, and is connected to the inlet pipe 19a and a cylindrical outer cylinder 19b located above the cyclone separator 19, The truncated cone portion 19c that is connected downward from the lower side of the outer cylinder 19b and whose inner diameter is gradually decreased, and the coarse particles that are connected to the lower side of the truncated cone portion 19c and have coarse particles having a particle diameter equal to or larger than the above-mentioned desired particle diameter The recovery reaction chamber 19d is connected to the recovery unit 20 as described in detail below, and protrudes from the inner tube 19e of the outer tube 19b.
自入口管19a，在反應室16內所生成的含有一次微粒子15之氣流，沿著外筒19b內周壁吹入，藉此使該氣流如第4圖中之箭頭T所示，自外筒19b之內周壁朝向圓錐台部19c的方向流動，形成回旋的下降流。From the inlet pipe 19a, the gas stream containing the primary particles 15 generated in the reaction chamber 16 is blown along the inner peripheral wall of the outer cylinder 19b, whereby the gas flow is as shown by the arrow T in Fig. 4, from the outer cylinder 19b. The inner peripheral wall flows in the direction of the truncated cone portion 19c to form a downward flow of the swirl.
其次，上述回旋的下降流，在圓錐台部19c之內周壁更為加速，再予以反轉，形成上昇流，自內管19e排出於系外。而且，部分氣流在流入粗大粒子回收反應室19d之前，在圓錐台部19c反轉，自內管19e排出於系外。粒子藉由回旋流賦予離心力，藉由離心力與抗力之平衡性，使粗大粒子朝壁方向移動。另外，自氣流所分離的碳化物微粒子，沿著圓錐台部19c側面下降，被粗大粒子回收反應室19d回收。此處，沒有被賦予充分的離心力之微粒子，與圓錐台部19c內周壁之反轉氣流同時排出於系外。Next, the downward flow of the above-described swirling is further accelerated in the inner peripheral wall of the truncated cone portion 19c, and is reversed to form an upward flow, which is discharged from the inner tube 19e. Further, before flowing into the coarse particle recovery reaction chamber 19d, the partial gas flow is reversed at the truncated cone portion 19c, and is discharged from the inner tube 19e. The particles impart centrifugal force by the swirling flow, and the coarse particles move toward the wall by the balance between the centrifugal force and the resistance. Further, the carbide fine particles separated from the gas flow are descended along the side surface of the truncated cone portion 19c, and are collected by the coarse particle recovery reaction chamber 19d. Here, the fine particles which are not provided with sufficient centrifugal force are discharged to the outside of the system simultaneously with the reverse flow of the inner peripheral wall of the truncated cone portion 19c.
然後，通過內管19e，自下方詳述的回收部20產生負壓(吸引力)。其次，藉由該負壓(吸引力)，自上述回旋的氣流所分離的碳化物微粒子，如第4圖中之箭頭U所示地被吸引，通過內管19e，送入回收部20。Then, a negative pressure (attractive force) is generated from the recovery portion 20 detailed below through the inner tube 19e. Then, by the negative pressure (attractive force), the carbide fine particles separated from the swirling airflow are sucked as indicated by an arrow U in FIG. 4, and sent to the collecting portion 20 through the inner tube 19e.
如第1圖所示，就延長旋風分離機19內之氣流出口的內管19e而言，設置回收具有企求的奈米尺寸之粒徑的二次微粒子(碳化物微粒子)18之回收部20。該回收部20係具備回收室20a與設置於回收室20a內之過濾器20b，經由設置於回收室20a內下方之管所連接的真空幫浦(圖中沒有表示)。自旋風分離機19所送出的微粒子，藉由真空幫浦(圖中沒有表示)吸引，引入回收室20a，形成停留於過濾器20b之表面的狀態，予以回收。As shown in Fig. 1, the inner tube 19e for extending the gas flow outlet in the cyclone separator 19 is provided with a recovery unit 20 for recovering secondary fine particles (carbide fine particles) 18 having a desired nanometer size. The recovery unit 20 includes a vacuum chamber (not shown) connected to the filter 20b provided in the recovery chamber 20a and the filter 20b provided in the recovery chamber 20a. The fine particles sent from the cyclone separator 19 are sucked by a vacuum pump (not shown), introduced into the recovery chamber 20a, and formed in a state of staying on the surface of the filter 20b, and are collected.
如下所述，說明如上述所構成的微粒子製造裝置10之作用，且說明有關使用該微粒子製造裝置10，本發明之實施形態的碳化物微粒子之製造方法，以及藉由該製造方法所生成的碳化物微粒子。The operation of the fine particle production apparatus 10 configured as described above will be described below, and a method of manufacturing the carbide fine particles according to the embodiment of the present invention and the carbonization generated by the production method using the fine particle production apparatus 10 will be described. Microparticles.
此處，於本實施形態中，金屬氧化物原料(金屬氧化物之粉末)係由碳化物微粒子之原料所成者。該金屬氧化物原料(金屬氧化物之粉末)，例如氧化鈦(TiO2 )、氧化鋯(ZrO2 )、氧化釩(V2 O5 )、氧化鈮(Nb2 O5 )、氧化矽(SiO2 )，及氧化鎢(WO3 )。Here, in the present embodiment, the metal oxide raw material (powder of the metal oxide) is made of a raw material of the carbide fine particles. The metal oxide raw material (powder of metal oxide), such as titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), vanadium oxide (V 2 O 5 ), niobium oxide (Nb 2 O 5 ), niobium oxide (SiO 2 ), and tungsten oxide (WO 3 ).
於本實施形態中，金屬氧化物係使用構成生成的碳化物微粒子之金屬元素的氧化物。In the present embodiment, an oxide of a metal element constituting the produced carbide fine particles is used as the metal oxide.
而且，金屬氧化物原料，容易在熱電漿焰中蒸發，其平均粒徑為50μm以下，較佳的平均粒徑為10μm以下。Further, the metal oxide raw material is easily evaporated in the hot plasma flame, and has an average particle diameter of 50 μm or less, and preferably has an average particle diameter of 10 μm or less.
於本實施形態中，含碳之液體狀物質(分散媒)，例如醇、酮、煤油、辛烷或汽油。In the present embodiment, a carbon-containing liquid material (dispersion medium) such as an alcohol, a ketone, kerosene, octane or gasoline.
另外，醇例如乙醇、甲醇、丙醇、異丙醇。Further, an alcohol such as ethanol, methanol, propanol or isopropanol.
如上所述，含碳之液體狀物質(分散媒)，係使金屬氧化物原料(金屬氧化物之粉末)還原，同時作用作為供應為形成碳化物時之碳的碳源。因此，含碳之液體狀物質以可藉由熱電漿焰24容易分解較佳。由此可知，含碳之液體狀物質，以低元醇較佳。As described above, the carbon-containing liquid material (dispersion medium) serves to reduce the metal oxide raw material (powder of the metal oxide) and acts as a carbon source for supplying carbon when the carbide is formed. Therefore, the carbon-containing liquid material is preferably easily decomposed by the pyroelectric flame 24. From this, it is understood that the carbon-containing liquid material is preferably a low-valent alcohol.
本實施形態的碳化物微粒子之製造方法，首先使金屬氧化物原料分散於分散媒中，製得漿料。此時，漿料中之金屬氧化物原料與分散媒之混合比例，例如6:4(60%:40%)。由於分散媒具有為使金屬氧化物還原，同時作為碳化時之碳源的作用者，故在產生多餘的碳下，可適當地改變該金屬氧化物原料與分散媒之質量比，調製漿料。In the method for producing carbide fine particles of the present embodiment, first, a metal oxide raw material is dispersed in a dispersion medium to obtain a slurry. At this time, the mixing ratio of the metal oxide raw material and the dispersion medium in the slurry is, for example, 6:4 (60%: 40%). Since the dispersing medium has a function as a carbon source for carbonization in order to reduce the metal oxide, the mass ratio of the metal oxide raw material to the dispersing medium can be appropriately changed to produce a slurry.
另外，於調整漿料14a時，亦可添加選自界面活性劑、高分子、偶合劑所成群中之1種或2種以上的混合物。界面活性劑例如使用非離子性界面活性劑之山梨糖醇酐脂肪酸酯。高分子例如使用聚丙烯酸銨。偶合劑例如使用矽烷偶合劑等。藉由在漿料14a中添加選自界面活性劑、高分子、偶合劑所成群中之1種或2種以上的混合物，可更為有效地防止藉由金屬氧化物原料在分散媒中凝聚，使漿料14a予以安定化。In addition, when adjusting the slurry 14a, one or a mixture of two or more selected from the group consisting of a surfactant, a polymer, and a coupling agent may be added. As the surfactant, for example, a sorbitan fatty acid ester of a nonionic surfactant is used. As the polymer, for example, ammonium polyacrylate is used. As the coupling agent, for example, a decane coupling agent or the like is used. By adding one or a mixture of two or more selected from the group consisting of a surfactant, a polymer, and a coupling agent to the slurry 14a, it is possible to more effectively prevent aggregation of the metal oxide raw material in the dispersion medium. The slurry 14a is stabilized.
如上述調整的漿料14a，加入第1圖所示之材料供應裝置14的容器14b內，以攪拌機14c進行攪拌。藉此防止分散媒中之金屬氧化物原料沉澱，且維持金屬氧化物原料分散於分散媒中之狀態的漿料14a。而且，亦可連續使金屬氧化物原料與分散媒供應給材料供應裝置14，調製漿料14a。The slurry 14a adjusted as described above is placed in the container 14b of the material supply device 14 shown in Fig. 1, and stirred by the agitator 14c. Thereby, the metal oxide raw material in the dispersion medium is prevented from being precipitated, and the slurry 14a in a state in which the metal oxide raw material is dispersed in the dispersion medium is maintained. Further, the metal oxide raw material and the dispersion medium may be continuously supplied to the material supply device 14 to prepare the slurry 14a.
其次，使用上述之二流體噴嘴機構，使漿料14a液滴化，經液滴化的漿料14a藉由供應給電漿炬12內，供應給電漿炬12內產生的熱電漿焰24中，在分散媒沒有被燃燒下，生成碳。Next, the slurry 14a is dropletized by using the above-described two-fluid nozzle mechanism, and the dropletized slurry 14a is supplied into the plasma torch 12 and supplied to the pyroelectric flame 24 generated in the plasma torch 12, The dispersing medium is not burned to generate carbon.
而且，不含氧氣之熱電漿焰24，係使經液滴化的漿料14a蒸發，在分散媒沒有被燃燒下進行分解、蒸發，生成碳。另外，熱電漿焰24係藉由該溫度與所生成的碳，使金屬氧化物原料還原後，形成與剩餘的碳進行反應碳化物。因此，熱電漿焰24之溫度，必須為漿料中所含的金屬氧化物原料(金屬氧化物)藉由碳予以還原的溫度、且較被碳化更高的溫度。Further, the oxygen-free hot plasma flame 24 evaporates the dropletized slurry 14a, decomposes and evaporates without dissolving the dispersion medium, and generates carbon. Further, the pyroelectric flame 24 forms a reaction carbide with the remaining carbon by reducing the metal oxide raw material by the temperature and the generated carbon. Therefore, the temperature of the hot plasma flame 24 must be a temperature at which the metal oxide raw material (metal oxide) contained in the slurry is reduced by carbon and a temperature higher than carbonization.
另外，熱電漿焰24之溫度愈高時，由於容易使金屬氧化物原料(金屬氧化物)還原及碳化，故較佳，沒有特別的限制，視金屬氧化物原料(金屬氧化物)被還原的溫度而定予以適當選擇。例如，可使熱電漿焰24之溫度為6000℃，且理論上可達到約10000℃者。Further, when the temperature of the hot plasma flame 24 is higher, since the metal oxide raw material (metal oxide) is easily reduced and carbonized, it is preferably not particularly limited, and the metal oxide raw material (metal oxide) is reduced. The temperature is appropriately selected. For example, the temperature of the hot plasma flame 24 can be made 6000 ° C, and theoretically can reach about 10000 ° C.
此外，電漿炬12內之壓力氣體環境，以在大氣壓以下較佳。此處，有關大氣壓以下之氣體環境，沒有特別的限制，例如可為5Torr～750Torr。Further, the pressurized gas atmosphere in the plasma torch 12 is preferably at most atmospheric pressure. Here, the gas atmosphere below atmospheric pressure is not particularly limited, and may be, for example, 5 Torr to 750 Torr.
其次，在不含氧氣之熱電漿焰24中，使漿料14a蒸發，再於甲烷等之分散媒沒有被燃燒下被分解，製得碳。該碳與金屬氧化物原料相比時，在多數生成下調整漿料14a之分散媒的量。產生的碳與金屬氧化物原料進行反應，且使金屬氧化物還原成金屬。然後，剩餘的碳與被還原的金屬進行反應，生成碳化物。該經生成的碳化物，經由氣體射出口28a，朝箭頭Q所示之方向射出的氣體予以急冷，藉由在反應室16內被急冷，製得由碳化物所成的一次微粒子15。Next, in the thermoelectric plasma flame 24 containing no oxygen, the slurry 14a is evaporated, and then the dispersion medium such as methane is decomposed without being burned to obtain carbon. When the carbon is compared with the metal oxide raw material, the amount of the dispersion medium of the slurry 14a is adjusted under a large number of generations. The resulting carbon reacts with the metal oxide feedstock and reduces the metal oxide to a metal. The remaining carbon then reacts with the reduced metal to form a carbide. The generated carbide is quenched by a gas emitted from the gas injection port 28a in the direction indicated by the arrow Q, and is quenched in the reaction chamber 16 to obtain primary fine particles 15 made of carbide.
因此，自上述氣體射出口28a所射出的氣體之量，於生成一次微粒子15的過程中，使金屬氧化物形成碳化物後，使該碳化物急冷時必須具有充分的供應量，以與該物同時自氣體射出口28b所射出的氣體之量，以及與下述之熱電漿焰中供應的氣體之量組合，可得使一次微粒子15以下游之旋風分離機19、以任意分級點進行分級的流速，且在不妨礙熱電漿焰安定的程度之量較佳。Therefore, the amount of gas emitted from the gas exit port 28a is such that, in the process of generating the primary fine particles 15, the metal oxide is formed into a carbide, and when the carbide is quenched, it is necessary to have a sufficient supply amount to At the same time, the amount of gas emitted from the gas ejection port 28b and the amount of gas supplied from the pyroelectric flame described below can be used to classify the primary fine particles 15 by the downstream cyclone 19 at any hierarchical point. The flow rate, and the amount that does not interfere with the thermo-plasma flame stability, is preferred.
而且，組合自上述之氣體射出口28a所射出的氣體之量與自氣體射出口28b所射出的氣體之量的射出量，可為供應給上述熱電漿焰中之氣體的200%～5000%。此處，供應給上述熱電漿焰中之氣體，係組合形成熱電漿焰之電漿氣體、形成電漿流時之氣體及噴霧氣體者。Further, the amount of the gas emitted from the gas injection port 28a and the amount of the gas emitted from the gas injection port 28b may be 200% to 5000% of the gas supplied to the pyrophoric flame. Here, the gas supplied to the pyrophoric flame is combined to form a plasma gas of a pyroelectric flame, a gas for forming a plasma stream, and a spray gas.
此外，只要是不妨礙熱電漿焰之安定性，對上述所射出的氣體之供應方法或供應位置等，沒有特別的限制。本實施形態之微粒子製造裝置10，係在天板17上形成圓周狀隙縫，射出氣體，惟自熱電漿焰至旋風分離機之經路上，只要是可確實地供應氣體之方法或位置即可，亦可為其他的方法、其他的位置。Further, there is no particular limitation on the method of supplying the gas to be emitted, the supply position, and the like as long as it does not interfere with the stability of the pyrophoric flame. In the fine particle manufacturing apparatus 10 of the present embodiment, a circumferential slit is formed in the top plate 17, and a gas is emitted, but the method or the position where the gas can be reliably supplied from the hot plasma flame to the cyclone separator can be used. Other methods and other locations are also available.
由最終在反應室16內所生成的碳化物所成的一次微粒子15，係自旋風分離機19之入口管19a，與氣流同時沿著外筒19b之內周壁吹入，藉此使該氣流沿著第4圖中箭頭T所示之外筒19b的內周壁流動，形成回旋流而下降。然後，該回旋流在圓錐台部19c內周壁更為加速，然後反轉形成上昇流，自內管19e排出至系外。而且，部分的氣流，於流入粗大粒子回收反應室19d前，以圓錐台部19c內周壁反轉，且自內管19e排出至系外。The primary fine particles 15 formed by the carbides finally formed in the reaction chamber 16 are blown from the inner peripheral wall of the outer cylinder 19b simultaneously with the air flow at the inlet pipe 19a of the cyclone 19, thereby causing the air flow along The inner peripheral wall of the outer cylinder 19b flows as indicated by an arrow T in Fig. 4, and forms a swirling flow to descend. Then, the swirling flow is further accelerated in the inner peripheral wall of the truncated cone portion 19c, and then reversed to form an upward flow, which is discharged from the inner tube 19e to the outside of the system. Further, a part of the air current is reversed by the inner peripheral wall of the truncated cone portion 19c before flowing into the coarse particle recovery reaction chamber 19d, and is discharged from the inner tube 19e to the outside of the system.
藉由回旋流賦予由碳化物所成的一次微粒子15具有離心力，藉由離心力與抗力之平衡性，於一次微粒子15中使粗大粒子朝向壁方向移動。而且，於一次微粒子15中，自氣流所分離的粒子沿著圓錐台部19c側面下降，以粗大回收反應室19d回收。此處，不具充分離心力之微粒子，與在圓錐台部19c內周壁之反轉氣流，同時自內管19e作為碳化物微粒子(二次微粒子)18排出至系外。此時至旋風分離機19內之氣流的流速，較佳者為10m/sec以上。The primary particles 15 formed of carbides are centrifugally driven by the swirling flow, and the coarse particles are moved in the wall direction in the primary fine particles 15 by the balance between the centrifugal force and the resistance. Further, in the primary fine particles 15, the particles separated from the gas flow are descended along the side surface of the truncated cone portion 19c, and are recovered in the coarse recovery reaction chamber 19d. Here, the fine particles having no sufficient centrifugal force are discharged from the inner tube 19e as carbide fine particles (secondary fine particles) 18 to the outside of the system, and the reverse flow of the inner peripheral wall of the truncated cone portion 19c. The flow rate of the gas stream to the cyclone separator 19 at this time is preferably 10 m/sec or more.
被排出的碳化物微粒子(二次微粒子)18，藉由自回收部20之負壓(吸引力)，如第4圖中箭頭U所示被吸引，通過內管19e，送至回收部20，以回收部20之過濾器20b回收。此時之旋風分離機19內之內壓，以大氣壓以下較佳。而且，碳化物微粒子(二次微粒子)18之粒徑，視目的而定規定奈米尺寸水準之任意粒徑。The discharged carbide fine particles (secondary fine particles) 18 are sucked by the negative pressure (attractive force) from the collecting portion 20, as indicated by an arrow U in Fig. 4, and sent to the collecting portion 20 through the inner tube 19e. It is recovered by the filter 20b of the recovery part 20. The internal pressure in the cyclone separator 19 at this time is preferably at most atmospheric pressure. Further, the particle diameter of the carbide fine particles (secondary fine particles) 18 is determined to have an arbitrary particle diameter at a nanometer level depending on the purpose.
如此於本實施形態中，可製得奈米尺寸之碳化物微粒子。Thus, in the present embodiment, carbide fine particles of a nanometer size can be obtained.
而且，於本發明之碳化物微粒子之製造方法中，使用的旋風分離機之個數，不限制為1個，亦可為2個以上。Further, in the method for producing a carbide fine particle of the present invention, the number of the cyclone separators used is not limited to one, and may be two or more.
藉由本實施形態之碳化物微粒子的製造方法所製造的碳化物微粒子，其粒度分布寬度狹窄，即具有均勻的粒徑，且幾乎完全沒有混入1μm以上之粗大粒子，具體而言，其平均粒徑為1～100nm之奈米尺寸的碳化物微粒子。The carbide fine particles produced by the method for producing a carbide fine particle according to the present embodiment have a narrow particle size distribution width, that is, have a uniform particle diameter, and are almost completely mixed with coarse particles of 1 μm or more, specifically, an average particle diameter thereof. It is a carbide fine particle having a nanometer size of 1 to 100 nm.
本實施形態之碳化物微粒子的製造方法，可製得例如碳化鈦(TiC)、碳化鋯(ZrC)、碳化釩(VC1-x )、碳化鈮(NbC)、碳化鉭(TaC)、碳化矽(SiC)或碳化鎢(WC1-x )之微粒子作為碳化物微粒子。In the method for producing carbide fine particles of the present embodiment, for example, titanium carbide (TiC), zirconium carbide (ZrC), vanadium carbide (VC 1-x ), niobium carbide (NbC), tantalum carbide (TaC), niobium carbide can be obtained. Fine particles of (SiC) or tungsten carbide (WC 1-x ) are used as carbide fine particles.
以本實施形態之碳化物微粒子的製造方法所得的碳化物微粒子，例如可使用於半導體基板、印刷基板、各種電絕緣零件等之電絕緣材料、切削工具、塑模、軸承等之高硬度高精度之機械工作材料、粒界電容器、濕度感應器等之機能性材料、精密燒結成形材料等燒結體之製造、引擎閥等之被要求高溫耐摩擦性的材料等之溶射零件製造，以及燃料電池之電極、電解質材料及各種觸媒等。The carbide fine particles obtained by the method for producing carbide fine particles of the present embodiment can be used for, for example, high hardness and high precision of electrical insulating materials, cutting tools, molds, and bearings for semiconductor substrates, printed boards, and various electrically insulating parts. Manufacturing of functional materials such as mechanical working materials, grain boundary capacitors, humidity sensors, and sintered bodies such as precision sintered molding materials, and manufacturing of molten parts such as engine valves that require high-temperature and friction-resistant materials, and fuel cells. Electrodes, electrolyte materials and various catalysts.
於本實施形態中，由於可使碳化物微粒子之粒徑為奈米尺寸，例如利用於燒結體時，可提高燒結性，製得高強度之燒結體。藉此例如可製得切削性良好的工具。而且，利用於觸媒時，由於可使粒徑變小，故可提高觸媒之性能。In the present embodiment, when the particle diameter of the carbide fine particles can be made into a nanometer size, for example, when it is used for a sintered body, the sinterability can be improved, and a sintered body having high strength can be obtained. Thereby, for example, a tool having good machinability can be obtained. Further, when the catalyst is used, since the particle diameter can be made small, the performance of the catalyst can be improved.
此外，於本實施形態中，由於金屬氧化物原料之還原、碳化時所使用的碳源中使用液體，對熱電漿焰而言可容易且均勻地供應金屬氧化物原料。另外，由於碳源為液體，與石墨等之固體的碳源相比，容易被分解，對金屬氧化物及被還原的金屬而言，可有效地與碳進行反應。藉此可使金屬氧化物對碳化物之反應效率變高，以高生產性製造碳化物。Further, in the present embodiment, the metal oxide raw material can be easily and uniformly supplied to the hot plasma flame by using a liquid in the carbon source used for reduction and carbonization of the metal oxide raw material. Further, since the carbon source is a liquid, it is easily decomposed as compared with a solid carbon source such as graphite, and the metal oxide and the reduced metal can be efficiently reacted with carbon. Thereby, the reaction efficiency of the metal oxide to the carbide can be made high, and the carbide can be produced with high productivity.
而且，於本實施形態中，例如使用TiO2 作為金屬氧化原料時，可抑制原料成本且可降低生產成本。Further, in the present embodiment, for example, when TiO 2 is used as the metal oxide raw material, the raw material cost can be suppressed and the production cost can be reduced.
另外，本實施形態之碳化物微粒子之製造方法，藉由供應氣體且任意控制裝置內之流速，可以裝置內所設置的旋風分離機分級微粒子。本實施形態之碳化物微粒子的製造方法，由於可在沒有改變反應條件下，藉由改變氣體之流速或旋風分離機內徑以任意分級點分離粗大粒子，可以高生產性製造粒徑微細且均勻、品質佳的高純度微粒子。Further, in the method for producing carbide fine particles of the present embodiment, the cyclone separator provided in the apparatus can be used to classify fine particles by supplying a gas and controlling the flow rate in the apparatus arbitrarily. In the method for producing carbide fine particles of the present embodiment, since the coarse particles can be separated at an arbitrary classification point by changing the flow rate of the gas or the inner diameter of the cyclone without changing the reaction conditions, the particle size can be made fine and uniform with high productivity. High-quality fine particles of good quality.
此外，本實施形態之碳化物微粒子之製造方法，為在旋風分離機內產生回旋流，由於滯留時間變長，在旋風分離機內使微粒子冷卻，故目前不一定必須設置作為冷卻機構所使用的翼片或冷卻路。因此，為除去翼片內所堆積的微粒子，不一定必須停止裝置之運作，可使裝置之運作時間長時間化。而且，藉由使旋風分離機全體形成水冷套管構造，可更為提高冷卻效果。Further, in the method for producing carbide fine particles of the present embodiment, the swirling flow is generated in the cyclone, and since the residence time is long, the fine particles are cooled in the cyclone. Therefore, it is not always necessary to provide a cooling mechanism. Flap or cooling path. Therefore, in order to remove the fine particles accumulated in the fins, it is not necessary to stop the operation of the apparatus, and the operation time of the apparatus can be prolonged. Further, by forming the entire structure of the cyclone into a water-cooled jacket structure, the cooling effect can be further enhanced.
如上所述，本實施形態之微粒子製造裝置10，其特徵為具備使氣相狀態之混合物急冷為主要目的之氣體供應裝置28。於下述中，追加說明有關該氣體供應裝置28。As described above, the fine particle production apparatus 10 of the present embodiment is characterized in that it includes a gas supply device 28 which is mainly used for quenching the mixture in the gas phase state. The gas supply device 28 will be additionally described below.
第1圖、第3圖所示之氣體供應裝置28，係由朝向熱電漿焰24之尾部，以上述特定的角度射出氣體之氣體射出口28a，沿著反應室16之側壁、自上方朝向下方射出氣體之氣體射出口28b，對反應室16內所供應的氣體施加押出壓力之壓縮機28c，在反應室16內所供應的上述氣體之供應源28d，及連接此等之管28e所構成。The gas supply device 28 shown in Figs. 1 and 3 is a gas injection port 28a that emits gas at a specific angle toward the tail of the pyroelectric flame 24, along the side wall of the reaction chamber 16, from above to below. The gas injection port 28b for injecting gas is constituted by a compressor 28c that applies a discharge pressure to the gas supplied in the reaction chamber 16, a supply source 28d for supplying the gas supplied in the reaction chamber 16, and a tube 28e connected thereto.
而且，壓縮機28c與氣體供應源28d，係經由管28e連接於反應室16之天板17。此處，熱電漿焰之尾部，係與電漿氣體供應口12c相反側之熱電漿焰的端部、即熱電漿焰之終端部。Further, the compressor 28c and the gas supply source 28d are connected to the top plate 17 of the reaction chamber 16 via a pipe 28e. Here, the tail portion of the hot plasma flame is the end portion of the pyroelectric flame opposite to the plasma gas supply port 12c, that is, the end portion of the pyroelectric flame.
如第3圖所示，氣體射出口28a與氣體射出口28b，形成於反應室16之天板17上。此處，天板17係含有以圓錐台形狀、部分上側為圓柱之內側部天板零件17a，與具有圓錐台形狀之孔的外側部天板零件17b，與具有使內側部天板零件17a垂直移動的移動機構之上部外側部天板零件17c所構成。As shown in Fig. 3, the gas ejection port 28a and the gas ejection port 28b are formed on the top plate 17 of the reaction chamber 16. Here, the top plate 17 includes an inner side plate member 17a having a truncated cone shape, a part of the upper side being a column, and an outer side slab part 17b having a truncated cone shape, and having the inner side slab part 17a perpendicular thereto. The moving moving mechanism is composed of an upper outer portion of the upper plate member 17c.
此處，內側部天板零件17a與上部外側部天板零件17c連接的部分(內側部天板零件17a為上部之圓柱部分)切斷螺絲，內側部天板零件17a可藉由回轉，朝垂直方向改變位置，內側部天板零件17a，可調節與外側部天板零件17b之距離。而且，內側部天板零件17a之圓錐台部分的坡度，與具有外側部天板零件17b之孔的圓錐台部分之坡度相同，形成互相吻合的構造。Here, the portion where the inner portion of the roof member 17a is connected to the upper outer portion of the slab member 17c (the inner portion of the slab member 17a is the upper cylindrical portion) cuts the screw, and the inner portion of the slab member 17a can be rotated by the vertical The direction change position, the inner side roof member 17a, the distance from the outer side roof member 17b can be adjusted. Further, the slope of the truncated cone portion of the inner side roof member 17a is the same as the slope of the truncated cone portion having the hole of the outer side roof member 17b, and forms a structure that coincides with each other.
此外，氣體射出口28a可調節形成內側部天板零件17a與外側部天板零件17b之間隙、即隙縫寬度，形成具有與天板同心的圓周狀的隙縫。其中，氣體射出口28a，只要是可朝向熱電漿焰24之尾部射出氣體的形狀即可，不限定於上述之隙縫形狀，例如可在圓周上配置多數的孔。Further, the gas ejection port 28a can adjust the gap between the inner portion of the inner surface member 17a and the outer portion of the outer surface member 17b, that is, the slit width, to form a circumferential slit having a concentricity with the sap. In addition, the gas injection port 28a is not limited to the above-described slit shape as long as it can emit a gas toward the tail of the pyroelectric flame 24. For example, a plurality of holes can be arranged on the circumference.
另外，於上部外側部天板零件17c之內部，設置為使經由管28e被送入的氣體通過時之通氣路17d。上述氣體通過通氣路17d，且送入具有形成上述內側部天板零件17a與外側部天板零件17b之隙縫的氣體射出口28a。送入氣體射出口28a之氣體，第1圖及第3圖中以箭頭Q所示之方向，朝向熱電漿焰之尾部(終端部)，如上所述以特定的供應量及特定的角度射出。Further, inside the upper outer portion of the roof member 17c, a ventilation passage 17d when the gas fed through the tube 28e passes is provided. The gas passes through the air passage 17d, and is fed into a gas injection port 28a having a slit forming the inner side roof member 17a and the outer side roof member 17b. The gas fed into the gas injection port 28a is directed toward the tail portion (terminal portion) of the pyroelectric flame in the direction indicated by the arrow Q in the first and third figures, and is emitted at a specific supply amount and a specific angle as described above.
此處，說明有關上述特定的供應量。如上所述(參照段落0048)，為使上述氣相狀態之混合物急冷時所生成的量，例如於上述氣相狀態之混合物急冷時供應給形成必要空間之反應室的氣體在反應室16內之平均流速(反應室內流速)，以0.001～60m/sec較佳，更佳者為0.5～10m/sec。此係使熱電漿焰24中所噴霧蒸發的氣相狀態的混合物急冷且生成微粒子，藉由所生成的微粒子間之衝突來防止凝聚時之充分的氣體供應量。Here, the specific supply amount described above is explained. As described above (refer to paragraph 0048), in order to quench the mixture in the gas phase state, for example, when the mixture in the gas phase state is quenched, the gas supplied to the reaction chamber forming the necessary space is in the reaction chamber 16. The average flow rate (flow rate in the reaction chamber) is preferably 0.001 to 60 m/sec, more preferably 0.5 to 10 m/sec. This causes the mixture in the gas phase state which is sprayed and evaporated in the pyroelectric flame 24 to be quenched and generates fine particles, thereby preventing a sufficient supply of gas at the time of agglomeration by the collision between the generated fine particles.
而且，該供應量係使氣相狀態之混合物急冷且凝固時之充分量，此外，藉由凝固所生成的微粒子間衝突，使沒有凝聚的氣相狀態之混合物稀釋時，必須具有充分量，藉由反應室16之形狀或大小，適當決定其值。Further, the supply amount is a sufficient amount for quenching the mixture in the gas phase state and solidifying, and further, when the mixture of the gas phase which is not agglomerated is diluted by the collision of the fine particles generated by the solidification, it is necessary to have a sufficient amount. The value is appropriately determined by the shape or size of the reaction chamber 16.
惟該供應量以在不妨礙熱電漿焰之安定性下予以控制較佳。However, the supply is preferably controlled without hindering the stability of the pyroelectric flame.
其次，使用第5(A)、(B)圖，說明有關氣體射出口28a為隙縫形狀時之上述特定的角度。第5(A)圖係表示通過反應室16之天板17的中心軸之垂直方向的剖面圖，另外，第5(B)圖係表示自下方觀察天板17之圖。而且，第5(B)圖，係表示對第5(A)圖所示之剖面圖而言垂直的方向。其中，第5(A)、(B)圖中所示之點X，係經由通氣路17d，自氣體供應源28d(參照第1圖)所送入的氣體，自氣體射出口28a射出至反應室16內部之射出點。實際上，由於氣體射出口28a為圓周狀隙縫，射出時之氣體形成帶狀氣流。因此，點X為假設的射出點。Next, the above-described specific angle when the gas injection port 28a is in the shape of a slit will be described using the fifth (A) and (B) drawings. Fig. 5(A) is a cross-sectional view showing the vertical direction of the center axis of the sky plate 17 passing through the reaction chamber 16, and Fig. 5(B) is a view showing the sky plate 17 viewed from below. Further, Fig. 5(B) shows a direction perpendicular to the cross-sectional view shown in Fig. 5(A). Here, the point X shown in the fifth (A) and (B) is emitted from the gas injection source 28d (see FIG. 1) through the air passage 17d, and is emitted from the gas injection port 28a to the reaction. The exit point inside the chamber 16. Actually, since the gas ejection port 28a is a circumferential slit, the gas at the time of injection forms a strip-shaped gas flow. Therefore, point X is the hypothetical exit point.
如第5(A)圖所示，以通氣路17d之開口部的中心為原點，使垂直上方為0°，採用紙面上反時鐘周圍之正方向，朝箭頭Q所示方向，使自氣體射出口28a所射出的氣體角度以角度α表示。該角度α係對上述之自熱電漿焰的初部至尾部(終端部)之方向的角度。As shown in Fig. 5(A), the center of the opening of the air passage 17d is taken as the origin, and the vertical direction is 0°, and the positive direction around the counterclock on the paper surface is used to make the self-gas in the direction indicated by the arrow Q. The angle of the gas emitted from the injection port 28a is represented by an angle α. The angle α is an angle to the direction from the first portion to the tail portion (terminal portion) of the self-heating plasma flame.
而且，如第5(B)圖所示，以上述假設的射出點X為原點，以朝向熱電漿焰24之中心的方向為0°，以在紙面上反時鐘方向為正方向，對自熱電漿焰24之初部至尾部(終端部)的方向而言之垂直面方向、箭頭Q所示之方向、自氣體射出口28a至所射出的氣體之角度以角度β表示。該角度β係在上述的自熱電漿焰之初部至尾部(終端部)之方向而言直行的面內，對熱電漿焰之中心部而言的角度。Further, as shown in Fig. 5(B), the above-mentioned assumed injection point X is taken as the origin, and the direction toward the center of the hot plasma flame 24 is 0°, and the counterclockwise direction on the paper surface is the positive direction. The direction perpendicular to the direction from the beginning to the end (end portion) of the hot plasma torch 24, the direction indicated by the arrow Q, and the angle from the gas exit port 28a to the emitted gas are indicated by the angle β. The angle β is an angle to the center portion of the pyroelectric flame in a plane that goes straight in the direction from the beginning to the end (end portion) of the pyroelectric plasma flame.
使用上述之角度α(通常為垂直方向之角度)及角度β(通常為水平方向之角度)時，上述特定的角度、即上述氣體之上述反應室內的供應方向，於上述反應室16內，對熱電漿焰24之尾部(終端部)而言，角度α為90°<α<240°(較佳者為100°<α<180°之範圍，更佳者為α=135°)，角度β為-90°<β<90°(較佳者為-45°<β<45°之範圍，更佳者為β=0°)。When the angle α (usually the angle in the vertical direction) and the angle β (usually the angle in the horizontal direction) are used, the specific angle, that is, the supply direction of the gas in the reaction chamber, is in the reaction chamber 16 In the tail portion (terminal portion) of the hot plasma flame 24, the angle α is 90° < α < 240° (preferably 100° < α < 180°, more preferably α = 135°), angle β It is -90 ° < β < 90 ° (preferably, the range of -45 ° < β < 45 °, more preferably β = 0 °).
如上所述，藉由朝熱電漿焰24之特定的供應量及以特定角度所射出的氣體，使上述氣相狀態之混合物急冷，生成一次粒子15。以上述特定的角度射出於反應室16內部之氣體，藉由在反應室16內部產生的亂流等之影響，不一定必須以其射出的角度到達熱電漿焰24之尾部，惟為有效地進行氣相狀態之混合物的冷卻處理，且有效地使熱電漿焰24安定，使微粒子製造裝置10運作時，以決定為上述角度者較佳。而且，上述角度就考慮裝置之尺寸、熱電漿焰之大小等之條件予以實驗性決定。As described above, the mixture in the gas phase state is rapidly cooled by the specific supply amount of the hot plasma flame 24 and the gas emitted at a specific angle to generate the primary particles 15. The gas that is incident on the inside of the reaction chamber 16 at the specific angle described above does not necessarily have to reach the tail of the pyroelectric flame 24 at the angle of the emission by the influence of turbulence or the like generated inside the reaction chamber 16, but is effectively performed. It is preferable to cool the mixture in the gas phase state and to effectively stabilize the pyroelectric flame 24 so that the microparticle manufacturing apparatus 10 operates. Moreover, the above angle is experimentally determined in consideration of the conditions of the size of the device, the size of the thermo-plasma flame, and the like.
藉由生成後之微粒子間產生衝突，且形成凝聚物，產生粒徑之不均勻性時，導致品質降低的要因。對此而言，於本發明之碳化物微粒子的製造方法中，經由氣體射出口28a，以特定的角度及供應量，朝向熱電漿焰之尾部(終端部)朝箭頭Q所示之方向射出的氣體，藉由稀釋一次微粒子15，以防止微粒子間產生衝突、凝聚情形。總之，自氣體射出口28a所射出的氣體，藉由使上述氣相狀態之混合物急冷，且防止所生成的微粒子之凝聚情形，具有粒徑之微細化及粒徑之均勻化之兩種作用。When a collision occurs between the generated fine particles and agglomerates are formed, and unevenness in particle diameter occurs, the cause of deterioration in quality is caused. On the other hand, in the method for producing carbide fine particles of the present invention, the gas injection port 28a is emitted toward the tail portion (terminal portion) of the pyroelectric flame at a specific angle and supply amount in the direction indicated by the arrow Q. The gas is diluted by the primary particles 15 to prevent collision and agglomeration between the particles. In short, the gas emitted from the gas injection port 28a has two functions of miniaturizing the particle diameter and uniformizing the particle diameter by quenching the mixture in the gas phase state and preventing aggregation of the generated fine particles.
此處，自氣體射出口28a所射出的氣體，不會有對熱電漿焰24之安定性的惡影響。然而，為使裝置全體連續運轉時，必須使熱電漿焰安定。因此，本實施形態之微粒子製造裝置10中氣體射出口28a，為形成圓周狀之隙縫，由於藉由調整該隙縫寬度，可調節氣體之供應量且朝中心方向射出均勻的氣體，故具有使熱電漿焰安定時之較佳形狀。而且，該調節亦可藉由改變射出的氣體之供應量進行。Here, the gas emitted from the gas injection port 28a does not have an adverse effect on the stability of the pyroelectric flame 24. However, in order to continuously operate the entire apparatus, it is necessary to stabilize the pyroelectric flame. Therefore, in the fine particle production apparatus 10 of the present embodiment, the gas injection port 28a is formed into a circumferential slit, and by adjusting the slit width, the supply amount of the gas can be adjusted and a uniform gas is emitted toward the center direction, so that the thermoelectricity is provided. The preferred shape of the slurry flame. Moreover, the adjustment can also be made by changing the supply amount of the emitted gas.
以上詳細說明有關本發明之碳化物粒子的製造方法，惟本發明不受上述實施形態所限制，在不會脫離本發明主旨之範圍內，可進行各種改良或改變。The method for producing the carbide particles of the present invention is described in detail above, but the present invention is not limited to the above-described embodiments, and various modifications and changes can be made without departing from the spirit and scope of the invention.
[實施例][Examples]
於下述中，具體地說明有關本發明之碳化物微粒子之製造方法的實施例。Hereinafter, examples of the method for producing carbide fine particles of the present invention will be specifically described.
於本實施例及比較例中，使構成上述微粒子製造裝置10之熱電漿焰的電漿氣體之種類，試行下述表1所示之實施例1～6及比較例1～6之電漿氣體欄所示進行改變，製造碳化鈦。In the present embodiment and the comparative example, the types of the plasma gas constituting the hot plasma flame of the fine particle production apparatus 10 were tested for the plasma gases of Examples 1 to 6 and Comparative Examples 1 to 6 shown in Table 1 below. Changes are made in the column to produce titanium carbide.
於本實施例中，使用以氧化鈦之粉末作為原料，以質量比1:1混合該氧化鈦之粉末與甲醇，進行攪拌所得的漿料濃度為50質量%之漿料。而且，原料所使用的氧化鈦，平均粒徑為5μm，具有第6(A)圖所示之結晶構造。In the present embodiment, the powder of titanium oxide was used as a raw material, and the powder of titanium oxide and methanol were mixed at a mass ratio of 1:1, and the slurry having a slurry concentration of 50% by mass was stirred. Further, the titanium oxide used in the raw material has an average particle diameter of 5 μm and has a crystal structure shown in Fig. 6(A).
此處，電漿炬12之高頻率發振用線圈12b，施加約4MHz、約80kVA之高頻率電壓，且各自電漿氣體供應源22如下述表1所示之電漿氣體供應給每一實施例，且在電漿炬12內產生熱電漿炬。而且，自材料供應裝置14之噴霧氣體供應源14e以10L/min供應氬氣作為噴霧氣體。Here, the high-frequency vibration coil 12b of the plasma torch 12 applies a high frequency voltage of about 4 MHz and about 80 kVA, and the respective plasma gas supply sources 22 are supplied to each of the plasma gases as shown in Table 1 below. For example, a hot plasma torch is generated within the plasma torch 12. Further, argon gas was supplied as a spray gas from the spray gas supply source 14e of the material supply device 14 at 10 L/min.
本實施例係使氧化鈦之漿料與噴霧氣體之氬氣同時供應給電漿炬12內之熱電漿焰24中。In this embodiment, the slurry of titanium oxide and the argon gas of the spray gas are simultaneously supplied to the hot plasma flame 24 in the plasma torch 12.
另外，藉由氣體供應裝置28供應給反應室16內之氣體，使用氬氣或氬氣與氦氣之混合氣體。此時之反應室內流速為5m/sec，供應量為1m3 /min。Further, the gas supplied to the reaction chamber 16 by the gas supply means 28 is used, and argon gas or a mixed gas of argon gas and helium gas is used. At this time, the flow rate in the reaction chamber was 5 m/sec, and the supply amount was 1 m 3 /min.
而且，旋風分離機19內之壓力為50kPa，且自反應室16至旋風分離機19之微粒子的供應速度為10m/sec(平均值)。Further, the pressure in the cyclone separator 19 was 50 kPa, and the supply speed of the fine particles from the reaction chamber 16 to the cyclone separator 19 was 10 m/sec (average value).
熱電漿焰之電漿氣體中，氫氣、氦氣、氬氣之比例相對於氦氣及氬氣之總量而言，氫氣之量為0～20vol%。In the plasma gas of the hot plasma flame, the ratio of hydrogen, helium, and argon is 0 to 20 vol% with respect to the total amount of helium and argon.
此外，電漿氣體為氫氣、氦氣等2種類時，相對於氦氣之總量而言，氫氣之量為0～20vol%；為氫氣、氬氣等2種類時，相對於氬氣之總量而言氫氣之量為0～20vol%。Further, when the plasma gas is two types of hydrogen gas or helium gas, the amount of hydrogen gas is 0 to 20 vol% with respect to the total amount of helium gas, and when it is two types of hydrogen gas or argon gas, the total amount of argon gas. The amount of hydrogen is 0 to 20 vol%.
而且，有關電漿氣體之供應量，氬氣為10～300L/min，氦氣為5～30L/min。Further, regarding the supply amount of the plasma gas, the argon gas is 10 to 300 L/min, and the helium gas is 5 to 30 L/min.
另外，於比較例中，使用與實施例相同的氧化鈦之粉末，僅以該原料、或該原料與還原劑與兼具碳源之石墨粉末混合者作為原料，直接以粉體供應給熱電漿焰。Further, in the comparative example, the same titanium oxide powder as in the example was used, and only the raw material or the raw material and the reducing agent and the graphite powder having the carbon source were mixed as a raw material, and the powder was directly supplied to the hot plasma. flame.
此外，於比較例中，製造條件除對熱電漿焰24中之供應形態沒有使用漿料外，與上述實施例相同的條件。Further, in the comparative example, the manufacturing conditions were the same as those of the above-described examples except that the slurry was not used in the supply form in the hot plasma flame 24.
其次，於下述表1所示之實施例1～6及比較例1～6中，有關所得的生成物使用X光繞射(XRD)觀察結晶構造。Next, in Examples 1 to 6 and Comparative Examples 1 to 6 shown in Table 1 below, the obtained product was observed by X-ray diffraction (XRD).
於下述表1之碳化物之欄中，僅呈現表示碳化鈦之組成的波峰者為「○」，呈現表示部分碳化鈦之組成的波峰者、惟呈現表示來自原料之氧化鈦之組成者為「△」，僅呈現表示氧化鈦之組成物者為「×」。In the column of the carbides in the following Table 1, only the peak indicating the composition of the titanium carbide is "○", and the peak indicating the composition of the partial titanium carbide is present, but the composition indicating the titanium oxide from the raw material is "△" indicates that only the composition indicating titanium oxide is "x".
於實施例1～6中，如第6(B)圖所示，皆可製得碳化鈦，粒徑約為25nm。In Examples 1 to 6, as shown in Fig. 6(B), titanium carbide was obtained, and the particle diameter was about 25 nm.
另外，於比較例1～6中，亦生成除碳化鈦外之組成。該除碳化鈦外之組成，係無法碳化的氧化鈦及來自原料之石墨。然而，比較例1～6與實施例1相比時，碳化鈦之收量較少。Further, in Comparative Examples 1 to 6, a composition other than titanium carbide was also formed. The composition other than the titanium carbide is titanium oxide which cannot be carbonized and graphite derived from a raw material. However, in Comparative Examples 1 to 6, when compared with Example 1, the amount of titanium carbide was small.
10．．．微粒子製造裝置10. . . Microparticle manufacturing device
12．．．電漿炬12. . . Electric torch
12a．．．石英管12a. . . Quartz tube
12b．．．高頻率發振用線圈12b. . . High frequency vibration coil
12c．．．電漿氣體供應口12c. . . Plasma gas supply port
14．．．材料供應裝置14. . . Material supply device
14a．．．漿料14a. . . Slurry
14b．．．容器14b. . . container
14c．．．攪拌機14c. . . Mixer
14d．．．幫浦14d. . . Pump
14e．．．噴霧氣體供應源14e. . . Spray gas supply
14f．．．供應管14f. . . Supply tube
15．．．一次微粒子15. . . Primary particle
16．．．反應室16. . . Reaction chamber
17．．．天板17. . . Sky
17a．．．內側部天板零件17a. . . Medial part
17b．．．外側部天板零件17b. . . Outer part of the sky
17c．．．上方外側部天板零件17c. . . Upper outer roof part
17d．．．通氣路17d. . . Ventilation road
18．．．微粒子(二次微粒子)18. . . Microparticles (secondary particles)
19．．．氣旋19. . . cyclone
19a．．．入口管19a. . . Inlet tube
19b．．．外筒19b. . . Outer tube
19c．．．圓錐台部19c. . . Conical table
19d．．．粗大粒子回收室19d. . . Coarse particle recovery room
20．．．回收部20. . . Recycling department
20a．．．回收室20a. . . Recycling room
20b．．．過濾器20b. . . filter
20c．．．管20c. . . tube
22．．．電漿氣體供應源twenty two. . . Plasma gas supply
24．．．熱電膠火焰twenty four. . . Thermoelectric glue flame
26．．．管26. . . tube
28．．．氣體供應裝置28. . . Gas supply device
28a．．．管28a. . . tube
28b．．．氣體射出口28b. . . Gas injection
28c．．．氣體射出口28c. . . Gas injection
28d．．．壓縮機28d. . . compressor
28e．．．管28e. . . tube
[第1圖]係表示為實施本發明實施形態的碳化物微粒子之製造方法時的微粒子製造裝置之全體構成的模式圖。[Fig. 1] is a schematic view showing the overall configuration of a fine particle production apparatus in the method of producing a carbide fine particle according to an embodiment of the present invention.
[第2圖]係表示擴大第1圖中電漿炬附近的剖面圖。[Fig. 2] is a cross-sectional view showing the vicinity of the plasma torch in the first drawing.
[第3圖]係表示擴大第1圖中之反應室(chamber)之天板及在該天板所具備的氣體射出口附近之剖面圖。[Fig. 3] is a cross-sectional view showing the expansion of the chamber of the reaction chamber in Fig. 1 and the vicinity of the gas ejection port provided in the sky plate.
[第4圖]係表示第1圖中之擴大旋風分離機(cyclone)之剖面圖。[Fig. 4] is a cross-sectional view showing an enlarged cyclone in Fig. 1.
[第5圖]係表示所射出的氣體之角度的說明圖，(A)係通過反應室之天板的中心軸之垂直方向的剖面圖，(B)自下方觀察天板的下面圖。[Fig. 5] is an explanatory view showing the angle of the gas to be emitted, (A) is a cross-sectional view in the vertical direction of the central axis of the sky plate passing through the reaction chamber, and (B) is a lower view of the sky plate viewed from below.
[第6圖](A)係表示本發明實施例之碳化物微粒子之製造方法所使用的氧化鈦藉由X光繞射法之結晶構造的分析結果圖，(B)係表示本發明實施例所得的碳化鈦藉由X光繞射法之結晶構造的分析結果圖。[Fig. 6] (A) shows an analysis result of a crystal structure of a titanium oxide used in a method for producing a carbide fine particle according to an embodiment of the present invention by an X-ray diffraction method, and (B) shows an embodiment of the present invention. The analysis result of the crystal structure of the obtained titanium carbide by the X-ray diffraction method.
10．．．微粒子製造裝置10. . . Microparticle manufacturing device
12．．．電漿炬12. . . Electric torch
12b．．．高頻率發振用線圈12b. . . High frequency vibration coil
14．．．材料供應裝置14. . . Material supply device
14a．．．漿料14a. . . Slurry
14b．．．容器14b. . . container
14c．．．攪拌機14c. . . Mixer
14d．．．幫浦14d. . . Pump
14e．．．噴霧氣體供應源14e. . . Spray gas supply
14f．．．供應管14f. . . Supply tube
15．．．一次微粒子15. . . Primary particle
16．．．反應室16. . . Reaction chamber
17．．．天板17. . . Sky
18．．．微粒子(二次微粒子)18. . . Microparticles (secondary particles)
19．．．氣旋19. . . cyclone
19a．．．入口管19a. . . Inlet tube
19b．．．外筒19b. . . Outer tube
19c．．．圓錐台部19c. . . Conical table
19d．．．粗大粒子回收室19d. . . Coarse particle recovery room
19e．．．內管19e. . . Inner tube
20．．．回收部20. . . Recycling department
20a．．．回收室20a. . . Recycling room
20b．．．過濾器20b. . . filter
20c．．．管20c. . . tube
22．．．電漿氣體供應源twenty two. . . Plasma gas supply
24．．．熱電膠火焰twenty four. . . Thermoelectric glue flame
26．．．管26. . . tube
28．．．氣體供應裝置28. . . Gas supply device
28c．．．氣體射出口28c. . . Gas injection
28d．．．壓縮機28d. . . compressor
28e．．．管28e. . . tube
R．．．箭頭R. . . arrow
Q．．．箭頭Q. . . arrow
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| US20080006954A1 (en) * | 2004-09-07 | 2008-01-10 | Kazuhiro Yubuta | Process and Apparatus for Producing Fine Particles |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201129499A (en) | 2011-09-01 |
| WO2011034129A1 (en) | 2011-03-24 |
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