TW200536776A - Method and device of manufacturing microparticles - Google Patents

Method and device of manufacturing microparticles Download PDF

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Publication number
TW200536776A
TW200536776A TW093140405A TW93140405A TW200536776A TW 200536776 A TW200536776 A TW 200536776A TW 093140405 A TW093140405 A TW 093140405A TW 93140405 A TW93140405 A TW 93140405A TW 200536776 A TW200536776 A TW 200536776A
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TW
Taiwan
Prior art keywords
fine particles
liquid
gas
fluid
powder
Prior art date
Application number
TW093140405A
Other languages
Chinese (zh)
Inventor
Seiichiro Takahashi
Hiroshi Watanabe
Original Assignee
Mitsui Mining & Smelting Co
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Publication date
Application filed by Mitsui Mining & Smelting Co filed Critical Mitsui Mining & Smelting Co
Publication of TW200536776A publication Critical patent/TW200536776A/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
    • C01B13/322—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005—Separating solid material from the gas/liquid stream
    • B01J8/0055—Separating solid material from the gas/liquid stream using cyclones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/026—Spray drying of solutions or suspensions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
    • C01B13/326—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the liquid state
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/34—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of sprayed or atomised solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/0821—Oxynitrides of metals, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00108—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00112—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00114—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant slurries
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00121—Controlling the temperature by direct heating or cooling
    • B01J2219/00123—Controlling the temperature by direct heating or cooling adding a temperature modifying medium to the reactants
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00159—Controlling the temperature controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0877—Liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0879—Solid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

This invention provides a method and a device of manufacturing microparticles, thereby the particles such as microparticles of oxides can be made at low cost through a simpler device. The method and device are suitable for the production of ITO particles. The method of this invention comprises the steps of: supplying the raw materials in the either state of liquid flow, liquid drop or particle to heat source, capturing the products as microparticle by using atomized liquid fluid, and recovering the above microparticles in the form of slurry by gas-liquid separation.

Description

200536776 九、發明說明： 【發明所屬之技術領域】 本舍明係有關氧化銦-氧 方法及减料末寺的微粒子之製造 【先前技術】 般’作為薄膜之成膜的方法之_ (sputtering)法。測* 土 〆σ、有贏鍵 實施職，藉以製=膜=濺Γ縣―enngta㈣ 能有效成膜高性能之膜故 方、大面積化的容易性、 月匕之版之故，而應用於工業上。7 &lt;么 來，作為濺鍍之方式而周知有在反應 = ‘靶之月面設置磁石以謀求薄膜來成 之同遝化的磁控濺鍍（magnetron邛似如^)等。 乳化錫（In2cvSn〇2之複合氧化物，以下簡稱「ιτ〇」）膜之 =見光穿，，且導電性良好之故，作為透明導電膜而 射膜等。 直飞破璃之防、‘路用發熱膜、紅外線反 因此，為能高效率且低成本成膜起見，目前仍繼 斷地改良濺鑛條件或滅鑛裝置，而如何有效運用裝置即 為重要課題。另外，在此種IT0濺鍍中，從設置新的濺射 用標靶後至起始電弧(異常放電)消失並能製造製品為止的 時間較短、或經設置後能使用多久時_積雜時間 萆巴耐用壽命）將成為問題。 丁 此種ιτο濺射標靶，係將氧化銦粉末與氧化錫粉末按 ^16619 200536776 既定比例混合並按乾式或濕式成型且燒結者（專利文獻 1 )、冒經提架有為製得高密度之ϊτ〇燒結體用的高分散性 之氧化銦粉末（參照專利文獻2、3、4等）。 又，周知有將由共沈澱法所成濕式合成的ΙΤ〇粉末作 成ITO I结體的作法（參照專利讀5)，亦多數提案有按 同樣方式為製得高密度燒結體的汀〇粉末之濕式合成方法 (參照專利文獻6至9等）。 再者，冒經有在電漿電弧中使銦-錫合金與氧反應，並 在馬赫（Mach) 1 α上之氣流中依既定之冷卻速度以上人 卻:藉以製造ΙΤ0粉末的提案（參照專利文獻Π))。然而二 =使用馬赫1以上之高速氣流時等’因其設備龐大而 能低成本且高效率之方式製造ΙΤ0粉末的問題。 另方面’雖然非為1τ〇粉末之製造方法，惟作為) 蜀氧化物微粒子之製造方法，有如下述之方法之提案。; 二將金屬粉末供給於燃燒器火焰中，以製造氧化物; :子，二以固氣相分離的各種方法之提案(參照專利3 ^ X 金屬噴射氣體使諸體化， 搬運㈣料人液體中使其產生 應，以製造微粉體的方法之提案(參照專利文獻： 金屬體或金屬氧化物棒等原料體。 =:行溶融蒸發，並對此蒸發氣體噴吹冷卻：， 形=微粒子的方法之提案(參照專利文㈣至^ 然而，此種乾式合成，可能因不適合 ） 渴應用1T〇粉末之乾式合成於工業生產方式1 3] 9 200536776 • » [專利文獻1]曰本專利特開昭62_2175】號公報 [專利文獻2]曰本專利特開平5_193939號公報 · [專利文獻3]曰本專利特開平6_191 846號公報 ‘ [專利文獻4]日本專利特開2〇〇1_261336號公報 [專利文獻5]日本專利特開昭62_21751號公報 [專利文獻6]日本專利特開平9_221322號公報 [專利文獻7]曰本專利特開2〇〇〇_281337號公報 [專利文獻8]曰本專利特開2〇〇卜172〇18號公報 [專利文獻9]日本專利特開2〇〇2_68744號公報 [專利文獻ίο]曰本專利特開平11-11946號公報 [專利文獻11]曰本專利特公平15520〗號公報 [專利文獻12]日本專利特公平5_776〇1號公報 [專利文獻13]日本專利第3253338號公報 [專利文獻14]日本專利第3253339號公報 [專利文獻15]日本專利第3229353號公報 [專利文獻I6]曰本專利第3225〇73號公報 φ [專利文獻17]曰本專利特開昭6〇_71〇37號公報 [專利文獻18]日本專利特開2〇〇2_253953號公報 [專利文獻19]曰本專利特開2〇〇2-253954號公報 [專利文獻20]日本專利特開2〇〇2_263474號公報 【發明内容】 (發明所欲解決之課題） 本發明，鑑於此種情況下，係以提供能使用更簡便的 裝置且低廉的成本製造氧化物微粒子等微粒子，適合於制 316619 7 200536776 造ITO粉末的微粒子之製造方法及製造裝置為課題。 (用以解決課題之手段） 為解決前述課題的本發明之第丨態樣為一種微粒子之 製造方法，係製造微粒子的方法，而其特徵為··將呈液體 流、液滴或者粉末狀態之原料供給於熱源中，藉由霧狀之 液狀流體而將生成物作成微粒子並加以捕獲，以及藉由氣 液分離回收前述呈漿料態之微粒子。 在此種第1態樣中，經供給原料於熱源中所得的生成 物，將為霧壯:之液狀流體作成微粒子所捕冑，再經氣液分 離而南效率地回收。 本發明之第2態樣，係在第i態樣之微粒子之製造方 法，其中從原料之熔融液形成液體流或者液滴，而供給於 該熱源中。 在此種弟2態樣中，來自作為原料之金屬或合金等的 熔融液的液流或者液滴將在熱源中視情況成為氧化物，並 稭由霧狀之液狀液體而作成微粒子加以财。 本t發明之第3態樣’係在第1態樣之微粒子之製造方 法，其中形成原料之霧化粉末，而供給於該熱源中。 在此種第3態樣中，；y v p 4、a 原枓之金屬或合金等將作成霧化 4末而供給於熱源中，並作成微粒子。 子之4態樣，係在第1至3之任—紐之微粒 離。 《中使用力疋風器(cycl〇ne)以實施該氣液分 在此種第4態樣中 微粒子將藉由旋風器實施氣液分 316619 200536776 離而作成液狀流體之漿料加以回收。 本發明之第5態樣， 子之製造方法，苴中兮气 #至4之任-態樣之微粒 火焰。 〃中d原，係乙诀火焰或叫直流）電聚 在此種第5態樣中，# 火焰而作成微粒子。原科將错由乙块火焰或此電聚 子之^:::第6態樣’係在第1至5之任-態樣之η粒 子之“方法，其中該液狀流體，係水。 …“立 在此種第6態樣中，生 《 加以回收。 成物即為水所捕獲而作成漿料 本赉明之第7態樣，係在繁 子之製造方法，’、 至6之任一態樣之微粒 子去其中该原料係選自金屬、合全、氧化你 氮化物以及氧氮化物中的至少一種。 …化物、 在此種第7態樣中，金屬、人入、於 及氧氮化物等原料，作成微粒子。减物乱化物以 子之二ϊ樣’係在第1至7之任'態樣之微粒· 任一者，可制―、§玄熱源，係氧化大氣或者氮化大氣之 任C 衣件氣化物、氮化物以及氧氮化物之任1粒 子0 8態樣中’原料將在氧化大氣或者在氧化大 狀，”、&quot;’、，作成氧化物、氮化物或者氧氮化物之 子。 ==之第9態樣’係在第]至7之任一態樣之微粒 子之Ά法，其中該原料，係In_Sn合金或者ITO粉末， 316619 200536776 而可製造氧化銦-氧化錫粉末者。 在此種第9態樣中，從In-Sn合金或者ITO粉末，可 製造1T 0粉末之料漿。 本發明之第1 0態樣，係在第9態樣之微粒子之製造方 法’其係製造錫含量’以換算成S n〇2計，為2 · 3至4 5質 里乂之氧化姻-氧化錫粉末。 在此種第1 0態樣中，藉由既定量之氧化錫而可保持 1丁〇之導電性。 本發明之第11態樣，係在第丨至10之任一態樣之微 粒子之製造方法，其中該生成物被該液狀液體所捕獲時之 最大速度為150m/秒以下。 在此種第11態樣中，可以比較低的流速製造微粒子t 、.本發明之第12態樣為—種微粒子之製造裝置，其特徵 為·具備將呈液體流'液滴或者粉末狀態之原料供給於熱 源所得的生成物與氣體流體—起導入的導入口、對所導^ mr射霧狀之液狀流體的流體噴射手段、將液狀流 隻的㈣子加以氣液分離以製得該微粒子之衆料的 子：刀雄手1又、以及將含有未能被液狀流體所捕獲的微粒 :::::體之—部分送回至流體滴喷射位置以二 在此種第12態樣中，原料經供給於熱源 物，即為霧狀之液狀产雕而从Λ、〜 厅仔生 广 肢而作成微粒子所捕獲並經氧 碓俊，氣氛流體之至少—邱八目 度加以ν夜分離而二 猶環手段之循環， 乳救刀離而可尚效率地回收。 316619 10 200536776 本發明之第13態樣，係 裝置’其中於該氣液分離手段之下：之微粒子之製造 能為液狀流體所捕獲的微粒子的：有未 時，噴射霧狀之液狀流體並加部分之同 之漿料的第2氣液分離手段。 ”離以衣得該微粒子 率地=二:3態樣中，藉由第2氣液分離手段而可有效 卞地回收未旎破回收的微粒子。 ’及 _ I:之第Μ態樣，係在第13態樣之微粒子之製造 :ι、、中於该氣液分離手段之下 &lt; 為液狀流體所捕獲的微粒子的大氣氣體之二、2: 第2氣液分離手段之導入部的第2循環手段:亥 在此種第態樣中，在第2氣液分離= 了的大氣流體將再度加以氣液分離，微 政率地回收。 j I J β hT月之第15態樣，係在第]2至】4之任-態樣之微 -子之表造裝置’其中該氣液分離手段，係旋風器。· 在此種第15態樣中，使用旋風器即可連續性且有 万式實施氣液分離。 本發明之第16態樣，係在第】2至15之任一態樣之微 :子之製造裝置，其中微粒子被該流體噴射手段所喷射的 ’之狀流體所捕獲時之最大速度，為l5〇m/#以下。 在此種第]6態樣中，可以比較低的流速製造微粒子。 【發明之效果] 如上所述，如採用本發明而將原料金屬或合金作成液 Π 316619 200536776 流、液滴或者粉末導入熱源中所得的生成物，藉由霧狀之 錄流體加以捕獲，即可發揮能有效率且簡便方式製造微 粒子的效果。 【實施方式】 [發明之最佳實施形態] ★ 明之微粒子的方法中，係將原料作成液 '*、液滴或者粉末’以供給於熱源中。 在此，原料係例如， 可例舉：峋、A1、) F或s金，而金屬或合金而言， 或此等的合金。又，:=Fe、Sl、In_、s_ew 等氧化物、氮化物及，，料而使用上述的金屬或合金 含有複合氧化物，而；：：。另外，在此，氧化物中， 此種原料，π·: 中則含有複合氮化物。 或作成粉末狀離…入1㈣的狀11之液流或液滴供給， 液流或液滴之;炫融液r曹等連續性作成 供給之方式。 s木用形成務化粉末後將此等 例如，如將In“Sii人 又，如將ITO粉末作為^為原料’則可得1丁〇粉末。 末。 ’’’、…4 ’亦可得性狀不相同的1丁〇粉200536776 IX. Description of the invention: [Technical field to which the invention belongs] The present invention is related to the indium oxide-oxygen method and the production of fine particles of the cut-off temple. [Prior technology] The method of (sputtering) is generally used as a film forming method . Measure * soil 〆σ, have a winning key to implement the post, so that = film = splash Γ county ―enngta ㈣ can effectively form high-performance film, the ease of large area, the reason of the version of the moon dagger, and applied to Industrially. 7 &lt; Well, as a method of sputtering, it is known that magnetron sputtering (magnetron like ^) which is provided with a magnet on the moon surface of the target to achieve a thin film to synchronize. Emulsified tin (In2cvSn〇2 composite oxide, hereinafter referred to as "ιτ〇") film = see through light, and because of its good conductivity, film as a transparent conductive film. Anti-flying glass protection, road heating film, infrared reflection. Therefore, in order to be able to form films with high efficiency and low cost, the splattering conditions or ore killing devices are still being improved. How to effectively use the devices is important topic. In addition, in this type of IT0 sputtering, the time from when a new sputtering target is set until the initial arc (abnormal discharge) disappears and the product can be manufactured is short, or how long can it be used after being set_ Time 萆 bar durable life) will become a problem. This type of ιτο sputtering target is made by mixing indium oxide powder and tin oxide powder at a predetermined ratio of ^ 16619 200536776 and molding it dry or wet and sintering (Patent Document 1). Density ϊτ〇 Highly dispersible indium oxide powder for sintered bodies (see Patent Documents 2, 3, and 4). In addition, it is known to make a wet-synthesized ITO powder made by the co-precipitation method into an ITO I structure (refer to Patent Reading 5), and many proposals have also been made for the preparation of high-density sintered tingo powder in the same manner. Wet synthesis method (refer to Patent Documents 6 to 9 and the like). Furthermore, it has been suggested that the indium-tin alloy reacts with oxygen in a plasma arc and is cooled at a predetermined cooling rate in a gas flow on Mach 1 α: a proposal to manufacture ITO powder (see patent Document ii)). However, two = when using high-speed airflow of Mach 1 and the like 'because of its large equipment, it can produce ITO powder at a low cost and high efficiency. On the other hand, although it is not a method for producing a 1τ〇 powder, it is proposed as a method for producing a fine particle of sulfide oxide as follows. Second, supply metal powder to the burner flame to produce oxides; Second, proposals for various methods of solid-gas phase separation (refer to patent 3 ^ X metal jet gas to make various bodies, transporting human liquids) Propose a method for producing micropowders in response to the problem (refer to Patent Documents: Raw materials such as metal bodies or metal oxide rods. =: Melt and evaporate, and evaporate the evaporative gas to cool it:, shape = fine particles Proposal of the method (refer to Patent Documents ㈣ to ^ However, this dry synthesis may not be suitable) Dry synthesis of 1T〇 powder is used in industrial production methods 1 3] 9 200536776 • »[Patent Document 1] Japanese Patent Laid-Open Sho 62_2175] [Patent Literature 2] Japanese Patent Laid-Open No. 5_193939 · [Patent Literature 3] Japanese Patent Laid-Open No. 6_191 846 '[Patent Literature 4] Japanese Patent Laid-Open No. 2000-261336 Patent Literature 5] Japanese Patent Laid-Open No. 62_21751 [Patent Literature 6] Japanese Patent Laid-Open No. 9_221322 [Patent Literature 7] Japanese Patent Laid-Open No. 2000-281337 [Patent Literature 8] Japanese Patent special Japanese Patent Publication No. 172〇18 [Patent Document 9] Japanese Patent Laid-Open Publication No. 2000-68744 [Patent Document ίο] Japanese Patent Publication No. 11-11946 [Patent Document 11] Japanese Patent Publication No. 15520 [Patent Document 12] Japanese Patent Publication No. 5_776〇1 [Patent Document 13] Japanese Patent No. 3253338 [Patent Document 14] Japanese Patent No. 3253339 [Patent Document 15] Japanese Patent No. 3293353 [Patent Document I6] Japanese Patent Publication No. 3225〇73 φ [Patent Literature 17] Japanese Patent Publication No. S60-71〇37 [Patent Literature 18] Japanese Patent Publication No. 2000-253953 [ Patent Literature 19] Japanese Patent Laid-Open No. 2000-253954 [Patent Literature 20] Japanese Patent Laid-Open No. 2000-263474 [Summary of the Invention] (Problems to be Solved by the Invention) The present invention is made in view of such problems. In this case, it is an object to provide a method and a device for manufacturing fine particles such as oxide particles, which can be used with simpler equipment and low cost, and are suitable for making 316619 7 200536776 for making ITO powder. (Means to solve the problem In order to solve the aforementioned problem, the first aspect of the present invention is a method for manufacturing fine particles, which is a method for manufacturing fine particles, and is characterized in that a raw material in a liquid flow, a droplet, or a powder state is supplied to a heat source by The product is made into fine particles by misting the liquid fluid and captured, and the fine particles in a slurry state are recovered by gas-liquid separation. In this first aspect, the product obtained by supplying the raw material to the heat source will be captured by the mist-like liquid fluid as fine particles, and then separated by gas-liquid separation and efficiently recovered in the south. A second aspect of the present invention is a method for manufacturing fine particles in the i-th aspect, wherein a liquid stream or a droplet is formed from a melt of a raw material and supplied to the heat source. In this second aspect, the liquid stream or droplets from the molten liquid such as a metal or an alloy as a raw material will become oxides as appropriate in the heat source, and the particles are made of fine particles from the misty liquid liquid. The third aspect 'of the present invention is a method for producing fine particles in the first aspect, in which atomized powder of a raw material is formed and supplied to the heat source. In this third aspect, y v p 4, a raw metal or alloy, etc. will be atomized 4 and supplied to a heat source, and made into fine particles. The 4th aspect of the son is in the first to the third-the particles of the button. << In the fourth aspect, the micro-particles will be separated by a cyclone to realize the gas-liquid separation. 316619 200536776 is used to separate the fine particles into a slurry of a liquid fluid and recovered. The fifth aspect of the present invention, the manufacturing method of the son, 苴 中西 气 # to 4 of any-aspect of the particle flame. In the 5th aspect of the fifth aspect, #Flame is made into particles. The original section will mistake the ^ ::: 6th aspect of the flame of this block or this polymer to the "n-state" of any of the first to fifth aspects of the "eta particle" method, wherein the liquid fluid is water. … "Stand in this sixth aspect and recycle it. The final product is the seventh aspect of the slurry that is captured by water. It is in the manufacturing method of the progenitor. Any of the fine particles in any of the aspects from to 6 is used. The raw material is selected from the group consisting of metal, alloy, and oxidation. At least one of your nitrides and oxynitrides. ... In this seventh aspect, the raw materials such as metal, manganese, and oxynitride are made into fine particles. Substances that are reduced in size are in the form of particles in any of the 1st to 7th styles. · Any of them can be made into §, § Xuan heat source, which is an oxidizing atmosphere or a nitriding atmosphere. Any one of the particles, nitrides, and oxynitrides in the 08 state, 'the raw material will be oxidized in the atmosphere or oxidized,' ", &quot; ', and will be the sons of oxides, nitrides, or oxynitrides. == The ninth aspect 'is a method of fine particles according to any one of the aspects] to 7, wherein the raw material is In_Sn alloy or ITO powder, 316619 200536776, and indium oxide-tin oxide powder can be manufactured. In the ninth aspect, a slurry of 1T 0 powder can be produced from an In-Sn alloy or ITO powder. The tenth aspect of the present invention is a method for manufacturing fine particles in the ninth aspect, which is to produce tin content 'In terms of Sn02, it is a powder of 2-3 to 4 5 mils of tin oxide-tin oxide powder. In this 10th aspect, 1 tin can be maintained by a given amount of tin oxide. 〇。 Electrical conductivity. The eleventh aspect of the present invention is a method for manufacturing fine particles in any one of aspects 丨 to 10, wherein the The maximum speed when an object is captured by the liquid liquid is 150 m / sec. In this eleventh aspect, the particles t can be produced at a relatively low flow rate. The twelfth aspect of the present invention is the production of a kind of particles The device is characterized in that it is provided with a product and a gaseous fluid obtained by supplying a raw material in the form of a liquid stream or a liquid state to a heat source and a gaseous fluid, an introduction port for introducing the fluid, and a mist-like liquid fluid guided to the guided fluid. The spraying method is to separate the maggots in the liquid state by gas-liquid separation to obtain the particles of the fine particles: the sword male hand 1 and the particles that have not been captured by the liquid fluid ::::: Part of the body-Partially returned to the fluid droplet ejection position. In this twelfth aspect, the raw materials are supplied to the heat source, that is, the misty liquid production carving is made from Λ, ~ Hall Tsai's wide limbs. The particles are captured and passed through the oxygen, the atmosphere fluid is at least-Qiu Bamu degrees separated by ν night and the cycle of the two still ring means, the milk is rescued and the knife can be recovered efficiently. 316619 10 200536776 The 13th state of the present invention In this way, the device 'is one of the means of gas-liquid separation Bottom: The production of fine particles can be captured by the liquid fluid: There is a second gas-liquid separation means that sprays the liquid fluid in the form of mist and adds a part of the same slurry. In the microparticle ratio = two: 3 aspect, the second gas-liquid separation means can effectively recover fine particles that have not been recovered. 'And _ I: The Mth aspect is the production of the microparticles in the 13th aspect: ι, under the gas-liquid separation means &lt; the second atmospheric gas of the microparticles captured by the liquid fluid, 2: The second circulation means of the introduction part of the second gas-liquid separation means: In this kind of aspect, the atmospheric fluid with the second gas-liquid separation = will be subjected to gas-liquid separation again, and it will be recovered with little effort. The fifteenth aspect of j I J β hT is in any of [2] to [4]-the micro-child's surface-making device ', wherein the gas-liquid separation means is a cyclone. • In this fifteenth aspect, the use of a cyclone enables continuous and gas-liquid separation. The sixteenth aspect of the present invention is a micro: zig manufacturing device according to any one of the second to fifteenth aspects, wherein the maximum speed at which the microparticles are captured by the 'like fluid' ejected by the fluid ejection means is l50m / # or less. In this aspect], fine particles can be produced at a relatively low flow rate. [Effects of the Invention] As described above, if the raw material metal or alloy is used as the liquid Π 316619 200536776 to introduce a stream, droplets, or powder into a heat source, and the product is captured by a misty recording fluid, The effect of producing fine particles efficiently and simply is exerted. [Embodiment] [The best embodiment of the invention] ★ In the method of the fine particles of the Ming, the raw material is made into liquid '*, droplet or powder' to be supplied to the heat source. Here, the raw material may be, for example, rhenium, Al, F or s gold, and in the case of a metal or an alloy, or an alloy thereof. In addition,: = Fe, Sl, In_, s_ew and other oxides, nitrides, and the above-mentioned metals or alloys are used to contain composite oxides, and ::. Here, in the oxide, such a raw material contains a composite nitride in π · :. Or it can be made into powder form, and it can be supplied in the form of liquid stream or liquid droplets in the shape of 1㈣, and the liquid stream or liquid droplets can be supplied continuously. After forming a chemical powder for wood, for example, if In "Sii" is used, and if ITO powder is used as a raw material, then 1 but 0 powder can be obtained. Finally, "", ... 4 "can also be obtained 1 different powder with different properties

又’熱源而言I 的熱源，例如，乙炔大氣或氮化大氣 祇要是能炼融金屬^ /* 63寺。熱源之溫度， 物，並充分使t氧者氣化物或氮化物或者氧氮化 况八虱化或虱化的程度 一般，W火焰時為數千U上 將叫別限定。 -电漿火焰時為數萬 316619 12 200536776 °c以上。 如對此種乙炔火焰或DC電聚火想將原料作成液、'“ 給時，則生成物即可與氣體流一起按繼 或氮化物或者氧氮化物而製得。原料按原狀之 二生成物製得，抑或按金屬或合金之氧化物或 :化物=氧氮化物製得，全靠熱源…之狀態所決 X作成氧化大氣，則可製得金屬或合金之氮化或氧氮 化物。又’即使作為原料而使用氧化物或氮化物或者氧氣 化物，仍能製得性狀不相同的氧化物或氮化物或者氧氮化 物0 本發明中，係藉由霧狀之液狀流體以捕獲所得的生成 勿亦即，對於與乙炔火焰或Dc電漿火焰之噴流一起流 動的生成物噴霧霧狀之液狀流體，較佳為霧狀之水。由此^ 生成物急冷而成為微粒子，結果成為經噴霧的液狀流體之 漿料。 ^在此，務狀之液狀流體之供給，祇要是作成能捕獲所 得的生成物並加以冷卻之方式則並不特別限定。例如，使 用水的情形，可使用常温之水，較佳為常溫之純水，惟亦 可使用冷卻水。 生成物作成微粒子而捕獲時，則捕獲時之最大速度為 例如’]5〇m/秒以下，較佳為1 00m/秒以下之程度。 本發明中，係將含有經噴霧的液狀流體所捕獲的微粒 十的液狀流體加以氣液分離，並將微粒子作為漿料加以回 收。在此，漿料之回收方法並不特別限定，惟較佳為可使 ^16619 200536776 用旋風器實施。 丄發日月，作為原料而使用心合金或IK)粉 I 造戲-氧化錫(ίΤ〇)粉末。如此方式所製造 的ΙΤΟ粉末，因hi9CK φ少e a ,L _ . 中之 Sn〇2 固溶體（solid 5〇1加1〇11)量 ^之:水準之故，燒結性高，可較容易製得高密度之燒 二肢’其結果可製得耐用壽命較長的標革巴。另外，如將由 各種製造方法所製造的ΙΤΩ 、 ^ ^ ^ ΤΤΠ 4.V i 4末，或粕碎經燒結的I丁〇燒 =〇 φ末作為原㈣，可製得與原料不相同的性狀 以3中之8吨之固溶體量為高水準的ιτ〇粉末。 另外’此種ΙΤ0粉東，可你炎TT。 田L ^ 不可作為Ιτ〇濺射用標靶材料使 用。此種ΙΤ0濺射用標靶之材料而t， 旦 算計，較佳為在2.3至45質量％/，3^Sn〇2換 以下，在麥照弟！圖之下說明實施本發 子之製造裝置之一例。 乃忐的U粒 t裝置具備有：形成氧化大氣或氮化大氣的熱源之乙 二八^或DC電毁火焰所成火焰i中能將所供給的金屬或 e金等原料2作成液流、液滴或者粉末供給〆 物3，i氧髅 '户顺 土、首 ^ 衣件的生成 /、孔妝級肢一起導入的導入口 10、及對所導入 立子嘴射霧狀之液狀流體的流體喷射手段2Q、 、广二 流體㈣獲的㈣子加錢液分離以製得前述微 料的虱液分離手段之旋風器3〇、以及將含有未能 ： 體捕獲的微粒子的大氣流體之一部分送回二（* 置並使其猶環的循環手段40。 吻射位 在此，導入口 10,祗要是能導入含有生成物的氣體流 316619 14 200536776 者’則並不拉兄丨丨服— 、 讨⑴限疋’惟亦可作成能吸引氣體流之方式。 &quot;丨L版ϋ貝射手段20，係經設置在設置有導入口 10的導 ^ 下兩1側而具有能噴射流體（例如，水）的複數個喷 射、貝窝21、及為對噴射噴嘴21導入流體用的泵22以及裝 滿流體用的洁〇 、， 七〜3。來自噴射噴嘴21的流體之喷射方 二' :彳寸別限疋，可為朝向能與從導入口 1 0所導入的流體 ’L動方向合流的方向喷射。從導入π 1 0所導入的氣體 二所3的生成物3，係經噴霧的流體，例如，水而冷卻， 並作為微粒子所捕獲。在此，雖然在導人管11之噴射噴嘴 1〜下游侧设置經縮小流路的文丘里加仙⑴部U以防 ^氣液混合物之流速之低落，惟文丘里部]2不-定需要設 ^二，噴射喷嘴21及系22不—定需要設置，亦可作成 ^孔月丑*之流動所引起的吸引力而吸引液體喷射之方 广：口 10的導入口 11，係連通於屬於氣液分 &quot;又、f風器30之導入口 31。從旋風器30之導入口 3 、、勺氣液心σ物，則成為沿著旋風器本體32之内壁c 二的屑而進行氣液分離，並作成液體成分，亦即，」 ::::的聚料即落下至下部，而氣體成分則從排氣口; 排出之方式。 即：實施形態中，在排氣口 34設置有循環手段40。功 印’排氣口 34上設置有盥導入其n令道\ 的循^ w 以〃、¥^ 11之導人σ附近連ϋ (J,V 1，並於循環管41之中途介裝有鼓風招 〇、叫42，此寺機件構成循環手段4G。藉由該猶環手段 316619 15 200536776 40 ’使未能完全捕獲的粉虫、、，+ 提升捕獲效率。 末运回嘴射喷嘴21之上游側，以 又，經旋風器30氣液分 環之:自:，得微;=:=物 末自紅風器30的排氣之 管41進行循環，惟作往循環 度則從第2排出口 35排出之方式。 +分之-程 本實施形態中，於第2排^口 35 ㈣有屬於第2氣液分離手段的第2旋風=㈣氣管43 &quot;5〇,基本上具有與旋風器30同樣構心且右! 2旋風 作用。亦即，從將連接排氣管43的導二/]、=液分離 液混合物，成為沿著旋風器本體52 =入的氣 而進行氣液分離，並作成液體成分，亦即人^渴流53 漿料即落下至下^卩彳乡 各有彳政粒子的 …式。再:：二:…排出，積存於流體槽 流路的文丘里部二並：='43,中途設置有經縮小 槽㈣水循環管62。由此，藉由文丘 ^^與流體 體流動，流體槽61中之水即經吸引而切於文之向速的氣 =成:體中所殘存的微粒子捕獲於液體内之A部： 〇有二口 55上連接有排氣管7】，而排氣二： 广機72’作成經由該第2鼓風機:2: 排…5的氣體之方式。另外，如欲將水槽:： 316619 16 200536776 水口A蔡於排氣管4 3内睹，日丨丄 泵與喷霧噴嘴以奋扩、，、丨〇上述的旋風器30般，使用 可設置過遽器(;C:，61上，如上述方㈠ 分離槽。再者，亦可作成使Λ置排中^麦分離微粒子的沈降 循環於排氣管43之 乳口 55的排氣之一部分 捕獲效率。 里部44之上游側之方式，以提升 另外’如僅用旋風哭 時，則不一定币 。。，&quot;被粒子之捕獲效率足夠 疒 要扠置第2旋風器50,又，如欲再楹古捕 後效率時，則亦可再連結複數個旋風哭。右人朴间捕 粒子^表示使用以上所說明的實施形態之裝置以製造微 (貫施例1) 將In-Sn合金（Sn9 6重量％)之霧化粉末（平均 :):。入於乙块火焰中以乾式合成聊一^ =里二）粉末，並使用袋式收座機mter)加以乾式回 收，作為實施例1之ΙΤΌ粉末。 (實施例2) ΙΤ〇==ηΓ樣方式經使用乙块火焰之乾式合成的 π、碏由°貝務水加以濕式回收，將此作為實施例2 之1το粉末。 (比較例1) 將經濕式合成的氧化銦粉末在1000t下煅燒的氧化 :知末90 I里/〇、與將同樣經濕式合成的氧化錫在1 〇〇〇 c下ife燒的氧化錫粉末10質量％一起在研鉢中混合者作 316619 17 200536776 為比較例i，並作為標準品]。 (比較例2) 作為比較例 將經依共沈澱法之濕式合成的ίτ〇粉末， 2之ΙΤΟ粉末。 依共沈澱法實施濕式合成之步驟，係如下所示。亦民 在常溫下’將In(4N)2Gg溶解於石肖酸（試藥特級/濃度^ ’ 至61%)133cc(pH叫_5)中，另外，在常溫下，將如(4&amp; 溶解於鹽酸（試藥特級：濃度35至36%)1〇〇cc(pH叫9)中g 混合兩者以作成混酸溶液。此時，並無析出物之存在，而 PH為-L5。接著，對此混酸中混合25%氨水（試藥特級）以 使1中和並作成ΡΗ ^ 6·5之結果，析出有白色沈㈣。數 小日寸後’棠去上清水’使用純水2公升⑴洗淨3小時後， ^(TC下乾燥並在_。口培、烤3小時以使其脫水反應而 製得濕式合成ITO粉末。 (比較例3) 一將使用經濕式合成的氧化銦粉末與氧化錫粉末的混合 物(氧化錫10重量％)之粉末在]55(rcu上所燒結的燒結體 加以粉碎者，作為比較例3 2IT〇粉末。 (試驗例1) 就貝轭例1、2及比較例丨至3之各Ιτ〇粉末，求出 S]叫固溶體量。其步驟為如下所示。另外，在未實施試驗 之前，就實施例卜2及比較例2、3之ΙΊΌ粉末，在大氣 中在10GGC下椴燒3小時以使作為微小粒子所析出的 Sn〇2成長，以便容易能作為Sn〇2檢測之方式。 316619 18 200536776 1. 首先，實施感應耦合高頻電漿光譜分析（icp光譜分析）。 由此結果，In、Sn以外均為氧氣◦，並假定該〇量可能有 不足心下，求出ln與Sn的比值，並算出該&amp;及％之全 部變成I】i2〇3、Sn〇2時的重量比。 2. 就實施例1、2及比較例i至3之ΙΤ〇粉末，實施採用粉 末X射線繞射（XRD:麥克科學公司製、μχρ18Γ[^^分析， 以求出Sn〇2析出量。亦即，從繞射結果確認有無存在夾 雜化合物（nuercalatl0n c〇mp〇und，In4Sn3〇]2)，如未能檢測 到夾雜化合物時，則作為比較例丨之標準品丨而從各試料 之Ill2〇3(222)積分繞射強度及Sn〇2( 11 0)積分繞射強度之 比长出Sn〇2析出里（質量％)。亦即，sn〇2之析出量（質量 %)，係可從X射線繞射之積分繞射強度比求出的“a之 含量，而假定未固溶於hl2〇3的Sn〇2係因1〇〇〇t：程度之煅 少兀而成長並成為X射線繞射之Sn〇2(i丨〇)之蜂值者。第2 圖至第6圖中表示x射線繞射之結果。 3·從1及2之結果，將雖然在icp分析經檢測，惟在X射 線繞射中則未能檢測為Sn〇2(11〇)的Sn〇2，作為中 之Sn〇2固溶體量。 一 將此專結果表示於表1中。 〜由此結果可知’在實施例卜2之ΪΤΟ粉末之Sn〇2固 冷里為2.35重量％、2 42重量％、而較經濕式合成之汀〇 粉末的比較例2之2·26重量％為多的事實。另外，將一度 作成燒結體者加以粉碎的比較例3之ΙΤ〇粉末中，則檢測 有夾雜化合物之存在，,准Sn〇2固溶體量則未能檢測二 316619 200536776 表1 試料 號碼 1CP之結杲 XRD之結果 Sn02 固溶砬量 (重量％) In (重量％) Sn (重量％) ]n2〇3 (重量％) Sn〇2 (重量％) 失雜 化合物 ]n〇3 (222) Sn〇， 010) Sn02 析出量 (重量％) 實施例1 74.1 8.26 89.52 10.48 無 6974596 35782] 8.13 2.35 實施例2 74.8 7.90 89.92 10.08 無 6875331 331124 7.66 2.42 比較例] 75.1 7.87 90.09 9.91 無 7]4]62】 455777 9.9】標準 0.00 比較例2 76.1 8.03 90.03 9.97 無 72734]] 352429 7.71 2.26 比較例3 74.8 7.90 90.02 9.98 有 7529677 105639 - - (實施例3) 將In-Sn合金（Sn為9.6重量％)之霧化粉末（平均粒徑馨 45//m)，導入於DC電漿火焰中以乾式合成IT〇（In2〇3: SnO2 = 90 ·· 10重量％)粉末，並將此使用噴霧水加以濕式回 收，作為實施例3之ITO粉末。 (比較例4) 與比較例1同樣方式，將經濕式合成的氧化銦粉末經 1 000°C下煅燒的氧化銦粉末90質量％、與將同樣經濕式合 成的氧化錫經l〇〇〇°C下鍛燒的氧化錫粉末10質量％—起 在研鉢中混合者作為比較例4，並作為標準品2。 β (試驗例2) 就實施例3及比較例4之各ΙΤΟ粉末，按與試驗例1 同樣方式求得Sn02固溶體量。在此，粉末X射線繞射 (XRD)，係採用斯培克特立斯公司製之X，PertPR〇MPD所 分析者。將此等結果表示於表2中。又，將X射線繞射之 結果表示於第7圖及第8圖。 由此結果可知，在實施例3之ITO粉末之Sn02固溶 體量為3.00重量％，而除不用DC電漿火焰而使用乙炔火 20 316619 200536776 焰以外其餘則按同樣方式實施之實施例2之s】]〇2固溶 量為顯著地大的事實。 試料號碼 In (重量％) __________ ICP^ Sn (重量％) :結果 双D之藏 ------ 1】12〇3 (重量〇/〇) 90.40 Sn02 (t*%) Q 夾雜 化合物 Ιη03 (222) Sn07 (Π0) ^ 1 i\r\r\ ~~SnO^ 析出量 (重量°/o) 實施例3 73.8^1 7.46 實施例4 75.1 7.86 90.10 -7.OU 9.90 0-/ i DoZ, 892303 jJ〇90 62325 「6.60As for the heat source, the heat source of I is, for example, acetylene atmosphere or nitriding atmosphere, as long as it can melt metals ^ / * 63 Temple. The temperature and temperature of the heat source are sufficient to make the gaseous compounds or nitrides or oxynitrides oxidized or nitrided. In general, the number of thousands of U in the case of a W flame is limited. -Plasma flame is tens of thousands 316619 12 200536776 ° c or more. If this kind of acetylene flame or DC electropolymerization fire wants to make the raw material into liquid, "", then the product can be produced together with the gas stream or nitride or oxynitride. The raw material is produced as the original two It can be made from oxides of metals or alloys, or oxides: oxynitrides, depending on the state of the heat source, X, and the oxidizing atmosphere can be made from metals or alloys. Also, even if oxides, nitrides, or oxynitrides are used as raw materials, oxides, nitrides, or oxynitrides with different properties can be produced. In the present invention, the mist-like liquid fluid is used to capture the obtained That is to say, for the product flowing together with the jet of acetylene flame or Dc plasma flame, spray the mist-like liquid fluid, preferably mist-like water. As a result, the product is rapidly cooled to become fine particles, resulting in The slurry of the sprayed liquid fluid. ^ Here, the supply of the liquid fluid is not limited as long as it can capture and cool the resulting product. For example, when water is used, Make Water at normal temperature is preferably pure water at normal temperature, but cooling water can also be used. When the product is captured as fine particles, the maximum speed at the time of capture is, for example, '50 m / s or less, preferably 100 m / s. It is less than a second. In the present invention, the liquid fluid containing the fine particles captured by the sprayed liquid fluid is separated into a gas and a liquid, and the fine particles are recovered as a slurry. Here, the method for recovering the slurry is It is not particularly limited, but it is preferable that it can be implemented with a cyclone ^ 16619 200536776. The sun and the moon are irradiated, and a core alloy or IK) powder is used as a raw material to make a play-tin oxide (ίΤ〇) powder. ΙΤΟ powder, because of the amount of Sn0 2 solid solution (solid 501 + 1011) in hi9CK φ less ea, L _. ^: The level, high sinterability, can be easily made high density Burning two limbs' can result in a long-lasting standard leather. In addition, for example, it will be manufactured by various manufacturing methods, ITO ^, ^ ^ ^ ΤΤΠ 4.V i 4 or sintered I Ding. Burning = 〇φ at the end as the raw material, can be made with different properties from the raw material, 8 tons of 3 The solid solution content is a high level of ιτ〇 powder. In addition, 'This kind of ITO powder can be used for TT. Tian L ^ cannot be used as a target material for Ιτ〇 sputtering. This kind of target material for ITO sputtering And t, once calculated, it is preferably changed from 2.3 to 45% by mass, and 3 ^ SnO2 is changed below, and an example of a manufacturing device for implementing the present invention will be described below under Mai Zhaodi! The device is provided with a raw material 2 such as metal or e-gold which can be supplied as a liquid stream, liquid droplet, or powder in a flame i formed by a heat source of oxidizing atmosphere or nitriding atmosphere. Object 3, i oxygen skull 'Hushun soil, the first generation of clothing / the introduction port 10 introduced with the pore makeup class limbs, and the fluid injection means 2Q, which sprays a mist-like liquid fluid into the introduced mouth Cyclone 30, which was obtained by Guanger Fluid, was separated with money and liquid to produce the aforementioned micro-particulate lice separation method, and a part of the atmospheric fluid containing particles that failed to: And make it still loop means 40. The kiss position is here, the introduction port 10, if it can introduce the gas stream containing the product 316619 14 200536776, then it will not pull the brother 丨 丨 service-, discuss the limit 疋, but it can also be made a way to attract the gas flow . &quot; 丨 L version ϋ shell shooting means 20, is provided on the lower two sides of the guide provided with the introduction port 10 and has a plurality of jets capable of jetting a fluid (for example, water), a shell 21, and a pair of jets. The nozzle 21 introduces a fluid pump 22 and a fluid-filled pump 22, 7 ~ 3. The second spraying method of the fluid from the spray nozzle 21: the size is not limited, and it can be sprayed in a direction that can merge with the fluid 'L moving direction introduced from the inlet 10. The product 3 introduced from the introduction of the gas π 10 to the product 3 is cooled by a sprayed fluid such as water, and is captured as fine particles. Here, although the venturi with a reduced flow path is provided at the injection nozzle 1 to the downstream side of the guide pipe 11 to prevent the flow velocity of the gas-liquid mixture from decreasing, the venturi is not necessarily set. ^ Second, the spray nozzles 21 and 22 are not necessarily required to be installed, and can also be made ^ The attraction caused by the flow of kongyue * to attract the liquid jet: the inlet 11 of the port 10 is connected to the gas Liquid &quot; in addition, the inlet 31 of the f fan 30. From the inlet 3 of the cyclone 30, the scoop of gas-liquid core σ becomes the chips along the inner wall c 2 of the cyclone body 32 to perform gas-liquid separation and make a liquid component, that is, "" ::: The polymer material falls to the lower part, and the gas component is discharged from the exhaust port; That is, in the embodiment, the exhaust port 34 is provided with a circulation means 40. The Gongyin 'exhaust port 34 is provided with a circulation path leading to its n-order path \ w 〃, ^, ¥ ^ 11 guide σ (J, V 1), and is installed in the middle of the circulation pipe 41 Inspired by the wind, called 42, this temple mechanism constitutes a 4G circulation means. By this method 316619 15 200536776 40 'Enhance the capture of mealworms that have not been fully captured, +, and increase the capture efficiency. At the end of the transport, return to the nozzle nozzle On the upstream side of 21, through the cyclone 30 gas-liquid separation ring: from :, get slightly; =: = the end of the object is circulated from the exhaust pipe 41 of the red winder 30, except for the degree of circulation from the first The method of discharging from the two outlets 35. + minutes-way In this embodiment, there is a second cyclone belonging to the second gas-liquid separation means at the second outlet ^ mouth 35 = the gas pipe 43 &quot; 50, which basically has It has the same structure and the right as the cyclone 30. 2 Cyclone action. That is, the gas mixture from the guide pipe /] and the liquid separation liquid that connects the exhaust pipe 43 is converted into the gas along the cyclone body 52. The liquid is separated and made into a liquid component, that is, the human ^ thirsty stream 53. The slurry is dropped to the next ^ 卩 彳 township each has 彳 political particles.... The middle part of the venturi in the flow path: = '43, a reduced trough 循环 water circulation pipe 62 is set in the middle. Thus, by the flow of the venturi ^^ and the fluid, the water in the fluid trough 61 is drawn and cut into the text. The speed of the gas = Cheng: The remaining particles in the body are captured in the liquid in the A part: 〇 There are two outlets 55 connected to the exhaust pipe 7], and the exhaust two: Guangji 72 'made through the second Blower: 2: The way of exhausting the gas of 5. In addition, if you want to sink the water tank :: 316619 16 200536776 The nozzle A Cai is in the exhaust pipe 4 3, and the pump and spray nozzle are expanded. 〇 Like the above cyclone 30, it is possible to use a separator (; C :, 61, as in the above-mentioned square separation tank. In addition, it is also possible to make the sedimentation cycle of Λ wheat in the row ^ separation particles in the exhaust air circulation A part of the exhaust of the nipple 55 of the pipe 43 captures the efficiency. The upstream side of the inner portion 44 is to improve the efficiency of the other side. "If you only cry with a whirlwind, it is not necessarily a coin ..." The capture efficiency of the particles is sufficient. If you want to fork the second cyclone 50, and if you want to improve the post-harvest efficiency, you can also connect multiple cyclones to cry. Right person Park The trapped particle ^ means that the device described in the embodiment described above was used to make micro (persistent Example 1) In-Sn alloy (Sn96 6% by weight) atomized powder (average :): put into a block of flame to The dry-formed synthetic powder was used to dry-recover the powder using a bag-type retractor mter) as the ΙΤΌ powder of Example 1. (Example 2) ITO == ηΓ-like method, dry-synthesized π and 使用 using a block of flame were wet-recovered from ° shell water, and this was taken as 1το powder of Example 2. (Comparative Example 1) Oxidation of wet-synthesized indium oxide powder at 1000t: oxidation of sage 90 I / o, and oxidation of the same wet-synthesized tin oxide at 1000c 10 mass% of tin powder was mixed together in a mortar as 316619 17 200536776 as Comparative Example i and used as a standard product]. (Comparative Example 2) As a comparative example, ττ powder, which is a wet-synthesized method according to the coprecipitation method, and ITO powder of 2 were used. The steps for carrying out the wet synthesis according to the co-precipitation method are shown below. Yimin 'dissolved In (4N) 2Gg in shiosaic acid (test grade / concentration ^' to 61%) 133cc (pH _5) at room temperature. In addition, at room temperature, such as (4 &amp; dissolve The two were mixed in 100 cc (pH 9) of hydrochloric acid (special grade of reagent: concentration 35 to 36%) to make a mixed acid solution. At this time, no precipitate was present and the pH was -L5. Next, In this mixed acid, 25% ammonia water (special grade of test reagent) was mixed to neutralize 1 to make PΗ ^ 6.5. As a result, a white sink was formed. After a few days, 'Tang went to clear water', 2 liters of pure water was used. After being washed for 3 hours, dried at TC and dried at _. Oral, roasted for 3 hours to make it dehydrated to obtain a wet synthetic ITO powder. (Comparative Example 3) First, a wet synthetic oxidation was used. A powder of a mixture of indium powder and tin oxide powder (10% by weight of tin oxide) at 55 ° C (sintered body sintered on rcu) was pulverized as Comparative Example 3 2ITO powder. (Experimental Example 1) As for yoke example 1 , 2 and Comparative Examples 丨 to 3 of each Iτ〇 powder, to determine the amount of S] called solid solution. The procedure is as follows. In addition, before the test is performed, Example 2 and comparison The powder of 2 to 3 is sintered in the atmosphere at 10 GGC for 3 hours to grow the Sn02 precipitated as fine particles, so that it can be easily used as a method for detecting Sn02. 316619 18 200536776 1. First, implement the induction Coupling high-frequency plasma spectroscopic analysis (icp spectroscopic analysis). From this result, except for In and Sn, it is oxygen. Assuming that the amount of 0 may be insufficient, find the ratio of ln to Sn, and calculate the &amp; All of the% and I% become the weight ratios when I2O3 and Sn02. 2. The powders of Examples 1 and 2 and Comparative Examples i to 3 were subjected to powder X-ray diffraction (XRD: Mike Science) Manufactured by the company, μχρ18Γ [^^ analysis to determine the amount of SnO2 precipitation. That is, the presence of inclusion compounds (nuercalatl0n commpund, In4Sn3〇] 2) was confirmed from the diffraction results, and if no inclusions were detected In the case of a compound, the ratio of the integral diffraction intensity of 11120 (222) and the integral diffraction intensity of Sn02 (110) as the comparative example 丨 was used as a comparative example. %). That is, the precipitation amount (mass%) of sn〇2 is the integral that can be obtained from X-ray diffraction. The content of "a" obtained from the diffraction intensity ratio, and it is assumed that Sn02 which is not solid-solubilized in hl203 is grown by 1000t: the degree of calcination and becomes Sn02 of X-ray diffraction. The bee value of (i 丨 〇). Figures 2 to 6 show the results of x-ray diffraction. 3. The results from 1 and 2 will be detected in the icp analysis, but in the x-ray diffraction. Then, Sn0 2 which is Sn0 2 (11 0) could not be detected as the amount of Sn 0 2 solid solution. The results are shown in Table 1. ~ From this result, it can be known that, in the SnO2 solid cooling of the ΪΤΪ powder of Example 2, 2.35 wt%, 2 42 wt%, and 2.26 wt. % Is more fact. In addition, in the ITO powder of Comparative Example 3, which was once pulverized into a sintered body, the presence of inclusion compounds was detected, and the amount of quasi-Sno2 solid solution was not detected. 316619 200536776 Table 1 Sample No. 1CP Result of XRD XRD Sn02 Solid solution amount (wt%) In (wt%) Sn (wt%)] n203 (wt%) Sn02 (wt%) Impurity compound] n03 (222) Sn 〇, 010) Precipitation amount (% by weight) of Sn02 Example 1 74.1 8.26 89.52 10.48 No 6974596 35782] 8.13 2.35 Example 2 74.8 7.90 89.92 10.08 No 6875331 331124 7.66 2.42 Comparative Example] 75.1 7.87 90.09 9.91 No 7] 4] 62] 455777 9.9] Standard 0.00 Comparative Example 2 76.1 8.03 90.03 9.97 No 72734]] 352429 7.71 2.26 Comparative Example 3 74.8 7.90 90.02 9.98 7529677 105639--(Example 3) In-Sn alloy (Sn 9.6% by weight) fog Powder (average particle size: 45 // m), introduced into DC plasma flame to dry synthesize IT0 (In2〇3: SnO2 = 90 ·· 10% by weight) powder, and spray-wet the powder with water Recovered and used as the ITO powder of Example 3. (Comparative Example 4) In the same manner as in Comparative Example 1, 90% by mass of the indium oxide powder calcined at 1,000 ° C was wet-synthesized indium oxide powder. 10 mass% of tin oxide powder calcined at 0 ° C.—Compared in a mortar as Comparative Example 4 and as Standard 2. β (Test Example 2) The Sn02 solid solution amount was determined for each ITO powder of Example 3 and Comparative Example 4 in the same manner as in Test Example 1. Here, the powder X-ray diffraction (XRD) is an analyzer using X, PertPROMD produced by Spike Tries. These results are shown in Table 2. The results of X-ray diffraction are shown in Figs. 7 and 8. From this result, it can be known that the Sn02 solid solution content of the ITO powder in Example 3 was 3.00% by weight, and except that the acetylene fire 20 316619 200536776 flame was used instead of a DC plasma flame, the same was performed in Example 2 as in Example 2. s]] 〇2 The fact that the amount of solid solution is significantly large. Sample No. In (% by weight) __________ ICP ^ Sn (% by weight): Results of double-D storage ------ 1] 12〇3 (wt. 〇 / 〇) 90.40 Sn02 (t *%) Q Inclusion compound Iη03 ( 222) Sn07 (Π0) ^ 1 i \ r \ r \ ~~ SnO ^ precipitation (weight ° / o) Example 3 73.8 ^ 1 7.46 Example 4 75.1 7.86 90.10 -7.OU 9.90 0- / i DoZ, 892303 jJ〇90 62325 「6.60

Sn〇2 固溶體量 (重量°/〇) 【圖式簡單說明】Sn〇2 solid solution amount (weight ° / 〇) [Schematic description]

第1圖係有關本發明之實施形態的微粒子之製造麥 之概略構成圖。 、 粉末之X射線 第2圖係表示本發明之實施例i之IT〇 繞射之結杲的圖。 第3圖係表示本發明之實施例2之ΙΤ〇粉末之X射線 繞射之結果的圖。 · 第4圖係表示本發明之比較例1之1丁〇粉末之χ射線 繞射之結果的圖。 第5圖係表示本發明之比較例2之1丁〇粉末之χ射線 繞射之結果的圖。 第6圖係表示本發明之比較例3之ΙΤ〇粉末之χ射線 繞射之結果的圖。 第7圖係表示本發明之實施例3之ΙΤ〇粉末之χ射線 繞射之結果的圖。 第8圖係表示本發明之比較例4之；[丁〇粉末之χ射線 繞射之結果的圖。 316619 200536776 [主要元件符號說明】 1 火焰 2 原料 3 生成物 10 導入口 11 導入管 12 文丘里部 20 喷射手段 21 喷射喷嘴 22 泵 23 流體槽 30 旋風器 31 導入口 32 旋風器本體 33 滿流 34 排氣口 35 第2排出口 36 水排出口 40 循環手段 41 循環管 42 鼓風機 43 排氣管 44 文丘里部 50 第2旋風器 51 導入口 52 旋風器本體 5 3 &gt;尚流 54 水排出口 55 排氣口 61 流體槽 62 水循環管 71 排氣管 72 第2鼓風機Fig. 1 is a schematic configuration diagram of a microparticle manufacturing wheat according to an embodiment of the present invention. X-rays of powder FIG. 2 is a diagram showing the results of IT0 diffraction in Example i of the present invention. Fig. 3 is a graph showing the results of X-ray diffraction of the ITO powder of Example 2 of the present invention. Fig. 4 is a graph showing the results of the X-ray diffraction of the 1-but powder in Comparative Example 1 of the present invention. Fig. 5 is a graph showing the results of X-ray diffraction of 1-but powder in Comparative Example 2 of the present invention. Fig. 6 is a graph showing the results of X-ray diffraction of the ITO powder of Comparative Example 3 of the present invention. Fig. 7 is a graph showing the results of X-ray diffraction of the ITO powder of Example 3 of the present invention. Fig. 8 is a graph showing the results of Comparative Example 4 of the present invention; 316619 200536776 [Description of main component symbols] 1 Flame 2 Raw material 3 Product 10 Introduction port 11 Introduction pipe 12 Venturi 20 Injection means 21 Injection nozzle 22 Pump 23 Fluid tank 30 Cyclone 31 Introduction port 32 Cyclone body 33 Full flow 34 Exhaust port 35 Second discharge port 36 Water discharge port 40 Circulation means 41 Circulation pipe 42 Blower 43 Exhaust pipe 44 Venturi 50 50 Second cyclone 51 Inlet port 52 Cyclone body 5 3 &gt; Still flow 54 Water discharge port 55 Exhaust port 61 Fluid tank 62 Water circulation pipe 71 Exhaust pipe 72 Second blower

Claims (1)

200536776 十、申請專利範圍： i 一種微粒子之製造方法，其特徵為：將原料以液體流、 液滴或者粉末狀態供給於熱源中，藉由霧狀之液狀流體 將生成物以微粒子形態加以捕獲，以及藉由氣液分離回 收王聚料狀之前述微粒子。 申明專利範圍第1項之微粒子之製造方法，其中，從 原料之熔融液形成液體流或者液滴，而供給於該埶 t 〇 ‘一、 3·如申請專利範圍帛1項之微粒子之製造方法，其中，形 成原料之務化粉末，而供給於該熱源中。 4·如申請專利範圍帛1項之微粒子之製造方法，其中，使 用旋風态（cyclone)實施該氣液分離。 5.如申請專利範圍帛1項之微粒子之製造方法，其中，該 熱源係乙炔火焰或Dc(直流）電漿火焰。 人 6·如申請專利範圍g !項之微粒子之製造方法，其中，該 液狀流體係水。 ^ 7·如申請專利範圍f }項之微粒子之製造方法，其中，該 原料备廷自金屬、合金、氧化物、氮化物以及氧氮化 中的至少一種。 ^ ^申請專利範圍帛1項之微粒子之製造方法，其中，該 …、源％軋化冡氣或者氮化蒙氣之任一種，可製得氧化 9物氮化物以及氧氮化物之任一種微粒子。 •如申請專利範圍f !項之微粒子之製造方法，其中，該 原料係hvSn合金或者ITO粉末，以製造氧化銦‘氧化 316619 23 200536776 錫粉末。 10·如申請專利範圍第9項之微粒子之製造方法，其中，係 製造以換算成SnCb計，錫含量為2.3至45質量。/。之氧 化銦-氧化錫粉末。 11. 如申請專利範圍第1項至第10項中任—項之微粒子之 製造方法，其中，該生成物被該液狀流體所捕獲時之最 大速度為150m/秒以下。 12. —種微粒子之製造裝置，其特徵為具備：將呈液體流、 液滴或者粉末狀態之原料供給於熱源所得的生成物與 氣體流體-起導入的導入口；肖所導入的生成物喷射霧 狀之液狀流體的流體喷射手段；將液狀流體所捕獲的微 粒子加以氣液分離而製得該微粒子之漿料的氣液分離 手段；以及將含有未能以液狀流體捕獲的微粒子的蒙氣 f體之-部分送回至流體滴喷射位置以使其循環的循 環手段。 13=申請專利範圍第12項之微粒子之製造裝置，其中， 於該氣液分離手段之下游側再具備第2氣液分離手段， 用以將含有未能為液狀流體捕獲的微粒子的蒙氣流體 ，-部分導入，同時喷射霧狀之液狀流體並加以氣液： 離，而製得該微粒子之漿料。 ❹申請專利範圍第13項之微粒子之製造裝置，其中， 於：氣液分離手段之下游側再具備第2循環手段，用以 I: I有未旎為液狀流體捕獲的微粒子的蒙氣流體之-°刀达回至該第2氣液分離手段之導入部。 3166J9 24 200536776 15. 16 如申请專利範圍第12項之微粒子之製造裝置，其中， 該氣液分離手段係旋風器。 申請專利範圍第12項至第15項中任一項之微粒子之 衣k衣置’其中’該微粒子被該流體噴射手段所噴射的 液狀流體所捕獲時之最大速度為15〇m/&amp;以下。200536776 10. Scope of patent application: i A method for manufacturing fine particles, characterized in that the raw material is supplied to a heat source in the form of a liquid stream, droplets or powder, and the product is captured in the form of fine particles by a misty liquid fluid. , And the aforementioned fine particles in the form of Wang Ju are recovered by gas-liquid separation. The method for manufacturing microparticles according to claim 1, wherein a liquid stream or droplet is formed from the molten material of the raw material, and supplied to the 埶 t 〇 ′ 一, 3. · The method for manufacturing microparticles according to claim 1 Among them, a raw powder is formed and supplied to the heat source. 4. The method for producing fine particles according to item 1 of the scope of patent application, wherein the gas-liquid separation is performed using a cyclone. 5. The method for manufacturing fine particles according to item 1 of the patent application scope, wherein the heat source is an acetylene flame or a DC (direct current) plasma flame. Person 6. The method for manufacturing fine particles according to the scope of patent application g, wherein the liquid flow system is water. ^ 7. The method for manufacturing fine particles according to the item f} in the patent application range, wherein the raw material is prepared from at least one of a metal, an alloy, an oxide, a nitride, and an oxynitride. ^ ^ The method for manufacturing fine particles of scope 1 of the patent application, wherein the ..., source% rolling radon gas or nitriding nitrogen gas can be used to produce 9 oxide nitrides and oxynitride fine particles . • The method for manufacturing fine particles according to the scope of patent application f !, wherein the raw material is an hvSn alloy or ITO powder to produce indium oxide, oxidized 316619 23 200536776 tin powder. 10. The method for manufacturing fine particles according to item 9 of the patent application scope, wherein the tin content is 2.3 to 45 mass in terms of SnCb. /. Of indium oxide-tin oxide powder. 11. The method for manufacturing fine particles according to any one of items 1 to 10 of the scope of patent application, wherein the maximum speed of the product when captured by the liquid fluid is 150 m / s or less. 12. An apparatus for manufacturing fine particles, comprising: an introduction port for introducing a product obtained by supplying a raw material in a liquid flow, droplet, or powder state to a heat source, and a gaseous fluid; and ejecting the product introduced by Shaw Fluid spraying means for a misty liquid fluid; gas-liquid separation means for preparing a slurry of the microparticles by gas-liquid separation of the microparticles captured by the liquid fluid; and Circulation means that part of the masked body f is returned to the fluid droplet ejection position to circulate it. 13 = The microparticle manufacturing device of the 12th scope of the patent application, wherein a second gas-liquid separation means is further provided downstream of the gas-liquid separation means, and is used for filtering the air current containing the particles that cannot be captured by the liquid fluid. The body is partially introduced, while spraying a mist-like liquid fluid and adding gas-liquid: away, to obtain a slurry of the fine particles. (1) The microparticle manufacturing device of the scope of application for patent No. 13, wherein: a second circulation means is further provided downstream of the gas-liquid separation means, and is used for the I: I fluid containing the fine particles captured by the liquid fluid The-° knife reaches the introduction part of the second gas-liquid separation means. 3166J9 24 200536776 15. 16 For the device for manufacturing fine particles according to item 12 of the patent application scope, wherein the gas-liquid separation means is a cyclone. The clothing of the microparticles in any of claims 12 to 15 of the application range 'wherein' the maximum velocity when the microparticles are captured by the liquid fluid ejected by the fluid ejection means is 15 m / &amp; the following. 316619316619
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