TW501940B - Method for producing a liquid dispersion substantially containing submicron sized metal particles - Google Patents
Method for producing a liquid dispersion substantially containing submicron sized metal particles Download PDFInfo
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- TW501940B TW501940B TW090126896A TW90126896A TW501940B TW 501940 B TW501940 B TW 501940B TW 090126896 A TW090126896 A TW 090126896A TW 90126896 A TW90126896 A TW 90126896A TW 501940 B TW501940 B TW 501940B
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- carbonyl
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- 239000007788 liquid Substances 0.000 title claims abstract description 45
- 239000006185 dispersion Substances 0.000 title claims abstract description 13
- 239000002923 metal particle Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title description 7
- 239000007789 gas Substances 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims abstract description 14
- 239000012159 carrier gas Substances 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 64
- 229910052759 nickel Inorganic materials 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 25
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 claims description 4
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 2
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 claims description 2
- 229940088601 alpha-terpineol Drugs 0.000 claims description 2
- 229910002090 carbon oxide Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000007885 magnetic separation Methods 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 238000000108 ultra-filtration Methods 0.000 claims description 2
- 239000003085 diluting agent Substances 0.000 claims 2
- 101100067761 Rattus norvegicus Gast gene Proteins 0.000 claims 1
- 230000004888 barrier function Effects 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims 1
- 229940087654 iron carbonyl Drugs 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 25
- 238000011437 continuous method Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 150000001728 carbonyl compounds Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- SKBXVAOMEVOTGJ-UHFFFAOYSA-N xi-Pinol Chemical compound CC1=CCC2C(C)(C)OC1C2 SKBXVAOMEVOTGJ-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- FDEJSJBWOCAQAD-UHFFFAOYSA-N [Ni].O=C=[Ni] Chemical compound [Ni].O=C=[Ni] FDEJSJBWOCAQAD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000003701 inert diluent Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- -1 nickel carbonyl compound Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
- H01G4/008—Selection of materials
- H01G4/0085—Fried electrodes
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/006—Metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/80—Porous plates, e.g. sintered carriers
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Dispersion Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Colloid Chemistry (AREA)
Description
五、發明説明（ 技術範_ 本發明係一般性關於金屬粉末，更特別關於製造次微細 粒金屬顆粒之連續方法。此等顆粒尤其用於包含在裝料和 糊料中，以用於電化學電池（如電池組）和電容器。 背景拮爇 如曼德（Mond)和朗格（Langer)在1889年所發現，四羰基鎳 m(co)4易在約150_315t溫度範圍分解成基本純金屬鎳和一 氧化疲。劇烈曼德方法的一個主要缺陷為，四乡炭基鎳為高 度危險毒素。同樣，一氧化碳也必須相當小心處理。所 以，世界上有限少組織利用此方法。 多層電容器糊料市場需要沒有大於約1微米聚結顆粒的 次微細粒（小於1微米）鎳粉末。 取工業化生產的細鎳粉末由化學相沉積（ 原或水性《方法製造。此等流衫藝代價„)。鼠^ 多層電谷器製造商使用的鎳粉末起初係為乾燥粉末購 侍。然後使細粉末分散進入液體，形成漿料，該漿料係作 為糊料製程一部分。製造糊料顯著增加最終產物成本。 ^幾十年來，受讓者使（四）羰基鎳蒸氣在氣相中分解，以 製造多種細純鎳粉末β基本顆粒大小小於約0·5微米的超細 粉末可在钓400°c以上溫度由氣相分解羰基鎳製造。遺憾的 是，在此等條件下，顆粒碰撞產生相當多熔結機會，使粉 末包含一些超過約丨微米的不合需要顆粒。 為製造所需槳料和糊料，製備含次微細粒顆分散液的所 有現行技術均需要高昂多步驟分批操作。 501940 A7 B7 五、發明説明（ 在末世紀之交早期開發羰基鎳工藝期間認識到，羰基鎳 與氫氣通過流體之通道產生催化作用，並生成有機化合 物。見德國專利第241,823號（1911年）[頒予沙可夫 (Shukoff)] 〇 美國專利第1，138,201號[頒予埃利斯（Ellis)]揭示熱油氫化。 羰基鎳在油内用作細催化鎳源。 在兩種貫例中，鎳顆粒均自液體分離，留下經氫化化合 物。但很明顯，其中夾帶鎳顆粒的後處理液體分散液（如 糊料或漿料）具有利用性未得到認識。 因此，需要一種於液體分散液中產生次細粒金屬粉末之 連續代價有效方法，由之縮簡一些中間處理步驟。 發明概要 本發明提供一種製造次微細粒純金屬顆粒之液體分散液 之連續低代價方法。 羰基金屬蒸氣泡係與惰性載氣引入經加熱液體。在氣泡 上升時，羰基金屬在不聚結下分解成次微細粒全屬顆斧， '同時遍及液體分散。所得鎳基本顆粒具有物微米平均 直控，其大小等級小於最流行工業生產的錄顆粒。 里簡軍隸明 圖1為本發明具體實施例之示意流程圖。 fcSA隹具體會旒你丨 ，考圖！’其顯示製造夾帶次微細粒鎳顆粒液體之原型
裝 訂
線 雖然討論重點針對鎳 但本發明方法亦 可用於形成羰基 I紙張尺度適財關家鮮(CNS) A4規格(2ΐ〇ϋΤ^ 化合物的其他金屬，如鐵、鈷、鉻及鉬。 /入微細粒”指小於約1小微米。 麵h性載氣”指不直接與羰基鎳蒸氣或熱液體反應之氣 m ;":而根據標準動力和熱力學原理，它可能影響反應 速度和程度。 氣怨羰基鎳板1 2經由惰性載氣供到靜態混合器丨4。自供 應為1 6的惰性載氣（較佳為一氧化碳）調節供應至混合器工4 f最終達到熱反應器18(較佳為高壓釜）的初(⑺)4流速和 里。如需要，可用選擇性氮氣或其它惰性稀釋氣體源2〇增 加對容器18的Ni(C0)4進料。一氧化碳用於防止羰基化合物 在與液體24接觸前分解，並可影響顆粒大小。 對熟謂此藝者而言顯而易見，由於羰基鎳的危險性質， 必須用嚴格適當的防護物保護工作人員和環境免受羰基化 合物和氧化敌戌漏危害。因此，必須額定所有泵、導 言、閥、傳感器等的羰基化合物量。 氣悲Ni(CO)4和載氣由導管22按線路送達容器18。較佳將 羰基化合物蒸氣引向容器18底部，以通過容器“内布置的 f體24發出氣泡26。除霧器28或類似裝置脫去由流出容 器18—氧化碳氣體遺留的液體。 測量儀表幫助調節和控制反應器丨8的過程，如壓力表 3〇、溫度探測器32及其它操作和安全設備（未顯示）。 釋放的一氧化碳氣體通過分解器34，以破壞毒性一氧化 碳氣體。最終火焰分解器38中和剩殘的一氧化碳，並對安 全範圍内的經消耗氣體流提供可觀驗證。 -；--——- _ 一 _· 6 - 本紙張尺度適用中國國家標準(CNS) A4規格(210X297公董） 501940 A7 B7 五、發明説明（4 ) 次微細粒鎳顆粒由羰基鎳蒸氣直接在容器1 8内布置的熱 液體中分解產生。在生成顆粒時，顆粒由液-周邊界層保 護不發生表面反應及碰撞。同時，藉由將液體保持在固定 均勻溫度，所得顆粒具有更均勻微細結構。 與載氣混合的氣態羰基鎳進入容器1 8，且由熟諳此藝者 已知的適用分配器引入經加熱液體2 4。例如，用冷却分配 器（如噴嘴、發泡器、多孔盤或穿孔板）使蒸氣通過液體24 起泡。使分配器冷却以防止鎳在裝置上積聚亦很有用。可 由調節流速、氣泡大小分布、氣體濃度和液體2 4溫度控制 鎳顆粒的物理大小。 · 惰性氣體充當流速促進劑。 在氣泡通過液體24上升時，羰基鎳在氣泡内分解和或在 分解前溶入液體。羰基鎳化合物分解產生次微細粒鎳顆粒 之液體分散液，並沒有顯著量大於約1微米聚結顆粒。分 解反應為溫度、所選擇液體的類型、羰基金屬的氣體濃度 及氣體流速流體動力的函數。 可由一些習知操作將所得固體/液體分散液增稠到所需固 體含量及黏度，如蒸發、離心、磁性分離及超過濾。 藉由直接製造夾帶鎳顆粒的液體分散液，消除一些製造 鎳顆粒組成糊所用的習知以前存在處理步驟。 利用系統1 0的兩個實驗證明本方法之效能。 實例1 將每分鐘2升的氣態氮氣（90%)、羰基鎳（5%)和一氧化 碳（5%)通過繞結盤分配器送入由350毫升經熱至160°C液體 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 501940 A7 ___B7 五、發明説明（5 ) 組成的容器柱18底部（見圖丨）。實驗在（丨）癸醇（CAS i 12-3〇_ 1) ’（2) Flutfec PP10低霜氣壓锬氟化合物（CAS 3〇7-〇8-〇4) ; ( 3 ) 矽油（CAS 63148-58-3)，（4)十二燒（CAS 112-40-3);及（5) α- 萜品醇（CAS 10482-56-1)中進行。完全分解由在分解器34中 焚燒期間火焰3 8顏色改變證實。在製造評估用足夠產物後 的約8分鐘後停止實驗。將液體冷却並於室溫清洗。由掃 描電子顯微鏡（“SEM”）、動態光散射及^射線衍射（“_，，) 分析法初步分析微結構證實，鎳顆粒大小近似為〇1微米。 掺加鎳顆粒的萜品醇特別用作電容器電極糊料。 實例2 將每分鐘2升的氣態氮氣（9〇%)、羰基鎳（5%)及一氧化 碳（5%)通過繞結盤經約8分鐘送入由35〇毫升熱萜品醇 (CAS 10482-56-1)組成的容器柱18底部。在12〇〇c、13(rc、刚 。。及160t重複實驗。我們發現，在12〇t沒有鎳粉末產 生，表明沒有反應，或者分解器34内部件上沒有顯著鎳積 累。較高溫度令鎳顆粒產生。 雖然在約8分鐘後停止實驗評估產物，但反應顯得幾乎 瞬時發生。因此，連續方法使產物以相對恒速流出；流速 為輸入填充參數、液體溫度和體積的函數。 雖然在此根據規定條款說明和描述本發明的明確具體實 施例，但熟諳此藝者應瞭解，可由申請專利範圍覆蓋的本 發明形式作出變化，有時可用本發明的某些特點在不需對 應使用其它特點下獲得益處。
Claims (1)
- 々、申請專利範圍 1·. 一種製備含次微細粒金屬顆粒之液體分散之方法，其包 括： a) 在容器中提供液體浴液； b) 將羰基金屬氣體與惰性載氣混合，以形成羰基金屬 氣體 >昆合物； Ο將羰基金屬氣體混合物引入液體浴液； d) 使羰基金屬氣體混合物通過液體浴液發出氣泡； e) 使至少部分羰基金屬氣體在液體浴液内分解，以形 成預定大小的金屬顆粒並在其中保持；及 f) 在液體浴液中形成具預定黏度的金屬顆粒之液體分 散液。 2·根據申請專利範圍第1項之方法，其中該液體浴液係經 加熱。 3.根據申請專利範圍第2項之方法，其中該液體浴液係以 大於約120°C溫度加熱。 4·根據申請專利範圍第1項之方法，其中該羰基金屬氣體 係選自由羰基鎳、羰基鐵、羰基姑、羰基鉻及羰基鉬所 組成之群。 5·根據申請專利範圍第1項之方法，其中至少大多數金屬 顆粒之大小係小於約1微米。 6·根據申請專利範圍第1項之方法，其中該液體浴液係選 自由癸醇、低蒸氣壓碳氟化合物、矽油、十二烷及α -萜品醇所組成之群。 7·根據申請專利範圍第1項之方法，其中該金屬顆粒之液 9-•體分散係經增稠。. 8·:據中請專利範圍第7項之方法，其中該金屬顆粒之液 月且刀政係藉由選自蒸發、離心、磁性分離及超過濾組成 之群之方法增稠。 9·根據中請專利範圍第^之方法，其中該液體分散液為 漿料或糊料。 1〇.te根據中請專利範圍第1項之方法，#中該惰性載氣為一 氧化礙。 11·根據申請專利範圍第i項之方法，其中該稀釋氣體係加 入羰基金屬氣體混合物。 12·根據申請專利範圍第丨丨項之方法，其包括將約9〇〇/。稀 釋氣體、約5 %羰基金屬氣體及約5 % 一氧化碳引入液體 浴液。 13·根據申請專利範圍第1 1項之方法，其中該稀釋氣體為 鼠氣。 14·根據申請專利範圍第1 1項之方法，其包括將約9 〇 %氮 氣、約5 %羰基鎳氣體及約5 % —氧化碳引入液體浴液。 •10- 本纸張尺度適用中國國家標準(CNS) A4規格(21〇x297公釐)
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| US20070283782A1 (en) * | 2005-08-10 | 2007-12-13 | Mercuri Robert A | Continuous process for the production of nano-scale metal particles |
| US20070283783A1 (en) * | 2005-08-10 | 2007-12-13 | Mercuri Robert A | Process for the production of nano-scale metal particles |
| DE102007045878B4 (de) * | 2007-09-25 | 2009-06-18 | Albert-Ludwigs-Universität Freiburg | Verfahren zur Herstellung von metallhaltigen Nanopartikeln |
| DE102009005923A1 (de) * | 2009-01-23 | 2010-07-29 | Linde Aktiengesellschaft | Verfahren und Vorrichtung zur Ableitung von Leckagegas aus einem Verdampfer |
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| US3504895A (en) | 1964-05-25 | 1970-04-07 | Int Nickel Co | Apparatus for the production of metal powders and metal-coated powders |
| US4252671A (en) | 1979-12-04 | 1981-02-24 | Xerox Corporation | Preparation of colloidal iron dispersions by the polymer-catalyzed decomposition of iron carbonyl and iron organocarbonyl compounds |
| US4808216A (en) * | 1987-04-25 | 1989-02-28 | Mitsubishi Petrochemical Company Limited | Process for producing ultrafine metal powder |
| US5064464A (en) * | 1988-11-10 | 1991-11-12 | Mitsubishi Petrochemical Company Limited | Process for producing ultrafine metal particles |
| US5137652A (en) | 1989-12-18 | 1992-08-11 | National Research Institute For Metals | Method of manufacturing particle colloid or a magnetic fluid containing metal nitrides |
| US6033624A (en) | 1995-02-15 | 2000-03-07 | The University Of Conneticut | Methods for the manufacturing of nanostructured metals, metal carbides, and metal alloys |
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| RU2237547C2 (ru) | 2004-10-10 |
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| CN1416362A (zh) | 2003-05-07 |
| US20020088306A1 (en) | 2002-07-11 |
| KR100505174B1 (ko) | 2005-08-03 |
| GB2380188A (en) | 2003-04-02 |
| NO20024199D0 (no) | 2002-09-03 |
| GB0218017D0 (en) | 2002-09-11 |
| JP3986964B2 (ja) | 2007-10-03 |
| CA2401026A1 (en) | 2002-07-11 |
| AU2001295323B8 (en) | 2010-03-25 |
| WO2002053315A3 (en) | 2002-09-06 |
| US6506229B2 (en) | 2003-01-14 |
| AU2001295323B1 (en) | 2004-07-22 |
| WO2002053315A2 (en) | 2002-07-11 |
| CN1200761C (zh) | 2005-05-11 |
| KR20020081689A (ko) | 2002-10-30 |
| CA2401026C (en) | 2005-03-29 |
| GB2380188B (en) | 2004-11-10 |
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