CN101905875A - 空心碳球 - Google Patents
空心碳球 Download PDFInfo
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- CN101905875A CN101905875A CN2010101809833A CN201010180983A CN101905875A CN 101905875 A CN101905875 A CN 101905875A CN 2010101809833 A CN2010101809833 A CN 2010101809833A CN 201010180983 A CN201010180983 A CN 201010180983A CN 101905875 A CN101905875 A CN 101905875A
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- carbon
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 157
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 151
- 230000001186 cumulative effect Effects 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 28
- 230000003197 catalytic effect Effects 0.000 claims description 13
- 239000011824 nuclear material Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 239000011149 active material Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 150000001721 carbon Chemical group 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- 239000010948 rhodium Substances 0.000 claims description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000000608 laser ablation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims 1
- 239000011257 shell material Substances 0.000 description 58
- 239000007789 gas Substances 0.000 description 36
- 239000002243 precursor Substances 0.000 description 33
- 239000000443 aerosol Substances 0.000 description 30
- 239000002245 particle Substances 0.000 description 14
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 10
- 229910052718 tin Inorganic materials 0.000 description 10
- 239000011135 tin Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 125000004429 atom Chemical group 0.000 description 8
- 239000003814 drug Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000011263 electroactive material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000975 bioactive effect Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000011162 core material Substances 0.000 description 3
- 239000003550 marker Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 102000008394 Immunoglobulin Fragments Human genes 0.000 description 2
- 108010021625 Immunoglobulin Fragments Proteins 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011852 carbon nanoparticle Substances 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000001989 lithium alloy Substances 0.000 description 2
- KUJOABUXCGVGIY-UHFFFAOYSA-N lithium zinc Chemical group [Li].[Zn] KUJOABUXCGVGIY-UHFFFAOYSA-N 0.000 description 2
- 229910021392 nanocarbon Inorganic materials 0.000 description 2
- -1 poly(lactic acid) Polymers 0.000 description 2
- 229920001515 polyalkylene glycol Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N Lactic Acid Natural products CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 1
- 240000003936 Plumbago auriculata Species 0.000 description 1
- 229920000954 Polyglycolide Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 1
- QWJYDTCSUDMGSU-UHFFFAOYSA-N [Sn].[C] Chemical compound [Sn].[C] QWJYDTCSUDMGSU-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 238000011275 oncology therapy Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920001606 poly(lactic acid-co-glycolic acid) Polymers 0.000 description 1
- 239000004633 polyglycolic acid Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000008521 reorganization Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B35/62828—Non-oxide ceramics
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- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
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- C04B2235/40—Metallic constituents or additives not added as binding phase
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- Y10T428/00—Stock material or miscellaneous articles
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- 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
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Abstract
本发明公开了具有碳壳和内核的空心碳球。该空心碳球具有等于碳壳体积加上碳壳中的内部自由体积的总体积。该内部自由体积占总体积的至少25%。在一些实例中,空心碳球的标称直径为10~180nm。
Description
政府利益
本发明是在由美国能源部制定的、基于合同编号为DE-AC52-06NA25396的政府支持下完成的。政府享有本发明的某些权利。
技术领域
本发明涉及一种空心碳球,尤其是一种具有大的内部自由体积的空心碳球。
背景技术
空心碳球是公知的。例如,Xiong等1报告了一种由CCl4在190~230℃的温度下制备的、直径为400~600nm的空心碳球,Zhang等2报告了一种使用金属锌粉和乙醇制备的、公称直径为400nm的空心碳球,Su等3报告了一种通过碳包覆氧化硅球制备的空心碳球,Win等4报告了直径为300nm~1μm的空心碳球。
关于直径小于200nm的空心碳球,美国专利No.7,156,958公开了一种制备直径为3~60nm的空心碳纳米囊的方法,美国专利申请公开Nos.2005/0079354和2007/0220873公开了一种直径小于20nm的空心碳球。然而,这些参考文献没有公开空心碳结构中内核或空腔的尺寸。与此相反,美国专利申请公开No.2007/0080054公开了在直径为20nm的空心碳纳米颗粒中的5nm的内部空腔,Phillips等5,6报告了制备直径小到30nm的空心石墨颗粒。
同样地,直径小于200nm的空心碳球已被公开,然而,在这个尺寸范围内具有相对大的内部自由体积的空心碳球未被公开。因此,期望得到一种直径小于200nm、具有相对大的内部自由体积的空心碳球。
发明内容
本发明公开了一种具有碳壳和内部自由体积的空心碳球。该空心碳球具有总体积,该总体积等于碳壳体积加上碳壳中的内部自由体积。内部自由体积占总体积的至少25%。在一些实例中,空心碳球的标称直径为10~180nm。
碳壳可以具有贯穿的通道,例如以孔隙形式的通道和/或以错配区域形式的通道,该错配区域位于至少形成部分碳壳的两个邻近碳晶粒之间。该通道能够使某种材料被封装在空心碳球中,例如电活性材料、催化材料和/或生物活性材料。另外,该催化材料可以位于碳壳表面上,在一些实例中位于碳壳的外表面上。该催化材料可以包括诸如铂、钯、铑、铼、铁、镍、钴、银、金及其合金的材料。
本发明还公开了制备空心碳球的方法,该方法包括提供碳要封装的牺牲核材料,由此形成碳壳。然后,将该牺牲材料从碳壳中去除以生成空心碳球。空心碳球具有占该球总体积至少25%的内部体积。
向牺牲材料上沉积碳可以包括通过碳原子浓缩沉积。例如,碳能够在等离子体中蒸发形成碳蒸气,随后是碳原子在牺牲材料上重排和/或沉积。另外,向牺牲核材料上沉积碳可以包括通过化学气相沉积法沉积、通过激光烧蚀沉积、通过电弧放电沉积和通过低温溶剂化沉积。牺牲材料可以通过酸溶解或碱溶解从碳壳中去除。
附图说明
图1是依照本发明实施方案的多个空心碳球的示意图;
图2是图1所示的在多个空心碳球中具有电活性材料的实施方案的示意图;
图3是图1所示的在多个空心碳球的表面上具有催化材料的实施方案的示意图;
图4是表示通过碳壳的潜在通道的TEM图像;
图5是制备空心碳球的方法的示意图;
图6是制备由碳封装的核材料的装置的示意图;
图7是在牺牲材料上的碳外壳的示意图;
图8是在牺牲材料上的碳外壳的TEM图像;
图9是形成由碳封装的核材料的装置的示意图;和
图10是空心碳球的TEM图像。
具体实施方式
本发明公开了一种具有有内部自由体积的碳壳的空心碳球。另外,还公开了制备该空心碳球的方法。该空心碳球可用来在其中封装材料和/或支撑催化材料。同样地,该空心碳球可用作电池材料、催化支撑结构材料等。另外,该方法可用于制备空心碳球。
该空心碳球具有总体积,该总体积等于碳壳体积加上碳壳中的内部自由空间的体积。内部自由体积占总体积的至少25%。在一些实例中,内部自由体积占总体积的至少50%,而在其他的实例中,内部自由体积占总体积的至少75%,以及在另外其他的实例中,内部体积占总体积的至少90%。
该空心碳球的标称直径可以为10~180nm,在一些实例中为50~150nm。在其他一些实例中,空心碳球的标称直径为80~120nm。该碳壳可以具有2~30nm的标称厚度,在一些实例中为5~20nm。在另外其他的实例中,碳壳的标称厚度为7~10nm。
该碳壳可以有贯穿的通道,该通道使得材料移动通过该壳并进出碳球。该通道可以是孔隙形式和/或在两个邻近碳晶粒之间的错配区域的形式,在该区域中原子和/或分子的扩散性被增强。
该空心碳球可用于在其中封装电活性材料。该电活性材料可以是与锂或含锂的材料形成合金的材料。该空心碳球也可用作催化材料的支撑结构,该催化材料在碳壳的表面上。该表面可以是碳壳的外表面,或可选择地是碳壳的内表面。催化材料可以是诸如铂、钯、铑、铼、铁、镍、钴、银、金和/或它们的合金的材料。
另外,通过在碳壳内和/或碳壳上具有生物活性材料,可将空心碳球用于药物输送。例如并仅作为示例性的目的,空心碳球可在其内包含要输送的生物活性材料或分子,以及可选地与该生物活性分子共价键合的聚合物(如抗体或抗体片段)。该生物活性分子可位于空心碳球内和/或外表面上。该生物活性分子可以是任何用于治疗患者的分子,举例来说包括蛋白质、碳水化合物或多糖、核酸、脂类、它们的组合或合成分子,包括有机和无机材料。
在一些实例中,该空心碳球可用作可注射的颗粒,该空心碳球具有要输送的物质和聚亚烷基二醇与聚(乳酸乙醇酸)(poly(lactic-co-glycolicacid))、聚乳酸、聚乙醇酸或聚酸酐的共聚物,其中聚亚烷基二醇与抗体或抗体片段共价键合。同样地,该空心碳球可用于在长的时间段内释放高活性和有效的药物,如抗癌药物,当系统给药时这种药物产生严重的副作用。已知这种受控释放通常降低与非封装药物的系统给药有关的毒副作用。聚合物基质也可以向具有短生物半衰期的药物提供药物保护以防止在等离子体中发生降解。
制备空心碳球的方法可以包括提供牺牲材料,向该牺牲材料上沉积碳以形成碳壳和去除牺牲材料以产生空心碳球。该牺牲材料可以是任何通过酸溶解或碱溶解从碳壳中可去除的材料。
在一些实例中,可以提供干燥前体粉末、液体和/或液体蒸汽形式的前体,该前体悬浮在气溶胶气体中形成含有前体的气溶胶。另外,气溶胶可以通过具有热区的等离子体,同时使气溶胶中的至少部分前体蒸发。在热区中,通过来自前体的原子和有时来自气溶胶气体的原子的重组可以产生新的颗粒。
气溶胶气体可将新的颗粒携带出热区并进入其中发生极快冷却的等离子体余辉区域。随后将这些颗粒带入接近环境温度的区域中,在那里通常可以使用过滤器将颗粒从气溶胶气体中去除。然后,可采用酸溶解或碱溶解从碳壳中去除核材料。
等离子体的热区可以是利用射频、微波能或直流放电产生的高电磁能的区域。等离子体可以是非氧化性等离子体,在一些实例中是低功率常压或近常压等离子体,所述等离子通过在耦合器中聚焦微波能而产生。
气溶胶气体可以是惰性气体,举例来说包括氦、氩和它们的组合。该方法可进一步包括传送除气溶胶外的等离子体气体通过等离子体热区,该等离子体气体也是惰性气体。在一些实例中,核材料是锂合金材料,可以包如锡、硅、铝、锗、它们的组合等的元素。
现在转向图1,一般用参考数字10表示空心碳球的一个实施方案。实施方案10可包括一个或多个空心碳球100,空心碳球100具有碳壳110和内部自由体积120。空心碳球100可以包括从球心102延伸至碳壳110的外表面116的半径112。另外,空心碳球100可具有从球心102延伸至内表面118的内径124。同样地,空心碳球100可以具有等于4/3πRt 3的总体积,其中Rt等于图1所示的半径112。同样地,空心碳球100可以具有等于4/3πRi 3的内部自由空间体积,其中Ri等于图1所示的内径124。
在一些实例中,对于空心碳球100,内部自由空间体积等于总体积的至少25%。在另一些实例中,内部自由空间体积是总体积的至少50%,在另一些实例中,内部自由空间体积是总体积的至少75%。甚至在其他一些实例中,内部自由空间体积是总体积的至少90%。
碳壳110可具有贯穿的通道。例如并仅作为示例性的目的,通道可以是如图1所示的孔隙114的形式。孔隙114能使原子和/或分子传送、迁移和/或扩散通过碳壳110。另外,通道可由作为碳壳110的一部分的邻近碳晶粒间的错配区域提供。例如,图4显示了具有两个邻近晶粒111的空心碳球的透射电子显微镜(TEM)图像,其中两个邻近晶粒111具有示意性地在113所示的不同取向。晶粒111具有示意地在其上绘制的对应于碳原子排列的线条,以此说明两个晶粒111不具有相同的取向。同样地,认为位于两个邻近晶粒111之间的区域113可使得穿过那里的原子和/或分子具有增强的扩散性。以这种形式,来自酸性或碱性溶液的原子和/或分子可以通过碳壳并与牺牲材料接触。同样地,已被溶解的牺牲材料能从空心碳球100中离开。
现在转向图2,空心碳球100可以将电活性材料135封装在里面。电活性材料135可包括锂合金材料。认为电活性材料135通过首先穿过碳壳110的如上所述的通道而沉积在空心碳球100中。
现在参看图3,空心碳球100具有由碳壳110支撑的催化材料140。催化材料140可存在于碳壳110的外表面116和/或内表面118上。认为生物活性材料或分子可位于碳壳110中和/或之上,由此使得空心碳球可用于药物输送。
现在转向图5,一般用参考标记20表示制备空心碳球的实施方案。方法20包括在步骤200提供粉末、液体和/或液体蒸气形式的前体并在步骤202将前体通过等离子体炬。在步骤202将前体通过等离子体炬时,包含于前体中的至少部分壳材料和至少部分核材料被蒸发。在步骤204被蒸发了的材料随后冷凝而形成核-壳结构纳米颗粒。然后,去除位于外壳中的牺牲材料,制得空心碳球。
图6提供了用参考标记30表示的、用于制备核-壳结构纳米颗粒的装置的示意图。如该图所示,气溶胶气体300通过进口管310进入包含前体322的前体容器320。以足够的流速进入前体容器320的气溶胶气体300的气流导致前体322悬浮在气溶胶气体300中以形成气溶胶。前体322可包含核材料和壳材料。前体322还可以包含在任何制得的核/壳结构纳米颗粒的核和/或壳中没有导入的元素,但这些元素可以存在从而以某种方式促进整个过程。
气溶胶生成后,其可以移动或流动通过出口管330,其中出口管330的至少一部分进入等离子体炬340。在一些实例中,出口管330具有通常终止于波导管360的中间的陶瓷部332。波导管360用于将微波能耦合到等离子体炬340。也可包括等离子体气体350,该等离子体气体350在等离子体炬340中通过,但处于气溶胶通过的出口管330的陶瓷部332的外面。在用波导管360将微波能聚焦到等离子体炬340时,等离子体可通过位于等离子体炬340中的热区342产生。当具有前体322的气溶胶通过等离子体炬340的热区342时,热区342的温度为可蒸发至少部分前体322的温度。被蒸发的前体322从等离子体炬340的热区342离开进入烟囱区域370。当离开热区342时,被蒸发的前体的原子冷凝成固体颗粒。
如果前体322包含核材料和壳材料,气溶胶通过或流过等离子体炬340的热区342会使至少部分核材料和至少部分壳材料蒸发。因此,核和壳材料原子冷凝成核-壳结构纳米颗粒。核-壳结构纳米颗粒可通过颗粒过滤器390、烟囱区域370的内侧壁和/或颗粒捕集器(未示出)收集。
核-壳结构纳米颗粒被收集后,可将它们放入酸性浴或碱性浴中。酸或酸性浴或碱性浴与牺牲材料或内核接触并导致它们溶解,由此制得空心碳球。
为了更好地阐明本发明的实施方式,下面提供了制备空心碳球的方法的实施例。
实施例1
参考图6,通过手动研磨微米锡颗粒和结晶蒽颗粒的混合物来提供干燥前体粉末以产生干燥前体粉末322。锡与蒽的重量比是50∶1,锡颗粒的平均直径为50μm,手动研磨锡颗粒和蒽晶体的混合物直至产物呈现充分均匀。将干燥前体粉末322放入前体粉末容器320中。将在标准温度和气压(STP)下流速为200立方厘米每分钟(cc/min)的氩气用作等离子体气体350并通过等离子体炬340。
为了生成含有干燥前体粉末322的气溶胶,将在STP下流速为300cc/min的氩气用作气溶胶气体300并允许其进入或流入前体粉末容器320。在流入前体粉末容器320并随后通过出口管330流出时,气溶胶气体300将来自干燥前体粉末322的锡颗粒和蒽颗粒悬浮在其中,由此生成气溶胶。含有锡和蒽颗粒的气溶胶从出口管330的陶瓷部332排出,进入通常在波导管部分360中间的等离子体热区。波导管部分360将微波能耦合到等离子体炬340,以使得出现约900W的吸收能量。在本实施例中,等离子体炬由石英管形成。等离子体本身被限制在石英炬340中,等离子体气体和气溶胶的驻留时间相对短,例如小于1秒。随后,新的颗粒从热区传递至余辉区域,最后到达接近环境温度的区域。使用这些参数,制备出具有锡核和碳壳的、平均纳米颗粒直径为50nm和粒径分布相对紧密的核-壳结构纳米颗粒。图7例举了这样的纳米颗粒(通常用参考标记210表示),核-壳结构纳米颗粒210具有内核212和外壳214。图8表示使用上述参数制备的真实的锡核-碳壳纳米颗粒的透射电子显微镜(TEM)图像。
核-壳结构纳米颗粒制备后,通过使用如美国专利No.3,986,970公开的溶解方法(该专利的全部引入本文作为参考)去除内核的牺牲材料。
尽管上述实施例制备了锡-碳纳米颗粒,可以理解可用其他前体粉末材料来制备其他核-壳结构纳米颗粒,例如并仅作为示例性目的,可以用微米尺寸的铝颗粒和蒽作为前体材料来制备铝-碳纳米颗粒。
实施例2
参考图9(其中相同的数字对应于图6的相同部分),除了以己烷(C6H14)和/或它的蒸气形式的液态碳源327之外,如上述的实施例1所述提供干燥前体粉末。已知己烷是在室温下无色的液体,在-95℃时熔化,在69℃时沸腾,在20℃和1个大气压下具有132mmHg的蒸气压。还可以理解在本发明的范围内可使用其他液态碳源以及其他将液滴和/或它们的蒸气导入惰性气体的方法(例如己烷的超声振动以生成直接的己烷气溶胶)。
如图9所示,将液态碳源327放入容器325中,气溶胶气体300流入容器325,并且在离开容器325前在碳源327上方流动。以这种方式,当它流出容器325并流向容器320时,碳源蒸气悬浮在气溶胶气体300中。对于这个具体的例子,在等离子体炬340存在有约900W的吸收能量,氩气被用作等离子体和气溶胶气体。另外,等离子体气体350的流速为250cc/min,气溶胶气体300的流速为30cc/min,气溶胶气体300的流速为160cc/min,由此生成锡核-碳壳纳米颗粒。
制得核-壳结构纳米颗粒后,如前面实施例中所述那样去除牺牲材料,图10表示以这种方式制备的空心碳球的TEM图象。
可以理解本发明不局限于具体的蒸气流速、组成或构造。另外,即使上述实施例公开了具有二重气流体系的方法,其中每个气流具有不同的总组成并仅在等离子体热区结合和混合,但其他气流和/或等离子体体系也包括在本发明的范围之内。例如并仅作为示例性目的,使用直流(DC)放电的、具有一种气流体系的等离子体(其中气溶胶气体和等离子体气体是一样的)的方法属于公开的本发明的方法的范围。这种方法会使所有流经等离子体的气体和前体在到达热区前很好地混合,而两种气流体系则与其相反,其中气溶胶气体和等离子体气体如上面实施例所述在热区的中心相互混合。
前述的附图、讨论和描述是本发明具体实施方式的举例,但它们不意味着受此操作的限制。根据本发明的教导,本发明的许多改进和变化对本领域技术人员来说是显而易见的。下面的权利要求,包括所有等效表述,限定了本发明的范围。
参考文献
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Claims (16)
1.一种空心碳球,包含:
具有总体积的碳壳;
具有内部自由体积的内核;
所述总体积等于所述碳壳的体积加上所述内部自由体积;
所述内部自由体积占总体积的至少25%。
2.根据权利要求1所述的空心碳球,其中所述标称直径为10~180nm。
3.根据权利要求1所述的空心碳球,进一步包含封装于所述内核中的生物活性材料。
4.根据权利要求1所述的空心碳球,进一步包含在所述碳壳表面上的催化材料。
5.根据权利要求4所述的空心碳球,其中所述表面是所述碳壳的外表面。
6.根据权利要求4所述的空心碳球,其中所述催化材料选自铂、钯、铑、铼、铁、镍、钴、银、金及它们的合金。
7.一种制备空心碳球的方法,包括:
提供用于内核材料的牺牲材料;
向内核材料上沉积碳以形成碳壳;及
去除内核材料以生成空心碳球,该空心碳球具有:
具有总体积的碳壳;
具有内部自由体积的内核;
所述总体积等于所述碳壳的体积加上所述内部自由体积;
所述内部自由体积占总体积的至少25%。
8.根据权利要求7所述的方法,其中空心碳球的标称直径为10~180nm。
9.根据权利要求7所述的方法,其中向内核材料上沉积碳是通过向牺牲材料上冷凝碳原子进行沉积。
10.根据权利要求7所述的方法,进一步包括使用等离子体蒸发碳以形成碳蒸气。
11.根据权利要求7所述的方法,其中向牺牲材料上沉积碳选自通过化学气相沉积进行沉积、通过激光烧蚀进行沉积、通过电弧放电进行沉积和通过低温溶剂化进行沉积。
12.根据权利要求7所述的方法,其中通过内核材料的酸溶解去除内核材料。
13.根据权利要求7所述的方法,其中通过内核材料的碱溶解去除内核材料。
14.根据权利要求7所述的方法,进一步包括在空心碳球中封装生物活性材料。
15.根据权利要求7所述的方法,进一步包括向空心碳球的表面上沉积催化材料。
16.根据权利要求15所述的方法,其中空心碳球的表面是空心碳球的外表面。
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US20110180513A1 (en) | 2011-07-28 |
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US8419998B2 (en) | 2013-04-16 |
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