CN106379948A - 一种制备纳米羟基氧化钴锰的方法 - Google Patents
一种制备纳米羟基氧化钴锰的方法 Download PDFInfo
- Publication number
- CN106379948A CN106379948A CN201610883535.7A CN201610883535A CN106379948A CN 106379948 A CN106379948 A CN 106379948A CN 201610883535 A CN201610883535 A CN 201610883535A CN 106379948 A CN106379948 A CN 106379948A
- Authority
- CN
- China
- Prior art keywords
- manganese
- cobalt
- cobalt oxide
- mixed solution
- acetate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 34
- RHBREZMHGBURNU-UHFFFAOYSA-M O[Mn]O[Co] Chemical compound O[Mn]O[Co] RHBREZMHGBURNU-UHFFFAOYSA-M 0.000 title abstract 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract description 13
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 11
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 8
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 6
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005273 aeration Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 235000013495 cobalt Nutrition 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 7
- 229910017052 cobalt Inorganic materials 0.000 description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000011572 manganese Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 3
- MZZUATUOLXMCEY-UHFFFAOYSA-N cobalt manganese Chemical compound [Mn].[Co] MZZUATUOLXMCEY-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- MSBWDNNCBOLXGS-UHFFFAOYSA-L manganese(2+);diacetate;hydrate Chemical compound O.[Mn+2].CC([O-])=O.CC([O-])=O MSBWDNNCBOLXGS-UHFFFAOYSA-L 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910008090 Li-Mn-O Inorganic materials 0.000 description 1
- 229910006369 Li—Mn—O Inorganic materials 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- SVMCDCBHSKARBQ-UHFFFAOYSA-N acetic acid;cobalt Chemical compound [Co].CC(O)=O SVMCDCBHSKARBQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 150000001869 cobalt compounds Chemical class 0.000 description 1
- XEUFSQHGFWJHAP-UHFFFAOYSA-N cobalt(2+) manganese(2+) oxygen(2-) Chemical compound [O--].[O--].[Mn++].[Co++] XEUFSQHGFWJHAP-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- DLHSXQSAISCVNN-UHFFFAOYSA-M hydroxy(oxo)cobalt Chemical compound O[Co]=O DLHSXQSAISCVNN-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- -1 manganese Hydroxy cobalt oxide Chemical compound 0.000 description 1
- WSHADMOVDWUXEY-UHFFFAOYSA-N manganese oxocobalt Chemical compound [Co]=O.[Mn] WSHADMOVDWUXEY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
本发明公开了一种制备纳米羟基氧化钴锰的方法,包括以下步骤:(1)调节乙酸锰与乙酸钴的混合溶液的pH值至2.5~6;(2)向步骤(1)后的混合溶液中通入氧化性气体进行氧化反应,反应后离心、洗涤、烘干,得到所述纳米羟基氧化锰钴。本发明的制备方法可一步加工得到纳米羟基氧化钴锰,该纳米羟基氧化钴锰可应用于超级电容器及锂离子电池等相关领域。本发明的制备方法所涉及原料廉价易得,成本低,合成工艺简单易实现,产品质量稳定且工艺重复性能好,反应可以在较短时间内完成,效率高。
Description
技术领域
本发明属于纳米材料领域,尤其涉及一种制备纳米羟基氧化钴锰的方法。
背景技术
锰、钴的氢氧化合物在电化学、电池、电致变色等领域都有着十分重要的用途。羟基氧化锰钴亦可作为Li-Mn-O尖晶石结构和参钴的锰氧化合物的前驱体,而参钴的锰氧化合物在二次电池,超级电容器方面有着十分优越的性能,一直受到科学界及工业界的广泛关注。中国专利申请201210578760.1,公开了一种掺杂微量锰的羟基氧化钴的制备方法,此方法是在钴盐及M盐中加入沉淀剂(KOH、NaOH等)及氧化剂(压缩空气),合成含有微量锰的羟基氧化钴,由于此方法在合成过程中加入沉淀剂及氧化剂会造成反应的不均匀,产品稳定性较差,反应需要在较长一段时间内才能完成,效率不高,不利于进行大批量生产。因此,研究一种合成工艺简单易实现,产品质量稳定且工艺重复性能好的羟基氧化锰钴的制备方法,是非常有必要的。
发明内容
本发明所要解决的技术问题是,克服以上背景技术中提到的不足和缺陷,提供一种制备纳米羟基氧化钴锰的方法。
为解决上述技术问题,本发明提出的技术方案为:
一种制备纳米羟基氧化钴锰的方法,包括以下步骤:
(1)调节乙酸锰与乙酸钴的混合溶液的pH值至2.5~6;
(2)向步骤(1)后的混合溶液中通入氧化性气体进行氧化反应,反应后离心、洗涤、烘干,得到所述纳米羟基氧化锰钴。
申请人通过反复研究和实验验证发现,当混合溶液的pH值低于2.5时,钴离子难以被氧化沉淀,在短时间内只有少量钴沉淀下来,反应效率过低;当pH值高于6时,反应速率过快、产物粒径难以控制;同时还发现,在相同pH下Co2+氧化电位较高,沉淀较Mn2+慢,在相同时间内两者沉淀量不同,因而可以通过调节pH来调节产物中钴锰的原子比,改变参杂钴的含量。
上述的方法,优选的,所述纳米羟基氧化锰钴的化学式为(CoxMn1-x)OOH,其中0<x<1;所述纳米羟基氧化锰钴呈球形,平均粒径为180nm~200nm。
上述的方法,优选的,所述乙酸锰与乙酸钴的混合溶液中,乙酸锰与乙酸钴的浓度为0.01mol/L~0.02mol/L。
上述的方法,优选的,所述氧化性气体为氯气、或者为臭氧与氧气的混合气体。
上述的方法,优选的,所述步骤(2)中氧化反应的时间为45min~75min。
上述的方法,优选的,所述步骤(2)中,在25℃~70℃下向混合溶液中通入氧化性气体,控制反应温度为25℃~70℃,能够改变锰、钴的成核与生长速率,调节产物粒径大小,调节沉淀速率,使产物为纳米颗粒;反应过程的温度低于25℃,反应变得较缓慢,生产效率低;反应温度高于70℃,反应迅速,且溶液水分挥发严重,不利于晶粒尺寸控制及体系稳定。
上述的方法,优选的,所述步骤(2)中,氧化性气体是经过曝气头通入混合溶液中的。氧化性气体经过曝气头可以在溶液中形成弥散的小气泡,氧化性气体均匀弥散在液体中,然后与溶液中的锰,钴离子反应生成沉淀,使反应更充分。
与现有技术相比,本发明的优点在于:
(1)本发明的制备方法可一步加工得到纳米羟基氧化钴锰,该纳米羟基氧化钴锰可应用于超级电容器及锂离子电池等相关领域。
(2)本发明的制备方法所涉及原料廉价易得,成本低,合成工艺简单易实现,产品质量稳定且工艺重复性能好,反应可以在较短时间内完成,效率高。
附图说明
图1是本发明实施例1制备的纳米羟基氧化钴锰的XRD图。
图2是本发明实施例2制备的纳米羟基氧化钴锰的FESEM图。
具体实施方式
为了便于理解本发明,下文将结合说明书附图和较佳的实施例对本文发明做更全面、细致地描述,但本发明的保护范围并不限于以下具体实施例。
除非另有定义,下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的,并不是旨在限制本发明的保护范围。
除非另有特别说明,本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。
实施例1:
一种本发明的制备纳米羟基氧化钴锰的方法,包括以下步骤:
(1)将四水合乙酸锰与四水合乙酸钴溶于200mL去离子水中,制得的乙酸锰与乙酸钴的浓度均为0.0125mol/L的混合溶液中;
(2)利用稀硫酸调节混合溶液的pH值至2.5;
(3)在35℃下,向步骤(2)处理后的混合溶液中通入臭氧,反应1h,然后离心,洗涤,最后在80℃烘干,得到纳米羟基氧化钴锰产物。
本实施例制备的纳米羟基氧化钴锰产物的XRD图如图1所示,表明产品为羟基氧化钴锰,化学式为(Coa,Mn1-a)OOH,标准卡片号为JCPDS 42-1316;本实施例所制备的纳米羟基氧化钴锰呈球形,粒径为181nm左右;经XPS检测进一步表明其化学式为(Co0.15Mn0.85)OOH。
将本实施例制备得到的纳米羟基氧化钴锰制备成电极片,并在6mol/L KOH溶液中进行恒流充放电检测,测得比容量为707F/g。
实施例2:
一种本发明的制备纳米羟基氧化钴锰的方法,包括以下步骤:
(1)将四水合乙酸锰与四水合乙酸钴溶于200mL去离子水中,制得的乙酸锰与乙酸钴的浓度均为0.0125mol/L的混合溶液中;
(2)利用稀硫酸调节混合溶液的pH值至3.5;
(3)在35℃下,向步骤(2)处理后的混合溶液中通入臭氧,反应45min,然后离心,洗涤,最后在80℃烘干,得到纳米羟基氧化钴锰产物。
本实施例制备的纳米羟基氧化钴锰产物的FESEM图如图2所示,由图可知,本实施例所制备的纳米羟基氧化钴锰呈球形,粒径在200nm左右;经XRD和XPS检测,表明本实施例的纳米羟基氧化钴锰产物的化学式为(Co0.27Mn0.73)OOH。
实施例3:
一种本发明的制备纳米羟基氧化钴锰的方法,包括以下步骤:
(1)将四水合乙酸锰与四水合乙酸钴溶于200mL去离子水中,制得的乙酸锰与乙酸钴混合溶液(混合溶液中乙酸锰浓度为0.0125mol/L,乙酸钴的浓度为0.025mol/L);
(2)利用稀硫酸调节混合溶液的pH值至2.5;
(3)在70℃下,向步骤(2)处理后的混合溶液中通入臭氧,反应1h,然后离心,洗涤,最后在80℃烘干,得到纳米羟基氧化钴锰产物。本实施例所制备的纳米羟基氧化钴锰呈球形,粒径为123nm左右;经XRD和XPS检测,表明本实施例的纳米羟基氧化钴锰产物的化学式为(Co0.48Mn0.52)OOH。
Claims (7)
1.一种制备纳米羟基氧化钴锰的方法,其特征在于,包括以下步骤:
(1)调节乙酸锰与乙酸钴的混合溶液的pH值至2.5~6;
(2)向步骤(1)后的混合溶液中通入氧化性气体进行氧化反应,反应后离心、洗涤、烘干,得到所述纳米羟基氧化锰钴。
2.如权利要求1所述的方法,其特征在于,所述纳米羟基氧化锰钴的化学式为(CoxMn1-x)OOH,其中0<x<1;所述纳米羟基氧化锰钴呈球形,平均粒径为180nm~200nm。
3.如权利要求1所述的方法,其特征在于,所述乙酸锰与乙酸钴的混合溶液中,乙酸锰与乙酸钴的浓度均为0.01mol/L~0.02mol/L。
4.如权利要求1所述的方法,其特征在于,所述氧化性气体为氯气、或者为臭氧与氧气的混合气体。
5.如权利要求1~4任一项所述的方法,其特征在于,所述步骤(2)中氧化反应的时间为45min~75min。
6.如权利要求1~4任一项所述的方法,其特征在于,所述步骤(2)中,在25℃~20℃下向混合溶液中通入氧化性气体。
7.如权利要求1~4任一项所述的方法,其特征在于,所述步骤(2)中,氧化性气体是经过曝气头通入混合溶液中的。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610883535.7A CN106379948B (zh) | 2016-10-10 | 2016-10-10 | 一种制备纳米羟基氧化钴锰的方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610883535.7A CN106379948B (zh) | 2016-10-10 | 2016-10-10 | 一种制备纳米羟基氧化钴锰的方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106379948A true CN106379948A (zh) | 2017-02-08 |
CN106379948B CN106379948B (zh) | 2020-06-26 |
Family
ID=57937261
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610883535.7A Active CN106379948B (zh) | 2016-10-10 | 2016-10-10 | 一种制备纳米羟基氧化钴锰的方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106379948B (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109256532A (zh) * | 2018-03-27 | 2019-01-22 | 清远佳致新材料研究院有限公司 | 一种锂离子电池三元正极材料前驱体合成过程母液综合利用的方法 |
CN112071659A (zh) * | 2020-08-05 | 2020-12-11 | 新昌县华发机械股份有限公司 | 一种聚苯胺水凝胶包覆Co3O4超级电容器电极材料及其制法 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101127398A (zh) * | 2007-06-28 | 2008-02-20 | 河南师范大学 | 一种球形羟基氧化镍钴锰及其制备方法 |
CN100577576C (zh) * | 2007-04-20 | 2010-01-06 | 南京大学 | 臭氧氧化制备α-FeOOH、β-MnO2和Co3O4纳米材料的简便方法 |
CN103904323A (zh) * | 2012-12-28 | 2014-07-02 | 北京当升材料科技股份有限公司 | 一种球形羟基氧化钴的制备方法 |
-
2016
- 2016-10-10 CN CN201610883535.7A patent/CN106379948B/zh active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100577576C (zh) * | 2007-04-20 | 2010-01-06 | 南京大学 | 臭氧氧化制备α-FeOOH、β-MnO2和Co3O4纳米材料的简便方法 |
CN101127398A (zh) * | 2007-06-28 | 2008-02-20 | 河南师范大学 | 一种球形羟基氧化镍钴锰及其制备方法 |
CN103904323A (zh) * | 2012-12-28 | 2014-07-02 | 北京当升材料科技股份有限公司 | 一种球形羟基氧化钴的制备方法 |
Non-Patent Citations (1)
Title |
---|
辛云涛: "含钴溶液臭氧氧化沉淀及其在冶金中的应用研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109256532A (zh) * | 2018-03-27 | 2019-01-22 | 清远佳致新材料研究院有限公司 | 一种锂离子电池三元正极材料前驱体合成过程母液综合利用的方法 |
CN109256532B (zh) * | 2018-03-27 | 2021-04-02 | 清远佳致新材料研究院有限公司 | 一种锂离子电池三元正极材料前驱体合成过程母液综合利用的方法 |
CN112071659A (zh) * | 2020-08-05 | 2020-12-11 | 新昌县华发机械股份有限公司 | 一种聚苯胺水凝胶包覆Co3O4超级电容器电极材料及其制法 |
Also Published As
Publication number | Publication date |
---|---|
CN106379948B (zh) | 2020-06-26 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Cong et al. | Shape control of cobalt carbonate particles by a hydrothermal process in a mixed solvent: an efficient precursor to nanoporous cobalt oxide architectures and their sensing property | |
CN107346824B (zh) | 一种梯度三元正极材料的制备方法及其应用 | |
CN112028126B (zh) | 一种小粒径补锂添加剂Li5FeO4的制备方法和应用 | |
US20190039142A1 (en) | A method for preparing silver powder by using micro-nano bubbles as crystal seeds | |
CN108373175A (zh) | 铝掺杂四氧化三钴及其制备方法和应用 | |
CN106025282B (zh) | 一种高纯超细草酸锰铁及其制备方法 | |
CN109179516B (zh) | 掺铝小颗粒球形四氧化三钴以及其制备方法 | |
Hu et al. | Synthesis of Mn-doped CeO 2 nanorods and their application as humidity sensors | |
CN111170375A (zh) | 一种三元正极材料前驱体及其制备方法 | |
CN105322154A (zh) | 一种特殊形貌的电极活性物质前驱体镍锰氧化物 | |
CN102790211B (zh) | 一种高性能锂离子电池负极材料铁酸铜超细粉的制备方法 | |
CN108598467A (zh) | 氧化铝包覆镍钴锰酸锂正极材料的制备方法及氧化铝包覆镍钴锰酸锂正极材料和锂离子电池 | |
Motlagh et al. | Structural properties of nickel hydroxide/oxyhydroxide and oxide nanoparticles obtained by microwave-assisted oxidation technique | |
CN104045113A (zh) | 一种八面体Mn3O4纳米颗粒的制备方法 | |
Yu et al. | Formation of TiO2 hollow spheres through nanoscale Kirkendall effect and their lithium storage and photocatalytic properties | |
Chu et al. | Hard-template-engaged formation of Co 2 V 2 O 7 hollow prisms for lithium ion batteries | |
CN108987740A (zh) | 镍钴铝酸锂正极材料、其制备方法及应用其的电池 | |
CN106379948A (zh) | 一种制备纳米羟基氧化钴锰的方法 | |
CN104810518A (zh) | 一种钴锰系尖晶石纳米材料及其制备方法和应用 | |
CN115520900A (zh) | 磷掺杂纳米级四氧化三锰及其制备方法和电池 | |
CN104671287A (zh) | 一种纳米氧化锰复合材料的绿色制备方法 | |
CN106006748B (zh) | 一种形貌可控的纳米二氧化锰及其制备方法和应用 | |
Song et al. | One-step template-free synthesis of hollow core–shell α-Fe 2 O 3 microspheres with improved lithium storage and gas-sensing properties | |
CN103066270A (zh) | 一种纳米尖晶石型LiMn2O4的制备方法 | |
CN109616308B (zh) | 一种球形纳米氧化铱dna提取磁性粉末及其生产方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |