CN108483495B - 一种BiOF材料的制备方法及其应用 - Google Patents
一种BiOF材料的制备方法及其应用 Download PDFInfo
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- 229910016295 BiOF Inorganic materials 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000003990 capacitor Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 6
- 239000011737 fluorine Substances 0.000 claims abstract description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 239000002135 nanosheet Substances 0.000 claims abstract description 3
- 239000002105 nanoparticle Substances 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003570 air Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
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- 229920002866 paraformaldehyde Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 235000003270 potassium fluoride Nutrition 0.000 claims description 3
- 239000011698 potassium fluoride Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 150000001720 carbohydrates Chemical class 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 239000000049 pigment Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000003682 fluorination reaction Methods 0.000 abstract description 2
- 238000006479 redox reaction Methods 0.000 abstract description 2
- 238000000713 high-energy ball milling Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- IPNGSXQUQIUWKO-UHFFFAOYSA-N bismuth;fluoro hypofluorite Chemical compound [Bi].FOF IPNGSXQUQIUWKO-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 4
- 239000012265 solid product Substances 0.000 description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229940073609 bismuth oxychloride Drugs 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
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- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
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- 239000003792 electrolyte Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
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- 235000019441 ethanol Nutrition 0.000 description 1
- -1 fluorine ions Chemical class 0.000 description 1
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
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- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
本发明涉及一种BiOF材料的制备方法及其应用。本发明以铋酸盐、还原剂、氟源、助剂为原料,将高能球磨的机械力同步作用于氧化还原与氟化反应,再经过热处理、洗涤除杂、固液分离、干燥制备出BiOF材料。所制备的BiOF材料由2~500nm纳米片或纳米颗粒构成,比表面积为3~300m2/g。本发明具有工艺简单、易于工业化生产、制造工艺成本低、环境友好等优势;所制备的BiOF材料在超级电容器、碱性二次电池、锂离子电池、光催化剂、珠光颜料、医药等领域具有广泛应用。
Description
技术领域
本发明涉及一种BiOF材料的制备方法及其应用,属于新型功能材料领域。
背景技术
氟氧化铋是一种重要的功能材料,由于其独特的微观结构及物理化学性质,并且无毒、成本低,将广泛应用在电极活性材料、催化剂、颜料、化妆品、气体传感器、电子材料、医药材料等领域。
材料的结构与性能与制备工艺方法密切相关。目前合成超细功能粉体的方法根据合成原理可分为物理法和化学法。物理法可制得粒径易控的超细粒子,但所需设备昂贵;化学法成本低,易于通过过程控制调整粒子大小,但工艺流程复杂、并有可能带来环境污染。机械化学法是将物理法与化学法相结合,其基本原理是反应物质通过研磨过程提供的能量,提高反应物的化学活性,使得通常需要在高温下进行的反应能在较低温度下快速进行。机械化学合成方法是一种价格低廉、环境友好、高效率和可控性高的合成方法,这一制备方法使得材料的结构与性能具有更多的设计可能性、且易于工业化生产。
Su等[Scripta Materialia 62(2010)345-348]以硝酸铋、氟化铵为原料,乙二醇为溶剂,采用液相沉淀及后续的热处理方法制备出BiOF材料并在紫外光下研究了它的光催化性能。Matar等[Solid State Ionics11(1983)77-81]以Bi2O3和BiF3为原料,通过600℃的高温固相法制备出BiOF材料。Teng等[RSC Adv.5(2015)88936-88942]以硝酸铋、氟化铵为原料,乙醇为溶剂,通过溶剂热法制备出(002)晶面暴露的BiOF纳米材料,并研究了在紫外光下降解罗丹明B的光催化性能。
发明专利[申请公布号CN104148094A]公开了“一种氟氧化铋/石墨烯复合可见光催化剂的制备方法”,该发明用乙二醇分别溶解硝酸铋和氟化钠,采用水解沉淀法制备出氟氧化铋。发明专利[申请公布号CN104891444A]公开了“一种制备BiOF光催化剂的方法及催化剂作用”,该发明以四氢呋喃水溶液为溶剂,以硝酸铋和氢氟酸为原料,通过水热法合成了BiOF光催化剂。
目前只有少量关于BiOF材料的制备研究,主要有水热法,溶剂热法等。但是这些方法普遍存在合成过程复杂,成本高,生产过程中会产生有害副产物,不适合大量生产等问题。
发明内容
本发明的目的在于提供一种BiOF材料的制备方法及其应用。将高能球磨的机械力同步作用于氧化还原与氟化反应,再经过热处理、洗涤除杂、固液分离、干燥制备出BiOF材料。
本发明通过以下技术方案实现:
一种BiOF材料的制备方法,包括如下步骤:
(1)将铋酸盐、还原剂、氟源和助剂按1:(0.25~2):(1~2):(0.001~0.3)的摩尔比(物质的量之比)混合均匀,得到原料混合物;
(2)将步骤(1)所得原料混合物和磨球按1:(1~100)的质量比放入球磨机中,在保护气氛下球磨0.2h~20h;
(3)将步骤(2)得到的球磨混合物置于高温炉中在100~600℃下热处理0.5~10h,将热处理后的产物分别用蒸馏水和无水乙醇进行洗涤除杂,然后进行固液分离、干燥,即得BiOF材料。
进一步地,所述的铋酸盐为铋酸钠、铋酸锂、铋酸钾、铋酸镁中的一种或两种以上。
进一步地,所述的氟源为含氟离子的化合物,优选氟化钠、氟化钾、氟化铵、氟化氢铵、氟化氢中的一种或两种以上。
进一步地,所述的还原剂为金属铋粉、碳粉、亚硫酸盐、甲醛(或多聚甲醛)、甲酸、还原糖、苯酚中的一种或两种以上。
进一步地,所述助剂为十二烷基磺酸钠、十二烷基苯磺酸钠、十六烷基三甲基溴化铵、聚乙烯吡咯烷酮、聚乙二醇、聚乙烯醇、三乙醇胺、乙二醇、丙三醇、非离子型表面活性剂、糖类物质、可溶性淀粉中的一种或两种以上。
进一步地,所述的保护气氛为氮气、氩气、二氧化碳、空气中的一种或两种以上。
进一步地,球磨机的转速为30~3000rpm。
进一步地,所述的球磨机选自市场上的各种机型;所述的磨球为玛瑙球、刚玉球、氧化锆球、瓷球、不锈钢球中的一种或两种以上。
上述制备方法所得到的BiOF材料在超级电容器、碱性二次电池、锂离子电池、光催化剂、医药等领域中的应用。
本发明的有益效果在于:
(1)本发明方法制备工艺简单、工艺条件较温和、易于工业化生产、生产过程环境友好,产品纯度高、产品微观形貌结构及大小易于控制。
(2)本发明所制备的氯氧化铋材料应用广泛,能够应用的领域包括但不限于在超级电容器、碱性二次电池、锂离子电池、光催化剂、珠光颜料、医药等领域。
附图说明
图1为实施例1所制备的BiOF材料的扫描电子显微镜图。
图2为实施例2所制备的BiOF材料的X射线衍射图。
图3为实施例3中BiOF/炭超级电容电池在不同电流密度下的恒电流充放电
测试图。
图4为实施例4所制备的BiOF材料的氮吸脱附等温线图。
具体实施方式
下面以具体实施例进一步说明本发明的技术方案,但本发明并不局限于实施例。
实施例1
(1)将2mmol铋酸钠,1mmol金属铋粉,2mmol氟化钾,0.15mmol聚乙烯吡咯烷酮混合均匀,得到原料混合物;将原料混合物和刚玉磨球按1:50的质量比加到球磨机中,通入空气,在转速为1000rpm条件下进行球磨8h,将球磨后的混合物在300℃下恒温热处理5h,再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离,最后将过滤所得的固体产物在110℃下干燥12h制备出BiOF材料。
(2)采用JEOLJEM-3010型扫描电子显微镜对实施例1所得BiOF材料进行表征,如图1所示,BiOF材料由10~20nm的纳米片状堆积组成。
实施例2
(1)将2mmol铋酸钾,2mmol亚硫酸钠,2mmol氟化铵,0.1mmol聚乙二醇混合均匀,得到原料混合物;将原料混合物和瓷质磨球按1:100的质量比加到球磨机中,通入氮气,在转速为1500rpm条件下进行球磨4h,将球磨后的混合物在450℃下恒温热处理4h,再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离,最后将过滤所得的固体产物在100℃下真空干燥8h制备出BiOF材料。
(2)采用XRD-6000型X-射线衍射仪对实施例2所制备的BiOF材料进行测试,如图2所示,所得BiOF产品晶相纯净,无其它杂质峰,结晶度好。
实施例3
(1)将2mmol铋酸镁,2mmol多聚甲醛,2mmol氟化钠,0.05mmol十六烷基三甲基溴化铵混合均匀,得到原料混合物;将原料混合物和氧化锆磨球按1:60的质量比加到球磨机中,通入氩气,在转速为1200rpm条件下进行球磨6h,将球磨后的混合物在300℃下恒温热处理3h,再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离,最后将过滤所得的固体产物在100℃下干燥8h制备出BiOF材料。
(2)采用上海辰华公司生产的CHI660A电化学工作站,将实施例3所制备的BiOF样品及活性炭分别制成电极片,采用6mol/L KOH溶液为电解质,组装成BiOF/炭超级电容电池,对所构造的电容电池在室温下进行恒流充放电测试。由图3可知,BiOF/炭超级电容电池在0.5A/g的电流密度下比容量达到138mAh/g,在电流密度为1、2、5A/g时的比容量分别为131、127、100mAh/g。
实施例4
(1)将2mmol铋酸钠,1mmol还原糖,2mmol氟化氢铵混合均匀得到原料混合物;将原料混合物和不锈钢磨球按1:50的质量比加到球磨机中,通入空气,在转速为800rpm条件下进行球磨10h,将球磨后的混合物在400℃下恒温热处理3h,再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离,最后将过滤所得的固体产物在110℃下干燥9h制备出BiOF材料。
(2)采用TriStar II 3020型比表面积和孔径分布仪对实施例4所得样品材料进行测试,如图4所示,氯氧化铋材料的比表面积为20.4m2/g。
Claims (5)
1.一种BiOF材料的制备方法,其特征在于,所述的掺杂BiOF材料应用于超级电容电池中,所述的BiOF材料由2~500nm纳米片或纳米颗粒构成,比表面积为3~300m2/g;其制备方法包括如下步骤:
(1) 将铋酸盐、还原剂、氟源和助剂按1:(0.25~2):(1~2):(0.001~0.3)的摩尔比混合均匀,得到原料混合物;
(2) 将步骤(1)所得原料混合物和磨球按1:(0.5~100)的质量比放入球磨机中,在保护气氛下球磨0.2h~20h;
(3) 将步骤(2)得到的球磨混合物置于高温炉中在100~600℃下热处理0.5~10h,将热处理后的产物分别用蒸馏水和无水乙醇进行洗涤除杂,然后进行固液分离、干燥,即得BiOF材料;
所述的氟源为氟化钠、氟化钾、氟化铵、氟化氢铵、氟化氢中的一种或两种以上;
所述的还原剂为金属铋粉、碳粉、亚硫酸盐、甲醛、多聚甲醛、甲酸、还原糖、苯酚中的一种或两种以上;
所述助剂为十二烷基磺酸钠、十二烷基苯磺酸钠、十六烷基三甲基溴化铵、聚乙烯吡咯烷酮、聚乙二醇、聚乙烯醇、三乙醇胺、乙二醇、丙三醇、非离子型表面活性剂、糖类物质、可溶性淀粉中的一种或两种以上。
2.根据权利要求1所述的BiOF材料的制备方法,其特征在于,所述的铋酸盐为铋酸钠、铋酸锂、铋酸钾中的一种或两种以上。
3.根据权利要求1所述的BiOF材料的制备方法,其特征在于,所述的保护气氛为氮气、氩气、二氧化碳、空气中的一种或两种以上。
4.根据权利要求1所述的BiOF材料的制备方法,其特征在于,球磨机的转速为30~3000rpm。
5.根据权利要求1所述的BiOF材料的制备方法,其特征在于,所述的球磨机选自市场上的各种机型;所述的磨球为玛瑙球、刚玉球、氧化锆球、瓷球、不锈钢球中的一种或两种以上。
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