CN107230551B - 一种TiO2/GQDs/NiS异质结光阳极及其制备方法 - Google Patents
一种TiO2/GQDs/NiS异质结光阳极及其制备方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
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- 239000002131 composite material Substances 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002071 nanotube Substances 0.000 claims abstract description 9
- 239000002096 quantum dot Substances 0.000 claims abstract description 9
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 8
- 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 claims abstract description 6
- 238000007743 anodising Methods 0.000 claims abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000012153 distilled water Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000011010 flushing procedure Methods 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 6
- 230000005693 optoelectronics Effects 0.000 claims description 6
- RLLPVAHGXHCWKJ-IEBWSBKVSA-N (3-phenoxyphenyl)methyl (1s,3s)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylate Chemical compound CC1(C)[C@H](C=C(Cl)Cl)[C@@H]1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 RLLPVAHGXHCWKJ-IEBWSBKVSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
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- 150000002815 nickel Chemical class 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- GAIQJSWQJOZOMI-UHFFFAOYSA-L nickel(2+);dibenzoate Chemical compound [Ni+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 GAIQJSWQJOZOMI-UHFFFAOYSA-L 0.000 claims description 2
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
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- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
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- 238000002513 implantation Methods 0.000 description 1
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- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
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Abstract
本发明公开了一种TiO2/GQDs/NiS复合光阳极及其制备方法，解决了TiO2光电转换效率较低的问题。本发明以钛片为基体，含有石墨烯量子点的乙二醇、氟化铵水溶液为电解液，通过阳极氧化法，制备出含有石墨烯量子点(GQDs)的TiO2复合膜。再通过连续离子层吸附‑沉淀反应将NiS纳米颗粒沉积到TiO2表面，然后在氮气管式炉中，退火20min得到TiO2/GQDs/NiS复合光阳极。TiO2/GQDs/NiS(浸渍8次)复合膜光电流密度是TiO2纳米管的2倍。本发明方法简便、易于操作，所制备的TiO2/GQDs/NiS复合光电极具有很高的光催化活性及稳定性。
Description
技术领域
本发明所属技术领域为光催化、光电化学材料技术领域，特别涉及二氧化钛异质结光催化剂开发及制备方法。
背景技术
TiO2纳米管阵列(TNA)由于其高的比表面积，优良的电荷传输性能、无毒、催化活性高、化学稳定性和低成本等优点而受到研究者们的青睐。TNA在气体传感器、太阳能电池、生物催化剂、生物医学植入材料和锂离子电池等方面的应用是很吸引人的。然而TiO2仅能吸收500nm以下波长的太阳光，无法充分利用太阳光的能源；并且光生电子空穴对易于复合，导致光电转换效率较低，在实际应用中仍有许多地方有待改进和完善。因此对TiO2光敏半导体通过改性形成异质结，以提高其光电化学性能。对光催化活性具有重要意义。
GQDs具有很强的sp2杂化碳结构，因此其稳定性非常好，在高强度紫外光条件下也不发生化学变化。而且石墨烯量子点是非金属的碳材料结构，稳定性好、成本低、污染小、在各方面都有很大的应用前景。然而，GQDs的研究还处于早期阶段，这种材料的潜能还没有完全探索出来，因此针对GQDs独特的物理化学性质，将GQDs与TiO2光敏半导体材料进行复合改性。
硫化镍是一种窄带隙的直接半导体，吸光系数较高，被应用于太阳能电池、光电导元件、光电设备的光敏薄膜、光敏涂料和红外探测器等。特别地，NiS因其带隙比较窄而具有非常宽的吸收光谱，使其成为一种高效的半导体光催化剂材料。所以本专利中将NiS作为助催化剂与TiO2构建异质结催化剂，以提高TiO2的光电化学性能及稳定性。
发明内容
本发明的目的是提供一种可见光催化剂纳米TiO2/GQDs/NiS光阳极及其制备方法，该方法操作简便、易于操作，所制备的TiO2纳米管复合膜具有很高的光催化活性。
具体步骤为：
(1)阳极氧化合成TiO2纳米管，将钛片分别在丙酮、乙醇、蒸馏水中各超声15分钟。电解液为0.3wt％的氟化铵和2wt％的蒸馏水以及100mL的乙二醇，向电解液中加入5～50mL的石墨烯量子点，设置直流稳压电源输出电压为 20～100V，阳极氧化时间进行0.5～5h后结束。最后将阳极氧化试片用蒸馏水冲洗，冷风吹干，得到包含GQDs的TiO2纳米管阵列膜。
(2)将步骤(1)中制备的光阳极浸入0.03M的乙醇化的镍盐溶液中 0.5～5min，然后用乙醇冲洗掉样品表面过量松散的吸附离子，再将光电极浸入 0.03M的硫源和甲醇水溶液中2～6min，硫源：甲醇体积比为1:1。最后将样品试片用蒸馏水冲洗，冷风吹干，保存待处理。
(3)将步骤(2)中的样品试片置于管式炉中，将管式炉中抽成真空，再充入氮气，待管式炉中充满氮气后，以5℃/min的升温速率升温至300～600℃，退火2h，待其降温后取出，得到钛箔表面沉积TiO2/GQDs/NiS复合膜光阳极。
所述的镍盐为硝酸镍、硫酸镍、氯化镍、氟化镍、苯甲酸镍中的一种。
所述硫源为硫化钠、硫化钾、硫化铵中的一种。
所述化学试剂纯度均为化学纯以上纯度。
本发明TiO2/GQDs/NiS复合物展示出了优异的吸光性能和很强的光电化学响应，光生电流密度为是纯TiO2的2倍；同时有较好的稳定性，因此， TiO2/GQDs/NiS作为一种可见光响应材料，在环境污染如降解染料、光催化处理污水，太阳能电池等方面具有很大的应用潜能。
附图说明
图1为本发明实施例1制备的浸渍不同次数的TiO2和TiO2/GQDs/NiS的 XRD图谱。
图2为本发明实施例1制备TiO2/GQDs/NiS的拉曼光谱图
图3为本发明实施例1制备TiO2/GQDs/NiS的透射电镜图。
图4为本发明实施例1制备的TiO2和TiO2/GQDs/NiS复合物的光生电流曲线。
具体实施方式
实施例1：
(1)阳极氧化合成TiO2纳米管，将钛片分别在丙酮、乙醇、蒸馏水中各超声15分钟。电解液为0.3wt％的氟化铵和2wt％的蒸馏水以及100mL的乙二醇，向电解液中加入10mL的石墨烯量子点，设置直流稳压电源输出电压为60V，阳极氧化时间进行2h后结束。最后将阳极氧化试片用蒸馏水冲洗，冷风吹干，保存待处理。
(2)将步骤(1)中制备的光阳极浸入0.03M的乙醇化的硝酸镍溶液中2min，然后用乙醇冲洗掉样品表面过量松散的吸附离子，再将光电极浸入0.03M的硫化钠水溶液中5min。将样品试片用蒸馏水冲洗，冷风吹干，重复此步骤5次，保存待处理。
(3)将步骤(2)中的样品试片置于管式炉中，将管式炉中抽成真空，再充入氮气，待管式炉中充满氮气后，以5℃/min的升温速率升温至380℃，退火 2h，待其降温后取出，得到钛箔表面沉积TiO2/GQDs/NiS复合膜光阳极。
此法获得的TiO2/GQDs/NiS复合膜光电流密度为是纯TiO2的2倍。
实施例2：
(1)阳极氧化合成TiO2纳米管，将钛片分别在丙酮、乙醇、蒸馏水中各超声15分钟。电解液为0.3wt％的氟化铵和2wt％的蒸馏水以及100mL的乙二醇，向电解液中加入15mL的石墨烯量子点，设置直流稳压电源输出电压为60V，阳极氧化时间进行2h后结束。最后将阳极氧化试片用蒸馏水冲洗，冷风吹干，保存待处理。
(2)将步骤(1)中制备的光阳极浸入0.03M的乙醇化的硫酸镍溶液中2min，然后用乙醇冲洗掉样品表面过量松散的吸附离子，再将光电极浸入0.03M的硫化钾水溶液中5min，再样品试片用蒸馏水冲洗，冷风吹干，重复此步骤3次，烘干，保存待处理。
(3)将步骤(2)中的样品试片置于管式炉中心，将管式炉中抽成真空，再充入氮气，待管式炉中充满氮气后，以5℃/min的升温速率升温至500℃，退火2h，待其降温后取出，得到钛箔表面沉积TiO2/GQDs/NiS复合膜光阳极。
此法获得的TiO2/GQDs/NiS复合膜光电流密度为是纯TiO2的1.8倍。
实施例3：
(1)阳极氧化合成TiO2纳米管，将钛片分别在丙酮、乙醇、蒸馏水中各超声15分钟。电解液为0.3wt％的氟化铵和2wt％的蒸馏水以及100mL的乙二醇，向电解液中加入20mL的石墨烯量子点，设置直流稳压电源输出电压为60V，阳极氧化时间进行2h后结束。最后将阳极氧化试片用蒸馏水冲洗，冷风吹干，保存待处理。
(2)将步骤(2)中制备的光阳极浸入0.03M的乙醇化的氯化镍溶液中4min，然后用乙醇冲洗掉样品表面过量松散的吸附离子，再将光电极浸入0.03M的硫化铵水溶液中6min，再将样品试片用蒸馏水冲洗，冷风吹干，重复此步骤8次，保存待处理。
(3)将步骤(2)中的样品试片置于管式炉中心，将管式炉中抽成真空，再充入氮气，待管式炉中充满氮气后，以5℃/min的升温速率升温至450℃，退火2h，待其降温后取出，得到钛箔表面沉积TiO2/GQDs/NiS复合膜光阳极。
此法获得的TiO2/GQDs/NiS复合膜光电流密度为是纯TiO2的1.6倍
以上实施例所述化学试剂纯度均为化学纯。
Claims (1)
1.一种TiO2/GQDs/NiS异质结光阳极,摩尔比组成为TiO2 85～99％，石墨烯量子点(GQDs)0.1～5％，NiS0.5～10％；所述TiO2/GQDs/NiS异质结光阳极的制备方法，具体步骤为：
(1)阳极氧化合成TiO2纳米管，将钛片分别在丙酮、乙醇、蒸馏水中各超声15分钟；电解液为0.3wt％的氟化铵和2wt％的蒸馏水以及100mL的乙二醇，向电解液中加入5～50mL的石墨烯量子点，设置直流稳压电源输出电压为20～100V，阳极氧化时间进行0.5～5h后结束；最后将阳极氧化试片用蒸馏水冲洗，冷风吹干，得到包含GQDs的TiO2纳米管阵列膜；
(2)将步骤(1)中制备的光阳极浸入0.03M的乙醇化的镍盐溶液中0.5～5min，然后用乙醇冲洗掉样品表面过量松散的吸附离子，再将光电极浸入0.03M的硫源和甲醇水溶液中2～6min，硫源：甲醇体积比为1:1；最后将样品试片用蒸馏水冲洗，冷风吹干，保存待处理；
(3)将步骤(2)中的样品试片置于管式炉中，将管式炉中抽成真空，再充入氮气，待管式炉中充满氮气后，以5℃/min的升温速率升温至300～600℃，退火2h，待其降温后取出，得到钛箔表面沉积TiO2/GQDs/NiS复合膜光阳极；
其特征在于：步骤(3)中镍盐为硝酸镍、硫酸镍、氯化镍、氟化镍、苯甲酸镍中的一种，硫源为硫化钠、硫化钾、硫化铵中的一种。
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