CN113881985B - 多孔树枝状泡沫镍、制备方法及应用 - Google Patents
多孔树枝状泡沫镍、制备方法及应用 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 53
- 239000006260 foam Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910018054 Ni-Cu Inorganic materials 0.000 claims abstract description 21
- 229910018481 Ni—Cu Inorganic materials 0.000 claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 21
- 239000000956 alloy Substances 0.000 claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000004070 electrodeposition Methods 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000003792 electrolyte Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 9
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- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000013354 porous framework Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- 241000588724 Escherichia coli Species 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims 1
- 241000894006 Bacteria Species 0.000 abstract description 19
- 230000005684 electric field Effects 0.000 abstract description 16
- 238000004720 dielectrophoresis Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 6
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- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 description 16
- 238000004659 sterilization and disinfection Methods 0.000 description 15
- 239000000758 substrate Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 3
- 239000007844 bleaching agent Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
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- 238000012360 testing method Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
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- 208000005623 Carcinogenesis Diseases 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 238000009440 infrastructure construction Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
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Abstract
本发明公开了一种多孔树枝状泡沫镍的制备方法,主要是通过电化学沉积法,在泡沫镍的三维多孔骨架上,生长出Ni‑Cu合金树枝状分支,再将带有Ni‑Cu合金树枝状分支的泡沫镍在由氢气和氮气构成的混合气体氛围中,于700‑1500℃保温5分钟进行退火,然后降温冷却得成品。采用本发明的显著效果是,在泡沫镍上的Ni‑Cu合金树枝状分支能够聚集大量电荷,从而提高分支处的电压,提高电场强度,强化介电泳去除细菌的效率和效果,细菌在变化电场作用下,向电极移动并最终吸附在带有Ni‑Cu合金树枝状分支的泡沫镍的微孔内,以分离和捕获细菌;此外,去除细菌的时间较短,能耗低,因而使用成本低,可适合于实际生产。
Description
技术领域
本发明涉及介电泳用的电极,具体涉及一种具有尖端电荷聚集效应的电极以及制备方法。
背景技术
目前对水中的细菌进行清除的方法有膜过滤、超声波消杀、紫外线杀菌等;这一般都需要大型的基础设施建设和净水设备投入,且能耗较高;不适合偏远及欠发达的地区。当然,在自来水中加入含氯的漂白粉是现阶段更为常用的杀菌手段,但在我国村镇供应的自来水中,原水中的细菌含量普遍很高,这就面临漂白粉加入量过大造成的氯含量高、气味大、易致癌的问题;而低漂白粉加入量杀菌效果不足的问题。
介电泳,也称双向电泳,是介电常数较低的物体在非均匀电场中受力的现象。介电力大小与物体是否带电无关,而与物体的大小、电学性质、周围介质的电学性质以及外加电场的场强、场强变化率、频率有关。
在前期研究中,有人提出基于介电泳原理捕捉血液中细菌的方法,这为采用介电泳去除水中细菌提供了参考,但在对大量水进行处理时,需要更一步考虑电极材料、能耗、除菌时间、以及除菌效率等问题。
发明内容
有鉴于此,本发明首先提供了一种多孔树枝状泡沫镍的制备方法,其技术方案如下:
步骤一、将片状的泡沫镍清洗备用;
步骤二、配制Ni2+和Cu2+混合电解液,通过电化学沉积法,在泡沫镍的三维多孔骨架上,生长出Ni-Cu合金树枝状分支,得金属半成品;
步骤三、将带有Ni-Cu合金树枝状分支的泡沫镍清洗干燥;
步骤四、将干燥后的带有Ni-Cu合金树枝状分支的泡沫镍在混合气体氛围中,于700-1500℃保温5分钟进行退火,然后降温冷却得成品;
所述混合气体由氢气和氮气构成。
其次,本发明提供一种多孔树枝状泡沫镍,由以上制备方案得到。
最后,本发明提供一种多孔树枝状泡沫镍在水处理除菌过程中作为电极的应用。
附图说明
图1为在成品②上随机选取的一处的1mm扫描电镜图;
图2为在成品②上随机选取的一处的50μm扫描电镜图;
图3为在成品②上随机选取的一处树枝状分支的成分表征图;
图4为实施例3中试验方盒的结构示意图;
图5a为未施加变化的非均匀电场前细菌的位置和分布图;
图5b为刚开始施加变化的非均匀电场时细菌的位置和分布图;
图5c为施加变化的非均匀电场2min后细菌的位置和分布图;
图5d为停止施加变化的非均匀电场后细菌的位置和分布图。
具体实施方式
以下结合实施例和附图对本发明作进一步说明。
实施例1:
一种多孔树枝状泡沫镍的制备方法,按以下步骤进行:
步骤一、将片状的泡沫镍基材用双辊压机压制成厚度为100μm的薄片,然后用丙酮、硫酸和去离子水依次清洗泡以去除其表面的氧化层,备用;
所述泡沫镍基材的孔径为250μm,厚度为1mm;
步骤二、将硫酸铜、氯化镍和硼酸混合形成电解液,所述电解液中硫酸铜的浓度为0.0001M,氯化镍的浓度为0.1M,硼酸的浓度为0.1M;
将泡沫镍置于所述电解液中,再通过电化学沉积法,在泡沫镍的三维多孔骨架上,生长出Ni-Cu合金树枝状分支,得金属半成品;
电化学沉积法参数以及条件:以Ag/AgCl为参比电极,以镍箔为对电极,电压为-0.6V;
步骤三、用去离子水和乙醇分别冲洗带有Ni-Cu合金树枝状分支的泡沫镍,然后将其置于真空干燥器中干燥过夜;
步骤四、将干燥后的带有Ni-Cu合金树枝状分支的泡沫镍置于管式炉中,在混合气体氛围中,于700℃保温5分钟进行退火,最后在所述混合气体氛围条件下随炉降温冷却,最后取出得成品①;
所述混合气体由氢气和氮气构成,其以流动状态通入管式炉内,氢气流速为0.1sccm的,氮气流速为0.1sccm。混合气体自泡沫镍置于管式炉中开始通入,一直保持到退火后冷却至室温停止。
实施例2:
一种多孔树枝状泡沫镍的制备方法,按以下步骤进行:
步骤一、将片状的泡沫镍基材用双辊压机压制成厚度为300μm的薄片,然后用丙酮、硫酸和去离子水依次清洗泡以去除其表面的氧化层,备用;
所述泡沫镍基材的孔径为250μm,厚度为3mm,长度为50mm,宽度为40mm;
步骤二、将硫酸铜、氯化镍和硼酸混合形成电解液,所述电解液中硫酸铜的浓度为0.01M,氯化镍的浓度为1M,硼酸的浓度为1M;
将泡沫镍置于所述电解液中,再通过电化学沉积法,在泡沫镍的三维多孔骨架上,生长出Ni-Cu合金树枝状分支,得金属半成品;
电化学沉积法参数以及条件:以Ag/AgCl为参比电极,以镍箔为对电极,电压为-2.5V;
步骤三、用去离子水和乙醇分别冲洗带有Ni-Cu合金树枝状分支的泡沫镍,然后将其置于真空干燥器中干燥过夜;
步骤四、将干燥后的带有Ni-Cu合金树枝状分支的泡沫镍置于管式炉中,在混合气体氛围中,于1500℃保温5分钟进行退火,最后在所述混合气体氛围条件下随炉降温冷却,最后取出得成品②;
所述混合气体由氢气和氮气构成,其以流动状态通入管式炉内,氢气流速为20sccm的,氮气流速为100sccm。混合气体自泡沫镍置于管式炉中开始通入,一直保持到退火后冷却至室温停止。
成品②的电镜图如图1和图2所示,可以看出,泡沫镍上具有若干树枝状结构的分支,进一步分析得到分支的长度为10-200μm,直径为2-5μm,长径比较高、比表面积显著提高,分支的长短、方向各异,其作为电极时有利于产生非均匀的电场。对树枝状结构的分支进行成分表征,其成分为Cu和Ni,如图3所示。
实施例3:
在试验方盒内布置16片相互平行的电极,每个电极的边缘通过铜箔接线,接线方式为交流/接地/交流/接地……,依次类推,如图4所示;电极采用实施例2制得的成品②,在方盒内注入原水,原水中含有初始浓度为106CFU/mL(菌落/毫升)的大肠杆菌,原水体积100mL;
分别设置多组除菌实验,实验后取样测定大肠杆菌的终止浓度,并计算除菌效率,除菌效率=(初始浓度-终止浓度)/初始浓度*100%,各组的除菌效率见下表:
电压 | 频率 | 持续时间 | 除菌效率 | |
1 | 0.5V | 1×107Hz | 20min | 90.534% |
2 | 4V | 1×107Hz | 20min | 99.126% |
3 | 8V | 1Hz | 20min | 68.765% |
4 | 8V | 1×105Hz | 20min | 99.999% |
5 | 8V | 1×107Hz | 1min | 52.872% |
6 | 8V | 1×107Hz | 5min | 96.365% |
7 | 8V | 1×107Hz | 20min | 99.999% |
从上表可以看出,通过电压为8V、频率为1×105Hz或1×107Hz、持续时间为20min的交流电除菌,原水中的大肠杆菌几乎完全被去除,除菌效果优异。
经计算,在第7组除菌实验中,方盒内电极除菌时所需要的能耗(功率)为435J/L,其远低于现目前主流的污水处理方法所需要的能耗。
实施例4
以金箔为电极,进行细菌在介电场效应作用下移动状态的测试,结果如图5a、5b、5c、5d所示,其展示了水中的细菌在施加变化的非均匀电场前中后的位置;可以看出,在施加变化的非均匀电场一定时间后,细菌向电极两侧移动并聚集,而未施加变化的非均匀电场时(包括施加电场前以及停止施加电场后),细菌在两电极之间随机杂乱分布。
本发明的有益效果:在泡沫镍上的Ni-Cu合金树枝状分支能够聚集大量电荷,从而提高分支处的电压,提高电场强度,强化介电泳去除细菌的效率和效果,细菌在变化电场作用下,向电极移动并最终吸附在带有Ni-Cu合金树枝状分支的泡沫镍的微孔内,以分离和捕获细菌;此外,去除细菌的时间较短,能耗低,因而使用成本低,可适合于实际生产。
最后需要说明的是,上述描述仅仅为本发明的优选实施例,本领域的普通技术人员在本发明的启示下,在不违背本发明宗旨及权利要求的前提下,可以做出多种类似的表示,这样的变换均落入本发明的保护范围之内。
Claims (1)
1.一种多孔树枝状泡沫镍在水处理去除大肠杆菌过程中的应用,其特征在于多孔树枝状泡沫镍作为电极;
对原水施加电压为8V、频率为1×105 Hz或1×107 Hz、持续时间为20min的交流电;
所述多孔树枝状泡沫镍的制备方法按以下步骤进行:
步骤一、将片状的泡沫镍清洗备用;
步骤二、配制Ni2+和Cu2+混合电解液,通过电化学沉积法,在泡沫镍的三维多孔骨架上,生长出Ni-Cu合金树枝状分支,得金属半成品;
步骤三、将带有Ni-Cu合金树枝状分支的泡沫镍清洗干燥;
步骤四、将干燥后的带有Ni-Cu合金树枝状分支的泡沫镍在混合气体氛围中,于700-1500℃保温5分钟进行退火,然后降温冷却得成品;
所述混合气体由氢气和氮气构成;
所述步骤一中,所述泡沫镍的孔径为250μm,厚度为1-3mm,将其用双辊压机压制成厚度为100-300μm的薄片,然后用丙酮、硫酸和去离子水依次清洗以去除其表面的氧化层;
所述步骤二中,将硫酸铜、氯化镍和硼酸混合形成所述电解液,所述电解液中硫酸铜的浓度为0.0001-0.01M,氯化镍的浓度为0.1-1M,硼酸的浓度为0.1-1M;
所述步骤二中,将所述泡沫镍置于所述电解液中,以Ag/AgCl为参比电极,以镍箔为对电极,在(-0.6)—(-2.5)V电压下,采用电化学沉积法在所述泡沫镍的三维多孔骨架上,生长出Ni-Cu合金树枝状分支;
所述步骤三中,用去离子水和乙醇分别冲洗带有Ni-Cu合金树枝状分支的泡沫镍,然后将其置于真空干燥器中干燥过夜;
所述步骤四中,将干燥后的带有Ni-Cu合金树枝状分支的泡沫镍置于管式炉中,并向其中通入流速为0.1-20sccm的氢气,以及流速为0.1-100sccm的氮气,以进行退火;
所述步骤四中,退火完成后,在所述混合气体氛围条件下随炉降温冷却,最后取出得成品。
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