CN102373491A - Method for preparing nanometer materials through electric deposition by reinforced micro electrolysis technology - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 49
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- 238000005516 engineering process Methods 0.000 title abstract description 9
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000002086 nanomaterial Substances 0.000 claims description 34
- 238000004070 electrodeposition Methods 0.000 claims description 32
- 239000012530 fluid Substances 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 13
- -1 metals ion Chemical class 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 239000000956 alloy Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 8
- 239000002659 electrodeposit Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 230000013011 mating Effects 0.000 claims description 4
- 230000002787 reinforcement Effects 0.000 claims description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229930002839 ionone Natural products 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 20
- 239000002245 particle Substances 0.000 abstract description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 2
- 230000003014 reinforcing effect Effects 0.000 abstract 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 229910021645 metal ion Inorganic materials 0.000 abstract 1
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- 239000008187 granular material Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 229910000906 Bronze Inorganic materials 0.000 description 5
- 239000010974 bronze Substances 0.000 description 5
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 4
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 4
- 239000013528 metallic particle Substances 0.000 description 4
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 4
- 238000009827 uniform distribution Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
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- 238000007714 electro crystallization reaction Methods 0.000 description 3
- 230000036647 reaction Effects 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
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- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
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- Water Treatment By Electricity Or Magnetism (AREA)
- Electroplating Methods And Accessories (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a method for preparing nanometer materials through electric deposition by the reinforced micro electrolysis technology, which belongs to the technical field of nanometer material preparation. The method is characterized in that micro electrolysis fillings consisting of an active anode and an inert cathode are placed into a reinforced micro electrolysis reactor, in addition, deposition liquid water solution is fed into the micro electrolysis reactor, metal ions in the deposition liquid are reduced into metal elementary substance on the surface of the fillings under the reinforcing effect of an external electric field after the reinforced micro electrolysis deposition reaction, the goal of controlling the micro electrolysis reaction process is reached through controlling the field intensity of the external electric field, different field intensities of the external electric field have different promotion and reinforcing effect on the micro electrolysis, the uniformity degrees and the nanometer degrees of the electric deposition particles are also different, and the nanometer materials conforming to the requirements of specific dimension, ingredients and the like are finally prepared. The method has the advantages that the particle diameter of the nanometer materials is controllable, the energy consumption is low, the reaction condition is mild, the operation is simple and convenient, and the like.
Description
Technical field
The present invention relates to a kind of method for preparing nano material, relate in particular to a kind of method, belong to the nano material preparation technical field with reinforcement micro electrolysis tech prepared by electrodeposition nano material.
Background technology
Nano material is the type material science that grows up the eighties in 20th century; Compare with common material; Make it have special magnetic, optics, mechanics, electricity, chemical catalysis performance because nano material has small-size effect, surface and interfacial effect, quantum size effect, macro quanta tunnel effect etc., thereby become one of the most attractive popular research of 21 century field of materials.
Preparation method of nano material is varied; Be divided into solid phase method, liquid phase method and vapor phase process from the angle of raw material; Be divided into physics method and chemical method from the angle of reaction, common preparation method has vacuum-evaporation condensation method, ball milled, the precipitator method, sol-gel method, water reaction method, electrodip process, microemulsion method and template synthesis method.Electrodip process more and more receives people's attention and favor in numerous preparing methods, and this is because electrodip process prepares nano material and has the following advantages:
is fit to preparation nano metal, alloy and matrix material;
main impellent of galvanic deposit crystallization-----overpotential; Can artificially control; Whole deposition process realizes computer monitoring easily, difficult technically less, technology is flexible; Thermal stresses that high temperature introduces at material internal etc. has been avoided in
normal temperature and pressure operation simultaneously.
Conventional electro-deposition techniques has dc electrodeposition, pulse electrodeposition and sprays galvanic deposit; These electro-deposition techniques all can obtain the nano material of specific dimensions size under the certain condition of control; But such electrodeposition process needs consumed power, and this must make that the material prepn cost is higher, and how cutting down the consumption of energy and then lowering the material prepn cost to become a research focus; Little electrolysis electrodeposit metals is not because deposition process needs consumed power can reach the purpose that reduces the material prepn cost; For a new route has been opened up in the preparation of nano material, this method adopts active anode particle and inert cathode granulometric composition micro-electrolysis stuffing, and the corrosion galvanic cell reaction takes place between the micro-electrolysis stuffing in deposit fluid; Make active anode dissolve; And treat that the metal refining ion-conductance is deposited on the inert cathode surface, finally accomplish the preparation of material, but the impellent of little electrolysis electro-deposition techniques reaction derives from the electric current and voltage that corrosion galvanic cell produces on the inert cathode surface; Receive metallic particles particle diameter that the restriction galvanic deposit of this electric current and voltage makes big (generally in micron level), do not reach the purpose of preparation nano material.
the big problem of material particle size to above little electrolysis electrodeposition technology for preparing; How through improve, improvement should technology or exploitation United Technologies; Under the prerequisite that keeps little electrolysis electro-deposition techniques advantage, effectively solve above-mentioned drawback problem, become an important techniques problem thereby make the nano material that meets the certain particle size requirement.
Summary of the invention
The present invention has overcome the deficiency and the shortcoming of little electrolysis electrodeposition technology for preparing material, provides a kind of to strengthen micro electrolysis tech prepared by electrodeposition preparation of nanomaterials.
For realizing the object of the invention; The present invention is when the little electrolysis prepared by electrodeposition of tradition metallic particles material; Through introducing an External Electrical Field on micro-electrolysis stuffing, promote the carrying out of corrosion galvanic cell reaction between micro-electrolysis stuffing, make galvanic cell react bigger galvanic cell voltage of violentization generation; And metallic particles high dispersingization, nanometer that this big voltage can impel galvanic deposit to obtain finally make nano material at filling surface.
Of the present invention a kind of to strengthen the method for micro electrolysis tech prepared by electrodeposition nano material; The concrete technical scheme that adopts is: the micro-electrolysis stuffing of active anode and inert cathode composition is placed the reinforcement micro-electrolysis reactor; Add the ratio of the 200-500ml deposit fluid aqueous solution in the 100g micro-electrolysis stuffing; In micro-electrolysis reactor, add the deposit fluid aqueous solution; After strengthening little electrolysis electrodeposit reaction through 5~120min under the external electric field strengthening effect of certain intensity; Metals ion is reduced into metal simple-substance at filling surface to be deposited in the deposit fluid, and to reach the purpose of control micro-electrolysis reaction process, different external electric field field intensity sizes are different to little electrolysis promotion, strengthening effect through control external electric field field intensity size; Galvanic deposit particulate homogenizing is also different with the nanometer degree, finally makes specific dimensions, becomes the nano material of the requirement that grades.
The deposit fluid aqueous solution described in the present invention comprises the metals ion of concentration 1~10000mg/L, the ionogen of concentration 1~100g/L, deposit fluid solution ph=1-9.
Ionogen of the present invention is Na
2SO
4, NaCl, K
2SO
4, a kind of among the KCl etc.
Metals ion of the present invention is one or more arbitrary combination in cupric ion, nickel ion, silver ions, platinum ion, the gold ion.
The external electric field of certain intensity of the present invention is a kind of electric field or several kinds of electric fields in DC electric field, alternating-electric field, the pulsed electrical field; External electric field is the electric field of strength of electric field >=0.1V/cm.
Micro-electrolysis stuffing of the present invention is the binary micro-electrolysis stuffing system of iron, aluminium, copper, carbon arbitrary combination formation; Or iron, copper, aluminium, zinc, carbon the arbitrary combination ternary or the above micro-electrolysis stuffing system of ternary that constitute, or iron, copper, aluminium, the alloy of zinc arbitrary combination and the micro-electrolysis stuffing system of carbon formation.
Ratio >=the 1:10 of anode and the quality of negative electrode in the micro-electrolysis stuffing system of binary micro-electrolysis stuffing system of the present invention or alloy and carbon, alloy is the commercial alloys material; By the active descending order of each composition, the mass ratio in the above micro-electrolysis stuffing system of ternary or ternary between each composition is equal >=1:10.
The form of micro-electrolysis stuffing of the present invention is a decentralized composite grain irregularity filler form, or mating type composite grain structured packing form.
The introducing of external electric field of the present invention mainly shows as the strengthening effect of little electrolytic metal electrodeposition process: little electrolytic metal electrodeposit reaction can impel the galvanic cell reaction to produce a bigger galvanic cell response voltage under the effect of extra electric field; Improve the reaction overpotential of metal electrodeposition; And then the formation of the required nucleus of promotion metal electric crystallization; The electrocrystallization process grows into the multinuclear transient growth again to the multinuclear continuous growth from monokaryon, and the abundant nucleus of filling surface helps metallic particles high dispersingization, the nanometer that electrocrystallization forms; Simultaneously, galvanic cell is reflected at and has changed GOLD FROM PLATING SOLUTION under the polarized action of extra electric field and belong to ionic chemistry potential energy, required activation energy when reducing metal electrodeposition, and then reduce the required overpotential of electrocrystallization nucleation, and nucleation rate increases, and makes the nucleus growth facilitation; And extra electric field can promote the migration of micro-electrolysis stuffing surface electronic, makes filling surface distribution of current homogenizing; Simultaneously can also promote GOLD FROM PLATING SOLUTION to belong to the migration of ion to filling surface, compression double electric layer reduces the electrostatic double layer current potential; Improve mass-transfer efficiency; Accelerate the carrying out of metal electrodeposition reaction, the metal electrodeposition reaction process has been strengthened in the introducing of external electric field, helps the preparation of metal nano material.
A kind of method with reinforcement micro electrolysis tech prepared by electrodeposition nano material of the present invention compared with prior art has the following advantages:
1, compare with the material of traditional micro-electrolysis method preparation, the material particle size of present method preparation is little, homogenizing, nanometer degree are high, and material particle size is controlled.
2, compare with conventional electrodip process, present method energy consumption is low, and the material prepn cost is low.
3, compare with other physico-chemical processes, present method has that technology is simple, easy and simple to handle, speed of response is fast, reaction conditions is gentle--characteristics such as-normal temperature and pressure.
Embodiment
Through embodiment the inventive method is done further to specify below, but protection scope of the present invention is not limited to said content.
Embodiment 1: this is to strengthen the method for micro electrolysis tech prepared by electrodeposition nano material, and concrete steps are following:
Preparation contains Ag
+The deposit fluid aqueous solution of=1mg/L, NaCl=1g/L, pH=9; In the ratio that the 100g micro-electrolysis stuffing adds 500ml deposit fluid solution, in strengthening micro-electrolysis reactor, add the deposit fluid aqueous solution, strengthen and fill iron carbon decentralized composite grain filler in the micro-electrolysis reactor; Iron carbon mass ratio is 1:10; Through parallel-plate electrode control input AC strength of electric field be the External Electrical Field of 0.1V/cm on packing layer, the silver ions in the deposit fluid solution is reduced into silver-colored simple substance at the iron carbon surface and separates out, thereby reaches the purpose of preparation nano material; After strengthening little electrolysis electrodeposit reaction 50min, take out filler; The separation, the carbon granule after the separation that carry out the iron carbon granule successively clean postlyophilization through clear water, absolute ethyl alcohol, observe carbon surface deposited silver layer pattern by ESEM (SEM, the S3400N of Hitachi) at last; Find the deposition of silver particle at the carbon surface uniform distribution, silver-colored grain diameter is about 95nm.
Embodiment 2: this is to strengthen the method for micro electrolysis tech prepared by electrodeposition nano material, and concrete steps are following:
Preparation contains Cu
2+The deposit fluid aqueous solution of=100mg/L, KCl=20g/L, pH=1; In the ratio that the 100g micro-electrolysis stuffing adds the 300ml deposit fluid aqueous solution, in strengthening micro-electrolysis reactor, add the deposit fluid aqueous solution, strengthen and fill aluminum bronze carbon mating type filler in the micro-electrolysis reactor; Aluminum bronze carbon mass ratio is 2:1:1; Through parallel-plate electrode control input pulse strength of electric field be the External Electrical Field of 3V/cm on packing layer, the cupric ion in the deposit fluid aqueous solution is reduced into copper simple substance at the aluminum bronze carbon surface and separates out, thereby reaches the purpose of preparation nano material; After strengthening little electrolysis electrodeposit reaction 120min, take out filler; The separation, the carbon granule after the separation that carry out the aluminum bronze carbon granule successively clean postlyophilization through clear water, absolute ethyl alcohol, observe carbon surface copper settled layer pattern by ESEM (SEM, the S3400N of Hitachi) at last; Find the copper deposited particles at the carbon surface uniform distribution, the copper grain diameter is about 30nm.
Embodiment 3: this is to strengthen the method for micro electrolysis tech prepared by electrodeposition nano material, and concrete operations are following:
Preparation contains Pt
2+=10000mg/L, K
2SO
4The deposit fluid aqueous solution of=100g/L, pH=4; In the ratio that the 100g micro-electrolysis stuffing adds the 200ml deposit fluid aqueous solution, in strengthening micro-electrolysis reactor, add the deposit fluid aqueous solution, strengthen filling aluminum copper alloy mating type filler in the micro-electrolysis reactor; The aluminum bronze mass ratio is 2:1; Through parallel-plate electrode control input dc power intensity of field be the External Electrical Field of 6V/cm on packing layer, the platinum ion in the deposit fluid solution is reduced into platinum simple substance on the aluminum-copper alloy surface and separates out, thereby reaches the purpose of preparation nano material; After strengthening little electrolysis electrodeposit reaction 5min, take out filler; Alloy packing successively cleans postlyophilization through clear water, absolute ethyl alcohol, observes alloy surface platinum settled layer pattern by ESEM (SEM, the S3400N of Hitachi) at last; Find the platinum deposited particles at the alloy surface uniform distribution, the platinum grain particle diameter is about 50nm.
Embodiment 4: this is to strengthen the method for micro electrolysis tech prepared by electrodeposition nano material, and concrete steps are following:
Preparation contains Cu
2+=300mg/L, Ni
2+=100mg/L, Na
2SO
4The deposit fluid aqueous solution of=20g/L, pH=4; In the ratio that the 100g micro-electrolysis stuffing adds the 300ml deposit fluid aqueous solution, in strengthening micro-electrolysis reactor, add the deposit fluid aqueous solution, strengthen filling aluminum carbon decentralized granular filler in the micro-electrolysis reactor; Aluminium carbon mass ratio is 6:1; Through parallel-plate electrode control input dc power intensity of field be the External Electrical Field of 5V/cm on packing layer, the Cu in the deposit fluid solution, Ni ion are reduced into alloyed metal simple substance at aluminium carbon surface codeposition, thereby reach the purpose of preparation nano-copper-nickel alloy material; After strengthening little electrolysis electrodeposit reaction 60min, take out filler; The separation, the carbon granule after the separation that carry out the aluminium carbon granule successively clean postlyophilization through clear water, absolute ethyl alcohol, at last by ESEM (SEM, the S3400N of Hitachi; EDAX E-550) observes carbon surface alloy deposition layer pattern, finds the alloy deposition particle at the carbon surface uniform distribution, and the alloying pellet particle diameter is about 60nm, and the EDS results of elemental analyses shows that copper nickel mass ratio is about 0.35 in this alloy.
Claims (8)
1. one kind to strengthen the method for micro electrolysis tech prepared by electrodeposition nano material; It is characterized in that: the micro-electrolysis stuffing of active anode and inert cathode composition is placed the reinforcement micro-electrolysis reactor; Add the ratio of 200~500ml deposit fluid aqueous solution in the 100g micro-electrolysis stuffing; In micro-electrolysis reactor, add the deposit fluid aqueous solution, strengthen little electrolysis electrodeposit reaction through 5~120min under the electric field-enhanced outside effect after, make metal nano material.
2. according to claim 1 to strengthen micro electrolysis tech prepared by electrodeposition nano material method, it is characterized in that: the deposit fluid aqueous solution comprises the metals ion of concentration 1~10000mg/L, the ionogen of concentration 1~100g/L, deposit fluid solution ph=1~9.
3. according to claim 2 to strengthen micro electrolysis tech prepared by electrodeposition nano material method, it is characterized in that: ionogen is Na
2SO
4, NaCl, K
2SO
4, a kind of among the KCl.
4. according to claim 2 to strengthen micro electrolysis tech prepared by electrodeposition nano material method, it is characterized in that: metals ion be in cupric ion, nickel ion, silver ions, platinum ion, the gold ion one or more.
5. according to claim 1 to strengthen micro electrolysis tech prepared by electrodeposition nano material method, it is characterized in that: external electric field is one or more electric fields in DC electric field, alternating-electric field, the pulsed electrical field, external electric field intensity >=0.1V/cm.
6. according to claim 1 to strengthen micro electrolysis tech prepared by electrodeposition nano material method; It is characterized in that: micro-electrolysis stuffing is the binary micro-electrolysis stuffing system of iron, aluminium, copper, carbon arbitrary combination formation; Or iron, copper, aluminium, zinc, carbon the arbitrary combination ternary or the above micro-electrolysis stuffing system of ternary that constitute, or iron, copper, aluminium, the alloy of zinc arbitrary combination and the micro-electrolysis stuffing system of carbon formation.
7. according to claim 6 to strengthen micro electrolysis tech prepared by electrodeposition nano material method, it is characterized in that: the ratio >=1:10 of anode and the quality of negative electrode in the micro-electrolysis stuffing system of binary micro-electrolysis stuffing system or alloy and carbon; By the active descending order of each composition, the mass ratio in the above micro-electrolysis stuffing system of ternary or ternary between each composition is equal >=1:10.
8. according to claim 1 to strengthen micro electrolysis tech prepared by electrodeposition nano material method, it is characterized in that: the form of micro-electrolysis stuffing is a decentralized composite grain irregularity filler form, or mating type composite grain structured packing form.
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CN103359813A (en) * | 2013-08-09 | 2013-10-23 | 中国矿业大学(北京) | Water sterilizing system |
CN105645525A (en) * | 2016-01-13 | 2016-06-08 | 北方工程设计研究院有限公司 | Catalytic microelectrolysis packing, as well as preparation method and application thereof |
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CN201713362U (en) * | 2010-04-13 | 2011-01-19 | 昆明理工大学 | Plate type compound electrochemical device used for recovering heavy metal in wastewater |
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CN201713362U (en) * | 2010-04-13 | 2011-01-19 | 昆明理工大学 | Plate type compound electrochemical device used for recovering heavy metal in wastewater |
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CN103359813A (en) * | 2013-08-09 | 2013-10-23 | 中国矿业大学(北京) | Water sterilizing system |
CN105645525A (en) * | 2016-01-13 | 2016-06-08 | 北方工程设计研究院有限公司 | Catalytic microelectrolysis packing, as well as preparation method and application thereof |
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