CN106564951A - Synthesis method of MoS2 nano-structure material - Google Patents
Synthesis method of MoS2 nano-structure material Download PDFInfo
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- CN106564951A CN106564951A CN201610980001.6A CN201610980001A CN106564951A CN 106564951 A CN106564951 A CN 106564951A CN 201610980001 A CN201610980001 A CN 201610980001A CN 106564951 A CN106564951 A CN 106564951A
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- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A synthesis method of a MoS2 nano-structure material is carried out with MoO2 as a precursor and L-cysteine as a sulfurizing agent under a hydrothermal condition. The synthesis method includes the steps of: (1) dissolving 5 parts by mass of MoO2 in 2 parts by mass of n-hexanol; (2) adding 1-5 parts by mass of L-cysteine to the solution prepared in the step (1), wherein the solution contains 8 parts by mass of the MoO2 and all the mass part values are integers; (3) uniformly stirring the solution in the step (2); (4) pouring the solution in the step (3) into a stainless steel hydrothermal reaction kettle to perform a reaction; (5) centrifuging a reaction product in the step (4) for 20-30 min; (6) performing ethanol ultrasonic cleaning to the centrifuged reaction product in the step (5); and (7) drying the cleaned product in the step (6).
Description
Technical field
The invention belongs to inorganic advanced material technical field, and in particular to a kind of that there are regular spherical morphology, uniform particle sizes
MoS2The synthetic method of nano structural material.
Background technology
With conventional fossil, the problem of environmental pollution petered out and increasingly highlight of coal equal energy source, find green, can
The lasting energy is extremely urgent., used as a kind of preferable energy carrier, with green, environmental protection, energy density is high and comes for hydrogen
The advantages of source is extensive, especially in conversion process of energy, final product is water, does not produce the pollutant such as nitride, sulfide,
Additionally, hydrogen serves not only as the fuel of cleaning, while also have important purposes at aspects such as chemical industry, oil and metallurgy, such as
Industry synthetic ammonia etc..Therefore, seek efficiently, the hydrogen preparation method of energy-conservation become one of current study hotspot.With tradition
Oil, coal it is different with natural gas equal energy source, there is no the pure hydrogen that directly can be utilized in nature, therefore, it is extensive cheap
The exploitation for preparing hydrogen technology is the matter of utmost importance that Hydrogen Energy needs to solve.The method for preparing hydrogen at present mainly has Pintsch process day
Three kinds of right gas method, water gas method and water electrolysis method, wherein, Pintsch process natural gas and water gas method are industrial at present conventional
Hydrogen preparation method, both approaches are both needed to carry out at high temperature, and energy consumption is larger, and is inevitably generated in hydrogen production process
Carbon dioxide with greenhouse effect, therefore, to take a long view, both preparation methoies do not meet wanting for sustainable development
Ask.And during the entire process of using electrocatalytic decomposition water, the hydrogen obtained by negative electrode is very pure, and preparation condition is relatively warm
With without the need for further separating-purifying；Meanwhile, the oxygen that anode is produced can be applied to medical science, diving as pure by-product
With space flight etc..This hydrogen production process is applied to sea water and fresh water, and abundant water resource reduces cost to a certain extent.Cause
This, electrolysis water prepares hydrogen will become the core technology of following industries, with very high Social benefit and economic benefit.And
With metal-oxide MoS2Film modified glass-carbon electrode, and the working electrode of electrolysis water is used as, because have preferably urging
Change activity and stability, there is in terms of electrolysis water prepares hydrogen high application prospect.The method for preparing MoS2 modified electrodes
Have a lot, experience one is generally required for containing MoS2Electrolyte carry out the process of pre-treatment.And adopt MoS2 nanoparticles
Modification is carried out to which and can omit this pretreatment process, and bigger electrode activity surface can be obtained, therefore suffered from more
Concern.Regrettably, it is such to study in default of high-quality MoS2Nano structural material is used as technical support, and does not obtain wide
General development.In prior art, MoS2The synthetic method of nano structural material is not also common, but Ye You research and development institutions invent
MoS2Preparation method.
For example, Chinese invention patent application file 201510436528.8 discloses a kind of preparation method of three-dimensional MoS 2,
Characterized in that, comprising the following steps：
(1) prepare reaction raw materials solution：(NH4) 2MoS4 and DMF is taken, the reaction raw materials of three-dimensional MoS 2 after mixing, are configured to
Solution, and the weight/mass percentage composition of (NH4) 2MoS4 described in reaction raw materials solution is 1.1-1.3%；
(2) prepare (NH4) 2MoS4/ nickel foam：The reaction that foamed nickel substrate is immersed step (1) the three-dimensional MoS2 is former
In material solution, and 15-20min is kept, then take out and be placed in vacuum drying oven, 25- is dried under 70-80 DEG C of temperature conditionss
35min, repeat the above steps 5 times obtain (NH4) 2MoS4/ nickel foam；
(3) prepare MoS2/ nickel foam：(NH4) 2MoS4/ nickel foam that step (2) is prepared is placed under atmosphere in pipe
2h is incubated under 700-800 DEG C of temperature conditionss in formula stove, room temperature is cooled to, MoS2/ nickel foam is obtained；
(4) prepare the MoS2/ nickel foam of cladding PMMA：The MoS2/ nickel foam that step (3) is prepared is put into into PMMA benzene
Take out after 1-2min is soaked in methyl ether solution, then 1h is vacuum dried under 120-130 DEG C of temperature conditionss, obtain coating PMMA
MoS2/ nickel foam；
(5) prepare the three-dimensional MoS2 of cladding PMMA：2/ nickel foam of the MoS leaching of the cladding PMMA that step (4) is prepared
Nickel is removed in the acid solution for entering 40-50 DEG C, then washing obtains the three-dimensional MoS2 for coating PMMA；
(6) prepare three-dimensional MoS2：The three-dimensional MoS 2 of the cladding PMMA that step (5) is prepared is in vacuum tube furnace
400-500 DEG C is heated to, vacuum is 8-11Pa, PMMA is removed after insulation 2-2.5h, obtain three-dimensional MoS2.
Although three-dimensional MoS can be prepared in prior art2But, because reaction designing defect, however it remains following
Problem：
1st, reaction condition is complicated, is difficult to promote；
2nd, generate product purity low, can purify again in application process；
3rd, limited by raw material itself, the pattern of product is difficult to control to；
4th, in dedoping step, the problems such as easily cause acid water pollution；
5th, equipment relatively falls behind, and generates the less efficient of product.
There is as above defect in prior art, it is difficult to adapt to current MoS2The development trend and reality of nano structural material is needed
Will.In order to overcome defect present in above-mentioned prior art, the present inventor to combine design for many years and knowhow, propose a kind of
MoS2The synthetic method of nano structural material.
The content of the invention
The purpose of the present invention is to propose to a kind of MoS with regular spherical morphology, uniform particle sizes2The system of nano structural material
Preparation Method.
The present invention is achieved through the following technical solutions, a kind of synthetic method of MoS2 nano structural materials, the conjunction
Into method with molybdenum dioxide as predecessor, L-Cysteine is vulcanizing agent, is carried out under hydrothermal conditions；The synthetic method is concrete
Comprise the steps：
Step 1, the hexanol that 5 parts of molybdenum dioxide is dissolved in 2 parts, each composition is by mass；
In step 2, the solution for adding step 1 to be formed 1～5 part of L-Cysteine, containing the two of 8 parts in the solution
Molybdenum oxide, each composition is by mass and number value is integer；
Step 3, will be the solution stirring formed in step 2 uniform；
Step 4, the solution for stirring is poured into rustless steel hydrothermal reaction kettle reacted in step 3；
Step 5, the reactant that completes will be reacted in step 4 to carry out centrifugal treating, time of the centrifugal treating is 20～
30 minutes；
Step 6, the reactant in step 5 through centrifugal treating is carried out into EtOH Sonicate cleaning；
Step 7, the product that completes will be cleaned in step 6 it is dried process.
Further, the step of solution that molybdenum dioxide is dissolved in hexanol is stirred, institute are also included in the step 1
The equipment for stating stirring is magnetic stirring apparatuss, and the time of the stirring is 0.5～1 hour.
Further, in the step 2, the addition of L-Cysteine is the 1/2 of molybdenum dioxide quality.
Further, the time stirred described in the step 3 is 0.2～0.5 hour.
Further, the rustless steel hydrothermal reaction kettle contains teflon lined layer.
Further, it is as follows the step of reaction in the step 4：
Step 4.1, pour the solution stirred in step 3 into rustless steel hydrothermal reaction kettle, sealed；
Step 4.2, by step 4.1 seal after rustless steel hydrothermal reaction kettle be put in baking oven, arrange 120～180 DEG C
Heating-up temperature, heats 10-20 hours；
Step 4.3, the rustless steel hydrothermal reaction kettle for completing will be reacted in step 4.2 cooling is stood under room temperature environment.
Further, in the step 5, centrifugal treating process comprises the steps：
Step 5.1, will react in step 4 during the reactant that completes adds centrifuge tube；
Step 5.2, by the reactant in centrifuge tube rotating speed be 1000～4000 revs/min under the conditions of be centrifuged 10～15 points
Clock, discards precipitate, and upper suspension is deposited in centrifuge tube；
Step 5.3, again by the reactant in centrifuge tube rotating speed be 8000～12000 revs/min under the conditions of centrifugation 10～
15 minutes, supernatant liquid is discarded, retain gained solid.
Further, the step of cleaning in the step 6 is as follows：
Step 6.1, the gained solid in step 5 through centrifugal treating is cleaned into 5～10 minutes with EtOH Sonicate；
Step 6.2, by step 6.1 Jing EtOH Sonicate cleaning after the reactant centrifugal treating for being mixed with ethanol, turn
Speed discards supernatant liquid to be centrifuged 10～15 minutes under conditions of 8000～12000 revs/min；
Step 6.3, repeated washing 1～2 time.
Further, it is as follows the step of dried in the step 7：
Step 7.1, pour the product that completes of cleaning into surface plate；
Step 7.2, again by the surface plate that product is poured into be placed under room temperature ventilation condition be dried 1～2 day.
Compared with prior art, superior effect of the invention is：
1st, MoS of the present invention2The synthetic method of nano structural material, by by the solution stirring formed in step 2
Uniformly, react fully.
2nd, MoS of the present invention2The synthetic method of nano structural material, by by step 5 through centrifugal treating
Reactant carries out EtOH Sonicate cleaning, and after making reaction, unnecessary impurity is peeled off in product.
3rd, MoS of the present invention2The synthetic method of nano structural material, makes this generating process by the setting of centrifuge tube
Product and impurity are repeatedly centrifuged, and improve the purity of product.
4th, MoS of the present invention2The synthetic method of nano structural material, by anti-with L-Cysteine as vulcanizing agent
MoS2 nano-particle should be obtained so that material has splendid purity, purification is carried out without the need for any last handling process.
5th, MoS of the present invention2The nanoparticle that nano structural material synthesis is obtained can be directly used for preparing MoS2Modification
Electrode, obtained electrode can electrolysis water prepare hydrogen, its overpotential be 150mV.
Description of the drawings
Building-up processes of the Fig. 1 described in the embodiment of the present invention 1 obtains spherical morphology MoS2The SEM figures of nano structural material；
Building-up processes of the Fig. 2 described in the embodiment of the present invention 2 obtains spherical morphology MoS2The SEM figures of nano structural material；
Building-up processes of the Fig. 3 described in the embodiment of the present invention 3 obtains spherical morphology MoS2The SEM figures of nano structural material.
Specific embodiment
Below the specific embodiment of the invention is described in further detail.
Embodiment 1
A kind of MoS2The synthetic method of nano structural material, synthesis step are as follows：Each composition by mass, by 25 parts of pentachloro-s
Change molybdenum to be dissolved in 500 parts of ethanol, stir 0.5～1 hour on magnetic stirring apparatuss, after being completely dissolved, take 40 parts of solution and proceed to
Capacity is 80 parts of teflon lined rustless steel hydrothermal reaction kettle, after sealing, is put into baking oven, is heated 20 hours at 180 DEG C,
Obtain presoma molybdenum dioxide.Take 100 parts of molybdenum dioxide to be dissolved in 40 parts of hexanol, then be added thereto to 15 parts of L-Cysteine
Solution, stirs 1 hour on magnetic stirring apparatuss, and gained black suspension is proceeded to teflon lined that capacity is 80 parts not
Rust steel hydrothermal reaction kettle, after sealing, is put into baking oven, heats 20 hours at 120 DEG C.After reaction terminates, by stainless steel water thermal response
Kettle stands cooling under room temperature environment.Products therefrom proceeds to centrifuge tube, under the conditions of rotating speed is for 2000 revs/min is centrifuged 10 points
Clock；Precipitation is discarded, upper suspension is proceeded to into centrifuge tube, be centrifuged 15 minutes under the conditions of rotating speed is for 9000 revs/min, discard
Layer liquid.Centrifugation products therefrom is cleaned by ultrasonic 8 minutes with excess ethyl alcohol, 10 is centrifuged under the conditions of rotating speed is for 9000 revs/min
Minute, discard supernatant liquid, repeated washing 1 time.Black solid product after washing is proceeded to into surface plate, in room temperature ventilation condition
Lower drying 1 day.As shown in figure 1, after obtained product Jing XRD, SEM, TEM and EDX etc. are characterized, being defined as hexagonal crystal phase MoS2Nanometer
Granule, with spherical morphology, about 1 μm of particle diameter.
Embodiment 2
A kind of MoS2The synthetic method of nano structural material, synthesis step are as follows：Each composition by mass, by 25 parts of pentachloro-s
Change molybdenum to be dissolved in 500 parts of ethanol, stir 0.5 hour on magnetic stirring apparatuss, after being completely dissolved, take 40 parts of solution and proceed to capacity
For 80 parts of teflon lined rustless steel hydrothermal reaction kettle, after sealing, baking oven is put into, heats 20 hours at 180 DEG C, obtain
Presoma molybdenum dioxide.Take 100 parts of molybdenum dioxide to be dissolved in 40 parts of hexanol, then to be added thereto to 15 parts of L-Cysteine molten
Liquid, stirs 1 hour on magnetic stirring apparatuss, gained black suspension is proceeded to the teflon lined that capacity is 80 parts stainless
Steel hydrothermal reaction kettle, after sealing, is put into baking oven, heats 20 hours at 150 DEG C.After reaction terminates, by rustless steel hydrothermal reaction kettle
Cooling is stood under room temperature environment.Products therefrom proceeds to centrifuge tube, is centrifuged 10 minutes under the conditions of rotating speed is for 2000 revs/min；
Precipitation is discarded, upper suspension is proceeded to into centrifuge tube, be centrifuged 15 minutes under the conditions of rotating speed is for 9000 revs/min, discard upper strata
Liquid.Centrifugation products therefrom is cleaned by ultrasonic 8 minutes with excess ethyl alcohol, 10 points is centrifuged under the conditions of rotating speed is for 9000 revs/min
Clock, discards supernatant liquid, repeated washing 1 time.Black solid product after washing is proceeded to into surface plate, under room temperature ventilation condition
It is dried 1 day.As shown in Fig. 2 after obtained product Jing XRD, SEM, TEM and EDX etc. are characterized, being defined as hexagonal crystal phase MoS2Nanometer
Grain, with spherical morphology, particle diameter is about 700nm.
Embodiment 3
A kind of MoS2The synthetic method of nano structural material, synthesis step are as follows：Each composition by mass, by 25 parts of pentachloro-s
Change molybdenum to be dissolved in 500 parts of ethanol, stir 0.5 hour on magnetic stirring apparatuss, after being completely dissolved, take 40 parts of solution and proceed to capacity
For 80 parts of teflon lined rustless steel hydrothermal reaction kettle, after sealing, baking oven is put into, heats 20 hours at 180 DEG C, obtain
Presoma molybdenum dioxide.Take 100 parts of molybdenum dioxide to be dissolved in 40 parts of hexanol, then to be added thereto to 15 parts of L-Cysteine molten
Liquid, stirs 1 hour on magnetic stirring apparatuss, gained black suspension is proceeded to the teflon lined that capacity is 80 parts stainless
Steel hydrothermal reaction kettle, after sealing, is put into baking oven, heats 20 hours at 180 DEG C.After reaction terminates, by rustless steel hydrothermal reaction kettle
Cooling is stood under room temperature environment.Products therefrom proceeds to centrifuge tube, is centrifuged 10 minutes under the conditions of rotating speed is for 2000 revs/min；
Precipitation is discarded, upper suspension is proceeded to into centrifuge tube, be centrifuged 15 minutes under the conditions of rotating speed is for 9000 revs/min, discard upper strata
Liquid.Centrifugation products therefrom is cleaned by ultrasonic 8 minutes with excess ethyl alcohol, 10 points is centrifuged under the conditions of rotating speed is for 9000 revs/min
Clock, discards supernatant liquid, repeated washing 1 time.Black solid product after washing is proceeded to into surface plate, under room temperature ventilation condition
It is dried 1 day.As shown in Fig. 2 after obtained product Jing XRD, SEM, TEM and EDX etc. are characterized, being defined as hexagonal crystal phase MoS2Nanometer
Grain, with spherical morphology, particle diameter is about 500nm.
The present invention is not limited to above-mentioned embodiment, in the case of the flesh and blood without departing substantially from the present invention, this area skill
Any deformation that art personnel are contemplated that, improvement, replacement each fall within protection scope of the present invention.
Claims (9)
1. a kind of MoS2The synthetic method of nano structural material, the synthetic method with molybdenum dioxide as predecessor, L-Cysteine
For vulcanizing agent, carry out under hydrothermal conditions；Characterized in that, the synthetic method specifically includes following steps：
Step 1, the hexanol that 5 parts of molybdenum dioxide is dissolved in 2 parts, each composition is by mass；
In step 2, the solution for adding step 1 to be formed 1～5 part of L-Cysteine, containing 8 parts of titanium dioxide in the solution
Molybdenum, each composition is by mass and number value is integer；
Step 3, will be the solution stirring formed in step 2 uniform；
Step 4, the solution for stirring is poured into rustless steel hydrothermal reaction kettle reacted in step 3；
Step 5, the reactant that completes will be reacted in step 4 carry out centrifugal treating, the time of the centrifugal treating is 20～30 points
Clock；
Step 6, the reactant in step 5 through centrifugal treating is carried out into EtOH Sonicate cleaning；
Step 7, the product that completes will be cleaned in step 6 it is dried process.
2. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that also wrap in the step 1
The step of solution that molybdenum dioxide is dissolved in hexanol is stirred is included, the equipment of the stirring is magnetic stirring apparatuss, described to stir
The time mixed is 0.5～1 hour.
3. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that L- half in the step 2
The addition of cystine for molybdenum dioxide quality 1/2.
4. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that described in the step 3
The time of stirring is 0.2～0.5 hour.
5. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that the institute in the step 4
State rustless steel hydrothermal reaction kettle and contain teflon lined layer.
6. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that be centrifuged in the step 5
Processing procedure comprises the steps：
Step 5.1, will react in step 4 during the reactant that completes adds centrifuge tube；
Step 5.2, by the reactant in centrifuge tube rotating speed be 1000～4000 revs/min under the conditions of be centrifuged 10～15 minutes,
Precipitate is discarded, upper suspension is deposited in centrifuge tube；
Step 5.3, again by the reactant in centrifuge tube rotating speed be 8000～12000 revs/min under the conditions of be centrifuged 10～15 points
Clock, discards supernatant liquid, retains gained solid.
7. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that clean in the step 6
The step of it is as follows：
Step 6.1, the gained solid in step 5 through centrifugal treating is cleaned into 5～10 minutes with excessive EtOH Sonicate；
Step 6.2, by step 6.1 Jing EtOH Sonicate cleaning after the reactant centrifugal treating for being mixed with ethanol, in rotating speed be
It is centrifuged 10～15 minutes under conditions of 8000～12000 revs/min, discards supernatant liquid；
Step 6.3, repeated washing 1～2 time.
8. MoS according to claim 12The synthetic method of nano structural material, it is characterised in that be dried in the step 7
The step of process, is as follows：
Step 7.1, pour the product that completes of cleaning into surface plate；
Step 7.2, again by the surface plate that product is poured into be placed under room temperature ventilation condition be dried 1～2 day.
9. MoS according to claim 52The synthetic method of nano structural material, it is characterised in that anti-in the step 4
The step of answering is as follows：
Step 4.1 into, the solution stirred in step 3 is poured rustless steel hydrothermal reaction kettle, seal；
Step 4.2, by step 4.1 seal after rustless steel hydrothermal reaction kettle be put in baking oven, arrange 120～180 DEG C heating
Temperature, heats 10-20 hours；
Step 4.3, the rustless steel hydrothermal reaction kettle for completing will be reacted in step 4.2 cooling is stood under room temperature environment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111058054A (en) * | 2020-01-03 | 2020-04-24 | 大连理工大学 | Device and method for synthesizing ammonia by electrocatalytic nitrogen reduction by using salt bridge to replace Nafion membrane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
| CN105329946A (en) * | 2015-11-16 | 2016-02-17 | 暨南大学 | Molybdenum disulfide nanosheet with rich active sites as well as preparation method and application of molybdenum disulfide nanosheet |
| CN105366725A (en) * | 2014-08-29 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source |
-
2016
- 2016-11-08 CN CN201610980001.6A patent/CN106564951A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366725A (en) * | 2014-08-29 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source |
| CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
| CN105329946A (en) * | 2015-11-16 | 2016-02-17 | 暨南大学 | Molybdenum disulfide nanosheet with rich active sites as well as preparation method and application of molybdenum disulfide nanosheet |
Non-Patent Citations (1)
| Title |
|---|
| QIQI ZHANG ET AL.: ""MoS2 yolk-shell microspheres with hierarchical porous structure for efficient hydrogen evolution"", 《NANO REARCH》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111058054A (en) * | 2020-01-03 | 2020-04-24 | 大连理工大学 | Device and method for synthesizing ammonia by electrocatalytic nitrogen reduction by using salt bridge to replace Nafion membrane |
| CN111058054B (en) * | 2020-01-03 | 2022-01-18 | 大连理工大学 | Device and method for synthesizing ammonia by electrocatalytic nitrogen reduction by using salt bridge to replace Nafion membrane |
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