CN107732256A - One kind prepares MFC electrode materials and its chemical property using agricultural wastes - Google Patents

One kind prepares MFC electrode materials and its chemical property using agricultural wastes Download PDF

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Publication number
CN107732256A
CN107732256A CN201710933076.3A CN201710933076A CN107732256A CN 107732256 A CN107732256 A CN 107732256A CN 201710933076 A CN201710933076 A CN 201710933076A CN 107732256 A CN107732256 A CN 107732256A
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porous carbon
electrode
ptfe
agricultural wastes
acetylene black
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张頔
孔勇
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Changzhou University
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Changzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
    • H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/96—Carbon-based electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Microbiology (AREA)
  • Biochemistry (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Composite Materials (AREA)
  • Inert Electrodes (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Abstract

One kind prepares MFC electrode materials and its chemical property using agricultural wastes.The present invention relates to a kind of novel porous carbon PTFE foam nickel electrodes, it mainly includes：Agricultural wastes Dehydrated Corn core, conductive agent acetylene black, polyfluortetraethylene of binding element (1%PTFE emulsions) and nickel foam etc..The present invention selects agricultural wastes corncob as the raw material for preparing porous carbon.Corncob is through natural air drying, hand breaking after high-purity N2Atmosphere pipe type reaction in furnace, is carbonized.KOH is selected to be mixed in high-purity N as activator and carbonizing production afterwards2Priming reaction is carried out in atmosphere pipe type stove porous carbon materials are made.Mix to roll and be cut into suitable size with conductive agent acetylene black and polyfluortetraethylene of binding element (1%PTFE emulsions) after porous carbon grinding is careful, it is applied to absolute ethyl alcohol wetting in nickel foam and flakiness is rolled on powder compressing machine, produces porous carbon modified electrode material.Electrode of the present invention can improve Bioelectrochemical device electricity generation ability compared with having more excellent chemical property before modification.And abundant raw material, cost are cheap, prepare simple, efficient productivity.

Description

One kind prepares MFC electrode materials and its chemical property using agricultural wastes
Technical field
The invention belongs to fuel cell field, and in particular to a kind of more by the use of agricultural wastes corncob as raw material preparation Hole carbon electrode material.
Background technology
China is large agricultural country, and annual corn total output up to 2.2 hundred million t, by-product corncob is in 0.4 hundred million t or so.It is although beautiful Rice core cost is cheap, aboundresources, but cannot reasonably utilize, most of to be finally taken as agricultural wastes processing.In original The rapid raising of material cost is present with demand for energy sustainable growth, and but there is backward in technique, utilization for China's using energy source Rate is low, the problems such as unreasonable structure.China is faced with dual " blocking " of lack of energy and high low cost materials.How to find A kind of cost is cheap and can to alleviate the new material of lack of energy present situation be current domestic and international research hot topic.
Microbiological fuel cell (Microbial Fuel Cell, MFC) is that one kind utilizes microbiological oxidation organic matter, from And chemical energy is directly translated into the device of electric energy, at present by extensive concern.Solid-state carrier electrode surface grows electricity in MFC Active biological film, can be to electronics caused by extracellular output microbiological oxidation organic pollution, again can be electric directly in environment of accepting Son, electron transfer process in electrode surface and nearby occurs, biological energy source is changed into electric energy.Can solve study hotspot in the world Energy problem.
Influenceing the principal element of MFC electricity generation performances includes：Reactor configuration, electrode material, electricity-producing microorganism number of species, Electrode surface biomembrane etc..It is in research to microbiological fuel cell (MFCs) at present to use carbon material as electrode more.Such as public affairs A kind of microbiological fuel cell that the number of opening CN101645515 is announced and its preparation method and application, inventor are heavy using surface electricity Product has the carbon felt of polypyrrole and anthraquinone -2,6- sodium disulfonate to do anode, negative electrode then by CNT, polytetrafluoroethylene (PTFE) and gamma - Iron oxide basic forms, and it has the problems such as high high energy consumption, cost of manufacture, complex process.
Electrode material of the present invention is China's agricultural wastes corncob, and its annual yield is considerable, and cost is cheap, and at present It is seldom for the commercial use of corncob, accomplish that discarded object secondary use meets ecological harmonious development again from corncob Need.
Found in actual application, the electro-chemical activity of electrode can be as the weight for weighing MFCs electricity generation performances quality Want index.Electrode of the present invention --- porous carbon-PTFE foam nickel electrodes have high-specific surface area and high density office because its is modified Domain electric charge and the electro-chemical activity of electrode can be effectively improved.
The content of the invention
It is insufficient present in above-mentioned technology it is an object of the invention to overcome, there is provided a kind of cost is cheap, prepares simple, production Efficiently, and it can apply to microbial fuel cell unit and implement to continue the new electrode materials of production capacity.
The technical solution adopted by the present invention is as follows：
A kind of novel porous carbon-PTFE foam nickel electrodes, mainly include：Agricultural wastes Dehydrated Corn core, conductive agent second Acetylene black, polyfluortetraethylene of binding element (1%PTFE emulsions) and nickel foam etc..The reagent mainly used has：Absolute ethyl alcohol, polytetrafluoro Ethene (PTFE emulsion), experimental water are Milli-Q deionized waters, 2.5% glutaraldehyde, HMDS, acetonitrile (HPLC Level), phosphate buffer, 1% osmium tetroxide, expoxy propane, Epon812 embedding mediums etc..
The preparation of agricultural wastes porous carbon materials：Agricultural wastes corncob is selected as the raw material for preparing porous carbon.It is beautiful Meter Xin is through natural air drying, hand breaking after high-purity N2Atmosphere pipe type reaction in furnace, is carbonized.Soaked successively with HCl, HF afterwards Bubble, wash to neutrality, KOH is selected after drying as activator.KOH and carbonizing production are mixed in high-purity N2Atmosphere pipe type stove Interior carry out priming reaction, after successively through pickling be washed to it is neutral, dry.
The above-mentioned carbonization rate of heat addition is 10 DEG C/min, and temperature control is 400 DEG C, reaction time 0.5h, is carbonized.Selected during activation Select activation ratio 2:1, the porous carbon of optimal property is made in 800 DEG C of reaction temperature, time 1h.Above-mentioned HCl and HF concentration is respectively 5wt% and 3wt%, soak time 6h, 80 DEG C of drying temperature.
The preparation of electrode material：Porous carbon grinding careful rear and conductive agent acetylene black and polyfluortetraethylene of binding element (1% PTFE emulsion) it is well mixed, it is transferred in absolute ethyl alcohol, taking-up is evaporated at 100 DEG C of ultrasonic disperse processing 5min vacuum drying chambers, Rolled (pressure 15Mpa time 1min) through roller machine, 100 DEG C of dry 2h.Dried blend sample is cut into suitable size, It is applied to be placed on powder compressing machine in the lump after drying in clean nickel foam with absolute ethyl alcohol wetting and rolls flakiness, (pressure 10Mpa, time 1min) produce porous carbon modified electrode material.Porous carbon, acetylene black and polytetrafluoroethylene (PTFE) (1%PTFE emulsions) Mixing quality ratio is 8:1:1.
The sludge of MFC reactors inoculation is derived from municipal sewage plant's anaerobic sludge, adds homemade Nutrient medium.Nutrient medium Before reactor is passed through first it is quick-fried enter N2Supplemented once per 24h.The nutritive medium contg and composition are 0.5g/L NH4Cl, 0.1g/L NaCl, 0.1g/L MgCl2·6H2O, 13g/L Na2HPO4·12H2O, 1.48g/L KH2PO4。
The reporting method of the bioelectrode, electrode obtained above embedment is derived to the anaerobism of Changzhou sewage treatment plant In sludge, nutrient solution is added daily, and electrode surface can cover a thick layer biomembrane after 5 days, and thus bioelectrode has been put on record Into.
The beneficial effects of the invention are as follows：This electrode material is electric come modifying foam nickel using porous carbon by binding agent of PTFE Pole, the electrode material is abundant, cost is cheap, prepares simple, efficient productivity, and bioelectrode can effectively facilitate pollutant removal and electricity Son transmits, and reaches the reliability service of electricity production and environment remediation function.Make full use of resource again environment-friendly, while and can solves The energy problem of World Focusing.
Brief description of the drawings
Fig. 1 is electrode pair of the present invention than blank foam nickel electrode, the foam nickel electrode, porous of blank-load biomembrane The SEM photograph of the foam nickel electrode of carbon-load biomembrane；
Fig. 2 is electrode of the present invention and blank foam nickel electrode electrochemical reduction cyclic voltammetry curve comparison diagram；
Fig. 3 is the electrochemical alternate impedance spectrum at electrode biomembrane initial stage and later stage of the present invention；
Table 1 is the electricity production data of microbial fuel cells system；
In Fig. 1：(a)~(d) is respectively blank foam nickel electrode, the foam nickel electrode of porous carbon modification, blank-load The foam nickel electrode of foam nickel electrode and porous carbon-load biomembrane of biomembrane.
Embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of SEM photograph of novel porous carbon-PTFE foam nickel electrodes shown in Fig. 1 (b).Novel foam nickel electrode surface quilt Porous carbon and PTFE coverings, and porous carbon and PTFE are uniformly covered with electrode surface, are completely embedded, and do not occur crack；
Fig. 1 (a) blank foam nickel electrodes surface is smooth laminated structure；The foam nickel surface that Fig. 1 (c) is adhered to by biomembrane omits Aobvious coarse, cavernous structure is obvious, and is evenly distributed, and such case is beneficial to the migration of electronics；Fig. 1 (d) is adhered to by biomembrane The a large amount of spheroidal particles not of uniform size of porous carbon foam nickel electrode surface connection, exist between these particulates compared with Multiple level and tight It is close to be attached to electrode surface, increase electrode surface roughness and specific surface area.Be advantageous to electrolyte material internal infiltration and Transmission effects between electronics, the utilization rate of electrode material can be improved.
The above-mentioned ESEMs of ESEM model Quanta 250, made electrode sample is rinsed with phosphate buffer before test Product, 24h is fixed in 2.5% glutaraldehyde solution, then gradient takes off step by step through 30%, 50%, 70%, 80%, 95%, 100% ethanol Water, finally passes sequentially through HMDS and acetonitrile dries 30min, metal spraying.
Embodiment 2
Under three-electrode system, using platinum electrode as to electrode, saturated calomel electrode is as reference electrode, by blank and more The foam nickel electrode of hole carbon modification is respectively in O2The 50mmol/L of saturation P-buffer (sodium dihydrogen phosphates：2.452g/L；Phosphoric acid Disodium hydrogen：Cyclic voltammetric and electrochemical impedance scanning 4.576g/L) are done in electrolyte solution.
Fig. 2 electrochemical reduction cyclic voltammetry curves, the results showed that do not detect oxygen on the CV curves of blank nickel foam Change reduction peak, significantly electrochemical oxidation phenomenon occur, by porous at -0.6~-0.1V current potentials on porous carbon CV curves The oxidation peak to peak current that carbon is formed is 3.48mAcm-2, experimental result explanation, which is modified processing to electrode, can optimize P- Electrocatalysis characteristics of the buffer on electrode, compared to blank electrode, electro-chemical activity is improved.
Fig. 3 is the electrochemical impedance spectroscopy measured by porous carbon electrodes biofilm development initial stage and later stage.It is it can be seen that electric Chemical impedance spectrum is made up of two sections of circular arcs and an oblique line, and each section of arc diameter can represent resistance value, and first paragraph circular arc exists High frequency region, it is Ohmic resistance, second segment circular arc appears in intermediate frequency zone, is polarization resistance.Early growth period Ohmic resistance is 8.52ohm, polarization resistance are about 23.97ohm, and with the formation of biomembrane, Ohmic resistance and polarization resistance are being gradually reduced, Biofilm formation later stage, Rs values are 6.65ohm, polarization resistance 19.27ohm.1.87ohm and 4.70ohm are reduced respectively.Say Transmission of the bright biomembrane to electric charge has facilitation.In the biofilm development later stage, impedance spectrum final stage oblique line is gradually to vertical seat Parameter is close, gradually shows electric charge saturated phenomenon.
The condition of work of above-mentioned electro-chemical test：When CV is tested, sweep speed：10mV/s, test voltage scope：-0.8- 0.6V；During ac impedance measurement, spoke value is exchanged：100mV, test frequency scope：0.01-1000KHz；Tafel curve test is surveyed During examination, test voltage scope：-0.8-0.6V.
Above-mentioned novel porous carbon-PTFE foam nickel electrodes are applied to microbial fuel cell unit by embodiment 3 [0036], Electrochemical workstation and data acquisition unit are connected, starter, the electricity production situation of battery is measured using data acquisition unit, is taken daily 3 numerical value, the data of continuous record one week, fetch according to the electric current and voltage for being battery.During the daily morning 9, noon 14 when, under Noon 19 notes down data, a length of 10 days during statistics, amounts to 30 numberings, is specifically shown in Table 1
The electricity production data of the microbial fuel cells system of table 1
The steady sequence of the electricity generation ability of this cell apparatus improves as can be seen from Table 2, and maximum current reaches 0.436mA, voltage Reach 553.4mV.
From embodiment 1~3, novel porous carbon-PTFE foam nickel electrodes of the invention are more excellent compared with having before modification Chemical property, Bioelectrochemical device electricity generation ability can be improved.

Claims (5)

  1. A kind of 1. novel porous carbon-PTFE foam nickel electrodes, it is characterised in that：Including agricultural wastes Dehydrated Corn core, conduction Agent acetylene black, polyfluortetraethylene of binding element (1%PTFE emulsions) and nickel foam etc..
    Agricultural wastes corncob is selected as the raw material for preparing porous carbon.Corncob is through natural air drying, hand breaking after high-purity N2 Atmosphere pipe type reaction in furnace, is carbonized.Soaked, washed to neutrality with HCl, HF successively afterwards, selected KOH to be used as after drying and live Agent.KOH and carbonizing production are mixed in high-purity N2Priming reaction is carried out in atmosphere pipe type stove, after be washed to successively through pickling It is neutral, dry.
  2. 2. the preparation of electrode according to claim 1, it is characterised in that：The above-mentioned carbonization rate of heat addition is 10 DEG C/min, temperature control For 400 DEG C, reaction time 0.5h, it is carbonized.Activation ratio 2 is selected during activation:1,800 DEG C of reaction temperature, the time, 1h was made The porous carbon of optimal property.Above-mentioned HCl and HF concentration is respectively 5wt% and 3wt%, soak time 6h, 80 DEG C of drying temperature.
  3. 3. the preparation of electrode according to claim 1, it is characterised in that：Porous carbon grinding it is careful after and conductive agent acetylene black and Polyfluortetraethylene of binding element (1%PTFE emulsions) is well mixed, is transferred in absolute ethyl alcohol, and ultrasonic disperse processing 5min vacuum is done Taking-up is evaporated at dry 100 DEG C of case, is rolled (pressure 15Mpa time 1min) through roller machine, 100 DEG C of dry 2h.Will be dried mixed Compound sample is cut into suitable size, is applied to absolute ethyl alcohol wetting after being dried in clean nickel foam and is placed on pressed powder in the lump Flakiness is rolled on machine, (pressure 10Mpa, time 1min) produces porous carbon modified electrode material.Porous carbon, acetylene black and poly- four PVF (1%PTFE emulsions) mixing quality ratio is 8:1:1.
  4. 4. the preparation of electrode according to claim 1, it is characterised in that：The sludge of MFC reactors inoculation is derived from municipal sewage Treatment plant's anaerobic sludge, add homemade Nutrient medium.Nutrient medium before reactor is passed through first it is quick-fried enter N2The supplement one per 24h It is secondary.The nutritive medium contg and composition are 0.5g/L NH4Cl, 0.1g/L NaCl, 0.1g/L MgCl2·6H2O, 13g/L Na2HPO4·12H2O, 1.48g/L KH2PO4。
  5. 5. the reporting method of the bioelectrode according to claim 4, electrode obtained above embedment is derived from Changzhou In the anaerobic sludge of sewage treatment plant of city, nutrient solution is added daily, electrode surface can cover a thick layer biomembrane after 5 days, Thus bioelectrode puts completion on record.
CN201710933076.3A 2017-10-10 2017-10-10 One kind prepares MFC electrode materials and its chemical property using agricultural wastes Pending CN107732256A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109841888A (en) * 2019-02-28 2019-06-04 山东理工大学 A kind of direct carbon solid oxide fuel cell group of micro-tubular based on corncob derivatived fuel
CN110310844A (en) * 2019-06-28 2019-10-08 华中科技大学 Sludge utilizes method and the nickel foam-nitrogen-doped nanometer carbon composite prepared by this method
CN110756166A (en) * 2019-12-03 2020-02-07 四川农业大学 Corncob-loaded magnesium-modified adsorption material and preparation method and application thereof
CN110981280A (en) * 2019-12-17 2020-04-10 大连理工大学 Preparation method and application of reed biochar-based composite electrode material
CN111755704A (en) * 2019-03-27 2020-10-09 中南大学 Preparation method of novel porous carbon cathode lithium air battery
CN116040627A (en) * 2022-12-22 2023-05-02 华中农业大学 Porous carbon, composite material, diaphragm modification material and application

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CN101850958A (en) * 2010-01-21 2010-10-06 中国石油天然气股份有限公司 Method for improving yield of biomass porous carbon
CN103579640A (en) * 2012-07-25 2014-02-12 中国科学院大连化学物理研究所 Anode material for lithium-air battery and preparation method thereof
CN105384162A (en) * 2015-12-04 2016-03-09 华南理工大学 Corncob-based porous carbon material, and preparation method and application thereof
CN105762372A (en) * 2016-04-21 2016-07-13 常州大学 Method for preparing microbial fuel cell anode electrodes from agricultural wastes
CN105845947A (en) * 2016-05-31 2016-08-10 常州大学 Method for preparing microbial fuel cell electrode material employing rape stalks
CN106299384A (en) * 2016-10-14 2017-01-04 北京理工大学 A kind of lithium sky anode electrode slice based on charcoal

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101850958A (en) * 2010-01-21 2010-10-06 中国石油天然气股份有限公司 Method for improving yield of biomass porous carbon
CN103579640A (en) * 2012-07-25 2014-02-12 中国科学院大连化学物理研究所 Anode material for lithium-air battery and preparation method thereof
CN105384162A (en) * 2015-12-04 2016-03-09 华南理工大学 Corncob-based porous carbon material, and preparation method and application thereof
CN105762372A (en) * 2016-04-21 2016-07-13 常州大学 Method for preparing microbial fuel cell anode electrodes from agricultural wastes
CN105845947A (en) * 2016-05-31 2016-08-10 常州大学 Method for preparing microbial fuel cell electrode material employing rape stalks
CN106299384A (en) * 2016-10-14 2017-01-04 北京理工大学 A kind of lithium sky anode electrode slice based on charcoal

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109841888A (en) * 2019-02-28 2019-06-04 山东理工大学 A kind of direct carbon solid oxide fuel cell group of micro-tubular based on corncob derivatived fuel
CN111755704A (en) * 2019-03-27 2020-10-09 中南大学 Preparation method of novel porous carbon cathode lithium air battery
CN110310844A (en) * 2019-06-28 2019-10-08 华中科技大学 Sludge utilizes method and the nickel foam-nitrogen-doped nanometer carbon composite prepared by this method
CN110756166A (en) * 2019-12-03 2020-02-07 四川农业大学 Corncob-loaded magnesium-modified adsorption material and preparation method and application thereof
CN110981280A (en) * 2019-12-17 2020-04-10 大连理工大学 Preparation method and application of reed biochar-based composite electrode material
CN110981280B (en) * 2019-12-17 2021-08-20 大连理工大学 Preparation method and application of reed biochar-based composite cathode material
CN116040627A (en) * 2022-12-22 2023-05-02 华中农业大学 Porous carbon, composite material, diaphragm modification material and application

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Application publication date: 20180223