CN110085432A - A kind of preparation method of high pressure resistant intensity capacitor material - Google Patents
A kind of preparation method of high pressure resistant intensity capacitor material Download PDFInfo
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- CN110085432A CN110085432A CN201910235990.XA CN201910235990A CN110085432A CN 110085432 A CN110085432 A CN 110085432A CN 201910235990 A CN201910235990 A CN 201910235990A CN 110085432 A CN110085432 A CN 110085432A
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- resistant intensity
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/40—Fibres
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention relates to a kind of preparation methods of high pressure resistant intensity capacitor material, belong to electronic material preparation technical field.The present invention is with bamboo chip, sawdust, iron powder etc. is that reaction solid is made in raw material, again will reaction solid high-temperature heat treatment and and silicon nitride, the materials such as zinc nitrate are mixed to prepare pre product, finally by pre product and triacetin, the material mixings such as neopelex, hot pressing, it calcines up to high pressure resistant intensity capacitor material, the present invention is from bamboo chip, bamboo fibre is extracted in sawdust, the organic principles such as lignin, bamboo fibre Surface Creation hydroxyl, the functional groups such as carboxyl, improve the mechanical strength of capacitor material microstructure, aluminium simple substance particulate component generates aluminium oxide in the present invention, absorption forms aluminum oxide film layer cladding carbon fiber between each aluminium oxide, it is improved the chemical stability of capacitor material, the electric conductivity of simultaneous oxidation aluminium is poor, the dielectric constant of capacitor material can also be improved, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high pressure resistant intensity capacitor material, belong to electronic material technology of preparing neck
Domain.
Background technique
Now with the sustainable growth of the rapid development of human society and energy demand, traditional fossil energy is caused sharply to subtract
Less, global ecological environment is worsening.It has been extremely urgent for greatly developing clean, the reproducible energy.Supercapacitor
As a kind of clean energy resource, the advantages that due to its high power density, fast charging and discharging and long circulation life, by scientific research circle and production
The close attention of industry.
Supercapacitor is a kind of new type of energy storage device of performance between physical capacitor and secondary cell, have than
The higher specific capacitance of ordinary capacitor and energy density, and there is power density more higher than battery simultaneously.Rely primarily on electricity
The electrochemical reaction or electric double layer of pole surface store charge, with charge and discharge are rapid, long service life, stability are good, work temperature
The advantages that degree is wide, circuit is simple, safe and reliable, environmentally protective, can be widely applied to auto industry, aerospace, science and techniques of defence,
The multiple fields such as information technology, electronics industry, have broad application prospects.
For electrode material as the deciding factor for determining performance of the supercapacitor, it decides the main property of supercapacitor
It can index.Ideal electrode material should specific capacitance, high rate capability and cyclical stability with higher.Supercapacitor root
Carbon electrode capacitor, metal oxide based capacitor and conducting polymer based capacitor can be divided into according to the difference of electrode material；Root
Double layer capacitor and faraday (counterfeit) capacity capacitor can be divided into according to the difference of energy storage mechnism.Faraday's capacitor is based on electricity
Reversible, quick redox reaction occurs on the interface of pole to store energy.Double layer capacitor is based on electrode and electrolyte
Between the interfacial electric double layer capacitor that is formed store energy.
Carbon material is the material for being used as supercapacitor active material earliest, and most commonly used electrode material at present.
Wherein, active carbon due to its large specific surface area, be easy preparation, price is low the features such as, be still and prepare electrode of super capacitor material
The preferred material of material, but its specific capacity and energy density compare it is lower.Using metal oxide or conducting polymer as electrode
The fake capacitance capacitor of material can not only form electric double layer in electrolyte and electrode interface, and occur in electrode material surface
Redox reaction, therefore, the latter have bigger specific capacitance than the former.Although transition metal oxide and conducting polymer are all
Higher specific capacitance and high-energy density are embodied, but their power density is barely satisfactory, and under high charge-discharge magnification
Energy density it is lower.
Capacitor material in the prior art often has that dielectric constant is smaller, is not able to satisfy the need of electronic circuit miniaturization
Ask, and pressure voltage is not high enough, structural instability, dielectric loss is higher, in production, use and scrapping process can to human body and
Environment causes certain harm.China Patent Publication No. CN106554201A discloses a kind of lead-free high-voltage ceramic capacitor material,
It is made of following component: barium titanate, titanium dioxide, calcium carbonate, zirconium dioxide, silica, modified additive.It is free of in formula
Lead element and yttrium, it is environmentally protective, it is at low cost, greatly improve ceramic material by being added to modified additive
Performance, substantially increases the dielectric constant and pressure voltage of ceramic material, and can reach lesser rate of temperature change, and capacitor is made to exist
Work process performance is more stable, but the product is using solid-phase synthesis, and the uniformity of final products is bad, and then influences
The performance of product.
Therefore it provides a kind of be free of noxious material, not can cause environmental pollution, and dielectric constant is high, pressure voltage is high
Capacitor material and preparation method thereof is those skilled in the art's urgent problem to be solved.
Summary of the invention
The technical problems to be solved by the invention: it is low for the dielectric constant of current existing capacitor material, it is applicable in model
It is with limit, and pressure voltage is insufficient, structural unstable defect provides a kind of preparation side of high pressure resistant intensity capacitor material
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The specific preparation step of high pressure resistant intensity capacitor material are as follows:
(1) heat-treated products are put into planetary ball mill, in the condition that ratio of grinding media to material is 10:1 and revolving speed is 300~350r/min
Milled mixtures are made in 40~50min of lower ground and mixed, and milled mixtures, silicon nitride, strontium carbonate, zinc nitrate, bismuth titanates are thrown
Enter blender and mixing and pre product is uniformly made；
(2) after mixing by pre product, triacetin, neopelex, vinyltrimethoxysilane
Put into hot press in, temperature be 140~150 DEG C and compacting pressure be 0.8~1.0MPa under conditions of constant temperature compacting 30~
40min, after compacting put into sintering furnace in, under argon atmosphere and temperature be 1100~1200 DEG C under conditions of sintering 50~
60min is up to high pressure resistant intensity capacitor material；
The specific preparation step of heat-treated products are as follows:
(1) it by acidic emulsion and aluminium chloride crystal powder investment beaker, places the beaker in sonic oscillation instrument, is 32 in frequency
1~2h is vibrated under conditions of~36kHz, and the potassium hydroxide solution that mass fraction is 5~8% is added dropwise after oscillation into beaker and adjusts
Iron powder is added into beaker, is mixed with blender with the revolving speed of 300~350r/min to the obtained preformed solution of neutrality for pH value
1~2h is up to mixed serum；
(2) mixed serum is put into suction filtration machine and filters removal filtrate, 3~5 times wash with distilled water, obtain reaction solid, it will
It reacts in solid investment tube furnace, nitrogen is continually fed into tube furnace, tubular type in-furnace temperature is increased to 105~115 DEG C, in advance
Tubular type in-furnace temperature is increased to 500~550 DEG C after preheating by 60~80min of heat, and heat treatment is made in 50~60min of high-temperature calcination
Product；
The specific preparation step of acidic emulsion are as follows:
(1) by bamboo chip and sawdust investment baking oven, dry 2~3h, is ground into after dry under conditions of temperature is 70~80 DEG C
Powder crosses 50 meshes and dry mixing is made, and dry mixing and water are put into reaction kettle, and reaction kettle is closed, increases in reaction kettle
For temperature to 120~130 DEG C, constant temperature stands 100~120min, and reacting slurry is made；
(2) sodium hydroxide solution that mass fraction is 6~10% is added dropwise into reaction kettle and adjusts pH value to 10~11, uses blender
50~60min is mixed with the revolving speed of 600~700r/min, air pressure in reaction kettle is increased to 0.8~1.2MPa, temperature liter
Up to 90~100 DEG C, constant temperature and pressure stands 2~3h, and the sulfuric acid solution that mass fraction is 20~25% is added dropwise after standing and adjusts pH value
To 4~5, acidic emulsion is made.
Preferably according to parts by weight, milled mixtures are 8~10 parts, silicon nitride is 0.5~0.7 part, strontium carbonate 1.1
~1.3 parts, zinc nitrate be 1.0~1.4 parts, bismuth titanates is 0.3~0.5 part.
Preferably according to parts by weight, pre product is 10~12 parts, triacetin is 1.2~1.4 parts, dodecane
Base benzene sulfonic acid sodium salt is 0.3~0.6 part, vinyltrimethoxysilane is 2~3 parts.
The mass ratio of acidic emulsion and aluminium chloride crystal powder is 15:1 in the specific preparation step (1) of heat-treated products.
The quality for the iron powder being added in the specific preparation step (1) of heat-treated products into beaker is preformed solution quality
5~9%.
The mass ratio of bamboo chip and sawdust is 5:1 in the specific preparation step (1) of acidic emulsion.
In the specific preparation step (1) of acidic emulsion bamboo chip be more preferably one of moso bamboo, fishpole bamboo, Fang Zhu or
A variety of to mix in any proportion, the sawdust is more preferably one of pine, poplar, mahogany or a variety of by any ratio
Example mixing.
The mass ratio of dry mixing and water is 1:5 in the specific preparation step (1) of acidic emulsion.
The method have the benefit that:
(1) present invention is dry by bamboo chip and sawdust first, cooks to obtain reacting slurry, then Xiang Fanying with water mixing high-temperature water after drying
Lye pyroreaction is added in slurries, pH value is adjusted after reaction to acidity, and aluminum chloride powder is added, then adjusts pH value into
Property, iron powder hybrid reaction is added, reaction solid is obtained by filtration after reaction, then reaction solid high-temperature is handled to obtain heat treatment production
Then the materials such as heat-treated products and silicon nitride, zinc nitrate are mixed to prepare pre product, finally by pre product and glycerol by object
The material mixings such as triacetate, neopelex put into hot pressing in hot press, and sintering furnace high temperature is put into after hot pressing and is forged
It burns up to high pressure resistant intensity capacitor material, bamboo chip, sawdust are carried out pyrohydrolysis and lye high-temperature process, Cong Zhongti by the present invention
The organic principles such as bamboo fibre, lignin are taken out, there is bamboo fibre good toughness and mechanical strength to make by pyrohydrolysis
Electricity improves to form the cross-linked structure that density is higher, bonding degree is high in the functional groups such as bamboo fibre Surface Creation hydroxyl, carboxyl
The mechanical strength of container material microstructure enhances capacitor pressure resistance performance, and this cross-linked structure can protect
Other ingredients in capacitor material, carbonize after high-temperature calcination, and fibre structure is condensed under the high temperature conditions, density itself mentions
Height, microstructure concentration are reinforced, and lignin also carbonizes, formed each hole in carbon particle filling capacitor material at
Point, and covalent bond absorption is formed between other ingredients around, reinforce the structural strength of capacitor material, makes capacitor material sheet
The chemical stability of body and pressure-resistant performance are strengthened；
(2) the effects of aluminium ion is introduced into bamboo fibre and lignin structure by the present invention, is adsorbed using complexing, ionic bond is inhaled
It invests in bamboo fibre surface and lignin structure, iron is then added, displacement reaction occurs, aluminium ion reaction is made to generate aluminium simple substance
Grain, be filled in bamboo fibre cross-linked structure, and by high-temperature calcination make aluminium simple substance particulate component generation aluminium oxide, each aluminium oxide it
Between can form covalent bond, intermolecular force adsorbs to form aluminum oxide film layer cladding carbon fiber, keep the chemistry of capacitor material steady
Qualitative to be improved, the electric conductivity of simultaneous oxidation aluminium is poor, moreover it is possible to improve the dielectric constant of capacitor material, have wide answer
Use prospect.
Specific embodiment
It is in mass ratio that 5:1 is put into baking oven by bamboo chip and sawdust, dry 2 under conditions of temperature is 70~80 DEG C~
3h, grind into powder crosses 50 meshes and dry mixing is made after drying, is in mass ratio that 1:5 puts into reaction kettle by dry mixing and water
In, reaction kettle is closed, reactor temperature is increased to 120~130 DEG C, and constant temperature stands 100~120min, and reaction slurry is made
Liquid；The sodium hydroxide solution that mass fraction is 6~10% is added dropwise into aforesaid reaction vessel and adjusts pH value to 10~11, uses blender
50~60min is mixed with the revolving speed of 600~700r/min, air pressure in reaction kettle is increased to 0.8~1.2MPa, temperature liter
Up to 90~100 DEG C, constant temperature and pressure stands 2~3h, and the sulfuric acid solution that mass fraction is 20~25% is added dropwise after standing and adjusts pH value
To 4~5, acidic emulsion is made；It is in mass ratio in 15:1 investment beaker, by beaker by acidic emulsion and aluminium chloride crystal powder
It is placed in sonic oscillation instrument, 1~2h is vibrated under conditions of frequency is 32~36kHz, quality point is added dropwise after oscillation into beaker
Number adjusts pH value to the obtained preformed solution of neutrality for 5~8% potassium hydroxide solution, be added into beaker preformed solution quality 5~
1~2h is mixed to get mixed serum with blender with the revolving speed of 300~350r/min in 9% iron powder；By above-mentioned mixing slurry
Liquid, which is put into suction filtration machine, filters removal filtrate, 3~5 times wash with distilled water, obtains reaction solid, reaction solid is put into tubular type
In furnace, it is continually fed into nitrogen into tube furnace, tubular type in-furnace temperature is increased to 105~115 DEG C, preheats 60~80min, preheating
Tubular type in-furnace temperature is increased to 500~550 DEG C, 50~60min of high-temperature calcination afterwards, heat-treated products are made；At above-mentioned heat
It manages in product investment planetary ball mill, ground and mixed 40 under conditions of ratio of grinding media to material is 10:1 and revolving speed is 300~350r/min
Milled mixtures are made in~50min, according to parts by weight, by 8~10 parts of milled mixtures, 0.5~0.7 part of silicon nitride, 1.1~
Prefabricated production is uniformly made in 1.3 parts of strontium carbonates, 1.0~1.4 parts of zinc nitrates, 0.3~0.5 part of bismuth titanates investment blender and mixing
Object；According to parts by weight, by 10~12 parts of above-mentioned pre products, 1.2~1.4 parts of triacetins, 0.3~0.6 part 12
Sodium alkyl benzene sulfonate, 2~3 parts of vinyltrimethoxysilanes are put into hot press after mixing, are 140~150 in temperature
DEG C and compacting pressure be 0.8~1.0MPa under conditions of constant temperature suppress 30~40min, after compacting put into sintering furnace in, in argon gas
50~60min is sintered under conditions of being 1100~1200 DEG C with temperature under atmosphere up to high pressure resistant intensity capacitor material.
Embodiment 1
Bamboo chip: moso bamboo
Sawdust: pine
The preparation of reacting slurry:
It is in mass ratio in 5:1 investment baking oven by bamboo plate and pine sawdust, dry 2h, dry under conditions of temperature is 70 DEG C
Grind into powder crosses 50 meshes and dry mixing is made afterwards, is in mass ratio that 1:5 is put into reaction kettle by dry mixing and water, will be anti-
It answers kettle closed, increases reactor temperature to 120 DEG C, constant temperature stands 100min, and reacting slurry is made.
The preparation of acidic emulsion:
The sodium hydroxide solution that mass fraction is 6% is added dropwise into aforesaid reaction vessel and adjusts pH value to 10, with blender with 600r/
50min is mixed in the revolving speed of min, air pressure in reaction kettle is increased to 0.8MPa, temperature is increased to 90 DEG C, and constant temperature and pressure is stood
The sulfuric acid solution that mass fraction is 20% is added dropwise after standing and adjusts pH value to 4, acidic emulsion is made by 2h.
The preparation of mixed serum:
It is in mass ratio to place the beaker sonic oscillation instrument in 15:1 investment beaker by acidic emulsion and aluminium chloride crystal powder
In, 1h is vibrated under conditions of frequency is 32kHz, the potassium hydroxide solution tune that mass fraction is 5% is added dropwise after oscillation into beaker
PH value is saved to the obtained preformed solution of neutrality, the iron powder of preformed solution quality 5% is added into beaker, with blender with 300r/min
Revolving speed be mixed 1h to get mixed serum.
The preparation of heat-treated products:
Above-mentioned mixed serum is put into suction filtration machine and filters removal filtrate, 3 times wash with distilled water, obtains reaction solid, it will be anti-
It answers in solid investment tube furnace, nitrogen is continually fed into tube furnace, tubular type in-furnace temperature is increased to 105 DEG C, preheating
Tubular type in-furnace temperature is increased to 500 DEG C, high-temperature calcination 50min after preheating by 60min, and heat-treated products are made.
The preparation of pre product:
Above-mentioned heat-treated products are put into planetary ball mill, are ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 300r/min
Milled mixtures are made in mill mixing 40min, according to parts by weight, by 8 parts of milled mixtures, 0.5 part of silicon nitride, 1.1 parts of carbonic acid
Pre product is uniformly made in strontium, 1.0 parts of zinc nitrates, 0.3 part of bismuth titanates investment blender and mixing.
The preparation of high pressure resistant intensity capacitor material:
According to parts by weight, by 10 parts of above-mentioned pre products, 1.2 parts of triacetins, 0.3 part of neopelex, 2
Part vinyltrimethoxysilane is put into hot press after mixing, and in temperature be 140 DEG C and compacting pressure is 0.8MPa's
Under the conditions of constant temperature suppress 30min, after compacting put into sintering furnace in, under argon atmosphere and temperature be 1100 DEG C under conditions of be sintered
50min is up to high pressure resistant intensity capacitor material.
Embodiment 2
Bamboo chip: fishpole bamboo
Sawdust: poplar
The preparation of reacting slurry:
It is in mass ratio in 5:1 investment baking oven by arhat bamboo chip and poplar sawdust, dry 2h, does under conditions of temperature is 75 DEG C
Dry rear grind into powder crosses 50 meshes and dry mixing is made, and is in mass ratio that 1:5 is put into reaction kettle by dry mixing and water, will
Reaction kettle is closed, increases reactor temperature to 125 DEG C, constant temperature stands 110min, and reacting slurry is made.
The preparation of acidic emulsion:
The sodium hydroxide solution that mass fraction is 8% is added dropwise into aforesaid reaction vessel and adjusts pH value to 10, with blender with 650r/
55min is mixed in the revolving speed of min, air pressure in reaction kettle is increased to 1.0MPa, temperature is increased to 95 DEG C, and constant temperature and pressure is stood
The sulfuric acid solution that mass fraction is 23% is added dropwise after standing and adjusts pH value to 4, acidic emulsion is made by 2h.
The preparation of mixed serum:
It is in mass ratio to place the beaker sonic oscillation instrument in 15:1 investment beaker by acidic emulsion and aluminium chloride crystal powder
In, 1h is vibrated under conditions of frequency is 34kHz, the potassium hydroxide solution tune that mass fraction is 7% is added dropwise after oscillation into beaker
PH value is saved to the obtained preformed solution of neutrality, the iron powder of preformed solution quality 6% is added into beaker, with blender with 325r/min
Revolving speed be mixed 1h to get mixed serum.
The preparation of heat-treated products:
Above-mentioned mixed serum is put into suction filtration machine and filters removal filtrate, 4 times wash with distilled water, obtains reaction solid, it will be anti-
It answers in solid investment tube furnace, nitrogen is continually fed into tube furnace, tubular type in-furnace temperature is increased to 110 DEG C, preheating
Tubular type in-furnace temperature is increased to 525 DEG C, high-temperature calcination 55min after preheating by 70min, and heat-treated products are made.
The preparation of pre product:
Above-mentioned heat-treated products are put into planetary ball mill, are ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 325r/min
Milled mixtures are made in mill mixing 45min, according to parts by weight, by 9 parts of milled mixtures, 0.6 part of silicon nitride, 1.2 parts of carbonic acid
Pre product is uniformly made in strontium, 1.2 parts of zinc nitrates, 0.4 part of bismuth titanates investment blender and mixing.
The preparation of high pressure resistant intensity capacitor material:
According to parts by weight, by 11 parts of above-mentioned pre products, 1.3 parts of triacetins, 0.4 part of neopelex, 2
Part vinyltrimethoxysilane is put into hot press after mixing, and in temperature be 1405 DEG C and compacting pressure is 0.9MPa's
Under the conditions of constant temperature suppress 35min, after compacting put into sintering furnace in, under argon atmosphere and temperature be 1150 DEG C under conditions of be sintered
55min is up to high pressure resistant intensity capacitor material.
Embodiment 3
Bamboo chip: Fang Zhu
Sawdust: mahogany
The preparation of reacting slurry:
It is in mass ratio in 5:1 investment baking oven by square bamboo bamboo chip and Peach sawdust, dry 3h, does under conditions of temperature is 80 DEG C
Dry rear grind into powder crosses 50 meshes and dry mixing is made, and is in mass ratio that 1:5 is put into reaction kettle by dry mixing and water, will
Reaction kettle is closed, increases reactor temperature to 130 DEG C, constant temperature stands 120min, and reacting slurry is made.
The preparation of acidic emulsion:
The sodium hydroxide solution that mass fraction is 10% is added dropwise into aforesaid reaction vessel and adjusts pH value to 11, with blender with 700r/
60min is mixed in the revolving speed of min, air pressure in reaction kettle is increased to 1.2MPa, temperature is increased to 100 DEG C, and constant temperature and pressure is quiet
3h is set, the sulfuric acid solution that mass fraction is 25% is added dropwise after standing and adjusts pH value to 5, acidic emulsion is made.
The preparation of mixed serum:
It is in mass ratio to place the beaker sonic oscillation instrument in 15:1 investment beaker by acidic emulsion and aluminium chloride crystal powder
In, 2h is vibrated under conditions of frequency is 36kHz, the potassium hydroxide solution tune that mass fraction is 8% is added dropwise after oscillation into beaker
PH value is saved to the obtained preformed solution of neutrality, the iron powder of preformed solution quality 9% is added into beaker, with blender with 350r/min
Revolving speed be mixed 2h to get mixed serum.
The preparation of heat-treated products:
Above-mentioned mixed serum is put into suction filtration machine and filters removal filtrate, 5 times wash with distilled water, obtains reaction solid, it will be anti-
It answers in solid investment tube furnace, nitrogen is continually fed into tube furnace, tubular type in-furnace temperature is increased to 115 DEG C, preheating
Tubular type in-furnace temperature is increased to 550 DEG C, high-temperature calcination 60min after preheating by 80min, and heat-treated products are made.
The preparation of pre product:
Above-mentioned heat-treated products are put into planetary ball mill, are ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 350r/min
Milled mixtures are made in mill mixing 50min, according to parts by weight, by 10 parts of milled mixtures, 0.7 part of silicon nitride, 1.3 parts of carbonic acid
Pre product is uniformly made in strontium, 1.4 parts of zinc nitrates, 0.5 part of bismuth titanates investment blender and mixing.
The preparation of high pressure resistant intensity capacitor material:
According to parts by weight, by 12 parts of above-mentioned pre products, 1.4 parts of triacetins, 0.6 part of neopelex, 3
Part vinyltrimethoxysilane is put into hot press after mixing, and in temperature be 150 DEG C and compacting pressure is 1.0MPa's
Under the conditions of constant temperature suppress 40min, after compacting put into sintering furnace in, under argon atmosphere and temperature be 1200 DEG C under conditions of be sintered
60min is up to high pressure resistant intensity capacitor material.
Comparative example 1: it is essentially identical with the preparation method of example 1, it has only the difference is that acidic emulsion is not added.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that heat-treated products are not added.
Comparative example 3: the capacitor material of company, Xuancheng City production.
Capacitor material in high pressure resistant intensity capacitor material produced by the present invention and comparative example is detected, is detected
The results are shown in Table 1:
Dielectric loss test
Capacitor material in high pressure resistant intensity capacitor material produced by the present invention and comparative example is 1 ± 0.1kHz in frequency,
It is tested in the range of 1 ± 0.1V of AC value using dielectric loss tester.
1 performance measurement result of table
From the data in table 1, it can be seen that high pressure resistant intensity capacitor material produced by the present invention, has dielectric constant height, pressure voltage height, is situated between
It the features such as matter loss small, stable structure, shows good cyclical stability, uses the longevity compared to common capacitor material
Life improves 2~3 times, and preparation method is simple, preparation process flow is easy to operate, is suitble to large-scale production, has extremely wide
Market prospects and application value.
Claims (8)
1. a kind of preparation method of high pressure resistant intensity capacitor material, it is characterised in that specific preparation step are as follows:
(1) heat-treated products are put into planetary ball mill, in the condition that ratio of grinding media to material is 10:1 and revolving speed is 300~350r/min
Milled mixtures are made in 40~50min of lower ground and mixed, and milled mixtures, silicon nitride, strontium carbonate, zinc nitrate, bismuth titanates are thrown
Enter blender and mixing and pre product is uniformly made；
(2) after mixing by pre product, triacetin, neopelex, vinyltrimethoxysilane
Put into hot press in, temperature be 140~150 DEG C and compacting pressure be 0.8~1.0MPa under conditions of constant temperature compacting 30~
40min, after compacting put into sintering furnace in, under argon atmosphere and temperature be 1100~1200 DEG C under conditions of sintering 50~
60min is up to high pressure resistant intensity capacitor material；
The specific preparation step of the heat-treated products are as follows:
(1) it by acidic emulsion and aluminium chloride crystal powder investment beaker, places the beaker in sonic oscillation instrument, is 32 in frequency
1~2h is vibrated under conditions of~36kHz, and the potassium hydroxide solution that mass fraction is 5~8% is added dropwise after oscillation into beaker and adjusts
Iron powder is added into beaker, is mixed with blender with the revolving speed of 300~350r/min to the obtained preformed solution of neutrality for pH value
1~2h is up to mixed serum；
(2) mixed serum is put into suction filtration machine and filters removal filtrate, 3~5 times wash with distilled water, obtain reaction solid, it will
It reacts in solid investment tube furnace, nitrogen is continually fed into tube furnace, tubular type in-furnace temperature is increased to 105~115 DEG C, in advance
Tubular type in-furnace temperature is increased to 500~550 DEG C after preheating by 60~80min of heat, and heat treatment is made in 50~60min of high-temperature calcination
Product；
The specific preparation step of the acidic emulsion are as follows:
(1) by bamboo chip and sawdust investment baking oven, dry 2~3h, is ground into after dry under conditions of temperature is 70~80 DEG C
Powder crosses 50 meshes and dry mixing is made, and dry mixing and water are put into reaction kettle, and reaction kettle is closed, increases in reaction kettle
For temperature to 120~130 DEG C, constant temperature stands 100~120min, and reacting slurry is made；
(2) sodium hydroxide solution that mass fraction is 6~10% is added dropwise into reaction kettle and adjusts pH value to 10~11, uses blender
50~60min is mixed with the revolving speed of 600~700r/min, air pressure in reaction kettle is increased to 0.8~1.2MPa, temperature liter
Up to 90~100 DEG C, constant temperature and pressure stands 2~3h, and the sulfuric acid solution that mass fraction is 20~25% is added dropwise after standing and adjusts pH value
To 4~5, acidic emulsion is made.
2. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: preferred
According to parts by weight, the milled mixtures are 8~10 parts, silicon nitride is 0.5~0.7 part, strontium carbonate is 1.1~1.3 parts,
Zinc nitrate is 1.0~1.4 parts, bismuth titanates is 0.3~0.5 part.
3. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: preferred
According to parts by weight, the pre product is 10~12 parts, triacetin is 1.2~1.4 parts, dodecyl benzene sulfonic acid
Sodium is 0.3~0.6 part, vinyltrimethoxysilane is 2~3 parts.
4. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: heat treatment
The mass ratio of acidic emulsion described in the specific preparation step (1) of product and aluminium chloride crystal powder is 15:1.
5. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: heat treatment
The quality for the iron powder being added described in the specific preparation step (1) of product into beaker is the 5~9% of preformed solution quality.
6. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: acid cream
The mass ratio of bamboo chip described in the specific preparation step (1) of liquid and sawdust is 5:1.
7. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: acid cream
Bamboo chip described in the specific preparation step (1) of liquid be more preferably one of moso bamboo, fishpole bamboo, Fang Zhu or it is a variety of by appoint
The mixing of meaning ratio, the sawdust are more preferably one of pine, poplar, mahogany or a variety of mix in any proportion.
8. a kind of preparation method of high pressure resistant intensity capacitor material according to claim 1, it is characterised in that: acid cream
The mass ratio of drying mixing described in the specific preparation step (1) of liquid and water is 1:5.
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| US6631073B1 (en) * | 1998-08-25 | 2003-10-07 | Kanebo, Limited | Electrode material and method for producing the same |
| CN1567493A (en) * | 2003-07-03 | 2005-01-19 | 中国科学院电工研究所 | A composite carbon-based electrode material for super capacitor and method for making same |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN106206043A (en) * | 2016-08-26 | 2016-12-07 | 中原工学院 | A kind of FeS2nanometer rods/Graphene is to electrode material and preparation method and application |
| CN108417410A (en) * | 2018-01-18 | 2018-08-17 | 燕山大学 | A kind of cellulose gel electrolyte and preparation method thereof |
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2019
- 2019-03-27 CN CN201910235990.XA patent/CN110085432B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6631073B1 (en) * | 1998-08-25 | 2003-10-07 | Kanebo, Limited | Electrode material and method for producing the same |
| CN1567493A (en) * | 2003-07-03 | 2005-01-19 | 中国科学院电工研究所 | A composite carbon-based electrode material for super capacitor and method for making same |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN106206043A (en) * | 2016-08-26 | 2016-12-07 | 中原工学院 | A kind of FeS2nanometer rods/Graphene is to electrode material and preparation method and application |
| CN108417410A (en) * | 2018-01-18 | 2018-08-17 | 燕山大学 | A kind of cellulose gel electrolyte and preparation method thereof |
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