CN107946600A - A kind of preparation method of the lightweight conductive ceramic plates of lead base storage battery - Google Patents
A kind of preparation method of the lightweight conductive ceramic plates of lead base storage battery Download PDFInfo
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- CN107946600A CN107946600A CN201711223031.3A CN201711223031A CN107946600A CN 107946600 A CN107946600 A CN 107946600A CN 201711223031 A CN201711223031 A CN 201711223031A CN 107946600 A CN107946600 A CN 107946600A
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- mould
- ceramic plates
- storage battery
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- base storage
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/82—Multi-step processes for manufacturing carriers for lead-acid accumulators
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method of the lightweight conductive ceramic plates of lead base storage battery, including cordierite powder and graphite powder, its preparation process mixes for a. cordierite powder with phenolic resin；B. graphite powder is mixed with the mixture of step a, is placed in mould；C. mould is placed in high temperature furnace and heated；D. it is being cooled to the sub- thin film of titanium oxide of one layer of ceramic plates matrix surface thermal spraying of room temperature.The present invention is applied to lead base storage battery, its light weight, structural strength is high, and the usage amount of heavy metal lead is greatly reduced, and has preferable thermal conductivity and conductivity, and current density is high, and battery performance and shelf characteric are good, and efficiency for charge-discharge is high and service life extends.
Description
Technical field：
The present invention relates to an a kind of component of lead base storage battery, the one kind used for particularly relating to lead base storage battery is conductive
The preparation method of ceramic plates.
Background technology：
Secondary power supply plays particularly important effect in modern society, is particularly that power battery is obtained as clean energy resource
To attention, the power battery typically now used is mainly two classes, and one kind is lithium battery, and another kind of is that traditional plumbic acid (base) stores
Battery.The former is that volume is relatively small, but shortcoming is expensive and fire or explosion easily occur in the case where temperature is slightly higher,
Also it is difficult to be received often as power battery, the latter is cheap, technology maturation, and performance safety is stablized, but relative volume
Weight is larger, and especially with substantial amounts of heavy metal lead, it is prepared and removal process can produce heavy metal pollution.Above-mentioned
Lead base storage battery in, the theory of lead base active material than energy be 170w.h/kg, and the ratio energy of the lead base storage battery of reality
Only above-mentioned theory is than 1/5th of energy.The main reason for lower than energy, first, active material reaction efficiency is less than
50%, the other is HSO4 -By electrode thickness, material restricts ion, grid and it is other it is non-account for nearly 40% into stream material, active matter
Relation between matter, grid quality, electrolyte density is extremely unreasonable.Therefore, the defects of how solving existing lead base storage battery, carries
The performance of plumbic acid storage battery, is still to solve the problems, such as a direction of power battery and anxious to be resolved.
The content of the invention：
The goal of the invention of the present invention is to disclose a kind of preparation method of the good unleaded conductivity ceramics pole plate of light weight, intensity.
Realize that the technical solution of the present invention is as follows：Including cordierite powder and graphite powder, the preparation of lightweight conductive ceramics
Step is following (component is by weight percentage)：
A.35 cordierite powder (granularity is 5~15 μm)~50% is mixed with 5~10% phenolic resin, after pinching pressure mixing
When standing 4~5 is small；
B.40 after graphite powder~50% is mixed with the mixture of step a, it is placed in mould and suppresses, mould is placed in heating
70~80 DEG C are heated in stove, when insulation 1~2 is small, with the mixed material and preliminarily dried being further plasticized in mould；
C. the mould with mixed material in step b is placed in high temperature furnace and heated, heating process is as follows：
1. being heated to 200~220 DEG C, 10~30 minutes are kept the temperature；
2. being heated to 800~850 DEG C, heating rate is 100 DEG C/h, while applies a vibration and pressure to mould；
3. being heated to 1300~1350 DEG C, heating rate is 150 DEG C/h, when insulation 1~2 is small, keeps pressure；
4. temperature-fall period is：1300~1350 DEG C are down to 800 DEG C, to mold decompression, are then naturally cooling to room temperature, are shed
Mould obtains Polar plate matrix；
D. the lightweight is obtained in the sub- thin film of titanium oxide of one layer of ceramic plates matrix surface thermal spraying for being cooled to room temperature to lead
Electroceramics finished product.
In the step b, when cordierite powder is mixed with phenolic resin, it is swollen to add the nanoscale that granularity is 5~20nm
Moisten soil particle.
In the step b, when mixed material mixes, metallic aluminium powder and/or ultra fine silicon carbide are added.
The composition of the ultra fine silicon carbide is containing the carborundum powder and 30 that 70~80% granularity is 50nm~200nm
~20% granularity is 10 μm~50 μm of carborundum powder.
The step c- 3. when, to mould apply pressure while, to mould apply a vibration force, vibration force
Amplitude is 0.5~1mm.
Step c- 4. during, decompression process is decline of the pressure with temperature, at the uniform velocity releases the pressure of application,
At 800 DEG C, the pressure releases of application.
The composition of the sub- thin film of titanium oxide is (by weight percentage)：10~15% polyvinyl alcohol, 0.3~
1% carboxymethylcellulose sodium, 10~12% sub- titanium oxide powder and surplus are water, it is heated with stirring to 50 after each component mixing~
80 DEG C must contain sub- titanium oxide liquid.
The sub- thin film of titanium oxide is latticed or is that spaced more strips are formed.
Lightweight conductive ceramic plates disclosed by the invention are to be applied to lead base storage battery, its advantage is light weight, and structure is strong
Degree is high, has the appropriate size of specific porosity and hole, has preferable thermal conductivity and conductivity.The present invention is used as electric power storage
The pole plate in pond is the usage amount that heavy metal lead is greatly reduced first, reduces lead contamination, while obtains a kind of current density height,
Battery performance and shelf characteric are good, and efficiency for charge-discharge height and the extended lead base storage battery of service life, are traditional lead base storage batteries
The major progress in field.
Embodiment：
The embodiment of the present invention is provided in detail below, it is necessary to which the detailed description to embodiment of explanation is
For ease of the comprehensive understanding of the technical spirit to the present invention, the limit to scope of the claims of the invention is not construed as
System.
The technical solution of the specific embodiment of the present invention is as follows：Including cordierite powder and graphite powder, it is important to lightweight
The preparation process of conductivity ceramics is following (component is by weight percentage)：
A.35 cordierite powder (granularity is 5~15 μm)~50% is mixed with 5~10% phenolic resin, after pinching pressure mixing
When standing 4~5 is small；
B.40 after graphite powder~50% is mixed with the mixture of step a, it is placed in mould and suppresses, mould is placed in heating
70~80 DEG C are heated in stove, when insulation 1~2 is small, with the mixed material and preliminarily dried being further plasticized in mould；
C. the mould with mixed material in step b is placed in high temperature furnace and heated, heating process is as follows：
1. being heated to 200~220 DEG C, 10~30 minutes are kept the temperature；
2. being heated to 800~850 DEG C, heating rate is 100 DEG C/h, while applies a vibration and pressure to mould；
3. being heated to 1300~1350 DEG C, heating rate is 150 DEG C/h, when insulation 1~2 is small, keeps pressure；
4. temperature-fall period is：1300~1350 DEG C are down to 800 DEG C, to mold decompression, are then naturally cooling to room temperature, are shed
Mould obtains Polar plate matrix；
D. the lightweight is obtained in the sub- thin film of titanium oxide of one layer of ceramic plates matrix surface thermal spraying for being cooled to room temperature to lead
Electroceramics finished product.
Above-mentioned cordierite material is a kind of commonly used in ceramic or glass industry raw material, belongs to oblique chip system, its thing
It is that thermal coefficient of expansion is small to manage characteristic, and the main function of cordierite is the matrix for forming ceramics in the present invention, and graphite powder is in this hair
Main function in bright is electric action and conduction of heat, while plays the role of certain basal body structure.In above-mentioned step a
In, after cordierite powder is mixed with phenolic resin, phenolic resin can immerse cordierite particle, and it is small to stand 4~5 after pressure mixing is pinched
When, phenolic resin is immersed cordierite particle, and cordierite is tentatively plasticized, in above-mentioned step b, with temperature
Increase, on the one hand improve cordierite gelation degree, the volatilizable component in phenolic resin is tentatively volatilized, make
Mixed material preliminarily dried in mould；Step c- 1. in, mixed material be heated to 200~220 DEG C and insulation, make mixture
Volatilizable component in material further volatilizees, shape need basic forming and basic curing of the mixed material by mould, great Liang Hui
The hole that the effusion of stimulating food helps to improve after sintering is small size hole, and helps to improve the structural strength of ceramic plates；
Above-mentioned step c- 2. in, phenolic resin carbonized, a part of gas componant escapes at high temperature, and a part of gas is in matrix
Hole is formed, it is 1~2Mpa to apply a vibration and pressure, pressure to mould, also can suitably increased or decrease, vibrate and be
5~10 times per second and amplitude are 3~5mm, and above-mentioned pressure can further improve the effusion of gas in matrix, and vibration can make hole
Quantity increases and forms the fine pore of large scale, so that graphite powder is distributed in substantial amounts of fine pore and improves the scattered of graphite powder
Uniformity, to improve the conduction of matrix and heat transfer property, the step for it is particularly significant, to improving conductive and heat transfer property to closing weight
Will, and phenolic resin is carbonized to form pyrolytic carbon in this stage, it plays between the ceramic component and graphite powder of matrix and is connected
Effect；Above-mentioned step c- 3. in, phenolic resin carbonization, and matrix is in 1300~1350 DEG C of also sinter moldings, the liter
Warm process is the developmental process of ceramic component, keeps above-mentioned pressure to make the crystal structure in the matrix of the ceramic plates of sheet
Grown to in-plane, make the structural strength of pole plate more preferably；Above-mentioned step c- 4. in, from 1300~1350 DEG C of sintering to
800 DEG C of temperature-fall period, release the foregoing pressure to mould, the decompression process be pressure as temperature declines, uniform descent is applied
The pressure added, at 800 DEG C, the pressure releases of application, since ceramic matrix is after the completion of high temperature sintering, in cool down
Thermal stress presence is had in ceramic matrix, on the one hand which can make ceramic matrix become fragile, on the other hand can be answered in part heat
Power produces substantial amounts of fine crack in ceramic matrix during disappearing, on the one hand the presence of these micro-cracks reduces ceramic matrix
Structural strength, on the one hand can reduce the conductivity of ceramic matrix, therefore in the above-mentioned temperature-fall period from the condition of high temperature, controlledly apply
Put the pressure of application, make ceramic matrix produced in temperature-fall period it is small be gradually deformed, so as to eliminate in ceramic matrix
The presence of thermal stress, has preferable raising to the performance for improving ceramic matrix.It is being cooled to the ceramic plates matrix surface of room temperature
The sub- thin film of titanium oxide of one layer of thermal spraying obtains the lightweight conductive ceramic product, and above-mentioned sub- thin film of titanium oxide can further improve
The conductivity of lightweight conductive ceramic plates.
To further improve the performance of above-mentioned lightweight conductive ceramic plates, in above-mentioned step b, cordierite powder with
When phenolic resin mixes, the nanoscale bentonite clay particle that granularity is 5~20nm is added；Bentonitic structure is layer structure, and
It is elecrtonegativity, on the one hand the structural strength of ceramic matrix can be increased in sintering process by adding nano-bentonite, on the other hand original
Layer structure form substantial amounts of small interlayer hole or gap again in matrix, have to the energy density for improving battery very big
Help.In above-mentioned step b, when mixed material mixes, metallic aluminium powder and/or ultra fine silicon carbide are added；Metallic aluminium
The part of powder forms metal between small lattice between the crystal of ceramic matrix or between graphite powder, this is to improving ceramic matrix
Conductivity it is helpful, and ultra fine silicon carbide can gasify in a condition of high temperature part and form small hole, a part with
Ceramic matrix forms structure division and improves the intensity of ceramic matrix.And the composition of above-mentioned ultra fine silicon carbide be containing 70~
Carborundum powder and 30~20% granularity that 80% granularity is 50nm~200nm are 10 μm~50 μm of carborundum powder, above-mentioned
The gasification of nano level silicon carbide portion when generate small stomata, and generation is relatively when micron-sized silicon carbide portion gasifies
Big stomata, forms the gas cell distribution of more rational proportion, part lead plaster component can be penetrated into above-mentioned larger stomata, this increasing
Add response area and improve the efficiency of discharge and recharge.Above-mentioned step c- 3. when, to mould apply pressure while, it is right
Mould applies a vibration force, and the amplitude of the vibration force be 0.5~1mm, i.e., amplitude at this time less than step c-- 2. in shake
Width, above-mentioned pressure and small vibration can further improve the quantity of the hole in ceramic matrix, and contribute to liquid metal
Expansion between lattice of the aluminium in ceramic matrix, and further improve conductivity, heat transfer performance and the raising energy of ceramic matrix
Metric density.4. above-mentioned step c- is the temperature-fall period of the ceramic matrix of high-temperature firing, in the drop that temperature is 1300~1350 DEG C
Warm process, at the same by step c- 3. during to mould apply pressure with temperature decline release, i.e., at the uniform velocity release apply
Pressure, at 800 DEG C, the pressure releases of application, gradually releasing is applied stressed process and can be reduced in temperature-fall period and makes pottery for this
Accumulation or the thermal stress formed in porcelain basal body, improve the toughness of ceramic matrix and reduce the fine crack formed in ceramic matrix.
In foregoing step d, be cooled to the ceramic plates of room temperature matrix surface spray sub- thin film of titanium oxide be by
Sub- thin film of titanium oxide is formed after ceramic plates matrix surface, drying containing sub- titanium oxide liquid spray.Above-mentioned sub- titanium oxide is thin
The composition of film is (by weight percentage)：10~15% polyvinyl alcohol, 0.3~1% carboxymethylcellulose sodium, 10~
12% sub- titanium oxide powder and surplus is water, and sub- titanium oxide liquid must be contained by being heated with stirring to 50~80 DEG C after each component mixing.It is dry
It can obtain sub- titanium oxide conductive film after dry, conductive film control is preferred in 0.1~0.5mm, and above-mentioned ceramic plates base
The thickness of body is 0.8~5mm, and the selection of thickness is depending on the requirement of storage battery.
The sub- thin film of titanium oxide is latticed or is that spaced more strips are formed, this need to be adjusted in coating
Coating method or technique can be achieved, this can make have infiltration between larger hole in lead plaster and pole plate.
It should be noted that the preparation method of lightweight conductive ceramic plates disclosed by the invention is by largely, repeatedly
Different component proportioning, combinations of particle sizes, heat the pole plate that the batch test of many influence factors such as speed and soaking time just obtains,
In fact the preparation of present ceramic composite generally or based on experiment, mechanism instruct supplemented by developing stage.This
The pole plate prepared is invented than the anode plate grid skeleton of the lead-calcium alloy of traditional lead-acid accumulator, considerably reduces lead base storage
Lead contamination, and above-mentioned lightweight conductive ceramics pole is greatly reduced up to 50% or so in the heavy metal lead dosage of battery, decrement
The unit mass of plate is also greatly reduced.The technical spirit of the conductivity ceramics pole plate of the present invention is a kind of the more of graphite/ceramic/metal
Hole composite conducting material, itself has concrete dynamic modulus, and the size scale of hole has rational distribution, and substantial amounts of fine pore can accommodate
Graphite powder, forms three-dimensional conductive network, and metallic aluminium further strengthens above-mentioned three-dimensional conductive network, and the hole shape that part is larger
Part lead plaster is entered the inside of pole plate into the interstitial space being mutually communicated, further improve the response area of active material
And reaction efficiency, so as to improve lead-acid accumulator efficiency for charge-discharge, improve the specific energy of lead-acid accumulator, mass ratio
Energy can improve 50~70%.It since ceramic plates have good intensity and toughness, therefore can be machined, such as can be made
The pole plate of standby larger area, then carry out as needed machine cuts obtain it is suitably sized.
Claims (8)
1. a kind of preparation method of the lightweight conductive ceramic plates of lead base storage battery, including cordierite powder and graphite powder, its feature
It is that the preparation process of lightweight conductive ceramics is following (component is by weight percentage)：
A.35 cordierite powder (granularity is 5~15 μm)~50% is mixed with 5~10% phenolic resin, is stood after pinching pressure mixing
4~5 it is small when；
B.40 after graphite powder~50% is mixed with the mixture of step a, it is placed in mould and suppresses, mould is placed in heating furnace
70~80 DEG C are heated to, when insulation 1~2 is small, with the mixed material and preliminarily dried being further plasticized in mould；
C. the mould with mixed material in step b is placed in high temperature furnace and heated, heating process is as follows：
1. being heated to 200~220 DEG C, 10~30 minutes are kept the temperature；
2. being heated to 800~850 DEG C, heating rate is 100 DEG C/h, while applies a vibration and pressure to mould；
3. being heated to 1300~1350 DEG C, heating rate is 150 DEG C/h, when insulation 1~2 is small, keeps pressure；
4. temperature-fall period is：1300~1350 DEG C are down to 800 DEG C, to mold decompression, are then naturally cooling to room temperature, are shed mould
Obtain Polar plate matrix；
D. the lightweight conductive pottery is obtained in the sub- thin film of titanium oxide of one layer of ceramic plates matrix surface thermal spraying for being cooled to room temperature
Porcelain finished product.
2. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 1, it is characterised in that institute
In the step b stated, when cordierite powder is mixed with phenolic resin, the nanoscale bentonite clay particle that granularity is 5~20nm is added.
3. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 1 or 2, it is characterised in that
In the step b, when mixed material mixes, metallic aluminium powder and/or ultra fine silicon carbide are added.
4. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 3, it is characterised in that institute
The composition for the ultra fine silicon carbide stated is containing the carborundum powder and 30~20% grain that 70~80% granularity is 50nm~200nm
Spend the carborundum powder for 10 μm~50 μm.
5. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 4, it is characterised in that institute
The step c- stated 3. when, while pressure is applied to mould, apply a vibration force to mould, the amplitude of vibration force is 0.5
~1mm.
6. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 5, it is characterised in that
Step c- 4. during, decompression process is decline of the pressure with temperature, at the uniform velocity releases the pressure of application, at 800 DEG C, apply
Pressure releases.
7. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 6, it is characterised in that institute
The composition for the sub- thin film of titanium oxide stated is (by weight percentage)：10~15% polyvinyl alcohol, 0.3~1% carboxymethyl
Cellulose is received, 10~12% sub- titanium oxide powder and surplus are water, and Asia must be contained by being heated with stirring to 50~80 DEG C after each component mixing
Titanium oxide liquid.
8. the preparation method of the lightweight conductive ceramic plates of lead base storage battery according to claim 7, it is characterised in that institute
The sub- thin film of titanium oxide stated is latticed or is that spaced more strips are formed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711223031.3A CN107946600B (en) | 2017-11-29 | 2017-11-29 | Preparation method of light conductive ceramic polar plate of lead-based storage battery |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711223031.3A CN107946600B (en) | 2017-11-29 | 2017-11-29 | Preparation method of light conductive ceramic polar plate of lead-based storage battery |
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| CN107946600A true CN107946600A (en) | 2018-04-20 |
| CN107946600B CN107946600B (en) | 2020-07-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109946145A (en) * | 2019-03-11 | 2019-06-28 | 哈尔滨理工大学 | A kind of multilayer sample preparation mold and preparation method thereof applying electrical pre-stress |
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| JPS5424222A (en) * | 1977-07-26 | 1979-02-23 | Dba Sa | Casting apparatus for making support grid for storage battery electrode |
| CN102515728A (en) * | 2011-12-16 | 2012-06-27 | 北京鸿源能信科技有限责任公司 | Conductive ceramic, method for preparing same and application for same |
| CN102522566A (en) * | 2011-12-16 | 2012-06-27 | 北京鸿源能信科技有限责任公司 | Storage battery grid |
| CN202405369U (en) * | 2011-12-16 | 2012-08-29 | 北京鸿源能信科技有限责任公司 | Storage battery slab lattice |
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2017
- 2017-11-29 CN CN201711223031.3A patent/CN107946600B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5424222A (en) * | 1977-07-26 | 1979-02-23 | Dba Sa | Casting apparatus for making support grid for storage battery electrode |
| CN102515728A (en) * | 2011-12-16 | 2012-06-27 | 北京鸿源能信科技有限责任公司 | Conductive ceramic, method for preparing same and application for same |
| CN102522566A (en) * | 2011-12-16 | 2012-06-27 | 北京鸿源能信科技有限责任公司 | Storage battery grid |
| CN202405369U (en) * | 2011-12-16 | 2012-08-29 | 北京鸿源能信科技有限责任公司 | Storage battery slab lattice |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109946145A (en) * | 2019-03-11 | 2019-06-28 | 哈尔滨理工大学 | A kind of multilayer sample preparation mold and preparation method thereof applying electrical pre-stress |
| CN109946145B (en) * | 2019-03-11 | 2024-03-19 | 哈尔滨理工大学 | Multilayer sample preparation mold capable of applying prestress and preparation method thereof |
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