CN110661039A - Low-temperature battery formation process - Google Patents
Low-temperature battery formation process Download PDFInfo
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- CN110661039A CN110661039A CN201910908796.3A CN201910908796A CN110661039A CN 110661039 A CN110661039 A CN 110661039A CN 201910908796 A CN201910908796 A CN 201910908796A CN 110661039 A CN110661039 A CN 110661039A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
- H01M10/12—Construction or manufacture
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
- H01M10/08—Selection of materials as electrolytes
- H01M10/10—Immobilising of electrolyte
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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
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- 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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a low-temperature battery formation process, which achieves the purposes of saving cost, reducing battery weight and improving the low-temperature performance of a battery by adjusting a formation process and a material preparation process. The invention adopts the constant temperature effect in the formation stage, the battery temperature is always controlled between 20 ℃ and 45 ℃, the charging current utilization rate is highest in the temperature state, the material in the electrode plate can not be oxidized, and the produced battery has the characteristics of high low-temperature capacity and long service life.
Description
Technical Field
The invention belongs to the technical field of production of lead-acid storage batteries, and particularly relates to a low-temperature battery formation process.
Background
The lead-acid storage battery is seen everywhere in our daily life as the secondary battery with the highest safety coefficient, and the product is durable for more than 150 years because the material of the product can be recycled, so that the cost is lower. Due to the electrolyte system relationship of the lead-acid storage battery, when the ambient temperature is high, the excellent battery performance is reflected in that the discharge time is long and the charge time is short, otherwise, the discharge time is short, the charged electric quantity is reduced, and the discharge quantity is lower due to the reduction of the charged quantity. In other words, in a low-temperature environment, if the low-temperature capacity of the lead-acid storage battery does not meet the national standard requirement, the battery enters a vicious cycle state. Therefore, the low-temperature capacity of the battery is an important index for measuring the performance of the battery. The quantity of goods returned by the products in northern markets of China in winter is 1.5 times of that in summer, and the goods returned by some large enterprises even reaches more than 2 times, so that the overall goods return rate reaches 20%.
Various production enterprises and colleges are continuously striving to attack and research materials, and hope to improve the low-temperature capacity of the lead-acid storage battery through optimizing the material properties, and the development of modified graphite, modified fumed silica, modified lignin, the introduction of a negative electrode material grinding process and the like is also greater in the years. The improvement of the anode material, although improving the low temperature performance, increases the cost much.
Disclosure of Invention
The invention aims to provide a battery formation process which is low in cost and can improve the low-temperature capacity of a lead-acid storage battery.
In order to achieve the purpose, the invention provides the following technical scheme:
a low-temperature battery formation process comprises the following steps:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2/2A-1m2Filling the positive plate active substance with the electrochemical equivalent of 0.3-3% in the solution A;
step two: charging current 1m2/5A-1m214A, filling 40-60% of the active material of the positive plate in an electrochemical equivalent;
step three: standing for 30 minutes;
step four: charging current 1m2/5A-1m2Charging 8% -12% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2/20.6A-1m2a/25A, discharging 3-8% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step six: charging current 1m2/4A-1m2Filling 3-8% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2/15A-1m2a/25A, discharging 4-9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eight: charging current 1m2/4A-1m2Charging 4% -9% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2/15A-1m2a/25A, discharging 5-9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m2/4A-1m2Filling 5-9% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eleven; discharge current 1m2/15A-1m2a/25A, discharging 6-11% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twelve: charging current 1m2/8A-1m2Filling 5.8-9% of active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step thirteen: charging current 1m2/5A-1m2Filling 20-52% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
fourteen steps: charging current 1m2/4A-1m2Filling 30-70% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
step fifteen: charging current 1m2/3A-1m2Filling 30-55% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2/15A-1m2a/25A, discharging 15-35% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2/15A-1m2a/25A, discharging 3-9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 seconds;
eighteen steps: charging current 1m2/7A-1m2Charging 10-25% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
nineteen steps: charging current 1m2/5A-1m2Filling 30-55% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
twenty steps: charging current 1m2/3A-1m2a/10A, charging 20-70% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
twenty one: charging current 1m2/2A-1m2Charging 15-35% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m2/0.2A-1m2and/1.5A, charging 1-6% of the active material electrochemical equivalent of the positive plate, automatically measuring the battery voltage in real time, and recording the measured value every 10 minutes.
Preferably, the low-temperature battery formation process comprises the following steps:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2a/4.1A, filling 1.3 percent of the active material electrochemical equivalent of the positive plate;
step two: charging current 1m28.24A, filling 52 percent of the electrochemical equivalent of the active substance of the positive plate;
step three: standing for 30 minutes;
step four: charging current 1m28.24A, charging 11.6 percent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is discharged by 5.1 percent at the A/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step six: charging current 1m28.24A, charging 5.4 percent of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is 6.3 percent at a/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step eight: charging current 1m28.24A, charging 6.4 percent of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2a/20.6A, discharging 7.5% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m28.24A, charging 7.6 percent of the active material of the positive plate into the electrochemical equivalent, automatically measuring the voltage of the battery in real time,record measurements every 10 minutes;
step eleven; discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is discharged by 8.7 percent at the A/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step twelve: charging current 1m2Filling 5.8% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step thirteen: charging current 1m2(iii)/7.99, charging 42.2% of the active material electrochemical equivalent of the positive plate, automatically measuring the battery voltage in real time, and recording the measured value every 10 minutes;
fourteen steps: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 58.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step fifteen: charging current 1m2Charging 44.5% of the active material of the positive plate in electrochemical equivalent, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2a/20.6A, discharging 25% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is 5.6 percent at 20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 seconds;
eighteen steps: charging current 1m2Filling 17.5 percent of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
nineteen steps: charging current 1m2The electrochemical equivalent of the active substance filled into the positive plate is 42.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
twenty steps: charging current 1m2(6.9A), charging 58.3% of the active material of the positive plate, automatically measuring the battery voltage in real time every 10%Recording one measurement in minutes;
twenty one: charging current 1m2Charging 24.5% of the active material of the positive plate into the electrochemical equivalent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m20.62A, charged with 2.6% of the electrochemical equivalent of the positive plate active material, the cell voltage was automatically measured in real time, and the measurement was recorded every 10 minutes.
Further, before the step one, the method further comprises the steps of: preparing a master batch;
raw materials: selecting industrial-grade silicon dioxide powder produced by a gas phase method, wherein the average particle size of the industrial-grade silicon dioxide powder is 0.1-0.2 mu m, the silicon dioxide content is more than 99.5% -99.99%, and the industrial-grade silicon dioxide powder is dried at 105 ℃ for 2 hours, has the density of 50g/L and is in a hydrophobic state;
preparing equipment: the rotating speed is 4000 to 5000r/min, the volume is 800 kg;
the configuration method comprises the following steps: adding 600kg of deionized water into the equipment, wherein the rotating speed of the equipment is 4000r/min, adding meteorological silica with the weight ratio of the ionized water being 15% by using a vacuum conveying device, increasing the rotating speed to 4800r/min, shearing at high speed for 20-30 minutes, and adjusting the temperature of cooling water to 20-35 ℃. Adding sodium hydroxide with the weight ratio of the deionized water being 0.0016 percent, then adding polyaspartic acid ammonia sodium salt with the weight ratio of the deionized water being 0.001 percent, and stirring for 3 to 5 minutes.
Further, before the step one, the method further comprises the steps of: preparing dilute sulfuric acid;
raw materials: analytical grade H2SO4
The configuration method comprises the following steps: according to 36%: 64% acid water mass ratio, analyzing the raw material to pure grade H2SO4Slowly adding into water to control the temperature within 25 + -5 deg.C, and adjusting the density of dilute sulfuric acid to 1.265g/cm3Anhydrous sodium sulfate with the total mass of 0.8 percent is added, the mixture is stirred for 20 minutes, and the preparation of dilute sulfuric acid is finished.
Further, before the step one, the method further comprises the steps of: preparing electrolyte;
mixing the prepared dilute sulfuric acid and the prepared masterbatch according to the mass ratio of 100: 3.5 adding the mixture into a stirring tank and mixing for 30 minutes to obtain electrolyte; then cooling, cooling temperature: if the using temperature is less than or equal to 15 ℃, cooling the electrolyte to 10 +/-1 ℃, and if the room temperature is more than or equal to 16 ℃, cooling the electrolyte to 1 +/-1 ℃; and cooling the electrolyte for later use.
Further, before the step one, the method further comprises the steps of: the prepared electrolyte is mixed according to the proportion of 1Ah/3.66g/cm3Adding the product of the concentrated acid quantity standard and the rated capacity of the product into the semi-finished battery within 80 seconds, then putting the semi-finished battery into cooling water with the constant temperature of 10 ℃, wherein the water level is 1 cm lower than the upper cover of the battery, and standing the semi-finished battery in the water for at least 25 minutes.
Furthermore, circulating water is needed in the battery formation process, and the temperature of the circulating water is between 20 and 45 ℃; sixthly, stopping circulating water; and when the operation is twenty-two, discharging the circulating water in the formation equipment.
The invention has the beneficial effects that: the battery formation process achieves the purposes of saving cost, reducing the weight of the battery and improving the low-temperature performance of the battery by adjusting the formation process and the material preparation process; the charging process used by the invention has the advantages that the current is fixed according to the area of a product to be formed, the charging and discharging amounts are fixed according to the amount of an active material, and the hydrogen evolution voltage is always taken as a control key point, so that the porosity of the cathode of the battery is ensured to the greater extent, and the charging process is more scientific and reasonable than other charging processes determined according to the charging time. In addition, the meteorological silica is adopted, is more uniform through high-speed cutting, has the average particle size of 0.1-0.2 mu m, and cannot be fused into micropores on the surface of the polar plate, so that the surface of the polar plate is not affected, and the application has the characteristic of high low-temperature discharge capacity; after the electrolyte is heated, sulfuric acid and lead oxide in the electrolyte are mixed and converted into lead sulfate, the lead sulfate is an exothermic reaction, the exothermic temperature rises to 80 ℃, and carbon materials in the polar plate are oxidized and deteriorated at high temperature. The electrolyte is added at low temperature, and then is placed in the cooling water for standing, and the time exceeds the heating time, so that the influence on the carbon material in the polar plate is minimum, and the integrity of the polar plate material is ensured to the maximum extent, so that the electrode plate has the characteristic of high low-temperature capacity, and the service life of the material is prolonged, so that the technical scheme of the electrode plate has an effect of prolonging the service life of the product; the invention adopts the constant temperature effect mainly in the formation stage, the battery temperature is always controlled between 20 and 45 ℃, the charging current utilization rate is highest in the temperature state, and the material in the electrode plate can not be oxidized, so the battery produced by the technical scheme of the application has the characteristics of high low-temperature capacity and long service life.
Detailed Description
Example 1
Before the formation of the battery, a battery semi-finished product needs to be manufactured for standby: the positive plate and the negative plate are manufactured by lead powder ball milling, grid casting, lead powder paste mixing, lead powder coating and pole plate curing, the positive plate and the negative plate are separated by AGM glass fiber cotton and assembled into a single lead-acid storage battery according to capacity, the positive electrode and the negative electrode are respectively connected in parallel, the voltage of each cell is nominal 2V, a single number of cells are connected in series according to needs to obtain a high-voltage battery level group, then the cells are connected in series after a battery shell made of ABS is installed, and then the semi-finished battery is obtained for standby after being sealed by a middle cover.
Preparing a master batch for later use:
raw materials: selecting industrial-grade silicon dioxide powder produced by a gas phase method, wherein the average particle size of the industrial-grade silicon dioxide powder is 0.17 mu m, the silicon dioxide content is more than 99.89%, and the industrial-grade silicon dioxide powder is dried at 105 ℃ for 2 hours to have a density of 50g/L and is in a hydrophobic state;
preparing equipment: the rotating speed is 4000 to 5000r/min, the volume is 800 kg;
the configuration method comprises the following steps: adding 600kg of deionized water into the equipment, wherein the rotating speed of the equipment is 4000r/min, adding meteorological silica (namely 90kg of meteorological silica) with the weight ratio of the ionic water of 15 percent by using a vacuum conveying device, increasing the rotating speed to 4800r/min, shearing at high speed for 20-30 minutes, and adjusting the temperature of cooling water to be 20-35 ℃. Sodium hydroxide (i.e., 10 g) was added in an amount of 0.0016% by weight of deionized water, and polyaspartic acid sodium salt (i.e., 6 g) was added in an amount of 0.001% by weight of deionized water, followed by stirring for 3 to 5 minutes.
Preparing dilute sulfuric acid for later use:
raw materials: analytical grade H2SO4
The configuration method comprises the following steps: according to 36%: 64% acid water mass ratio, analyzing the raw material to pure grade H2SO4Slowly adding into water to control the temperature within 25 + -5 deg.C, and adjusting the density of dilute sulfuric acid to 1.265g/cm3Anhydrous sodium sulfate with the total mass of 0.8 percent is added, the mixture is stirred for 20 minutes, and the preparation of dilute sulfuric acid is finished.
Preparing electrolyte for later use:
mixing the prepared dilute sulfuric acid and the prepared masterbatch according to the mass ratio of 100: 3.5 adding the mixture into a stirring tank and mixing for 30 minutes to obtain electrolyte; then cooling, cooling temperature: if the using temperature is less than or equal to 15 ℃, cooling the electrolyte to 10 +/-1 ℃, and if the room temperature is more than or equal to 16 ℃, cooling the electrolyte to 1 +/-1 ℃; the electrolyte after cooling is standby, and indoor temperature is different, and the problem of electrolyte also needs to be correspondingly adjusted, because if indoor temperature is high, the temperature of electrolyte is also high, and electrolyte can produce a large amount of exothermic reactions after adding the battery this moment, can damage the polar plate structure, causes the battery low temperature capacity to reduce.
Further, before the step one, the method further comprises the steps of: the prepared electrolyte is mixed according to the proportion of 1Ah/3.66g/cm3Adding the product of the concentrated acid quantity standard and the rated capacity of the product into the semi-finished battery within 80 seconds, then putting the semi-finished battery into cooling water with the constant temperature of 10 ℃, wherein the water level is 1 cm lower than the upper cover of the battery, and standing the semi-finished battery in the water for at least 25 minutes.
The battery formation process comprises the following steps:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2a/4.1A, filling 1.3 percent of the active material electrochemical equivalent of the positive plate; the purpose of this step is to reduce the polarization voltage to prevent gassing caused by too fast a voltage rise during large current charging;
step two: charging current 1m28.24A, filling 52 percent of the electrochemical equivalent of the active substance of the positive plate;
step three: standing for 30 minutes to balance the concentration of electrolyte in the lead-acid storage battery, playing the aim of rehydration and providing enough sulfate ions for secondary formation;
step four: charging current 1m28.24A, charging 11.6 percent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is discharged by 5.1 percent at the A/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step six: charging current 1m28.24A, charging 5.4 percent of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is 6.3 percent at a/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step eight: charging current 1m28.24A, charging 6.4 percent of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2a/20.6A, discharging 7.5% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m28.24A, charging 7.6 percent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eleven; discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is discharged by 8.7 percent at the A/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step twelve: charging current 1m2Filling 5.8% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step thirteen: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 42.2 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
fourteen steps: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 58.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step fifteen: charging current 1m2Charging 44.5% of the active material of the positive plate in electrochemical equivalent, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2a/20.6A, discharging 25% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is 5.6 percent at 20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 seconds;
eighteen steps: charging current 1m2Filling 17.5 percent of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
nineteen steps: charging current 1m2The electrochemical equivalent of the active substance filled into the positive plate is 42.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
twenty steps: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 58.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
twenty one: charging current 1m2Charging 24.5% of the active material of the positive plate into the electrochemical equivalent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m20.62A, charged with 2.6% of the electrochemical equivalent of the positive plate active material, the cell voltage was automatically measured in real time, and the measurement was recorded every 10 minutes.
Furthermore, circulating water is needed in the battery formation process, and the temperature of the circulating water is between 20 and 45 ℃; sixthly, stopping circulating water; and when the operation is twenty-two, discharging the circulating water in the formation equipment.
Furthermore, the current precision of the formation equipment used in the formation process is +/-0.03% A, the voltage precision is +/-0.02% V, the total voltage of a single loop is 310V, the charging rated current is 15A, and the discharging rated current is 20A; the total volume ratio of the formation tank to the required formation quantity of batteries is 3: 1.
further, referring to the voltage data recorded in the seventeenth step, selecting and recording the average voltage at 10.3V/time, dividing different gears according to the requirements that the error of the discharge time is within 20 seconds and the error of the discharge voltage is within 0.15V, and naming the gears as 1, 2 and 3 … … 10. And in addition, according to the sorted batteries in each grade, the open-circuit voltage is measured after the batteries stand still for 24 hours, and the single batteries with the open-circuit voltage error less than or equal to 0.02V are divided into the batteries in the same group.
Example 2
Before the formation of the battery, a battery semi-finished product needs to be manufactured for standby: the positive plate and the negative plate are manufactured by lead powder ball milling, grid casting, lead powder paste mixing, lead powder coating and pole plate curing, the positive plate and the negative plate are separated by AGM glass fiber cotton and assembled into a single lead-acid storage battery according to capacity, the positive electrode and the negative electrode are respectively connected in parallel, the voltage of each cell is nominal 2V, a single number of cells are connected in series according to needs to obtain a high-voltage battery level group, then the cells are connected in series after a battery shell made of ABS is installed, and then the semi-finished battery is obtained for standby after being sealed by a middle cover.
Preparing master batch for later use;
raw materials: selecting industrial-grade silicon dioxide powder produced by a gas phase method, wherein the average particle size of the industrial-grade silicon dioxide powder is 0.13 mu m, the silicon dioxide content is more than 99.5%, and the industrial-grade silicon dioxide powder is dried at 105 ℃ for 2 hours to have a density of 50g/L and is in a hydrophobic state;
preparing equipment: the rotating speed is 4000 to 5000r/min, the volume is 800 kg;
the configuration method comprises the following steps: 600kg of deionized water is added into the equipment, the rotating speed of the equipment is 4000r/min, meteorological silica (60 kg of meteorological silica) with the weight ratio of the ionic water of 10 percent is added by a vacuum conveying device, the rotating speed is increased to 4800r/min, high-speed shearing is carried out for 20 to 30 minutes, and cooling water is adjusted until the colloid temperature is 20 to 35 ℃. Sodium hydroxide (i.e., 10 g) was added in an amount of 0.0016% by weight of deionized water, and polyaspartic acid sodium salt (i.e., 6 g) was added in an amount of 0.001% by weight of deionized water, followed by stirring for 3 to 5 minutes.
Preparing dilute sulfuric acid for later use:
raw materials: analytical grade H2SO4
The configuration method comprises the following steps: according to 36%: 64% acid water mass ratio, analyzing the raw material to pure grade H2SO4Slowly adding into water to control the temperature within 25 + -5 deg.C, and adjusting the density of dilute sulfuric acid to 1.265g/cm3Anhydrous sodium sulfate with the total mass of 0.8 percent is added, the mixture is stirred for 20 minutes, and the preparation of dilute sulfuric acid is finished.
Preparing electrolyte for later use;
mixing the prepared dilute sulfuric acid and the prepared masterbatch according to the mass ratio of 100: 3.5 adding the mixture into a stirring tank and mixing for 30 minutes to obtain electrolyte; then cooling, cooling temperature: if the using temperature is less than or equal to 15 ℃, cooling the electrolyte to 10 +/-1 ℃, and if the room temperature is more than or equal to 16 ℃, cooling the electrolyte to 1 +/-1 ℃; the electrolyte after cooling is standby, and indoor temperature is different, and the problem of electrolyte also needs to be correspondingly adjusted, because if indoor temperature is high, the temperature of electrolyte is also high, and electrolyte can produce a large amount of exothermic reactions after adding the battery this moment, can damage the polar plate structure, causes the battery low temperature capacity to reduce.
Further, before the step one, the method further comprises the steps of: the prepared electrolyte is mixed according to the proportion of 1Ah/3.66g/cm3Adding the product of the concentrated acid quantity standard and the rated capacity of the product into the semi-finished battery within 80 seconds, then putting the semi-finished battery into cooling water with the constant temperature of 5 ℃, wherein the water level is 1 cm lower than the upper cover of the battery, and standing the semi-finished battery in the water for at least 25 minutes.
The battery after leaving the water area was charged within 30 minutes, during which the charging clip was connected, the charging stand was filled with cooling water, and the excess electrolyte on the surface was treated.
A battery formation step:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2Filling 0.3 percent of the active material of the positive plate in an electrochemical equivalent; the purpose of this step is to reduce the polarization voltage to prevent large current chargingWhen the voltage rises too fast, gas is generated;
step two: charging current 1m2Filling 40% of the active material of the positive plate in an electrochemical equivalent;
step three: standing for 30 minutes to balance the concentration of electrolyte in the lead-acid storage battery, playing the aim of rehydration and providing enough sulfate ions for secondary formation;
step four: charging current 1m2Charging 10% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2a/25A, discharging 4% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step six: charging current 1m2Charging 3% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2a/15A, discharging 4% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eight: charging current 1m2Charging 4% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2a/15A, discharging 5% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m2Charging 5% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eleven; discharge current 1m2a/15A, discharging 6% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twelve: charging current 1m2/8A, filling positive plate active materialThe battery voltage is automatically measured in real time at 4% of the electrochemical equivalent, and the measured value is recorded every 10 minutes;
step thirteen: charging current 1m2Charging 20% of the active material electrochemical equivalent of the positive plate, automatically measuring the battery voltage in real time, and recording the measured value every 10 minutes;
fourteen steps: charging current 1m2Charging 30% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step fifteen: charging current 1m2Charging 30% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2a/15A, discharging 15% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2a/15A, discharging 3% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 seconds;
eighteen steps: charging current 1m2The battery voltage is automatically measured in real time after 10 percent of the electrochemical equivalent of the active substance of the positive plate is charged, and the measured value is recorded every 10 minutes;
nineteen steps: charging current 1m2Charging 30% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
twenty steps: charging current 1m2Charging 20% of the active material electrochemical equivalent of the positive plate, automatically measuring the battery voltage in real time, and recording the measured value every 10 minutes;
twenty one: charging current 1m2Charging 15% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m20.2A, charging 1% of active material of positive plate with real-time automationThe cell voltage was measured and the measurements were recorded every 10 minutes.
Furthermore, circulating water is needed in the battery formation process, and the temperature of the circulating water is between 25 and 45 ℃; sixthly, stopping circulating water; and when the operation is twenty-two, discharging the circulating water in the formation equipment.
Furthermore, the current precision of the formation equipment used in the formation process is +/-0.03% A, the voltage precision is +/-0.02% V, the total voltage of a single loop is 310V, the charging rated current is 15A, and the discharging rated current is 20A; the total volume ratio of the formation tank to the required formation quantity of batteries is 3: 1.
further, referring to the voltage data recorded in the seventeenth step, selecting and recording the average voltage at 10.3V/time, dividing different gears according to the requirements that the error of the discharge time is within 20 seconds and the error of the discharge voltage is within 0.15V, and naming the gears as 1, 2 and 3 … … 10. And in addition, according to the sorted batteries in each grade, the open-circuit voltage is measured after the batteries stand still for 24 hours, and the single batteries with the open-circuit voltage error less than or equal to 0.02V are divided into the batteries in the same group.
Example 3
Before the formation of the battery, a battery semi-finished product needs to be manufactured for standby: the positive plate and the negative plate are manufactured by lead powder ball milling, grid casting, lead powder paste mixing, lead powder coating and pole plate curing, the positive plate and the negative plate are separated by AGM glass fiber cotton and assembled into a single lead-acid storage battery according to capacity, the positive electrode and the negative electrode are respectively connected in parallel, the voltage of each cell is nominal 2V, a single number of cells are connected in series according to needs to obtain a high-voltage battery level group, then the cells are connected in series after a battery shell made of ABS is installed, and then the semi-finished battery is obtained for standby after being sealed by a middle cover.
Preparing master batch for later use;
raw materials: selecting industrial-grade silicon dioxide powder produced by a gas phase method, wherein the average particle size of the industrial-grade silicon dioxide powder is 0.2 mu m, the silicon dioxide content is more than 99.99 percent, and the industrial-grade silicon dioxide powder is dried at 105 ℃ for 2 hours to have a density of 50g/L and is in a hydrophobic state;
preparing equipment: the rotating speed is 4000 to 5000r/min, the volume is 800 kg;
the configuration method comprises the following steps: 600kg of deionized water is added into the equipment, the rotating speed of the equipment is 4000r/min, meteorological silica (60 kg of meteorological silica) with the weight ratio of the ionic water of 10 percent is added by a vacuum conveying device, the rotating speed is increased to 4800r/min, high-speed shearing is carried out for 20 to 30 minutes, and cooling water is adjusted until the colloid temperature is 20 to 35 ℃. Sodium hydroxide (i.e., 10 g) was added in an amount of 0.0016% by weight of deionized water, and polyaspartic acid sodium salt (i.e., 6 g) was added in an amount of 0.001% by weight of deionized water, followed by stirring for 3 to 5 minutes.
Preparing dilute sulfuric acid for later use:
raw materials: analytical grade H2SO4
The configuration method comprises the following steps: according to 36%: 64% acid water mass ratio, analyzing the raw material to pure grade H2SO4Slowly adding into water to control the temperature within 25 + -5 deg.C, and adjusting the density of dilute sulfuric acid to 1.265g/cm3Anhydrous sodium sulfate with the total mass of 0.8 percent is added, the mixture is stirred for 20 minutes, and the preparation of dilute sulfuric acid is finished.
Preparing electrolyte for later use;
mixing the prepared dilute sulfuric acid and the prepared masterbatch according to the mass ratio of 100: 3.5 adding the mixture into a stirring tank and mixing for 30 minutes to obtain electrolyte; then cooling, cooling temperature: if the using temperature is less than or equal to 15 ℃, cooling the electrolyte to 10 +/-1 ℃, and if the room temperature is more than or equal to 16 ℃, cooling the electrolyte to 1 +/-1 ℃; the electrolyte after cooling is standby, and indoor temperature is different, and the problem of electrolyte also needs to be correspondingly adjusted, because if indoor temperature is high, the temperature of electrolyte is also high, and electrolyte can produce a large amount of exothermic reactions after adding the battery this moment, can damage the polar plate structure, causes the battery low temperature capacity to reduce.
Further, before the step one, the method further comprises the steps of: the prepared electrolyte is mixed according to the proportion of 1Ah/3.66g/cm3Adding the product of the concentrated acid quantity standard and the rated capacity of the product into the semi-finished battery within 80 seconds, then putting the semi-finished battery into cooling water with the constant temperature of 5 ℃, wherein the water level is 1 cm lower than the upper cover of the battery, and standing the semi-finished battery in the water for at least 25 minutes.
The battery after leaving the water area was charged within 30 minutes, during which the charging clip was connected, the charging stand was filled with cooling water, and the excess electrolyte on the surface was treated.
A battery formation step:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2Filling 3% of the active material of the positive plate in an electrochemical equivalent; the purpose of this step is to reduce the polarization voltage to prevent gassing caused by too fast a voltage rise during large current charging;
step two: charging current 1m214A, filling 60% of the active material electrochemical equivalent of the positive plate;
step three: standing for 30 minutes to balance the concentration of electrolyte in the lead-acid storage battery, playing the aim of rehydration and providing enough sulfate ions for secondary formation;
step four: charging current 1m2A 14A, charging 16% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2a/25A, discharging 8% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step six: charging current 1m2a/14A, charging 8% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2a/25A, discharging 9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eight: charging current 1m2a/14A, charging 9% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2a/25A, discharging 9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m2a/14A, charging 9% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eleven; discharge current 1m2a/25A, discharging 11% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twelve: charging current 1m2a/15A, charging 9% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step thirteen: charging current 1m2Filling 52% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
fourteen steps: charging current 1m2Filling 70% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step fifteen: charging current 1m2Filling 55% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2a/25A, discharging 35% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2a/25A, discharging 9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 seconds;
eighteen steps: charging current 1m2Charging 25% of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
nineteen steps: charging current 1m2Filling 55% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
twenty steps: charging current 1m2Filling 70% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
twenty one: charging deviceElectric current 1m2a/10A, charging 35% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m2The cell voltage was automatically measured in real time with charging 6% of the electrochemical equivalent of the positive plate active material at 1.5A, and the measurement was recorded every 10 minutes.
Furthermore, circulating water is needed in the battery formation process, and the temperature of the circulating water is between 25 and 45 ℃; sixthly, stopping circulating water; and when the operation is twenty-two, discharging the circulating water in the formation equipment.
Furthermore, the current precision of the formation equipment used in the formation process is +/-0.03% A, the voltage precision is +/-0.02% V, the total voltage of a single loop is 310V, the charging rated current is 15A, and the discharging rated current is 20A; the total volume ratio of the formation tank to the required formation quantity of batteries is 3: 1.
further, referring to the voltage data recorded in the seventeenth step, selecting and recording the average voltage at 10.3V/time, dividing different gears according to the requirements that the error of the discharge time is within 20 seconds and the error of the discharge voltage is within 0.15V, and naming the gears as 1, 2 and 3 … … 10. And in addition, according to the sorted batteries in each grade, the open-circuit voltage is measured after the batteries stand still for 24 hours, and the single batteries with the open-circuit voltage error less than or equal to 0.02V are divided into the batteries in the same group.
The prior art comprises the following steps:
before the formation of the battery, a battery semi-finished product needs to be manufactured for standby: the positive plate and the negative plate are manufactured by lead powder ball milling, grid casting, lead powder paste mixing, lead powder coating and pole plate curing, the positive plate and the negative plate are separated by AGM glass fiber cotton and assembled into a single lead-acid storage battery according to capacity, the positive electrode and the negative electrode are respectively connected in parallel, the voltage of each cell is nominal 2V, a single number of cells are connected in series according to needs to obtain a high-voltage battery level group, then the cells are connected in series after a battery shell made of ABS is installed, and then the semi-finished battery is obtained for standby after being sealed by a middle cover.
Preparing master batch for later use;
raw materials: selecting industrial-grade silicon dioxide powder produced by a gas phase method, wherein the average particle size of the industrial-grade silicon dioxide powder is 0.2 mu m, the silicon dioxide content is more than 99%, and the industrial-grade silicon dioxide powder is dried at 105 ℃ for 2 hours to have a density of 50g/L and is in a hydrophobic state;
preparing equipment: the rotating speed is 3000-4000 r/min, and the volume is 800 kg;
the configuration method comprises the following steps: 600kg of deionized water is added into the equipment, the rotating speed of the equipment is 3500r/min, meteorological silica (60 kg of meteorological silica) with the weight ratio of the ionic water of 10 percent is added by a vacuum conveying device, the rotating speed is increased to 3800r/min, the high-speed shearing is carried out for 20 to 30 minutes, and the cooling water is adjusted to the colloid temperature of 20 to 35 ℃. Sodium hydroxide (i.e., 10 g) was added in an amount of 0.0014% by weight of deionized water, and polyaspartic acid sodium salt (i.e., 6 g) was added in an amount of 0.001% by weight of deionized water, followed by stirring for 3 to 5 minutes.
Preparing dilute sulfuric acid for later use:
raw materials: analytical grade H2SO4
The configuration method comprises the following steps: according to 36%: 64% acid water mass ratio, analyzing the raw material to pure grade H2SO4Slowly adding into water to control the temperature within 25 + -5 deg.C, and adjusting the density of dilute sulfuric acid to 1.265g/cm3Anhydrous sodium sulfate with the total mass of 0.8 percent is added, the mixture is stirred for 20 minutes, and the preparation of dilute sulfuric acid is finished.
Preparing electrolyte for later use;
mixing the prepared dilute sulfuric acid and the prepared masterbatch according to the mass ratio of 100: 3.0 adding the mixture into a stirring tank and mixing for 30 minutes to obtain electrolyte; then cooling and cooling the temperature.
Further, before the step one, the method further comprises the steps of: the prepared electrolyte is mixed according to the proportion of 1Ah/3.66g/cm3The product of the concentrated acid amount standard and the rated capacity of the product is added into the semi-finished battery within 70 seconds, and the battery added with the electrolyte is kept still in a water area for 10 minutes.
The battery after leaving the water area was charged within 60 minutes, during which the charging clip was connected, the charging stand was filled with cooling water, and the excess electrolyte on the surface was treated.
A battery formation step:
the method comprises the following steps: the current at the initial charging stage is 0.05C/3h, and the time interval is recorded once every 10 minutes;
step two, charging current is 0.15C/6h, and the time interval is recorded once every 10 minutes;
step three: standing for 60 min;
step four: the charging current is 0.2C/10h, and the time interval is recorded once every 10 minutes;
step five: the charging current is 0.3C/3h, and the time interval is recorded once every 10 minutes;
step six: the discharge current is 0.3C/0.5h, and the time interval is recorded once every 10 minutes;
step seven: the charging current is 0.2C/10h, and the time interval is recorded once every 10 minutes;
step eight: the charging current is 0.3C/3h, and the time interval is recorded once every 10 minutes;
step nine: the discharge current is 0.3C/0.8h, and the recording time interval is once every 10 minutes;
step ten: the charging current is 0.2C/10h, and the time interval is recorded once every 10 minutes;
step eleven: the charging current is 0.3C/3h, and the time interval is recorded once every 10 minutes;
step twelve: the discharge current is 0.3C/1h, and the time interval is recorded once every 10 minutes;
step thirteen: the charging current is 0.2C/10h, and the time interval is recorded once every 10 minutes;
fourteen steps: the charging current is 0.3C/3h, and the time interval is recorded once every 10 minutes;
step fifteen: the charging current is 0.1C/8h, and the time interval is recorded once every 10 minutes;
sixthly, the steps are as follows: the discharge current is 0.5C/1.9h, and the time interval is recorded once every 10 minutes;
seventeen steps: the discharge current is 0.5C/0.2h, and the recording time interval is once every 10 seconds;
eighteen steps: the charging current is 0.2C/10h, and the time interval is recorded once every 10 minutes;
nineteen steps: the charging current is 0.3C/2h, and the time interval is recorded once every 10 minutes;
twenty steps: the charging current is 0.2C/2h, and the time interval is recorded once every 10 minutes;
twenty one: the charging current is 0.1C/2h, and the time interval is recorded once every 10 minutes;
step twenty-two: the charging current is 0.023C/5h, and the time interval is recorded once every 10 minutes;
controlling the temperature of circulating water in the formation charging process in the formation stage: within 20-55 ℃, discharging the circulating water after twenty-two 2 hours of the operation steps.
The battery formation process steps of examples 1, 2 and 3 were performed twice and compared with the battery comprehensive parameters of the formation process in the prior art, and the comparison results were as follows:
wherein, the detection equipment that charges, discharges: a Jiangsu Jinfan microcomputer storage battery comprehensive parameter detector;
the model is as follows: uC-ZS 08
High low temperature check out test set: a Taizhou power electronics device;
the model is as follows: XGDW-800C
The model is as follows: XGDW-800C
As can be seen from the above table, the weight of the samples using the process of the present invention was 6.05kg, which is a 5.39% reduction over the prior art. Wherein the average capacity at the low temperature of-18 ℃ reaches 14.97Ah, the average energy density is 42.02Wh/kg, Cb2 is more than Cb 1101.95, the cycle life of the battery manufactured by the formation process is 387 times and 100 percent DOD through tests, the estimated service life is 32.2 months, and the index exceeds the requirement in the new national standard GB/T32620.1-2016.
Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present invention and not to limit the same; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (7)
1. A low-temperature battery formation process is characterized by comprising the following steps:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2/2A-1m2Filling the positive plate active substance with the electrochemical equivalent of 0.3-3% in the solution A;
step two: charging current 1m2/5A-1m214A, filling 40-60% of the active material of the positive plate in an electrochemical equivalent;
step three: standing for 30 minutes;
step four: charging current 1m2/5A-1m2Charging 8% -12% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2/20.6A-1m2a/25A, discharging 3-8% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step six: charging current 1m2/4A-1m2Filling 3-8% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2/15A-1m2a/25A, discharging 4-9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eight: charging current 1m2/4A-1m2Charging 4% -9% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2/15A-1m2a/25A, discharging 5-9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m2/4A-1m2Filling 5-9% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eleven; discharge current 1m2/15A-1m2a/25A, discharging 6-11% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twelve: charging current 1m2/8A-1m2Filling 5.8-9% of active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step thirteen: charging current 1m2/5A-1m2Filling 20-52% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
fourteen steps: charging current 1m2/4A-1m2Filling 30-70% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
step fifteen: charging current 1m2/3A-1m2Filling 30-55% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2/15A-1m2a/25A, discharging 15-35% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2/15A-1m2a/25A, discharging 3-9% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 seconds;
eighteen steps: charging current 1m2/7A-1m2Charging 10-25% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
nineteen steps: charging current 1m2/5A-1m2/11A, charging positive plate active materialChanging the equivalent to 30-55%, automatically measuring the battery voltage in real time, and recording the measured value every 10 minutes;
twenty steps: charging current 1m2/3A-1m2a/10A, charging 20-70% of the active material electrochemical equivalent of the positive plate, automatically measuring the voltage of the battery in real time, and recording a measured value every 10 minutes;
twenty one: charging current 1m2/2A-1m2Charging 15-35% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m2/0.2A-1m2and/1.5A, charging 1-6% of the active material electrochemical equivalent of the positive plate, automatically measuring the battery voltage in real time, and recording the measured value every 10 minutes.
2. The low temperature battery formation process of claim 1, comprising the steps of:
the method comprises the following steps: the battery is preliminarily charged with the charging current of 1m2a/4.1A, filling 1.3 percent of the active material electrochemical equivalent of the positive plate;
step two: charging current 1m28.24A, filling 52 percent of the electrochemical equivalent of the active substance of the positive plate;
step three: standing for 30 minutes;
step four: charging current 1m28.24A, charging 11.6 percent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step five: discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is discharged by 5.1 percent at the A/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step six: charging current 1m28.24A, charging 5.4 percent of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step seven: discharge current 1m2/20.6A, 6.3% of the electrochemical equivalent of the positive plate active material was discharged in real timeAutomatically measuring the battery voltage, recording the measured value every 10 minutes;
step eight: charging current 1m28.24A, charging 6.4 percent of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step nine: discharge current 1m2a/20.6A, discharging 7.5% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step ten: charging current 1m28.24A, charging 7.6 percent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step eleven; discharge current 1m2The electrochemical equivalent of the active substance of the positive plate is discharged by 8.7 percent at the A/20.6A, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step twelve: charging current 1m2Filling 5.8% of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step thirteen: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 42.2 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
fourteen steps: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 58.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
step fifteen: charging current 1m2Charging 44.5% of the active material of the positive plate in electrochemical equivalent, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
sixthly, the steps are as follows: discharge current 1m2a/20.6A, discharging 25% of the electrochemical equivalent of the active substance of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
seventeen steps: discharge current 1m2/20.6A, 5.6% of the electrochemical equivalent of the positive plate active material was discharged, and the cell voltage was automatically measured in real time per unit timeRecord one measurement for 10 seconds;
eighteen steps: charging current 1m2Filling 17.5 percent of the active material of the positive plate into the battery, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
nineteen steps: charging current 1m2The electrochemical equivalent of the active substance filled into the positive plate is 42.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
twenty steps: charging current 1m2The electrochemical equivalent of the active substance of the positive plate is charged to 58.3 percent, the voltage of the battery is automatically measured in real time, and the measured value is recorded every 10 minutes;
twenty one: charging current 1m2Charging 24.5% of the active material of the positive plate into the electrochemical equivalent of the active material of the positive plate, automatically measuring the voltage of the battery in real time, and recording the measured value every 10 minutes;
step twenty-two: charging current 1m20.62A, charged with 2.6% of the electrochemical equivalent of the positive plate active material, the cell voltage was automatically measured in real time, and the measurement was recorded every 10 minutes.
3. The low temperature battery formation process of claim 1 or 2, further comprising, before step one, the steps of: preparing a master batch;
raw materials: selecting industrial-grade silicon dioxide powder produced by a gas phase method, wherein the average particle size of the industrial-grade silicon dioxide powder is 0.1-0.2 mu m, the silicon dioxide content is more than 99.5% -99.99%, and the industrial-grade silicon dioxide powder is dried at 105 ℃ for 2 hours, has the density of 50g/L and is in a hydrophobic state;
preparing equipment: the rotating speed is 4000 to 5000r/min, the volume is 800 kg;
the configuration method comprises the following steps: adding 600kg of deionized water into the equipment, wherein the rotating speed of the equipment is 4000r/min, adding meteorological silica with the weight ratio of the ionized water being 15% by using a vacuum conveying device, increasing the rotating speed to 4800r/min, shearing at high speed for 20-30 minutes, and adjusting the temperature of cooling water to 20-35 ℃. Adding sodium hydroxide with the weight ratio of the deionized water being 0.0016 percent, then adding polyaspartic acid ammonia sodium salt with the weight ratio of the deionized water being 0.001 percent, and stirring for 3 to 5 minutes.
4. The low temperature battery formation process of claim 3, further comprising, before step one, the steps of: preparing dilute sulfuric acid;
raw materials: analytical grade H2SO4
The configuration method comprises the following steps: according to 36%: 64% acid water mass ratio, analyzing the raw material to pure grade H2SO4Slowly adding into water to control the temperature within 25 + -5 deg.C, and adjusting the density of dilute sulfuric acid to 1.265g/cm3Anhydrous sodium sulfate with the total mass of 0.8 percent is added, the mixture is stirred for 20 minutes, and the preparation of dilute sulfuric acid is finished.
5. The low temperature battery formation process of claim 4, further comprising, before step one, the steps of: preparing electrolyte;
adding the prepared dilute sulfuric acid and the prepared masterbatch into a stirring tank according to the mass ratio of 100: 3.5, and mixing for 30 minutes to obtain electrolyte; then cooling, cooling temperature: if the using temperature is less than or equal to 15 ℃, cooling the electrolyte to 10 +/-1 ℃, and if the room temperature is more than or equal to 16 ℃, cooling the electrolyte to 1 +/-1 ℃; and cooling the electrolyte for later use.
6. The low temperature battery formation process of claim 5, further comprising, before step one, the steps of: the prepared electrolyte is mixed according to the proportion of 1Ah/3.66g/cm3Adding the product of the concentrated acid quantity standard and the rated capacity of the product into the semi-finished battery within 80 seconds, then putting the semi-finished battery into cooling water with the constant temperature of 10 ℃, wherein the water level is 1 cm lower than the upper cover of the battery, and standing the semi-finished battery in the water for at least 25 minutes.
7. The low-temperature battery formation process according to claim 1 or 2, wherein circulating water is required in the battery formation process, and the temperature of the circulating water is between 20 ℃ and 45 ℃; sixthly, stopping circulating water; and when the operation is twenty-two, discharging the circulating water in the formation equipment.
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