CN109437335A - A kind of method of explosion method synthesis NCA battery material - Google Patents
A kind of method of explosion method synthesis NCA battery material Download PDFInfo
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- CN109437335A CN109437335A CN201811301789.9A CN201811301789A CN109437335A CN 109437335 A CN109437335 A CN 109437335A CN 201811301789 A CN201811301789 A CN 201811301789A CN 109437335 A CN109437335 A CN 109437335A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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Abstract
The present invention relates to a kind of methods of explosion method synthesis NCA battery material, add water that mixed solution is made to nickel source, cobalt source and silicon source by elder generation, it adds density balance instrumentality and precursor solution is made, the obtained composite explosives of detonator are added after going water, cooling in precursor solution heating, explosion ash is collected after ignition, through sieving, separation, drying, calcination process, be prepared object mutually uniformly, the stable NCA battery material of good dispersion, product thermochemical property between Nano grade, particle；Data show, the partial size of the NCA battery material is 50-100nm, nickeliferous, cobalt, three kinds of elements of aluminium molar ratio be 8:1.5:0.5, be suitable as anode material of lithium battery.Shock-synthesis technique of the present invention, process flow is simple, and high production efficiency is, it can be achieved that large-scale production.
Description
Technical field
The invention belongs to battery material technical fields, and in particular to a kind of method of explosion method synthesis NCA battery material.
Background technique
Lithium ion battery has that voltage is high, energy density is big, has extended cycle life, and operating temperature range is wide, pollution-free etc. excellent
Point makes it have broad application prospects in various aspects such as portable electronic device, electric car, space technology, national defense industry,
Especially under the fossil energy situation that increasingly valuableness, environmental pollution are on the rise, lithium ion battery is as a kind of green high-capacity
Battery becomes research hotspot in recent years.
Positive electrode is the important component of lithium ion battery, high Ni-based lithium-nickel-cobalt-oxygen binary material (LiNixCo1-xO2)
It is a kind of very attractive high-capacity battery positive electrode, especially in power battery field, LiNixCo1-xO2Binary material
It is either ideal positive electrode in terms of specific energy or power characteristic.However, due to LiNixCo1-xO2Binary material
Structural stability Shortcomings, especially overcharging and, there are safety issue, leading to its practicalization under the condition of high temperature
Seriously it is obstructed.To improve its thermal safety, usually in LiNixCo1-xO2Aluminium is mixed in binary material, forms nickel cobalt lithium aluminate ternary
Positive electrode (i.e. NCA material), not only increases the structural stability of binary material, and improve thermal safety, is made
Lithium-ions battery also there is very high reversible specific capacity (0.5C, 180rnAh/g or more) and good stable circulation performance,
But this method synthesis difficulty is big, technique requires complexity, stability poor, it is difficult to realize the large-scale commercial of NCA positive electrode
Production.
Summary of the invention
In order to solve the above problems existing in the present technology, simple, production efficiency that the present invention provides a kind of process flows
The method of high explosion method synthesis NCA battery material.The partial size of the NCA battery material of the preparation method synthesis is 50-
100nm, nickel, cobalt, three kinds of elements of aluminium molar ratio be 8:1.5:0.5.
The technical scheme adopted by the invention is as follows:
A kind of method of explosion method synthesis NCA battery material, includes the following steps:
(1) taking nickel source, cobalt source and silicon source respectively and controlling the mass ratio of nickel source, cobalt source and silicon source is 0.732-0.789:
0.132-0.148:0.063-0.078 is sufficiently mixed uniformly, deionized water is added, obtains mixed solution after mixing；
(2) density balance instrumentality is added in Xiang Suoshu mixed solution, precursor solution is made；
(3) step (2) described precursor solution is subjected to heating concentration, it is cooling, concentrate is obtained, is added in Xiang Suoshu concentrate
Enter detonator and composite explosives are made；
(4) step (3) described composite explosives are ignited, after the completion of explosive reaction, collects the explosion ash of generation, successively
Through sieving, separation, drying, calcination process to get the NCA battery material.
The nickel source is six water nickel nitrates and/or nickelic oxide, and the cobalt source is cobalt nitrate hexahydrate and/or six water protochlorides
Cobalt, source of aluminium are nine water aluminum nitrates.
In step (1), the ratio between the quality of deionized water and the gross mass of nickel source, cobalt source and silicon source three 0.5- is added
0.67:0.5-0.33。
In step (2), the density balance instrumentality is azo-compound, sulfonyl hydrazines compound, nitroso compound
One or more of mixture.
In step (2), the additive amount of the density balance instrumentality accounts for the 3%-10% of mixed solution quality.
In step (3), 2/3 that volume is original volume is concentrated into described in progress.
In step (3), the detonator is C3H6O6N6、C5H8O12N4、C7H5O8N5、C7H5O6N3、C6H3O7N3One of
Or several mixture.
The addition quality of the detonator accounts for the 1%-5% of concentrate quality.
The partial size of the sieving is 150-250 mesh.
In step (4), the temperature for carrying out the drying is 80-120 DEG C, and the time for carrying out the drying is 0.5-2h, into
The temperature of the row roasting is 700-800 DEG C, and the time for carrying out the roasting is 1-3h.
The invention has the benefit that
The method of explosion method synthesis NCA battery material of the present invention, adds water system to nickel source, cobalt source and silicon source by elder generation
Mixed solution, add density balance instrumentality and be made precursor solution, precursor solution heating go water, it is cooling after be added and draw
Composite explosives are made in detonator, and explosion ash is collected after ignition, through sieving, separation, drying, calcination process, be prepared object mutually uniformly,
The stable NCA battery material of good dispersion, product thermochemical property between Nano grade, particle；Data show, the NCA battery
The partial size of material be 50-100nm, nickeliferous, cobalt, three kinds of elements of aluminium molar ratio be 8:1.5:0.5, be suitable as lithium battery just
Pole material.Shock-synthesis technique of the present invention, process flow is simple, and high production efficiency is, it can be achieved that large-scale production.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
The present embodiment provides a kind of methods of explosion method synthesis NCA battery material, include the following steps:
(1) six water nickel nitrate of 0.732g is taken respectively, and nine water aluminum nitrate of 0.132g cobalt nitrate hexahydrate and 0.063g is sufficiently mixed
Uniformly, 0.927g deionized water is added, is uniformly mixed and obtains mixed solution；
(2) azodicarbonamide of 0.028g is added in Xiang Suoshu mixed solution, precursor solution is made；
(3) step (2) described precursor solution is carried out being heated to 100 DEG C, being concentrated by evaporation to volume is original volume
2/3rds, it is cooling, the C of 0.093g is added3H6O6N6, density is made (for 1.8g/cm3Composite explosives；The composite explosives
Performance index is as follows: QV(kJ/kg)=4024, T (DEG C)=3007, VD(m/s)=5284, PCJ(GPa)=8.60, V (L/kg)
=747.26；
(4) step (3) described composite explosives are suspended in specific destructor, the volume of device is 14.14m3, dress
It is set to a thickness of 5mm, radius 3m, the steel drum that volume is 14.14 cubic metres, inner wall posts ceramics, and ceramics are outer also to be pasted
There is the electro-insulating rubber of wiped clean；In use, plugging No. 8 commercial electric detonators one and sending out manufactured composite explosives pack, then will
It, which hangs, is fixed on the half of steel drum height at 2/3rds, connects conducting wire, by steel drum it is each into
Outlet is sealed to be shut with collection port valve, by exploder, the composite explosives with a small amount of detonator is ignited, explosion is anti-
After the completion of answering, explosion ash precipitating is waited to finish, using row of exhausting-gas hole removing exhaust gas, collects the explosion ash of generation, first cross 150 meshes, then
Gained sample is further separated with differential centrifugation machine, 80 DEG C of dry 2h, 700 DEG C of calcination process 3h are to get the NCA battery material
Material.
With x-ray fluorescence analysis (XPFS), from the x-ray fluorescence spectral line of every kind of element at its corresponding peak of characteristic wave long value
The content of element in nickel cobalt aluminium nano composite oxide powder (NCA battery material) of the value intensity quantitatively to measure synthesis, through examining
It surveys, NCA cell positive material is nickeliferous, the molar ratio of three kinds of cobalt, aluminium elements is 8:1.5:0.5.
Embodiment 2
The present embodiment provides a kind of methods of explosion method synthesis NCA battery material, include the following steps:
(1) six water nickel nitrate of 0.741g is taken respectively, and nine water aluminum nitrate of 0.138g cobalt nitrate hexahydrate and 0.072g is sufficiently mixed
Uniformly, 1.236g deionized water is added, is uniformly mixed and obtains mixed solution；
(2) the bis oxide benzene sulfonyl hydrazide of 0.038g is added in Xiang Suoshu mixed solution, precursor solution is made；
(3) step (2) described precursor solution is carried out being heated to 100 DEG C, being concentrated by evaporation to volume is original volume
2/3rds, it is cooling, the C of 0.012g is added5H8O12N4, it is 2.5g/cm that density, which is made,3Composite explosives；The composite explosives
Performance index is as follows: QV(kJ/kg)=4024, T (DEG C)=3007, VD(m/s)=5284, PCJ(GPa)=8.60, V (L/kg)
=747.26；
(4) step (3) described composite explosives are suspended in specific destructor, the volume of device is 14.14m3, dress
It is set to a thickness of 5mm, radius 3m, the steel drum that volume is 14.14 cubic metres, inner wall posts ceramics, and ceramics are outer also to be pasted
There is the electro-insulating rubber of wiped clean；In use, plugging No. 8 commercial electric detonators one and sending out manufactured composite explosives pack, then will
It, which hangs, is fixed on the half of steel drum height at 2/3rds, connects conducting wire, by steel drum it is each into
Outlet is sealed to be shut with collection port valve, by exploder, the composite explosives with a small amount of detonator is ignited, explosion is anti-
After the completion of answering, explosion ash precipitating is waited to finish, using row of exhausting-gas hole removing exhaust gas, collects the explosion ash of generation, first cross 250 meshes, then
Gained sample is further separated with differential centrifugation machine, 120 DEG C of dry 0.5h, 800 DEG C of calcination process 1h are to get the NCA electricity
Pond material.
Through detecting, NCA cell positive material is nickeliferous, the molar ratio of three kinds of cobalt, aluminium elements is 8:1.5:0.5.
Embodiment 3
The present embodiment provides a kind of methods of explosion method synthesis NCA battery material, include the following steps:
(1) 0.789g nickelic oxide is taken respectively, and nine water aluminum nitrate of six water cobalt chloride of 0.148g and 0.078g is sufficiently mixed
Uniformly, 1.726g deionized water is added, is uniformly mixed and obtains mixed solution；
(2) azodicarbonamide and bis oxide benzene sulfonyl hydrazide for 0.036g being added in Xiang Suoshu mixed solution are according to mass ratio
The mixture of 1:1 composition, is made precursor solution；
(3) step (2) described precursor solution is carried out being heated to 100 DEG C, being concentrated by evaporation to volume is original volume
2/3rds, it is cooling, the C of 0.018g is added7H5O6N3, it is 1.0g/cm that density, which is made,3Composite explosives；The composite explosives
Performance index is as follows: QV(kJ/kg)=4024, T (DEG C)=3007, VD(m/s)=5284, PCJ(GPa)=8.60, V (L/kg)
=747.26；
(4) step (3) described composite explosives are suspended in specific destructor, the volume of device is 14.14m3, dress
It is set to a thickness of 5mm, radius 3m, the steel drum that volume is 14.14 cubic metres, inner wall posts ceramics, and ceramics are outer also to be pasted
There is the electro-insulating rubber of wiped clean；In use, plugging No. 8 commercial electric detonators one and sending out manufactured composite explosives pack, then will
It, which hangs, is fixed on the half of steel drum height at 2/3rds, connects conducting wire, by steel drum it is each into
Outlet is sealed to be shut with collection port valve, by exploder, the composite explosives with a small amount of detonator is ignited, explosion is anti-
After the completion of answering, explosion ash precipitating is waited to finish, using row of exhausting-gas hole removing exhaust gas, collects the explosion ash of generation, first cross 200 meshes, then
Gained sample is further separated with differential centrifugation machine, 100 DEG C of dry 1.2h, 750 DEG C of calcination process 2h are to get the NCA electricity
Pond material.
Through detecting, NCA cell positive material is nickeliferous, the molar ratio of three kinds of cobalt, aluminium elements is 8:1.5:0.5.
Embodiment 4
The present embodiment provides a kind of methods of explosion method synthesis NCA battery material, include the following steps:
(1) six water nickel nitrate of 0.781g is taken respectively, and nine water aluminum nitrate of 0.144g cobalt nitrate hexahydrate and 0.078g is sufficiently mixed
Uniformly, 1.404g deionized water is added, is uniformly mixed and obtains mixed solution；
(2) the N'- dinitrosopentamethylenetetramine of 0.039g is added in Xiang Suoshu mixed solution, precursor solution is made；
(3) step (2) described precursor solution is carried out being heated to 100 DEG C, being concentrated by evaporation to volume is original volume
2/3rds, it is cooling, the C of 0.014g is added6H3O7N3, it is 1.0g/cm that density, which is made,3Composite explosives；The composite explosives
Performance index is as follows: QV(kJ/kg)=4024, T (DEG C)=3007, VD(m/s)=5284, PCJ(GPa)=8.60, V (L/kg)
=747.26；
(4) step (3) described composite explosives are suspended in specific destructor, the volume of device is 14.14m3, dress
It is set to a thickness of 5mm, radius 3m, the steel drum that volume is 14.14 cubic metres, inner wall posts ceramics, and ceramics are outer also to be pasted
There is the electro-insulating rubber of wiped clean；In use, plugging No. 8 commercial electric detonators one and sending out manufactured composite explosives pack, then will
It, which hangs, is fixed on the half of steel drum height at 2/3rds, connects conducting wire, by steel drum it is each into
Outlet is sealed to be shut with collection port valve, by exploder, the composite explosives with a small amount of detonator is ignited, explosion is anti-
After the completion of answering, explosion ash precipitating is waited to finish, using row of exhausting-gas hole removing exhaust gas, collects the explosion ash of generation, first cross 200 meshes, then
Gained sample is further separated with differential centrifugation machine, 100 DEG C of dry 1.2h, 780 DEG C of calcination process 1.5h are to get the NCA
Battery material.
Through detecting, NCA cell positive material is nickeliferous, the molar ratio of three kinds of cobalt, aluminium elements is 8:1.5:0.5.
Embodiment 5
The present embodiment provides a kind of methods of explosion method synthesis NCA battery material, include the following steps:
(1) six water nickel nitrate of 0.783g is taken respectively, and nine water aluminum nitrate of 0.135g cobalt nitrate hexahydrate and 0.071g is sufficiently mixed
Uniformly, 1.187g deionized water is added, is uniformly mixed and obtains mixed solution；
(2) azodicarbonamide of 0.034g is added in Xiang Suoshu mixed solution and N'- dinitrosopentamethylenetetramine is pressed
According to the mixture of mass ratio 1:1 composition, precursor solution is made；
(3) by step (2) described precursor solution be heated to 100 DEG C be concentrated by evaporation to volume be original three/
Two, it is cooling, the C of 0.025g is added6H3O7N3, it is 1.0g/cm that density, which is made,3Composite explosives；The performance of the composite explosives refers to
Number is as follows: QV(kJ/kg)=4024, T (DEG C)=3007, VD(m/s)=5284, PCJ(GPa)=8.60, V (L/kg)=
747.26；
(4) step (3) described composite explosives are suspended in specific destructor, the volume of device is 14.14m3, dress
It is set to a thickness of 5mm, radius 3m, the steel drum that volume is 14.14 cubic metres, inner wall posts ceramics, and ceramics are outer also to be pasted
There is the electro-insulating rubber of wiped clean；In use, plugging No. 8 commercial electric detonators one and sending out manufactured composite explosives pack, then will
It, which hangs, is fixed on the half of steel drum height at 2/3rds, connects conducting wire, by steel drum it is each into
Outlet is sealed to be shut with collection port valve, by exploder, the composite explosives with a small amount of detonator is ignited, explosion is anti-
After the completion of answering, explosion ash precipitating is waited to finish, using row of exhausting-gas hole removing exhaust gas, collects the explosion ash of generation, first cross 200 meshes, then
Gained sample is further separated with differential centrifugation machine, 100 DEG C of dry 1.5h, 720 DEG C of calcination process 2.5h are to get the NCA
Battery material.
Through detecting, NCA cell positive material is nickeliferous, the molar ratio of three kinds of cobalt, aluminium elements is 8:1.5:0.5.
The present invention is not limited to above-mentioned preferred forms, anyone can show that other are various under the inspiration of the present invention
The product of form, however, make any variation in its shape or structure, it is all that there is skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (10)
1. a kind of method of explosion method synthesis NCA battery material, which comprises the steps of:
(1) taking nickel source, cobalt source and silicon source respectively and controlling the mass ratio of nickel source, cobalt source and silicon source is 0.732-0.789:0.132-
0.148:0.063-0.078 is sufficiently mixed uniformly, deionized water is added, obtains mixed solution after mixing；
(2) density balance instrumentality is added in Xiang Suoshu mixed solution, precursor solution is made；
(3) step (2) described precursor solution is subjected to heating concentration, it is cooling, concentrate is obtained, is added and draws in Xiang Suoshu concentrate
Composite explosives are made in detonator；
(4) step (3) described composite explosives are ignited, after the completion of explosive reaction, collects the explosion ash of generation, successively pass through
Sieve, separation, dry, calcination process are to get the NCA battery material.
2. the method for explosion method synthesis NCA battery material according to claim 1, which is characterized in that the nickel source is six
Water nickel nitrate and/or nickelic oxide, the cobalt source are cobalt nitrate hexahydrate and/or six water cobalt chlorides, and source of aluminium is nine water nitre
Sour aluminium.
3. the method for explosion method synthesis NCA battery material according to claim 1, which is characterized in that in step (1), add
Enter the ratio between the quality of deionized water and the gross mass of nickel source, cobalt source and silicon source three 0.5-0.67:0.5-0.33.
4. the method for explosion method synthesis NCA battery material according to claim 1, which is characterized in that in step (2), institute
State the mixing that density balance instrumentality is one or more of azo-compound, sulfonyl hydrazines compound, nitroso compound
Object.
5. the method for explosion method synthesis NCA battery material according to claim 4, which is characterized in that in step (2), institute
The additive amount for stating density balance instrumentality accounts for the 3%-10% of mixed solution quality.
6. the method for explosion method synthesis NCA battery material according to claim 1, which is characterized in that in step (3), into
2/3 that volume is original volume is concentrated into described in row.
7. the method for explosion method synthesis NCA battery material according to claim 1, which is characterized in that in step (3), institute
Stating detonator is C3H6O6N6、C5H8O12N4、C7H5O8N5、C7H5O6N3、C6H3O7N3One or more of mixture.
8. the method for explosion method synthesis NCA battery material according to claim 7, which is characterized in that the detonator
Addition quality accounts for the 1%-5% of concentrate quality.
9. the method for explosion method synthesis NCA battery material according to claim 8, which is characterized in that the grain of the sieving
Diameter is 150-250 mesh.
10. the method for explosion method synthesis NCA battery material according to claim 1, which is characterized in that in step (4), into
The temperature of the row drying is 80-120 DEG C, and the time for carrying out the drying is 0.5-2h, and the temperature for carrying out the roasting is
700-800 DEG C, the time for carrying out the roasting is 1-3h.
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| CN201811301789.9A CN109437335B (en) | 2018-11-02 | 2018-11-02 | Method for synthesizing NCA battery material by explosion method |
| ZA2018/08081A ZA201808081B (en) | 2018-11-02 | 2018-11-29 | Method for synthesizing nca battery material by explosion method |
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| CN201811301789.9A CN109437335B (en) | 2018-11-02 | 2018-11-02 | Method for synthesizing NCA battery material by explosion method |
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Cited By (2)
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| CN110357151A (en) * | 2019-06-20 | 2019-10-22 | 安徽理工大学 | A kind of method of explosive synthesizing nano composite oxides |
| CN114507107A (en) * | 2022-03-02 | 2022-05-17 | 安徽理工大学 | Preparation method of special explosive for catalyst doping |
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| BE1029015B1 (en) * | 2021-07-27 | 2022-08-17 | Univ Anhui Sci & Technology | Process for synthesizing the NCA battery material by an explosive process |
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| CN109437335B (en) | 2020-11-03 |
| ZA201808081B (en) | 2021-07-28 |
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