CN103094579A - Method for preparing cathode material-lithium iron phosphate of lithium ion battery by utilizing steel slag - Google Patents
Method for preparing cathode material-lithium iron phosphate of lithium ion battery by utilizing steel slag Download PDFInfo
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Abstract
The invention relates to a method for preparing a cathode material-lithium iron phosphate of a lithium ion battery by utilizing steel slag. The method comprises the steps as follows: mixing the steel slag with a water-soluble carbon source compound water solution, and carrying out microwave heat treatment, reduction and magnetic separation to obtain a steel slag extract; reacting the steel slag extract with a mixed solution of diluted sulfuric acid, hydrogen peroxide and phosphoric acid, and extracting to obtain a calcium-free steel slag filter cake; adding lithium carbonate and the water-soluble carbon source compound water solution into the filter cake to obtain a precursor; and carrying out microwave sintering on the precursor to obtain the cathode material-lithium iron phosphate. Part of conventional raw materials are replaced with the steel slag as raw materials, so that the cost can be reduced by more than 30% and the obtained product is good in cycle performance; the conventional processes of ball-milling, drying and the like are removed, so that the process and the control operation are simple, inert gas does not need to be used in the sintering process, harmful gas such as nitrogen oxide and the like is not generated, the pollution is avoided, and the environment is protected; and the method is widely suitable for industrial production.
Description
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries, particularly relate to a kind of slag that utilizes and process preparation anode material for lithium-ion batteries LiFePO by microwave thermal
4Method.
Background technology
Along with the fast development of Chinese national economy, the contradiction of shortage of resources, ambient pressure is increasing.Developing Circulation Economy, raising resource utilization are the inevitable approach that solves current china natural resources, environmental constraints economic development, need to improve energetically the comprehensive utilization ratio of first resource, develop simultaneously secondary resource.A kind of industrial solid wastes of blast furnace slag are the slags of discharging in the blast furnace ironmaking process, claim again blast-furnace cinder.Chinese large-sized steel mill is more, annual blast furnace slag discharge capacity is huge, only there is small part to be secondary use, approximately 4,000,000 tons of the blast furnace slags that discharges as annual in Baogang, be used for the Year's consumption of slag cement 800,000 tons of left and right, the approximately 3,200,000 tons of air storages of annual residue need to take tract during stacking, work the mischief to biological environment.Except the essential elements such as Ca, Si, Mg, P, Fe, O, also contain a small amount of metallic element such as Mn, V, Cr, Ni, Nb in slag.How slag is taken full advantage of, extract useful element wherein, and then prepare the technical barrier that anode material for lithium-ion batteries is the needs solution.
Studies show that, utilizing metal ion mixing to process is to improve anode material for lithium-ion batteries LiFePO
4One of effective means of conductivity, the doping of a lot of metal ions is to anode material for lithium-ion batteries LiFePO
4The raising of conductivity has better effect.
Summary of the invention
The technical problem to be solved in the present invention:Overcome anode material for lithium-ion batteries LiFePO in prior art
4Cost is high, the shortcoming of poor performance, provides a kind of discarded object slag that utilizes to be primary raw material, preparation anode material for lithium-ion batteries LiFePO
4Method, the method cost and energy consumption are low, work simplification, and the positive electrode charge/discharge capacity that makes is high, good cycle, can be widely used in suitability for industrialized production.
Technical scheme of the present invention:
A kind of standby anode material for lithium-ion batteries LiFePO of prepared from steel slag that utilizes
4Method, comprise the following steps:
(1) take slag and pulverizing, take water-soluble carbon-source cpd of slag weight 3-8% and the water of 10-20%, water-soluble carbon-source cpd is added to the water and stirs, obtain the aqueous solution of carbon-source cpd; The aqueous solution of carbon-source cpd is added in slag, stir, obtain compound;
(2) compound is put into non-metallic vessel, then send into industrial microwave oven, process through microwave thermal and reduce; The product that obtains is carried out magnetic separation, obtain the slag extract;
(3) press the weight ratio metering dilute sulfuric acid of slag extract, 30-35wt% dilute sulfuric acid 1:3-5, the slag extract is added in dilute sulfuric acid, 80-90 ℃ of lower stirring reaction 2-4h obtains filtrate through standing, suction filtration, washing; Adding the hydrogen peroxide of slag extract weight 20-30% and 30-40% concentration in the filtrate is the phosphoric acid of 85 wt%, stir, at 40-50 ℃ of lower isothermal reaction 4-5h, then the pH value of conditioned reaction liquid is to 3.0-5.0, continue to stir 25-30 min after pH is stable, standing 24-36h washs, suction filtration, obtain the slag filter cake after deliming, the water content of the slag filter cake after described deliming is 15 wt %;
(4) add the phosphoric acid of lithium carbonate and 85 wt % in the slag filter cake, the weight ratio of slag filter cake, lithium carbonate, phosphoric acid is 1:0.229-0.240:0.1016-0.1036, mixes, and obtains the mixture of slag filter cake, lithium carbonate and phosphoric acid;
(5) take the weight of lithium carbonate as benchmark, the water of the metering water-soluble carbon-source cpd of 30-50% and 70-90%; Water-soluble carbon-source cpd is added to the water, stirs, obtain the aqueous solution of carbon-source cpd; The aqueous solution of carbon-source cpd is joined in the mixture of slag filter cake, lithium carbonate and phosphoric acid of step (4), stir, obtain presoma;
(6) with described presoma ageing 24-36h, be placed in non-metallic vessel, then put into industrial microwave oven and carry out microwave sintering under air-tight state, prepare described anode material for lithium-ion batteries LiFePO
4
2, preparation anode material for lithium-ion batteries LiFePO according to claim 1
4Method, it is characterized in that: water-soluble carbon-source cpd described in described step (1), step (5) is one or more in oxalic acid, citric acid, glucose, sucrose, lactose, maltose.
Non-metallic vessel in described step (2), step (6) is silicon carbide crucible, graphite crucible or alumina crucible.
The power output of industrial microwave oven is 10-20KW in described step (2), and it is that speed with 2-10 per minute ℃ is warming up to 550-650 ℃ that microwave thermal is processed, and is incubated 10-15min at this temperature.
The power output of industrial microwave oven is 10-20KW in described step (6), and microwave sintering is to be warming up to 600-700 ℃ with the speed of 2-10 per minute ℃, and is incubated 20-35min at this temperature.
Magnetic field intensity during described magnetic separation is 30-95KA/m.
Positive beneficial effect of the present invention:
(1) after the present invention extracts the slag discarded object through removal of impurities, be used in and substitute the conventional raw materials such as iron, phosphorus and doped chemical in battery raw material, the method can obviously reduce cost of material, reduces cost of material more than 30%; On the other hand, the method is utilized the industrial solid castoff slag in a large number, turns waste into wealth, and is beneficial to reduce the environmental protection input, is beneficial to the exploitation secondary resource, meets the national industrial policies of recycling economy, and is great to the question meaning of alleviating the current shortage of resources of China.
(2) the present invention adopts industrial microwave that the weak magnetic substance in slag is reduced to ferromagnetic substance, realizes separating by magnetic separation, simultaneously the phosphorus in slag is effectively separated and utilizes, and has really realized the secondary utilization to trade waste.
(3) the slag extract of the present invention after with deliming directly mixes with the aqueous solution of lithium carbonate, carbon-source cpd, not only batch mixing is even, and the paste presoma that obtains further reacts between composition in mixed process, is conducive to the synthetic of positive electrode and carrying out that carbon coats.
(4) the present invention has omitted ball milling, the dry run in traditional positive electrode preparation technology, work simplification, and control procedure is simple, can effectively guarantee the quality of product; Carbon-source cpd plays coated carbon in sintering process, and sintering process does not need blanketing with inert gas, has further reduced production cost; sintering process produces without pernicious gases such as oxynitrides simultaneously; pollution-free, be conducive to environmental protection, can be widely used in suitability for industrialized production.
(5) the present invention adopts industrial microwave processing slag advantage obvious, and microwave is directly absorbed by slag, and reaction can accurately be controlled, and firing rate is fast, saves the reaction time, the sample grain refinement, the even structure that obtain.
(6) the present invention directly adulterates after extracting by carbon coated with the metallic element in slag, when increasing substantially the LiFePO4 conductivity, has effectively improved charge/discharge capacity and the cycle-index of positive electrode, and the quality of product is better.Referring to Fig. 3, Fig. 4.
Performance test: with the LiFePO of preparation
4Mix by the weight ratio of 80:10:10 with acetylene black, Kynoar, add wherein appropriate organic solvent NMP(N-methyl pyrrolidone) be dissolved into pasty state, then pastel is evenly coated on aluminium foil, after 120 ℃ of vacuumize as anode, adopt the lithium sheet as negative pole, polyethene microporous membrane Celgard 2400 is barrier film, and electrolyte adopts 1 molL
-1LiPF
6/ EC+DMC(is ethylene carbonate and dimethyl carbonate), be assembled into experimental cell in being full of the glove box of argon gas, be used for charge-discharge test.Adopt the LAND battery test system to discharge and recharge with the electric current of 20 mA/g at normal temperatures, in the voltage range of 2.5-4.1V to LiFePO
4The charge/discharge capacity of positive electrode and cycle life test.
After measured, when product of the present invention at room temperature discharged and recharged with the electric current of 20 mA/g, discharge capacity was 136-141.6mAh/g first, was 132.5-135.8mAh/g after 10 circulations, showed good cycle performance.
Description of drawings
Fig. 1: the XRD collection of illustrative plates of extract after the slag deliming;
Fig. 1 can find out, extract fits like a glove with the XRD figure of conventional synthetic ferric phosphate precursor.
Fig. 2: the XRD figure of the extract after the slag deliming after 680 ℃ of sintering;
Fig. 2 can find out, with the extract after the slag deliming after heat treatment, has obtained very pure Fe
7(PO
4)
6, other element there is no appearance.
Fig. 3: the sample LiFePO of the present invention's preparation
4XRD figure;
Do not see the diffraction maximum that contains other phase in Fig. 3, this be due to the amount of leaving over other element in slag seldom, obtained very pure LiFePO
4Sample.
Fig. 4: the sample LiFePO of the present invention's preparation
4Scanning electron microscope (SEM) photograph;
Fig. 4 can find out, the sample particle is tiny, and distribution of particles is more even, and maximum particle is 5 μ m left and right.
Embodiment
Embodiment one: utilize the standby anode material for lithium-ion batteries LiFePO of prepared from steel slag
4Method, comprise the following steps:
(1) take 80 Kg slags, be ground into granularity less than 100 purpose powders; Take 4Kg glucose, add 10 Kg water, stirring and dissolving obtains D/W; D/W is added in the slag powder, put into mixer and stir, obtain compound; Wherein the chemical composition of slag sees Table 1, and is lower same;
Table 1: the chemical composition of slag (mass fraction %)
| Composition | CaO | FeO | Al 2O 3 | SiO 2 | MgO | MnO | P 2O 5 |
| Content | 30-60 | 15-26 | 3-8 | 8-23 | 4-9 | 5-10 | 0.5-2 |
(2) compound of preparation is put into silicon carbide crucible, then send in industrial microwave oven, utilize microwave to be warming up to 550 ℃ with the speed of 10 ℃ per minute, and keep 15min at this temperature; Be magnetic separation in the magnetic separation tube of 45KA/m with the reduzate that obtains in magnetic field intensity, select slag extract 30Kg;
(3) the dilution heat of sulfuric acid 100Kg with 30wt% joins in the slag extract, 80 ℃ of lower stirring reaction 4h; Standing 1h, then suction filtration, washing obtain filtrate, and adding 8Kg hydrogen peroxide, 10Kg concentration in filtrate is the phosphoric acid of 85 wt %, stir, 40 ℃ of reaction 4h of constant temperature regulate pH value to 4.0 with NaOH solution, after pH is stable, continue to stir 25 min, standing 24h goes to suction filtration, washing, obtains filter cake (water content 15%, be the slag extract after deliming), the XRD collection of illustrative plates of filter cake is seen Fig. 1;
(4) take the 10Kg filter cake, add the phosphatase 11 .036Kg of lithium carbonate 2.39Kg and 85wt%, obtain the mixture of filter cake, lithium carbonate and phosphoric acid;
(5) metering 1.0Kg citric acid, 2.0Kg water, be added to the water citric acid, stirs, and obtains aqueous citric acid solution; Aqueous citric acid solution is joined in the mixture of filter cake, lithium carbonate and phosphoric acid in step (4), stir, obtain presoma;
(6) with presoma ageing 24h, then be placed in silicon carbide crucible, crucible is put into microwave oven, be warming up to 680 ℃ with the speed of 5 ℃ per minute, keep 25min at this temperature, prepare LiFePO
4
Embodiment two: utilize the standby anode material for lithium-ion batteries LiFePO of prepared from steel slag
4Method, comprise the following steps:
(1) take 80 Kg slags, be ground into granularity less than 100 purpose powders; Take the 3Kg citric acid, add 8 Kg water, stirring and dissolving obtains aqueous citric acid solution; Aqueous citric acid solution is added in the slag powder, and stirring obtains compound;
(2) compound of preparation is put into alumina crucible, send into industrial microwave oven and utilize microwave to be warming up to 600 ℃ with the speed of 8 ℃ per minute, keep 12min at this temperature; Be magnetic separation in the magnetic separation tube of 35KA/m with the reduzate that obtains in magnetic field intensity, select slag extract 30Kg;
(3) the dilution heat of sulfuric acid 100Kg with 30wt% adds in the slag extract, 80 ℃ of lower stirring reaction 4h; Standing 1h, then obtain filtrate after suction filtration, washing, adding 6Kg hydrogen peroxide, 9Kg concentration in filtrate is the phosphoric acid of 85 wt %, stir, 40 ℃ of reaction 4h of constant temperature regulate pH value to 3.0 with NaOH solution, continue to stir 25 min after pH is stable, go to suction filtration, washing after standing 24h, obtain filter cake (water content 15%, i.e. slag extract after deliming);
(4) take the 10Kg filter cake, adding the lithium carbonate of 2.32Kg and 1.026Kg concentration is the phosphoric acid of 85 wt %, obtains the mixture of filter cake, lithium carbonate and phosphoric acid;
(5) metering 0.90Kg sucrose and 1.80Kg water, be added to the water sucrose, and stirring obtains sucrose solution; Sucrose solution is joined in the mixture of filter cake, lithium carbonate and phosphoric acid of step (4), stir, obtain presoma;
(6) with presoma ageing 24h, then be placed in alumina crucible, crucible is put into industrial microwave oven, be warming up to 650 ℃ with the speed of 6 ℃ per minute, keep 15min at this temperature, prepare LiFePO
4
Embodiment three: utilize the standby anode material for lithium-ion batteries LiFePO of prepared from steel slag
4Method, comprise the following steps:
(1) take 90 Kg slags, be ground into granularity less than 100 purpose powders; Take 4Kg oxalic acid, add 10 Kg water, stirring and dissolving obtains oxalic acid aqueous solution; Oxalic acid aqueous solution is added in the slag powder, and stirring obtains compound;
(2) compound of preparation is put into alumina crucible, and send in industrial microwave oven, utilize microwave to be warming up to 600 ℃ with the speed of 10 ℃ per minute, and keep 15min at this temperature; Be magnetic separation in the magnetic separation tube of 55KA/m with the reduzate that obtains in magnetic field intensity, select slag extract 40Kg;
(3) the dilution heat of sulfuric acid 120Kg with 30wt% joins in the slag extract, 80 ℃ of lower stirring reaction 4h; Standing 1h, then obtain filtrate after suction filtration, washing, adding 12Kg hydrogen peroxide, 16Kg concentration in filtrate is the phosphoric acid of wt 85%, stir, and 40 ℃ of reaction 4h of constant temperature, regulate pH value to 5.0 with NaOH solution, after pH is stable, continue to stir 25 min, go to suction filtration, washing after standing 24h, obtain filter cake (water content 15%, i.e. slag extract after deliming);
(4) get the 10Kg filter cake, adding 2.35Kg lithium carbonate and 1.016Kg concentration is 85% phosphoric acid, obtains the mixture of filter cake, lithium carbonate and phosphoric acid;
(5) measure the glucose of 0.6Kg, the citric acid of 0.6Kg, then add the water of 2.10Kg, stir, obtain glucose, lemon aqueous acid; Glucose, lemon aqueous acid are joined in the mixture of filter cake, lithium carbonate and phosphoric acid of step (4), stir, obtain presoma;
(6) with presoma ageing 24h, then be placed in alumina crucible, crucible is put into microwave oven, be warming up to 620 ℃ with the speed of 3 ℃ per minute, keep 35min at this temperature, prepare LiFePO
4
Embodiment four: and embodiment one is basic identical, difference is following steps:
(1) take 100 Kg slags, pulverize; Take the 8Kg lactose, add 20 Kg water, stirring and dissolving obtains lactose solution; Lactose solution is added in the slag powder, stir, obtain compound;
(2) compound of preparation is put into graphite crucible, the speed with 2 ℃ per minute when industrial microwave oven heats up is warming up to 650 ℃, keeps 10min at this temperature; Be magnetic separation in the magnetic separation tube of 95KA/m with the reduzate that obtains in magnetic field intensity, select slag extract 40Kg;
(3) the dilution heat of sulfuric acid 100Kg with 35wt% adds in the slag extract, 90 ℃ of lower stirring reaction 2h; Standing 1h, then suction filtration, washing obtain filtrate, and adding 10Kg hydrogen peroxide, 15Kg concentration in filtrate is the phosphoric acid of 85 wt %, stirs, 50 ℃ of reaction 5h of constant temperature, the pH value to 4.0 of conditioned reaction liquid after pH is stable, continues to stir 30 min, standing 36h, go to suction filtration, washing, obtain filter cake (water content 15%, i.e. slag extract after deliming);
(4) take the 10Kg filter cake, add the phosphatase 11 .020Kg of lithium carbonate 2.35Kg and 85wt%, obtain the mixture of filter cake, lithium carbonate and phosphoric acid;
(5) metering 1.0Kg lactose, 2.0Kg water, be added to the water lactose, stirs, and obtains lactose aqueous solution; Lactose aqueous solution is joined in the mixture of filter cake, lithium carbonate and phosphoric acid in step (4), stir, obtain presoma;
(6) with presoma ageing 30h, then be placed in graphite crucible, crucible is put into microwave oven, be warming up to 700 ℃ with the speed of 2 ℃ per minute, keep 20min at this temperature, prepare LiFePO
4
Embodiment five: and embodiment one is basic identical, difference is following steps:
(1) take 100 Kg slags, pulverize; Take 8Kg maltose, add 15 Kg water, stirring and dissolving obtains maltose solution; Maltose solution is added in the slag powder, stir, obtain compound;
(2) compound of preparation is put into graphite crucible, be warming up to 600 ℃ with industrial microwave oven with the speed of 5 ℃ per minute, and keep 12min at this temperature; Be magnetic separation in the magnetic separation tube of 80KA/m with the reduzate that obtains in magnetic field intensity, select slag extract 30Kg;
(3) the dilution heat of sulfuric acid 100Kg with 35wt% joins in the slag extract, 85 ℃ of lower stirring reaction 3h; Standing 2h, then suction filtration, washing obtain filtrate, and adding 7Kg hydrogen peroxide, 10Kg concentration in filtrate is the phosphoric acid of 85 wt %, stirs, 45 ℃ of reaction 5h of constant temperature, the pH value to 4.0 of conditioned reaction liquid after pH is stable, continues to stir 30 min, standing 30h, go to suction filtration, washing, obtain filter cake (water content 15%, i.e. slag extract after deliming);
(4) take the 10Kg filter cake, add the phosphatase 11 .030Kg of lithium carbonate 2.30Kg and 85wt%, obtain the mixture of filter cake, lithium carbonate and phosphoric acid;
(5) metering 1.0Kg maltose, 2.0Kg water, be added to the water maltose, stirs, and obtains maltose solution; Maltose solution is joined in the mixture of filter cake, lithium carbonate and phosphoric acid in step (4), stir, obtain presoma;
(6) with presoma ageing 30h, then be placed in graphite crucible, crucible is put into microwave oven, be warming up to 680 ℃ with the speed of 5 ℃ per minute, keep 30min at this temperature, prepare LiFePO
4
?
Claims (6)
1. one kind is utilized the standby anode material for lithium-ion batteries LiFePO of prepared from steel slag
4Method, it is characterized in that: the method comprises the following steps:
(1) take slag and pulverizing, take water-soluble carbon-source cpd of slag weight 3-8% and the water of 10-20%, water-soluble carbon-source cpd is added to the water and stirs, obtain the aqueous solution of carbon-source cpd; The aqueous solution of carbon-source cpd is added in slag, stir, obtain compound;
(2) compound is put into non-metallic vessel, then send into industrial microwave oven, process through microwave thermal and reduce; The product that obtains is carried out magnetic separation, obtain the slag extract;
(3) press the weight ratio metering dilute sulfuric acid of slag extract, 30-35wt% dilute sulfuric acid 1:3-5, the slag extract is added in dilute sulfuric acid, 80-90 ℃ of lower stirring reaction 2-4h obtains filtrate through standing, suction filtration, washing; Adding the hydrogen peroxide of slag extract weight 20-30% and 30-40% concentration in the filtrate is the phosphoric acid of 85 wt%, stir, at 40-50 ℃ of lower isothermal reaction 4-5h, then the pH value of conditioned reaction liquid is to 3.0-5.0, continue to stir 25-30 min after pH is stable, standing 24-36h washs, suction filtration, obtain the slag filter cake after deliming, the water content of the slag filter cake after described deliming is 15 wt %;
(4) add the phosphoric acid of lithium carbonate and 85 wt % in the slag filter cake, the weight ratio of slag filter cake, lithium carbonate, phosphoric acid is 1:0.229-0.240:0.1016-0.1036, mixes, and obtains the mixture of slag filter cake, lithium carbonate and phosphoric acid;
(5) take the weight of lithium carbonate as benchmark, the water of the metering water-soluble carbon-source cpd of 30-50% and 70-90%; Water-soluble carbon-source cpd is added to the water, stirs, obtain the aqueous solution of carbon-source cpd; The aqueous solution of carbon-source cpd is joined in the mixture of slag filter cake, lithium carbonate and phosphoric acid of step (4), stir, obtain presoma;
(6) with described presoma ageing 24-36h, be placed in non-metallic vessel, then put into industrial microwave oven and carry out microwave sintering under air-tight state, prepare described anode material for lithium-ion batteries LiFePO
4
2. preparation anode material for lithium-ion batteries LiFePO according to claim 1
4Method, it is characterized in that: water-soluble carbon-source cpd described in described step (1), step (5) is one or more in oxalic acid, citric acid, glucose, sucrose, lactose, maltose.
3. preparation anode material for lithium-ion batteries LiFePO according to claim 1
4Method, it is characterized in that: the non-metallic vessel in described step (2), step (6) is silicon carbide crucible, graphite crucible or alumina crucible.
4. preparation anode material for lithium-ion batteries LiFePO according to claim 1
4Method, it is characterized in that: the power output of industrial microwave oven is 10-20KW in described step (2), it is that speed with 2-10 per minute ℃ is warming up to 550-650 ℃ that microwave thermal is processed, and is incubated 10-15min at this temperature.
5. preparation anode material for lithium-ion batteries LiFePO according to claim 1
4Method, it is characterized in that: the power output of industrial microwave oven is 10-20KW in described step (6), microwave sintering is to be warming up to 600-700 ℃ with the speed of 2-10 per minute ℃, and is incubated 20-35min at this temperature.
6. according to claim 1-5 described preparation anode material for lithium-ion batteries of any one LiFePO
4Method, it is characterized in that: the magnetic field intensity during described magnetic separation is 30-95KA/m.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103904326A (en) * | 2014-04-02 | 2014-07-02 | 莱芜钢铁集团有限公司 | Preparation method for doping type lithium iron phosphate using rotary hearth furnace metallized pellet |
| CN103956487A (en) * | 2014-04-02 | 2014-07-30 | 莱芜钢铁集团有限公司 | Method for preparing lithium iron phosphate by using rotary furnace metallized pellets |
| CN112289991A (en) * | 2020-10-20 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Ni and Cr co-doped carbon-coated lithium iron phosphate and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844756A (en) * | 2009-03-25 | 2010-09-29 | 宝山钢铁股份有限公司 | Method for preparing lithium iron phosphate by using steel slag |
| CN101898757A (en) * | 2009-05-26 | 2010-12-01 | 宝山钢铁股份有限公司 | Method for preparing multi-component doped lithium ferrous phosphate by utilizing high phosphorus slag |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844756A (en) * | 2009-03-25 | 2010-09-29 | 宝山钢铁股份有限公司 | Method for preparing lithium iron phosphate by using steel slag |
| CN101898757A (en) * | 2009-05-26 | 2010-12-01 | 宝山钢铁股份有限公司 | Method for preparing multi-component doped lithium ferrous phosphate by utilizing high phosphorus slag |
Non-Patent Citations (1)
| Title |
|---|
| Z.J.WU ET AL.: "Synthesis and electrochemical properties of multi-doped LiFePO4/C prepared from the steel slag", 《JOURNAL OF POWER SOURCES》, vol. 195, 9 December 2009 (2009-12-09) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103904326A (en) * | 2014-04-02 | 2014-07-02 | 莱芜钢铁集团有限公司 | Preparation method for doping type lithium iron phosphate using rotary hearth furnace metallized pellet |
| CN103956487A (en) * | 2014-04-02 | 2014-07-30 | 莱芜钢铁集团有限公司 | Method for preparing lithium iron phosphate by using rotary furnace metallized pellets |
| CN112289991A (en) * | 2020-10-20 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Ni and Cr co-doped carbon-coated lithium iron phosphate and preparation method and application thereof |
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