CN109841825B - Method for preparing lithium ion battery cathode material by recycling tin in electroplating sludge - Google Patents
Method for preparing lithium ion battery cathode material by recycling tin in electroplating sludge Download PDFInfo
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- 239000010802 sludge Substances 0.000 title claims abstract description 57
- 238000009713 electroplating Methods 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 29
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000010406 cathode material Substances 0.000 title claims abstract description 8
- 238000004064 recycling Methods 0.000 title claims description 11
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 229920002749 Bacterial cellulose Polymers 0.000 claims abstract description 28
- 239000005016 bacterial cellulose Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 3
- 239000007773 negative electrode material Substances 0.000 claims abstract description 3
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 claims abstract 3
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 claims abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 2
- 239000010405 anode material Substances 0.000 claims 9
- 239000000243 solution Substances 0.000 claims 7
- 239000011259 mixed solution Substances 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- 229910052718 tin Inorganic materials 0.000 description 10
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000009736 wetting Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000008104 plant cellulose Substances 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
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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 invention belongs to the technical field of electroplating sludge treatment, and discloses a method for preparing a lithium ion battery cathode material by recovering tin from electroplating sludge. Drying, grinding and sieving the electroplating sludge, adding an inorganic alkali solution, uniformly stirring, carrying out hydrothermal reaction, and filtering to obtain an electroplating sludge purified solution; adding bacterial cellulose into a PDDA solution, oscillating, stirring and mixing, and then rinsing with distilled water to obtain modified bacterial cellulose; and adding the obtained modified bacterial cellulose into the electroplating sludge purification solution, stirring and mixing, washing and drying to obtain a composite material precursor, and finally calcining at high temperature in an inert or reducing atmosphere to obtain the Sn @ C lithium battery negative electrode material. The preparation method provided by the invention not only solves the environmental problem of electroplating sludge, but also utilizes the unique morphology of the bacterial cellulose to prepare the high-valued lithium ion battery cathode material, thereby providing a feasible idea for changing environmental wastes into valuables.
Description
Technical Field
The invention belongs to the technical field of electroplating sludge treatment, and particularly relates to a method for preparing a lithium ion battery cathode material by recovering tin from electroplating sludge.
Background
The electroplating sludge is one of dangerous wastes, has the characteristics of instability, strong mobility and high water content, and mainly contains metal ions such as Sn, Fe, Cu, Ni, Cr, Cd and the like. And various electroplating sludge generated by different types of electroplating are different, and different metal ion treatment methods are different. Electroplating sludge is mainly divided into two types, one type is quality-divided sludge, and the metal ions contained in the sludge are single, so that the sludge is easier to recycle; the other is mixed sludge, which contains more complex components, more kinds of metal ions, and some dangerous metal ions such as Cr, Cd and the like, and brings great difficulty to post-treatment and separation. Sn is widely used in the electroplating industry, and is one of the main metal ions of electroplating sludge, and is also one of the sludge that is difficult to recycle. The currently and generally used electroplating sludge treatment methods mainly comprise: curing agent treatment, heat treatment, pyrogenic process, wet process, acid leaching, ammonia leaching, biological treatment method and the like, and treatment of leachate or solid waste products is required after the treatment method. Therefore, it is very important to develop a new method for treating electroplating sludge.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a method for preparing a lithium ion battery cathode material by recovering tin from electroplating sludge. The method utilizes the electroplating sludge in a high-value manner, provides a new idea for harmless treatment of the electroplating sludge and also provides a new idea for preparing an electrochemical energy storage material.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a lithium ion battery cathode material by recovering tin in electroplating sludge comprises the following preparation steps:
(1) drying, grinding and sieving the electroplating sludge, adding an inorganic alkali solution, uniformly stirring, carrying out hydrothermal reaction, and filtering to obtain an electroplating sludge purified solution;
(2) adding bacterial cellulose into a PDDA (poly dimethyl diallyl ammonium chloride) solution, oscillating, stirring and mixing, and then rinsing with distilled water to obtain modified bacterial cellulose;
(3) adding the modified bacterial cellulose obtained in the step (2) into the electroplating sludge purification liquid obtained in the step (1), stirring and mixing, and then washing and drying to obtain a composite material precursor;
(4) and (4) calcining the composite material precursor obtained in the step (3) at high temperature in an inert or reducing atmosphere to obtain the Sn @ C lithium battery negative electrode material.
Further, the drying, grinding and sieving in the step (1) means drying at 90 ℃ for 12 hours, and grinding and sieving by a 200-mesh sieve.
Further, the inorganic alkali solution in the step (1) is a sodium hydroxide, potassium hydroxide or lithium hydroxide solution with the concentration of 0.1-3 mol/L.
Further, the hydrothermal reaction temperature in the step (1) is 150-230 ℃, and the time is 12-18 h.
Further, the adding amount of the bacterial cellulose in the step (2) is 0.1-3 g/L.
Further, the mass concentration of the PDDA solution in the step (2) is 1-10%.
Further, the time for shaking, stirring and mixing in the step (2) is 0.5-2 h.
Further, the stirring and mixing time in the step (3) is 1-48 h.
Further, the washing solution in the step (3) is one or a mixture of distilled water and absolute ethyl alcohol.
Further, the drying in the step (3) is at least one of atmospheric drying, vacuum drying and freeze drying.
Further, the inert or reducing atmosphere in the step (4) is any one or a mixed atmosphere of two or more of nitrogen, argon and hydrogen.
Further, the high-temperature calcination in the step (4) is to heat the mixture to 500-900 ℃ at a heating rate of 1-10 ℃/min for 1-10 h.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the bacterial cellulose adopted by the invention is used as a natural nanofiber material, is simple to prepare, has high purity, does not contain lignin and hemicellulose in plant cellulose, has high crystallinity, and is in a special hyperfine nanometer three-dimensional network structure in the aspect of structure; the carbon skeleton after carbonization of the bacterial cellulose is used as a carrier of the tin micro-nano particles, so that the tin particles can be coated, the mechanical stress generated by Sn metal in the charging and discharging process is reduced, and the agglomeration of the Sn metal micro-nano particles is prevented to a certain extent, so that the material is prevented from being damaged, and the circulation stability of the material is improved; meanwhile, the bacterial cellulose has excellent mechanical properties, can bring a buffering effect to tin particles in the charging and discharging processes, and the obtained material has excellent cycle stability and higher capacity and can meet the requirements of the current market.
(2) The bacterial cellulose in the composite material prepared by the invention is partially graphene-bonded after high-temperature calcination, which is beneficial to the transfer and diffusion of Li ions.
(3) The invention utilizes the electroplating sludge of industrial waste in a high-value way and can solve the environmental problem.
(4) The preparation method has simple process, easy operation and easy control.
Drawings
FIG. 1 is an XRD pattern of the Sn @ C composite prepared in example 1;
FIG. 2 is an SEM image of a Sn @ C composite prepared in example 1;
FIG. 3 is a graph of the cycling performance of a button cell assembled from the composite prepared in example 2 at a current density of 1A/g;
FIG. 4 is a Raman spectrum of the composite prepared in example 2;
FIG. 5 is a graph of the cycling performance of a button cell assembled from the composite prepared in example 3 at a current density of 0.1A/g;
fig. 6 is a graph of rate performance of button cells assembled from the composite material prepared in example 3 at different current densities.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) Electroplating sludge purification liquid: the electroplating sludge is placed in an oven, dried for 12 hours at 90 ℃, ground and sieved by a two-hundred-mesh sieve. Taking 10g of dried electroplating sludge, adding 50ml of 0.7mol/L sodium hydroxide, carrying out hydrothermal treatment at 150 ℃ for 48h, and filtering to obtain filtrate, namely electroplating sludge purification solution.
(2) Modification of bacterial cellulose: adding 100mg of bacterial cellulose into 1 wt.% of PDDA solution, stirring for 1h at the speed of 200rpm in an oscillating way, and then rinsing for three times by using distilled water to obtain modified bacterial cellulose;
(3) and adding the modified bacterial cellulose into 50ml of electroplating sludge purification liquid, and stirring and mixing for 24 hours in a shaking way.
(4) And (3) wetting and washing the composite material for three times by using distilled water, and then freeze-drying to obtain a composite material precursor.
(5) And heating the composite material precursor to 600 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, calcining for 2h, and cooling to obtain the Sn @ C composite material.
The physical and chemical properties of the composite material prepared in the example are shown in figures 1 and 2, wherein figure 1 is an XRD (X-ray diffraction) spectrum of the prepared Sn @ C composite material, and figure 2 is an SEM (scanning Electron microscope) image of the prepared Sn @ C composite material.
XRD shows that simple substance tin exists in the Sn @ C composite material prepared by the method, SEM shows that the composite material is good in appearance, and tin particles are uniformly distributed in a three-dimensional network structure of bacterial cellulose.
Example 2
(1) Electroplating sludge purification liquid: the electroplating sludge is placed in an oven, dried for 12 hours at 90 ℃, ground and sieved by a two-hundred-mesh sieve. Taking 10g of dried electroplating sludge, adding 50ml of 1.0mol/L sodium hydroxide, carrying out hydrothermal treatment at 230 ℃ for 48h, and filtering to obtain filtrate, namely electroplating sludge purification solution.
(2) Modification of bacterial cellulose: adding 100mg of bacterial cellulose into a 2% PDDA solution, oscillating and stirring at the speed of 150rpm for 2 hours, and then wetting and washing with distilled water for three times;
(3) and adding the modified bacterial cellulose into 50ml of electroplating sludge purification liquid, and stirring and mixing for 24 hours in a shaking way.
(4) And (3) wetting and washing the composite material for three times by using distilled water, and then freeze-drying to obtain a composite material precursor.
(5) And heating the composite material precursor to 700 ℃ at the heating rate of 1 ℃/min in the nitrogen atmosphere, calcining for 2h, and cooling to obtain the Sn @ C composite material.
The product obtained in the embodiment is assembled into a button cell to test the discharge capacity, and the charge and the discharge are carried out within the range of 0.01-3V. The long cycle stability test at a current density of 1A/g is shown in FIG. 3. Meanwhile, the composite material can stably circulate for more than 2000 circles. The physical and chemical properties of the prepared Sn @ C composite material are shown in figure 4, figure 4 is Raman data of the prepared Sn @ C composite material, and figure 4 shows that bacterial cellulose in the composite material is partially graphene-based in a high-temperature annealing process, so that lithium ion diffusion is facilitated, and the specific capacity of the material is improved.
Example 3
(1) Electroplating sludge purification liquid: the electroplating sludge is placed in an oven, dried for 12 hours at 90 ℃, ground and sieved by a two-hundred-mesh sieve. Taking 10g of dried electroplating sludge, adding 50ml of 1.5mol/L sodium hydroxide, carrying out hydrothermal treatment at 200 ℃ for 24h, and filtering to obtain filtrate, namely electroplating sludge purification solution.
(2) Modification of bacterial cellulose: adding 250mg of bacterial cellulose into a 5% PDDA solution, oscillating and stirring at the speed of 200rpm for 0.5h, and then wetting and washing with distilled water for three times;
(3) and adding the modified bacterial cellulose into 50ml of electroplating sludge purification liquid, and stirring and mixing for 12 hours in a shaking way.
(4) And (3) wetting and washing the composite material for three times by using distilled water, and then freeze-drying to obtain a composite material precursor.
(5) And heating the composite material precursor to 700 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, calcining for 2h, and cooling to obtain the Sn @ C composite material.
The Sn @ C composite material obtained in the embodiment is assembled into a button cell to test the charge-discharge capacity of the button cell, and the cycle life test is carried out within the range of 0.01-3V. FIG. 5 is a graph showing the cycle stability test of the composite material. As shown in fig. 6, the rate capability of the button cell is shown under different current densities, and it can be seen that the Sn @ C composite material has excellent rate capability.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing a lithium ion battery cathode material by recovering tin in electroplating sludge is characterized by comprising the following preparation steps:
(1) drying, grinding and sieving the electroplating sludge, adding an inorganic alkali solution, uniformly stirring, carrying out hydrothermal reaction, and filtering to obtain an electroplating sludge purified solution;
(2) adding bacterial cellulose into a PDDA solution, oscillating, stirring and mixing, and then rinsing with distilled water to obtain modified bacterial cellulose;
(3) adding the modified bacterial cellulose obtained in the step (2) into the electroplating sludge purification liquid obtained in the step (1), stirring and mixing, and then washing and drying to obtain a composite material precursor;
(4) and (4) calcining the composite material precursor obtained in the step (3) at high temperature in an inert or reducing atmosphere to obtain the Sn @ C lithium battery negative electrode material.
2. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the drying, grinding and sieving in the step (1) means drying at 90 ℃ for 12 hours, and grinding and sieving by a 200-mesh sieve.
3. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the inorganic alkali solution in the step (1) is a sodium hydroxide, potassium hydroxide or lithium hydroxide solution with the concentration of 0.1-3 mol/L.
4. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the hydrothermal reaction temperature in the step (1) is 150-230 ℃, and the time is 24 or 48 hours.
5. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the adding amount of the bacterial cellulose in the step (2) is 0.1-3 g/L; the mass concentration of the PDDA solution is 1-10%.
6. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the time for oscillating, stirring and mixing in the step (2) is 0.5-2 h; and (4) stirring and mixing for 1-48 h in the step (3).
7. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the washing solution in the step (3) is one or a mixed solution of distilled water and absolute ethyl alcohol.
8. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: and (3) drying is at least one of normal pressure drying, vacuum drying and freeze drying.
9. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the inert or reducing atmosphere in the step (4) is any one or a mixed atmosphere of more than two of nitrogen, argon and hydrogen.
10. The method for preparing the lithium ion battery anode material by recycling tin in electroplating sludge according to claim 1, characterized by comprising the following steps: the high-temperature calcination in the step (4) is to heat the mixture to 500-900 ℃ at a heating rate of 1-10 ℃/min for 1-10 h.
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