CN108565423A - A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material - Google Patents
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material Download PDFInfo
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- CN108565423A CN108565423A CN201810320892.1A CN201810320892A CN108565423A CN 108565423 A CN108565423 A CN 108565423A CN 201810320892 A CN201810320892 A CN 201810320892A CN 108565423 A CN108565423 A CN 108565423A
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- H01M10/05—Accumulators with non-aqueous electrolyte
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Abstract
The invention discloses the preparation methods of a kind of LiFePO4 and cadmium phosphate lithium composite material, using sol-gal process self-assembling technique, the composite material of cadmium phosphate lithium and LiFePO4 has been prepared by two-step synthesis method under high-temperature calcination, and its structure, magnetic property have been studied.By adjusting mass ratio, calcination temperature and the calcination time of cadmium phosphate lithium and LiFePO4, it is found that the change of the mass ratio, calcination temperature and calcination time of cadmium phosphate lithium and LiFePO4 has certain adjustment effect to the structure and magnetism of composite material.
Description
Technical field
The invention belongs to technical field of composite preparation, more particularly to a kind of LiFePO4 and cadmium phosphate lithium composite material
Preparation method.
Background technology
LiFePO4 (LiFePO4) it is a kind of lithium ion cell positive material that J.B.Goodenough etc. was proposed in 1997
Material.Because of LiFePO4 (LiFePO4) there is abundant cheap, the battery theoretical specific capacity height of service life length, raw material sources, nothing
Malicious, pollution-free, environmentally friendly, cycle performance is good, the advantages that having a safety feature so that LiFePO4 (LiFePO4) by
Extensive work person's likes and furthers investigate.In olivine-type LiFePO4 (LiFePO4) in crystal structure, all atoms are
It is arranged in a manner of six side's solid matters, is rhombic system, phosphorus atoms (P) therein and four oxygen atoms (O) but with slight distortion
Constitute PO4Structure；And lithium atom (Li) and iron atom (Fe) then form LiO with six oxygen atoms (O) of surrounding respectively6With FeO6
Octahedral structure.When below Ne＆1＆el temperature, LiFePO4 (LiFePO4) magnetism characteristic show as anti-ferromagnetism.
For lithium ion battery anode material lithium iron phosphate (LiFePO4) research it is more, achieve certain achievement.Than
Such as Miran Gaberscek are prepared for the LiFePO of carbon modification using sol-gal process (sol-gel)4Composite cathode material,
Research finds sample activity ingredient for submicron size particle and with the presence of pore, this makes electronic conductivity improve well.
Yaping Xu and Jian Mao are prepared for by sol-gal process containing Ti2O3The composite ferric lithium phosphate material of coating improves multiple
The specific capacity and cyclical stability of condensation material.Zhang S.C. etc. use CTAB as the amount control of surfactant by hydro-thermal method
The growth of LiFePO4 crystal processed, synthesizing iron lithium phosphate, in 0.1C multiplying powers, specific capacity reaches 145.70mAh/g.
Although the research of LiFePO4 cathode material achieves certain achievement, it there is also some need further it is complete
Kind defect, such as electron energy density is small, conductivity is low, poor performance at low temperatures etc..For these disadvantages, each researcher uses
Different methods improve the performance of LiFePO4.And the magnetic performance of LiFePO4 cathode material has closely with electrical property
Contact, but LiFePO4 is combined the preparation method of synthetic composite material and to phosphoric acid every lithium and phosphorus with cadmium phosphate lithium at present
The research of sour iron lithium composite material magnetic performance has not been reported.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of LiFePO4s and cadmium phosphate lithium composite material
Preparation method.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, includes the following steps：
S1, it ferrous oxalate is dissolved in distilled water obtains ferrous oxalate aqueous solution, ethylene glycol is dissolved in distilled water and is obtained
Phosphoric acid is dissolved in distilled water and obtains phosphate aqueous solution by glycol water, and lithium hydroxide is dissolved in distilled water and obtains hydrogen-oxygen
Change lithium aqueous solution, cadmium phosphate lithium is dissolved in distilled water and obtains cadmium phosphate lithium aqueous solution, glycol water is added dropwise to oxalic acid
The glycol water that ferrous oxalate is obtained in ferrous aqueous solution, the ethylene glycol that phosphate aqueous solution is added dropwise to ferrous oxalate are water-soluble
Mixed solution is obtained in liquid, lithium hydroxide aqueous solution is added dropwise to the mixed solution that lithium hydroxide is obtained in mixed solution, then
Cadmium phosphate lithium aqueous solution is added dropwise in the mixed solution of lithium hydroxide and obtains reaction solution, needs continuously to stir in the above mixed process
It mixes；Wherein, ferrous oxalate, ethylene glycol, phosphoric acid, lithium hydroxide, cadmium phosphate lithium molar ratio be 5:8:4:4:0.03~0.5.
S2, the reaction solution obtained in S1 is stirred in 50~80 DEG C of water-baths, mixing time is 5~10h, is obtained wet
Gel；
S3, the class wet gel obtained in S2 is dried, 90~120 DEG C of drying temperature, 8~15h of drying time is obtained
Xerogel；
S4, the xerogel that S3 is obtained is ground to obtain powder, then powder is positioned in crucible, is protected using carbon
The three anti-oxidation measures of crucible formula, in Muffle furnace at 650~800 DEG C calcine 10~13h, natural cooling after the completion of calcining
To room temperature, using mortar grinder to get to the LiFePO4 and cadmium phosphate lithium composite material.
The features of the present invention also characterized in that in S1, the cadmium phosphate lithium is made by the steps：
S11, it lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol is added in distilled water carries out mixed dissolution, in 80 DEG C of water
H is stirred in bath, obtains gel；Wherein, the molar ratio of lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol is 1:1:1:1~3；
S12, by the gel obtained in S11, at 100~140 DEG C then dry 5~10h is existed then using mortar grinder
Under active powdered carbon protective condition, 600~900 DEG C of 4~16h of calcining are to get to the cadmium phosphate lithium material in Muffle furnace.
The features of the present invention also characterized in that in S3,750 DEG C of calcining 10h in Muffle furnace.
The features of the present invention also characterized in that in S2, bath temperature is 60 DEG C, mixing time 7h.
Compared with prior art, preparation method of the invention has the advantages that：
(1) the present invention provides the preparation method of a kind of LiFePO4 and cadmium phosphate lithium composite material, by cadmium phosphate lithium with
LiFePO4 is combined, and particle size has successfully been prepared using sol-gel method in the composite material of 700nm or so, this hair
Bright method is at low cost, toxicity is low, easy to operate, mild condition, take short, mechanism understand, the LiFePO4 being prepared with
Not only crystallinity and order are high for cadmium phosphate lithium composite material, but also reduce cost, have sizable application development prospect.
(2) improvement in terms of phase structure：By studying cadmium phosphate lithium and LiFePO4 mass ratio, calcination time and calcining
Influence of the temperature to LiFePO4 and cadmium phosphate lithium composite material phase structure, the results showed that when LiFePO4 and cadmium phosphate lithium
Mass ratio is 100:When 10, the crystallinity highest of composite material is further added by the dosage of cadmium phosphate lithium, under the crystallinity of composite material
Drop；By adjusting calcination temperature, find to gradually increase with the increase of calcination temperature, the crystallinity of composite material；Pass through adjusting
Calcination time finds that the increase with calcination time, the crystallinity of sample decline.
(3) improvement of magnetic aspect：Saturation magnetization reduces with the increase of cadmium phosphate lithium addition, and coercivity
Hc is as the increase of cadmium phosphate lithium addition is substantially in the trend of reduction after first increasing.
Description of the drawings
Fig. 1 be different quality than cadmium phosphate lithium and composite ferric lithium phosphate material XRD diffraction patterns；
Fig. 2 be different quality than cadmium phosphate lithium and composite ferric lithium phosphate material hysteresis loop figure；
Fig. 3 is LiFePO4 and cadmium phosphate lithium mass ratio is 100:The composite material scanning electron microscope prepared under the conditions of 10
Figure；
Fig. 4 is LiFePO4 and cadmium phosphate lithium mass ratio is 100:The composite material granular statistics prepared under the conditions of 10
Figure；
Fig. 5 is the XRD diffraction patterns that composite material is prepared using different calcination temperatures；
Fig. 6 is the hysteresis loop figure of the cadmium phosphate lithium and composite ferric lithium phosphate material that are synthesized under different calcination temperatures；
Fig. 7 is LiCdPO prepared by different calcination times4With phosphorus LiFePO4The XRD diffraction patterns of composite material；
Fig. 8 is the hysteresis loop figure of the cadmium phosphate lithium and composite ferric lithium phosphate material that are synthesized under different calcination times.
Specific implementation mode
The specific implementation mode of invention is described in detail below, it is to be understood that protection scope of the present invention not by
The limitation of specific implementation mode.The test method of actual conditions is not specified in the following example, usually according to normal condition, or
According to the condition proposed by each manufacturer.
Cadmium phosphate lithium in following embodiment is prepared by following specific steps：
S11,1.6784g lithium hydroxides, 12.3386g cadmium nitrates, 3.9199g phosphoric acid and 4.9654g ethylene glycol are added to
Mixed dissolution is carried out in 300mL distilled water, in 80 DEG C of stirred in water bath 8h, obtains gel；
S12, the gel obtained in S11 at 130 DEG C is dried into 5h, mortar grinder is then used, then in active powdered carbon
Under protective condition, 800 DEG C of calcining 12h are to get to the cadmium phosphate lithium material in Muffle furnace.
The mass ratio of 1 LiFePO4 of embodiment and cadmium phosphate lithium is 100:1
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, is as follows：
S1, it 7.3428g ferrous oxalates is dissolved in 40mL distilled water obtains ferrous oxalate aqueous solution, by 4.9657g second two
Alcohol, which is dissolved in 10mL distilled water, obtains glycol water, and 3.9201g phosphoric acid is dissolved in 10mL distilled water to obtain phosphoric acid water-soluble
1.6785g lithium hydroxides are dissolved in 30mL distilled water and obtain lithium hydroxide aqueous solution by liquid, and 0.0631g cadmium phosphate lithiums are dissolved in
Cadmium phosphate lithium aqueous solution is obtained in 10mL distilled water, and glycol water is added dropwise in ferrous oxalate aqueous solution and obtains oxalic acid Asia
Phosphate aqueous solution is added dropwise in the glycol water of ferrous oxalate and obtains mixed solution by the glycol water of iron, by hydrogen
Lithia aqueous solution is added dropwise to the mixed solution that lithium hydroxide is obtained in mixed solution, is then added dropwise to cadmium phosphate lithium aqueous solution
Reaction solution is obtained in the mixed solution of lithium hydroxide, needs to continuously stir using glass bar in the above mixed process；
S2, the reaction solution obtained in S1 is stirred, mixing time 7h in 60 DEG C of water-baths, it is wet solidifying obtains class
Glue；
S3, it is covered with the beaker equipped with the class wet gel obtained in S2 with a large beaker, then puts it to drying box
In be dried, 100 DEG C of drying temperature, drying time 10h obtains class xerogel；
S4, the xerogel that S3 is obtained is ground to obtain powder, then powder is positioned in crucible, is protected using carbon
The three anti-oxidation measures of crucible formula, 13h is calcined at 750 DEG C in Muffle furnace, cooled to room temperature after the completion of calcining makes
With mortar grinder to get to the LiFePO4 and cadmium phosphate lithium composite material.
The mass ratio of 2 LiFePO4 of embodiment and cadmium phosphate lithium is 100:4
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 1, and difference is only
It is that the quality of the cadmium phosphate lithium used in S1 is 0.2524g.
The mass ratio of 3 LiFePO4 of embodiment and cadmium phosphate lithium is 100:7
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 1, and difference is only
It is that the quality of the cadmium phosphate lithium used in S1 is 0.4417g.
The mass ratio of 4 LiFePO4 of embodiment and cadmium phosphate lithium is 100:10
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 1, and difference is only
It is that the quality of the cadmium phosphate lithium used in S1 is 0.6310g.
The mass ratio of 5 LiFePO4 of embodiment and cadmium phosphate lithium is 100:13
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 1, and difference is only
It is that the quality of the cadmium phosphate lithium used in S1 is 0.8203g.
The mass ratio of 6 LiFePO4 of embodiment and cadmium phosphate lithium is 100:16
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 1, and difference is only
It is that the quality of the cadmium phosphate lithium used in S1 is 1.0096g.
The mass ratio of 7 LiFePO4 of embodiment and cadmium phosphate lithium is 100:7
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 1, and difference is only
It is that the quality of the cadmium phosphate lithium used in S1 is 0.4417g.
Embodiment 8
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 4, and difference is only
It is in S4 that the calcination temperature in Muffle furnace is 650 DEG C.
Embodiment 9
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 4, and difference is only
It is in S4 that the calcination temperature in Muffle furnace is 700 DEG C.
Embodiment 10
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 4, and difference is only
It is in S4 that the calcination temperature in Muffle furnace is 800 DEG C.
Embodiment 11
A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material, specific steps are same as Example 4, and difference is only
It is in S4 that the calcination time in Muffle furnace is 10h.
One, we illustrate different cadmium phosphate lithium dosages to LiFePO4 by taking composite material prepared by Examples 1 to 7 as an example
With the influence of cadmium phosphate lithium composite material
Fig. 1 be different quality than cadmium phosphate lithium and composite ferric lithium phosphate material XRD diffraction patterns.It can be seen that in Fig. 1
There is LiFePO4 peak type in each composite material, main diffraction peak includes 200,101,111,211 and 311, with LiFePO4 mark
Quasi- card value corresponds；In addition each composite material is there is also cadmium phosphate lithium peak type, main diffraction peak has 200,101,111,
020,301,311 and 410, it is corresponded with cadmium phosphate lithium standard card chip value；Each diffraction maximum peak type is sharp, and crystallinity is good, says
It is bright to successfully synthesize cadmium phosphate lithium/composite ferric lithium phosphate material, and illustrate crystal of the introducing to LiFePO4 of cadmium phosphate lithium
Structure does not influence significantly, and as seen in Figure 1 when the mass ratio of LiFePO4 and cadmium phosphate lithium is 100:When 10,
The diffraction peak intensity of composite material is most strong, therefore the mass ratio of subsequent experimental LiFePO4 and cadmium phosphate lithium is 100:10.
1 different quality of table than LiFePO4 and cadmium phosphate lithium composite material magnetic parameter table
Fig. 2 be different quality than cadmium phosphate lithium and composite ferric lithium phosphate material hysteresis loop figure, all samples exist
It is tested at room temperature.It is larger to can be seen that the magnetic characteristic of the composite ferric lithium phosphate material of different content cadmium phosphate lithium has in Fig. 2
Variation, table 1 be different quality than LiFePO4 and cadmium phosphate lithium composite material magnetic parameter table.It can be seen from Table 1 that
Saturation magnetization Ms (emu/g) reduces with the increase of cadmium phosphate lithium addition, and coercivity H adds with cadmium phosphate lithium
Enter the increase of amount substantially in the trend of reduction after first increasing.
Fig. 3 is LiFePO4 and cadmium phosphate lithium mass ratio is 100:The composite material scanning electron microscope prepared under the conditions of 10
Figure, Fig. 4 is LiFePO4 and cadmium phosphate lithium mass ratio is 100:The composite material granular statistical chart prepared under the conditions of 10.Fig. 3
Show that the graininess of composite material is apparent, dispersibility is preferably.Fig. 4 results show that particle size distribution obeys class normal distribution,
Grain size is concentrated mainly on 700nm or so.
To sum up, the mass ratio of LiFePO4 and cadmium phosphate lithium is 100 in embodiment 4:The material prepared when 10 has good
Magnetism and structure.
Two, we illustrate influence of the different calcination temperatures to sample by taking composite material prepared by embodiment 4,8~10 as an example
Fig. 5 is the XRD diffraction patterns that composite material is prepared using different calcination temperatures.It can be seen that each composite material in Fig. 5
There are LiFePO4Peak type, main diffraction peak include 200,101,111,211,311 etc., one by one with LiFePO4 standard card chip value
Corresponding, in addition there is also LiCdPO4Peak type, main diffraction peak have 200,101,111,020,301,311,410 etc., with cadmium phosphate
Lithium standard card chip value corresponds, and each diffraction maximum peak type is sharp, and crystallinity is good, illustrates successfully to synthesize under different calcination temperatures
The composite material of cadmium phosphate lithium and LiFePO4 is gone out, and calcination temperature does not have prodigious shadow to the crystal structure of LiFePO4
It rings, from, it can also be seen that when calcination temperature is 750 DEG C in S4, the intensity of each diffraction maximum of the composite material of preparation is most in Fig. 5
By force, i.e., the crystallinity of the composite material prepared under this condition is best.
Fig. 6 is the hysteresis loop figure of the cadmium phosphate lithium and composite ferric lithium phosphate material that are synthesized under different calcination temperatures, is owned
Sample is tested at room temperature.It can be seen that the LiFePO4 of the cadmium phosphate lithium prepared under different calcination temperatures is multiple in Fig. 6
The magnetic characteristic of condensation material has a greater change, and table 2 is the LiFePO4 prepared under different calcination temperatures and cadmium phosphate lithium composite
Expect magnetic parameter table.It can be seen from Table 2 that saturation magnetization Ms (emu/g) is in after first increasing with the increase of calcination temperature
The trend of reduction, and coercivity H is in increased trend after first reducing substantially with the increase of calcination temperature.It can by the above results
To find out, when the calcination temperature in S4 is 750 DEG C, the properties of sample can reach best.
The LiFePO4 and cadmium phosphate lithium composite material magnetic parameter table prepared under the different calcination temperatures of table 2
Three, we illustrate influence of the different calcination times to sample by taking composite material prepared by embodiment 4 and 11 as an example
Fig. 7 is cadmium phosphate lithium (LiCdPO prepared by different calcination times4) and LiFePO4 (LiFePO4) composite material
XRD diffraction patterns.It can be seen that each composite material synthesized under different calcination times has LiFePO4 peak type, mainly in Fig. 7
Diffraction maximum include 200,101,111,211,311 etc., with LiFePO4 standard card chip value correspond, in addition there is also
LiCdPO4Peak type, main diffraction peak have 200,101,111,020,301,311,410 etc., with cadmium phosphate lithium standard card chip value one
One corresponds to, and each diffraction maximum peak type is sharp, and crystallinity is good, illustrate successfully to have synthesized under different calcination times cadmium phosphate lithium with
The composite material of LiFePO4, and calcination time does not have a great impact to the crystal structure of LiFePO4, can be with from Fig. 7
Find out that the intensity of each diffraction maximum of the composite material of preparation is most strong, i.e., prepares under this condition when calcination time is 10h in S4
The crystallinity of composite material is best.
Fig. 8 is the hysteresis loop figure of the cadmium phosphate lithium and composite ferric lithium phosphate material that are synthesized under different calcination times, is owned
Sample is tested at room temperature.It can be seen that the LiFePO4 of the cadmium phosphate lithium prepared under different calcination times is multiple in Fig. 8
The magnetic characteristic of condensation material has a greater change, and table 2 is the LiFePO4 prepared under different calcination times and cadmium phosphate lithium composite
Expect magnetic parameter table.It can be seen from Table 2 that saturation magnetization Ms (emu/g) increases with the increase of calcination time, and
Coercivity H reduces with the increase of calcination time.It can be seen from the above results when the calcination time in S4 is 10h,
The properties of sample can reach best.
To sum up, the present invention uses sol-gel method self-assembling technique, is prepared by two-step synthesis method under high-temperature calcination
The composite material of cadmium phosphate lithium and LiFePO4, and its structure, magnetic property studied.XRD shows in ferrous oxalate, second
Glycol, phosphoric acid, lithium hydroxide, cadmium phosphate lithium collective effect under, be successfully prepared and prepared using sol-gel self-assembling technique
Cadmium phosphate lithium and composite ferric lithium phosphate material of the particle size in 700nm or so.By adjusting cadmium phosphate lithium and LiFePO4
Mass ratio, calcination temperature and calcination time, find cadmium phosphate lithium and LiFePO4 mass ratio, calcination temperature and calcination time
Change to the structure of composite material and magnetic have certain adjustment effect.
To sum up, it is believed that the preparation method of embodiment 11 is preferred plan, remaining embodiment can be prepared by cadmium phosphate
Lithium and composite ferric lithium phosphate material, only effect is a bit weaker.
It should be noted that involved in claims of the present invention when numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, since the step method of use is identical as embodiment,
It repeats in order to prevent, the present invention describes preferred embodiment and its effect, and once a person skilled in the art knows bases
This creative concept, then additional changes and modifications may be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (4)
1. the preparation method of a kind of LiFePO4 and cadmium phosphate lithium composite material, which is characterized in that include the following steps：
S1, it ferrous oxalate is dissolved in distilled water obtains ferrous oxalate aqueous solution, ethylene glycol is dissolved in distilled water and obtains second two
Phosphoric acid is dissolved in distilled water and obtains phosphate aqueous solution by alcohol solution, and lithium hydroxide is dissolved in distilled water and obtains lithium hydroxide
Cadmium phosphate lithium is dissolved in distilled water and obtains cadmium phosphate lithium aqueous solution, glycol water is added dropwise to ferrous oxalate by aqueous solution
The glycol water that ferrous oxalate is obtained in aqueous solution, phosphate aqueous solution is added dropwise in the glycol water of ferrous oxalate
Mixed solution is obtained, lithium hydroxide aqueous solution is added dropwise to the mixed solution for obtaining lithium hydroxide in mixed solution, then by phosphorus
Sour cadmium lithium aqueous solution, which is added dropwise in the mixed solution of lithium hydroxide, obtains reaction solution, needs to continuously stir in the above mixed process；
Wherein, ferrous oxalate, ethylene glycol, phosphoric acid, lithium hydroxide, cadmium phosphate lithium molar ratio be 5:8:4:4:0.03~0.5；
S2, the reaction solution obtained in S1 is stirred in 50~80 DEG C of water-baths, mixing time is 5~10h, is obtained wet solidifying
Glue；
S3, the wet gel obtained in S2 is dried, 90~120 DEG C, 8~15h of drying time of drying temperature, it is dry solidifying obtains class
Glue；
S4, the xerogel that S3 is obtained is ground to obtain powder, then powder is positioned in crucible, using the three of carbon protection
The anti-oxidation measure of crucible formula calcines 10~13h at 650~800 DEG C in Muffle furnace, room is naturally cooled to after the completion of calcining
Temperature, using mortar grinder to get to the LiFePO4 and cadmium phosphate lithium composite material.
2. the preparation method of a kind of LiFePO4 according to claim 1 and cadmium phosphate lithium composite material, which is characterized in that
In S1, the cadmium phosphate lithium is made by the steps：
S11, it lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol is added in distilled water carries out mixed dissolution, in 50~80 DEG C of water
5~10h is stirred in bath, obtains gel；Wherein, the molar ratio of lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol is 1:1:1:1~
3；
S12, the gel obtained in S11 at 100~140 DEG C is dried into 5~10h, mortar grinder is then used, then in activity
Under powdered carbon protective condition, 600~900 DEG C of 4~16h of calcining are to get to the cadmium phosphate lithium material in Muffle furnace.
3. the preparation method of a kind of LiFePO4 according to claim 1 and cadmium phosphate lithium composite material, which is characterized in that
In S4,750 DEG C of calcining 10h in Muffle furnace.
4. the preparation method of a kind of LiFePO4 according to claim 1 and cadmium phosphate lithium composite material, which is characterized in that
In S2, bath temperature is 60 DEG C, mixing time 7h.
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