CN107673321B - A kind of cadmium phosphate lithium material and its synthetic method - Google Patents
A kind of cadmium phosphate lithium material and its synthetic method Download PDFInfo
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- CN107673321B CN107673321B CN201711137184.6A CN201711137184A CN107673321B CN 107673321 B CN107673321 B CN 107673321B CN 201711137184 A CN201711137184 A CN 201711137184A CN 107673321 B CN107673321 B CN 107673321B
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- 239000000463 material Substances 0.000 title claims abstract description 51
- VFCHTESWBCQZRZ-UHFFFAOYSA-K [Li+].P(=O)([O-])([O-])[O-].[Cd+2] Chemical compound [Li+].P(=O)([O-])([O-])[O-].[Cd+2] VFCHTESWBCQZRZ-UHFFFAOYSA-K 0.000 title claims abstract description 47
- 238000010189 synthetic method Methods 0.000 title abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 47
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 42
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 42
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 12
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 12
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 239000011240 wet gel Substances 0.000 claims abstract description 8
- 239000008236 heating water Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000000499 gel Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000005415 magnetization Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- NRGIRRZWCDKDMV-UHFFFAOYSA-H cadmium(2+);diphosphate Chemical compound [Cd+2].[Cd+2].[Cd+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O NRGIRRZWCDKDMV-UHFFFAOYSA-H 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- YYVXOEQBDYYRKU-UHFFFAOYSA-K lithium;zinc;phosphate Chemical compound [Li+].[Zn+2].[O-]P([O-])([O-])=O YYVXOEQBDYYRKU-UHFFFAOYSA-K 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910013275 LiMPO Inorganic materials 0.000 description 1
- 229910001305 LiMPO4 Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910014880 LixPO4 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- PLDDNNMQJMAEGX-UHFFFAOYSA-K [Li+].P(=O)([O-])([O-])[O-].[Sr+2] Chemical compound [Li+].P(=O)([O-])([O-])[O-].[Sr+2] PLDDNNMQJMAEGX-UHFFFAOYSA-K 0.000 description 1
- CUQSVGNVMULJSV-UHFFFAOYSA-K [Li+].[Mg++].[O-]P([O-])([O-])=O Chemical compound [Li+].[Mg++].[O-]P([O-])([O-])=O CUQSVGNVMULJSV-UHFFFAOYSA-K 0.000 description 1
- YSZKOFNTXPLTCU-UHFFFAOYSA-N barium lithium Chemical compound [Li].[Ba] YSZKOFNTXPLTCU-UHFFFAOYSA-N 0.000 description 1
- 229910000011 cadmium carbonate Inorganic materials 0.000 description 1
- KOHRTFCSIQIYAE-UHFFFAOYSA-N cadmium;carbonic acid Chemical compound [Cd].OC(O)=O KOHRTFCSIQIYAE-UHFFFAOYSA-N 0.000 description 1
- JKDBPVARNVYJPG-UHFFFAOYSA-K calcium;lithium;phosphate Chemical compound [Li+].[Ca+2].[O-]P([O-])([O-])=O JKDBPVARNVYJPG-UHFFFAOYSA-K 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 phosphoric acid Cadmium lithium Chemical compound 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- QVLTXCYWHPZMCA-UHFFFAOYSA-N po4-po4 Chemical compound OP(O)(O)=O.OP(O)(O)=O QVLTXCYWHPZMCA-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a kind of cadmium phosphate lithium material and its synthetic methods, are related to technical field of inorganic material synthesis.This method comprises: lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol are weighed according to the ratio between the amount of substance of 1:1:1:2; then addition distilled water, which is dissolved, is mixed to get mixed solution; mixed solution is subjected to heating water bath and is stirred using blender; obtain wet gel; wet gel is dried to obtain xerogel; xerogel is ground and enters in Muffle furnace to calcine in the protection down of active carbon powder, is ground to obtain cadmium phosphate lithium sample after calcining.The present invention synthesizes cadmium phosphate lithium material by sol-gal process, preparation process is easy to operate, preparation condition is mild and low in cost, the cadmium phosphate lithium material crystal structure degree of synthesis is good, good dispersion, stable structure, and determine that the magnetic property for the cadmium phosphate lithium material being prepared under 800 DEG C and 12h of calcination condition is relatively best, there is fine application prospect.
Description
Technical field
The present invention relates to technical field of inorganic material synthesis, specially a kind of cadmium phosphate lithium material and its synthetic method.
Background technique
The development and utilization of the energy and the development of human society are closely bound up, with the development of science and technology lithium ion battery because
It has many advantages, such as that high density energy, long circulation life, low self-discharge rate and green non-pollution cause to study extensively.Wherein make
For the LiMPO of anode material4The visual field of the advantages such as high, cheap into everybody with specific capacity (M=Fe, Co, Mn, V etc.).With
To the LiMPO4The research of type anode material has similar LiXPO4The substance of structural formula attracts attention, including phosphorus
Sour barium-lithium (LiBaPO4), calcium phosphate lithium (LiCaPO4), magnesium phosphate lithium (LiMgPO4), strontium phosphate lithium (LiSrPO4), lithium zinc phosphate
(LiZnPO4) and cadmium phosphate lithium (LiCdPO4) etc..
But at present for cadmium phosphate lithium (LiCdPO4) research it is relatively fewer, only ELAMMARIL and ELOUADIB etc.
Li was used in 19882CO3、CdCO3、(NH4)2HPO4Cadmium phosphate lithium (LiCdPO is prepared for for raw material4), and carry out finishing structure and grind
Study carefully, and passed through X ray diffracting data to cadmium phosphate lithium (LiCdPO in 19924) carry out refine again.But current phosphoric acid
Cadmium lithium (LiCdPO4) preparation method it is still less, preparation method is immature, and causing the material in application aspect, there are technology bottles
Neck.
Summary of the invention
In order to solve the deficiencies in the prior art, a kind of utilization sol-gal process synthesis cadmium phosphate provided by the invention
The method of lithium material, easy to operate, mild condition and low in cost.
A kind of method using sol-gal process synthesis cadmium phosphate lithium material provided by the invention, comprising the following steps:
S1, lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol are weighed according to the ratio between amount of substance of 1:1:1:2, so
After prepare mixed solution；
S2, the mixed solution for obtaining S1 carry out heating water bath, while being stirred continuously, water bath heating temperature 70-
90 DEG C, the heating water bath time is 5-6h, obtains wet gel；
S3, the wet gel for obtaining S2 are dried, and drying temperature is 110-130 DEG C, and drying time 10-15h is obtained
Xerogel；
Powder is placed in three layers of ceramic crucible of active carbon powder protection by S4, the xerogel grind into powder for obtaining S3
In, it is then calcined in Muffle furnace, calcination time 4-16h, calcination temperature is 600-900 DEG C；
S5, sample calcined in S4 is ground to obtain cadmium phosphate lithium sample.
Preferably, the preparation process of the mixed solution in S1 are as follows:
Distilled water is added first into phosphoric acid and obtains phosphoric acid solution, weigh cadmium nitrate and ethylene glycol and distilled water progress is added
Dissolution obtains the ethylene glycol solution of cadmium nitrate, lithium hydroxide is dissolved to obtain lithium hydroxide solution with distilled water, then by nitric acid
The ethylene glycol solution of cadmium is added dropwise in phosphoric acid solution, while being stirred continuously to obtain solution A, finally drips lithium hydroxide solution
It is added in solution A, and is stirred continuously during dropwise addition, obtain mixed solution.
Preferably, the placement process of three layers of ceramic crucible of the active carbon powder protection in S4 are as follows:
Crucible A, crucible B and the crucible C for selecting specification different, wherein the size of crucible A is less than crucible B, the size of crucible B
Less than crucible C, powder obtained in S3 is placed in crucible A and is covered crucible cover, then crucible A is integrally put into crucible B
And crucible cover is covered, crucible B is integrally put into crucible C, and be packed into active carbon powder into crucible C, covers crucible cover, obtain
Three layers of ceramic crucible of active carbon powder protection.
Preferably, the calcination atmosphere in S4 is air atmosphere.
Compared with prior art, preparation method of the invention has the advantages that
The present invention prepares mixed solution by weighing and dissolving lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol in proportion,
Mixed solution is subjected to heating water bath, drying and calcining and obtains cadmium phosphate lithium material.The preparation method is easy to operate, condition temperature
Cheap with cost of manufacture, the cadmium phosphate lithium material graininess being prepared is obvious, and dispersibility is preferable, stable structure, wherein different
Calcine technology has large effect to the magnetic property of cadmium phosphate lithium material, with the increase of calcination temperature and calcination time, satisfies
The trend of first increases and then decreases is presented with the intensity of magnetization, accordingly, it is determined that the optimum condition of calcining is 800 DEG C and 12h.
Detailed description of the invention
Fig. 1 is cadmium phosphate lithium (LiCdPO prepared by embodiment 14) material scanning electron microscope (SEM) photograph；
Fig. 2 is cadmium phosphate lithium (LiCdPO prepared by embodiment 14) material granularmetric analysis figure；
Fig. 3 is the cadmium phosphate lithium (LiCdPO of different calcination temperatures preparation4) material X-ray diffractogram；
Fig. 4 is the cadmium phosphate lithium (LiCdPO of different calcination temperatures preparation4) material hysteresis loop figure；
Fig. 5 is the cadmium phosphate lithium (LiCdPO of different calcination times preparation4) material X-ray diffractogram；
Fig. 6 is the cadmium phosphate lithium (LiCdPO of different calcination times preparation4) material hysteresis loop figure；
Specific embodiment
Embodiment 1
A method of cadmium phosphate lithium material is prepared using sol-gal process, comprising the following steps:
S1, by lithium hydroxide (LiOHH2O), cadmium nitrate (Cd (NO3)2·4H2O), phosphoric acid (H3PO4) and ethylene glycol
(C2H6O2) 1.6784g, 12.3389g, 3.9201g and 4.9657g are weighed respectively, 50ml distilled water is then added into phosphoric acid
Phosphoric acid solution is obtained, 100ml distilled water is added after cadmium nitrate and ethylene glycol are mixed and dissolves to obtain the ethylene glycol solution of cadmium nitrate,
Lithium hydroxide is dissolved to obtain lithium hydroxide solution with 50ml distilled water, the ethylene glycol solution of cadmium nitrate is then added dropwise to phosphoric acid
It in solution, while being stirred continuously to obtain mixed solution A, finally lithium hydroxide solution is added drop-wise in mixed solution A, and
It is stirred continuously, obtains mixed solution；
S2, the mixed solution that S1 is obtained is subjected to heating water bath at 80 DEG C while being stirred continuously, stirred 5h, obtain
Wet gel；
S3, the resulting wet gel of S2 is dried at 120 DEG C, drying time 10h obtains xerogel；
S4, S3 is obtained to xerogel grind into powder, crucible A, crucible B and the crucible C for then selecting specification different, wherein
The size of crucible A is less than crucible B, and the size of crucible B is less than crucible C, is placed in crucible A and covers crucible cover for powder, then
Crucible A is integrally put into crucible B and is covered crucible cover, crucible B is integrally put into crucible C, and is packed into activity into crucible C
Carbon powder covers crucible cover, obtains three layers of ceramic crucible of active carbon powder protection, which is placed in Muffle furnace and is calcined,
Calcination temperature is 800 DEG C, calcination time 12h；
S5, sample calcined in S4 is ground to obtain cadmium phosphate lithium sample powder.
Embodiment 2
Preparation method is same as Example 1, the difference is that calcination temperature of the dry gel powder in Muffle furnace is 600 DEG C.
Embodiment 3
Preparation method is same as Example 1, the difference is that calcination temperature of the dry gel powder in Muffle furnace is 700 DEG C.
Embodiment 4
Preparation method is same as Example 1, the difference is that calcination temperature of the dry gel powder in Muffle furnace is 900 DEG C.
The cadmium phosphate lithium material that we prepare embodiment 1 is scanned testing electronic microscope, and Fig. 1 is the system of embodiment 1
The SEM spectrum of standby cadmium phosphate lithium material, Fig. 2 are the grain size distribution obtained according to scanning electron microscope test, can from Fig. 1
To find out, the graininess of the material is obvious, and dispersibility is preferable, from figure 2, it is seen that the particle size distribution of the material obeys class normal state
Distribution, granular size are concentrated mainly on 1.5um or so.
The cadmium phosphate lithium material prepared under the different calcination temperatures that we provide embodiment 1- embodiment 4 carries out XRD survey
Examination and hysteresis loop test.
Fig. 3 is the XRD spectrum of the cadmium phosphate lithium material of different calcination temperatures preparation, and calcination temperature is respectively 600 DEG C, 700
DEG C, 800 DEG C and 900 DEG C, table 1 is the XRD parameter list of the cadmium phosphate lithium material of different calcination temperature preparations, according to Fig. 3 and table 1
Obtain the corresponding crystal face value (200) of main diffraction peak of the material sample, (101), (111), (020), (301), (410) etc.
Corresponded with standard card (PDF#81-0508), illustrating each material all has complete pure phase cadmium phosphate lithium peak type, and
Crystallinity is good, and minor change only occurs for the lattice parameter of the sample, illustrate when calcination temperature is between 600-900 DEG C for
Cadmium phosphate lithium (LiCdPO4) synthesis influence it is smaller.
The XRD parameter list of the cadmium phosphate lithium material of the different calcination temperature preparations of table 1
Fig. 4 and table 2 are respectively that the magnetic hysteresis of the cadmium phosphate lithium material of different calcination temperatures prepared by embodiment 1- embodiment 4 is returned
Line chart and the magnetic parameter table obtained according to hysteresis loop, obtain different calcination temperatures according to hysteresis loop test result and prepare material
The magnetic characteristic of material has a greater change, and wherein saturation magnetization, remanent magnetization and coercivity are with calcination time
Increase and variation tendency is had nothing in common with each other, saturation magnetization and remanent magnetization presentation first increase the trend reduced afterwards, coercive
The trend for being first significantly increased and then reducing is presented in power.From each magnetism of material energy Parameter analysis, the material of 800 DEG C of calcinings has maximum
Saturation magnetization, relatively illustrate 800 DEG C calcining have better magnetic property.
The magnetic parameter table of the cadmium phosphate lithium material of the different calcination temperature preparations of table 2
Embodiment 5
Preparation method is same as Example 1, the difference is that calcination time of the dry gel powder in Muffle furnace is 4h.
Embodiment 6
Preparation method is same as Example 1, the difference is that calcination time of the dry gel powder in Muffle furnace is 8h.
Embodiment 7
Preparation method is same as Example 1, the difference is that calcination time of the dry gel powder in Muffle furnace is 16h.
The cadmium phosphate for the different calcination times preparation that we provide embodiment 1, embodiment 5, embodiment 6 and embodiment 7
Lithium material carries out XRD test and hysteresis loop test.
Fig. 5 is the XRD spectrum of the cadmium phosphate lithium material of different calcination time preparations, and calcination time is respectively 4h, 8h, 12h
And 16h, table 3 are the XRD parameter lists of the cadmium phosphate lithium material of different calcination time preparations, obtain difference according to Fig. 5 and table 3 and forge
Burn the corresponding crystal face value (200) of main diffraction peak of material sample of time preparation, (101), (111), (020), (301),
(410) etc. it is corresponded with standard card (PDF#81-0508), illustrating each material all has complete pure phase cadmium phosphate lithium peak
Type, and crystallinity is good, and minor change only occurs for the lattice parameter of the sample, illustrates calcination time for cadmium phosphate lithium
(LiCdPO4) synthesis influence it is smaller.
The XRD parameter list of the cadmium phosphate lithium material of the different calcination time preparations of table 3
Fig. 6 and table 4 are respectively the cadmium phosphate lithium (LiCdPO of different calcination time preparations4) material hysteresis loop figure and root
The magnetic parameter table obtained according to hysteresis loop, according to Fig. 6 and table 4 obtain different calcination times prepare material magnetic characteristic have it is larger
Variation, wherein saturation magnetization, remanent magnetization and coercivity are with the increase of calcination time and variation tendency is each
Different, then saturation magnetization and remanent magnetization, which first increase, to be reduced, coercivity present first reduce then it is increased become
Gesture.From each magnetism of material energy Parameter analysis, the material for calcining 12h has maximum saturation magnetization, relatively illustrates to calcine
12h has better magnetic property.
The magnetic parameter table of the cadmium phosphate lithium material of the different calcination time preparations of table 4
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of method using sol-gal process synthesis cadmium phosphate lithium material, which comprises the following steps:
S1, lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol are weighed according to the ratio between amount of substance of 1:1:1:2, is then made
Standby mixed solution；
S2, the mixed solution for obtaining S1 carry out heating water bath, while being stirred continuously, and water bath heating temperature is 70-90 DEG C,
The heating water bath time is 5-6h, obtains wet gel；
S3, the wet gel for obtaining S2 are dried, and drying temperature is 110-130 DEG C, drying time 10-15h, obtain dry solidifying
Glue；
Powder is placed in three layers of ceramic crucible of active carbon powder protection, so by S4, the xerogel grind into powder for obtaining S3
It is calcined in Muffle furnace afterwards, calcination time 4-16h, calcination temperature is 600-900 DEG C；
S5, sample calcined in S4 is ground to obtain cadmium phosphate lithium sample.
2. a kind of method using sol-gal process synthesis cadmium phosphate lithium material as described in claim 1, which is characterized in that institute
State the preparation process of mixed solution in S1 are as follows:
Distilled water is added first into phosphoric acid and obtains phosphoric acid solution, weighs cadmium nitrate and ethylene glycol and distilled water is added and obtain nitric acid
The ethylene glycol solution of cadmium dissolves lithium hydroxide with distilled water to obtain lithium hydroxide solution, then that the ethylene glycol of cadmium nitrate is molten
Liquid is added dropwise in phosphoric acid solution, while being stirred continuously to obtain solution A, and finally lithium hydroxide solution is added drop-wise in solution A,
And it is stirred continuously in dropwise addition process, obtains mixed solution.
3. a kind of method using sol-gal process synthesis cadmium phosphate lithium material as described in claim 1, which is characterized in that institute
State the placement process for three layers of ceramic crucible that active carbon powder is protected in S4 are as follows:
Crucible A, crucible B and the crucible C for selecting specification different, wherein the size of crucible A is less than crucible B, and the size of crucible B is less than
Dry gel powder obtained in S3 is placed in crucible A and is covered crucible cover, crucible A is integrally then put into crucible B by crucible C
In, crucible cover is covered, crucible B is integrally put into crucible C, and is packed into active carbon powder into crucible C, crucible cover is covered, obtains
The three layers of ceramic crucible protected to active carbon powder.
4. a kind of method using sol-gal process synthesis cadmium phosphate lithium material as described in claim 1, which is characterized in that institute
Stating the calcination atmosphere in step S4 is air atmosphere.
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| CN108520948A (en) * | 2018-04-11 | 2018-09-11 | 广西师范大学 | A method of preparing magnesia coated LiFePO 4 for lithium ion batteries carbon composite using sol-gal process |
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