CN107673321A - 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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- CN107673321A CN107673321A CN201711137184.6A CN201711137184A CN107673321A CN 107673321 A CN107673321 A CN 107673321A CN 201711137184 A CN201711137184 A CN 201711137184A CN 107673321 A CN107673321 A CN 107673321A
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 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 49
- 238000010189 synthetic method Methods 0.000 title claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 48
- 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
- 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 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 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
- 230000008569 process Effects 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
- 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
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- 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
- 238000005516 engineering process Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000011160 research 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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-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
- 230000008859 change Effects 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
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 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
- 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
- ADCXHZZSUADYMI-UHFFFAOYSA-N cadmium lithium Chemical compound [Li].[Cd] ADCXHZZSUADYMI-UHFFFAOYSA-N 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
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 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
- 239000002245 particle Substances 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 method, it is related to technical field of inorganic material synthesis.This method includes：By lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol according to 1:1:1:The ratio between 2 amount of material is weighed; then addition distilled water, which is dissolved, is mixed to get mixed solution; mixed solution is subjected to heating water bath and stirred using agitator; obtain wet gel; wet gel is dried to obtain xerogel; xerogel is ground and calcined in the protection down of active carbon powder enters Muffle furnace, 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 simple to operate, preparation condition is gentle and cost is cheap, the cadmium phosphate lithium material crystal structure degree of synthesis is good, good dispersion, Stability Analysis of Structures, and determine that the magnetic property of cadmium phosphate lithium material that is prepared under 800 DEG C and 12h calcination conditions is relatively best, has 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 technology
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 is widely studied that it has the advantages that high density energy, long circulation life, low self-discharge rate and green non-pollution cause.Wherein make
For the LiMPO of anode material4(M=Fe, Co, Mn, V etc.) is so that specific capacity is high, the advantage such as cheap enters everybody visual field.With
To the LiMPO4The research of type anode material, there is similar LiXPO4The material 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 ELAMMARI L and ELOUADI B
Li was used equal to 19882CO3、CdCO3、(NH4)2HPO4Cadmium phosphate lithium (LiCdPO is prepared for for raw material4), and carry out finishing structure
Research, and in 1992 by X ray diffracting data to cadmium phosphate lithium (LiCdPO4) carry out refine again.But current phosphorus
Sour cadmium lithium (LiCdPO4) preparation method it is still less, preparation method is immature, causes the material technology to be present in application aspect
Bottleneck.
The content of the invention
In order to solve the deficiencies in the prior art, one kind provided by the invention utilizes sol-gal process synthesis cadmium phosphate
The method of lithium material, simple to operate, mild condition and cost is cheap.
A kind of method that cadmium phosphate lithium material is synthesized using sol-gal process provided by the invention, is comprised the following steps：
S1, by lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol according to 1:1:1:The ratio between 2 amount of material is weighed, so
After prepare mixed solution；
S2, the mixed solution for obtaining S1 carry out heating water bath, while are 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, drying time 10-15h, is obtained
Xerogel；
S4, the xerogel grind into powder for obtaining S3, powder is placed in three layers of ceramic crucible of active carbon powder protection
In, then calcined in Muffle furnace, calcination time 4-16h, calcining heat is 600-900 DEG C；
S5, by S4 calcine after sample grind to obtain cadmium phosphate lithium sample.
Preferably, the preparation process of the mixed solution in S1 is：
Distilled water is added first into phosphoric acid and obtains phosphoric acid solution, cadmium nitrate and ethylene glycol is weighed and adds distilled water progress
Dissolving obtains the ethylene glycol solution of cadmium nitrate, lithium hydroxide is dissolved with distilled water to obtain lithium hydroxide solution, then by nitric acid
The ethylene glycol solution of cadmium is added dropwise in phosphoric acid solution, while is stirred continuously to obtain solution A, finally drips lithium hydroxide solution
It is added in solution A, and is stirred continuously during dropwise addition, obtains mixed solution.
Preferably, the placement process of three layers of ceramic crucible of the active carbon powder protection in S4 is：
Specification different crucible A, crucible B and crucible C are selected, wherein crucible A size is less than crucible B, crucible B size
Less than crucible C, the powder obtained in S3 is placed in crucible A and covers 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 load active carbon powder into crucible C, crucible cover is covered, is obtained
Three layers of ceramic crucible of active carbon powder protection.
Preferably, the calcination atmosphere in S4 is air atmosphere.
The present invention also protects the cadmium phosphate lithium material being prepared by above-mentioned preparation method.
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 simple to operate, condition temperature
Cheap with, cost of manufacture, the cadmium phosphate lithium material graininess being prepared is obvious, dispersiveness preferably, Stability Analysis of Structures, wherein different
Calcine technology has large effect to the magnetic property of cadmium phosphate lithium material, with the increase of calcining heat 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.
Brief description of the drawings
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 cadmium phosphate lithium (LiCdPO prepared by different calcining heats4) material X-ray diffractogram；
Fig. 4 is cadmium phosphate lithium (LiCdPO prepared by different calcining heats4) material hysteresis curve figure；
Fig. 5 is cadmium phosphate lithium (LiCdPO prepared by different calcination times4) material X-ray diffractogram；
Fig. 6 is cadmium phosphate lithium (LiCdPO prepared by different calcination times4) material hysteresis curve figure；
Embodiment
Embodiment 1
A kind of method that cadmium phosphate lithium material is prepared using sol-gal process, is comprised 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, adding 100ml distilled water after cadmium nitrate and ethylene glycol are mixed dissolves to obtain the ethylene glycol solution of cadmium nitrate,
Lithium hydroxide is dissolved with 50ml distilled water to obtain lithium hydroxide solution, the ethylene glycol solution of cadmium nitrate is then added dropwise to phosphoric acid
In solution, while it is 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 is stirred continuously, stirred 5h, obtain
Wet gel；
S3, the wet gel obtained by S2 is dried at 120 DEG C, drying time 10h, obtains xerogel；
S4, S3 is obtained to xerogel grind into powder, then select specification different crucible A, crucible B and crucible C, wherein
Crucible A size is less than crucible B, and crucible B size is less than crucible C, powder is placed in crucible A and covers crucible cover, then
Crucible A is integrally put into crucible B and covers crucible cover, crucible B is integrally put into crucible C, and loads activity into crucible C
Carbon powder, crucible cover is covered, obtains three layers of ceramic crucible of active carbon powder protection, the crucible is placed in Muffle furnace and calcined,
Calcining heat is 800 DEG C, calcination time 12h；
S5, by S4 calcine after sample grind to obtain cadmium phosphate lithium sample powder.
Embodiment 2
Preparation method is same as Example 1, the difference is that calcining heat 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 calcining heat 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 calcining heat of the dry gel powder in Muffle furnace is 900 DEG C.
The cadmium phosphate lithium material that we prepare to embodiment 1 is scanned testing electronic microscope, and Fig. 1 is that embodiment 1 is made
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 dispersiveness 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 calcining heats that we are provided embodiment 1- embodiments 4 carries out XRD surveys
Examination and hysteresis curve test.
Fig. 3 is the XRD spectrum of cadmium phosphate lithium material prepared by different calcining heats, and calcining heat is respectively 600 DEG C, 700
DEG C, 800 DEG C and 900 DEG C, table 1 is the XRD parameter lists of cadmium phosphate lithium material prepared by different calcining heats, according to Fig. 3 and table 1
Obtain the corresponding crystal face value (200) of the main diffraction peak of the material sample, (101), (111), (020), (301), (410) etc.
Corresponded with standard card (PDF#81-0508), illustrate that each material all has complete pure phase cadmium phosphate lithium peak type, and
Crystallinity is good, and minor variations only occur for the lattice parameter of the sample, illustrate calcining heat when between 600-900 DEG C for
Cadmium phosphate lithium (LiCdPO4) synthesis influence it is smaller.
The XRD parameter lists of cadmium phosphate lithium material prepared by 1 different calcining heats of table
Fig. 4 and table 2 are respectively that the magnetic hysteresis of the cadmium phosphate lithium material of different calcining heats prepared by embodiment 1- embodiments 4 is returned
Line chart and the magnetic parameter table obtained according to hysteresis curve, different calcining heats are obtained according to hysteresis curve 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, which are presented, first increases 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 of calcinings there is more preferable magnetic property.
The magnetic parameter table of cadmium phosphate lithium material prepared by 2 different calcining heats of table
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 that we prepare to the different calcination times that embodiment 1, embodiment 5, embodiment 6 and embodiment 7 provide
Lithium material carries out XRD tests and hysteresis curve test.
Fig. 5 is the XRD spectrum of cadmium phosphate lithium material prepared by different calcination times, and calcination time is respectively 4h, 8h, 12h
And 16h, table 3 are the XRD parameter lists of cadmium phosphate lithium material prepared by different calcination times, 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 prepared by the time, (101), (111), (020), (301),
Etc. (410) corresponded with standard card (PDF#81-0508), illustrate that each material all has complete pure phase cadmium phosphate lithium peak
Type, and crystallinity is good, and minor variations only occur for the lattice parameter of the sample, illustrate calcination time for cadmium phosphate lithium
(LiCdPO4) synthesis influence it is smaller.
The XRD parameter lists of cadmium phosphate lithium material prepared by 3 different calcination times of table
Fig. 6 and table 4 are respectively cadmium phosphate lithium (LiCdPO prepared by different calcination times4) material hysteresis curve figure and root
The magnetic parameter table obtained according to hysteresis curve, according to Fig. 6 and table 4 obtain different calcination times prepare material magnetic characteristic have it is larger
Change, wherein saturation magnetization, remanent magnetization and coercivity are with the increase of calcination time and variation tendency is each
Have a difference, saturation magnetization and remanent magnetization first increase and then 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 explanation calcining
12h has more preferable magnetic property.
The magnetic parameter table of cadmium phosphate lithium material prepared by 4 different calcination times of table
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
- A kind of 1. method that cadmium phosphate lithium material is synthesized using sol-gal process, it is characterised in that comprise the following steps：S1, by lithium hydroxide, cadmium nitrate, phosphoric acid and ethylene glycol according to 1:1:1:The ratio between 2 amount of material is weighed, and is then made Standby mixed solution；S2, the mixed solution for obtaining S1 carry out heating water bath, while are 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；S4, the xerogel grind into powder for obtaining S3, powder is placed in three layers of ceramic crucible of active carbon powder protection, so After being calcined in Muffle furnace, calcination time 4-16h, calcining heat is 600-900 DEG C；S5, by S4 calcine after sample grind to obtain cadmium phosphate lithium sample.
- A kind of 2. method that cadmium phosphate lithium material is synthesized using sol-gal process as claimed in claim 1, it is characterised in that institute The preparation process for stating mixed solution in S1 is：Distilled water is added first into phosphoric acid and obtains phosphoric acid solution, cadmium nitrate and ethylene glycol is weighed and adds distilled water and obtain nitric acid The ethylene glycol solution of cadmium, lithium hydroxide is dissolved with distilled water to obtain lithium hydroxide solution, it is then that the ethylene glycol of cadmium nitrate is molten Liquid is added dropwise in phosphoric acid solution, while is 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.
- A kind of 3. method that cadmium phosphate lithium material is synthesized using sol-gal process as claimed in claim 1, it is characterised in that institute The placement process for stating three layers of ceramic crucible that active carbon powder in S4 is protected is：Specification different crucible A, crucible B and crucible C are selected, wherein crucible A size is less than crucible B, and crucible B size is less than Crucible C, the dry gel powder obtained in S3 is placed in crucible A and covers crucible cover, crucible A is integrally then put into crucible B In, crucible cover is covered, crucible B is integrally put into crucible C, and load active carbon powder into crucible C, crucible cover is covered, is obtained To three layers of ceramic crucible of active carbon powder protection.
- A kind of 4. method that cadmium phosphate lithium material is synthesized using sol-gal process as claimed in claim 1, it is characterised in that institute It is air atmosphere to state the calcination atmosphere in step S4.
- 5. a kind of cadmium phosphate lithium material, it is characterised in that synthesized using the synthetic method described in claim any one of 1-4 Arrive.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108565423A (en) * | 2018-04-11 | 2018-09-21 | 海南医学院 | A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material |
| CN112158821A (en) * | 2020-09-06 | 2021-01-01 | 桂林理工大学 | Preparation method and application of cadmium-fluorapatite solid solution |
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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 |
| CN108565423A (en) * | 2018-04-11 | 2018-09-21 | 海南医学院 | A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material |
| CN108565423B (en) * | 2018-04-11 | 2019-08-09 | 海南医学院 | A kind of preparation method of LiFePO4 and cadmium phosphate lithium composite material |
| CN112158821A (en) * | 2020-09-06 | 2021-01-01 | 桂林理工大学 | Preparation method and application of cadmium-fluorapatite solid solution |
| CN112158821B (en) * | 2020-09-06 | 2023-08-11 | 桂林理工大学 | Preparation method and application of cadmium-fluorapatite solid solution |
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