CN106353269B - The detection method of simple substance iron content in a kind of LiFePO4 - Google Patents
The detection method of simple substance iron content in a kind of LiFePO4 Download PDFInfo
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- CN106353269B CN106353269B CN201610796441.6A CN201610796441A CN106353269B CN 106353269 B CN106353269 B CN 106353269B CN 201610796441 A CN201610796441 A CN 201610796441A CN 106353269 B CN106353269 B CN 106353269B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The present invention discloses a kind of detection method of simple substance iron content in LiFePO4 comprising: iron phosphate powder is weighed by weight 8:1:1 and slurry is made in conductive agent, binder, is then coated with, is toasted；It is anode with the positive plate after toasting, copper foil is cathode, and CR2016 type is made and buckles electricity；Obtained CR2016 type is buckled after electricity carries out constant-voltage charge and is disassembled, and copper foil is retained；With the iron content of Atomic Absorption Spectrometry examination copper foil surface, the content of fe as in LiFePO4.Present invention firstly provides the test method of simple substance iron content in LiFePO4, this method test result is accurate and reliable, and cost is relatively low.
Description
Technical field
The invention belongs to field of lithium ion battery anode, the detection of simple substance iron content in specifically a kind of LiFePO4
Method.
Background technique
The LiFePO4 of olivine-type as a kind of anode active material of lithium ion battery, because its is safe and environment-friendly, price just
Preferably, energy density height, good cycle, are widely used in power battery and energy-storage battery field.
In the preparation process of LiFePO4, high-temperature calcination need to be passed through, iron oxide is easy quilt under high-temperature reductibility atmosphere
It is reduced into fe.Micro simple substance iron tramp is inevitably introduced in the LiFePO4 of preparation, will cause the micro- of battery
Short circuit, the defects of self discharge is big, it is therefore desirable to which the simple substance iron content of LiFePO4 is correctly evaluated.There is presently no lists
The effective ways of matter iron content detection, therefore find a kind of method of simple substance iron content in measurement LiFePO4 and have very high industry
Value.
Summary of the invention
The purpose of the present invention is to provide a kind of detection methods of simple substance iron content in LiFePO4.
The purpose of the present invention can be achieved through the following technical solutions:
The detection method of simple substance iron content in a kind of LiFePO4, which comprises the following steps:
(1) 8:1:1 in mass ratio weighs iron phosphate powder, conductive agent, binder, is mixed and made into slurry, with solvent point
It is coated on aluminum foil current collector surface after dissipating, toasts 2-6h at a temperature of 85 DEG C, the disk being punched into, weighing is denoted as m1；Take aluminium
Foil is punched into the disk of same size, and weighing is denoted as m2；
It (2) is anode with the positive plate after toasting, copper foil is cathode, and CR2016 type is made and buckles electricity；
(3) CR2016 type obtained by is buckled after electricity carries out constant-voltage charge and is disassembled, and negative copper foil is retained；
(4) it by step (3) negative copper foil 10mL dissolving with hydrochloric acid, dissolves by heating and keeps slightly boiled 30min, filtering to 100mL
Volumetric flask, constant volume are denoted as c with the iron content in Atomic Absorption Spectrometry examination solution1；
(5) copper foil is separately taken, step (4) operation is repeated, is tested as blank control, tries solution with Atomic Absorption Spectrometry
In iron content, be denoted as c2, the content of fe in LiFePO4 is calculated according to following formula:
With the iron content of Atomic Absorption Spectrometry examination copper foil surface, the content of fe as in LiFePO4.
Further scheme, the conductive agent is in conductive black, electrically conductive graphite, carbon nanotube, carbon fiber, graphene
One or more mixtures, binder are Kynoar, and solvent is N-Methyl pyrrolidone.
Further scheme, step (3) the button electricity carry out 3.8V constant-voltage charge, cut-off current 0.01C.
Beneficial effects of the present invention: the content of fe in LiFePO4, this method can be effectively detected in the method for the present invention
Test result is accurate and reliable, and cost is relatively low, and whole operation process is convenient, easily controllable, is compared with the traditional method environment friendly and pollution-free.
Specific embodiment
Present invention is further described in detail combined with specific embodiments below.
Embodiment 1
1. the preparation of positive plate
1) iron phosphate powder 1.6g is weighed, according to LiFePO4: conductive black: Kynoar=8:1:1 ratio
Conjunction slurry is carried out in 50mL beaker, is dispersed with N-Methyl pyrrolidone；
2) slurry is coated on 20 μm of aluminium foils, is then placed in 85 DEG C of baking ovens；
3) it is taken out after toasting 2h, is punched into the disk of Φ 12mm, weighed, be denoted as m1=197.5mg；
4) 20 μm of aluminium foils are taken, the disk of same size is punched into, weighs, is denoted as m2=44.1mg.
2. assembling button electricity
9 μm of copper foils are taken, the disk of same size is punched into, the negative electrode tab as button electricity；The positive plate weighed with step 1
It is assembled into CR2016 type in glove box and buckles electricity.
3. detaining electrical testing and dismantling
After CR2016 type made from step 2 buckles electricity standing 6-12h, 3.8V constant-voltage charge is carried out in new prestige test cabinet, is cut
Only electric current 0.01C；Dismantling button electricity, takes negative copper foil to test after charging.
4. iron content is tested
1) the resulting negative copper foil of step 3 is dissolved by heating with 10mL top grade pure hydrochloric acid, keeps slightly boiled 30min；
2) it filters to 100mL volumetric flask, constant volume；
3) with the iron content in Atomic Absorption Spectrometry examination solution, it is denoted as c1=0.301mg/L；
4) copper foil for being punched into Φ 12mm separately is taken, repeated the above steps, tested as blank control, experimental result is denoted as c2
=0.254mg/L.
It is 38.3ppm according to the content that following formula calculates fe in LiFePO4.
Embodiment 2
1. the preparation of positive plate
1) iron phosphate powder 1.6g is weighed, according to LiFePO4: electrically conductive graphite: Kynoar=8:1:1 ratio
Conjunction slurry is carried out in 50mL beaker, is dispersed with N-Methyl pyrrolidone；
2) slurry is coated on 20 μm of aluminium foils, is then placed in 85 DEG C of baking ovens；
3) it is taken out after toasting 6h, is punched into the disk of Φ 12mm, weighed, be denoted as m1=183.9mg；
4) 20 μm of aluminium foils are taken, the disk of same size is punched into, weighs, is denoted as m2=44.1mg.
2. assembling button electricity
9 μm of copper foils are taken, the disk of same size is punched into, the negative electrode tab as button electricity；The positive plate weighed with step 1
It is assembled into CR2016 type in glove box and buckles electricity.
3. detaining electrical testing and dismantling
After CR2016 type made from step 2 buckles electricity standing 6-12h, 3.8V constant-voltage charge is carried out in new prestige test cabinet, is cut
Only electric current 0.01C；Dismantling button electricity, takes negative copper foil to test after charging.
4. iron content is tested
1) the resulting negative copper foil of step 3 is dissolved by heating with 10mL top grade pure hydrochloric acid, keeps slightly boiled 30min；
2) it filters to 100mL volumetric flask, constant volume；
3) with the iron content in Atomic Absorption Spectrometry examination solution, it is denoted as c1=0.31mg/L；
4) copper foil for being punched into Φ 12mm separately is taken, repeated the above steps, tested as blank control, experimental result is denoted as c2
=0.26mg/L.
It is calculated according to following formula, the content of fe is 44.7ppm in LiFePO4.
Embodiment 3
1. the preparation of positive plate
1) iron phosphate powder 1.6g is weighed, according to LiFePO4: carbon fiber: Kynoar=8:1:1 ratio exists
Conjunction slurry is carried out in 50mL beaker, is dispersed with N-Methyl pyrrolidone；
2) slurry is coated on 20 μm of aluminium foils, is then placed in 85 DEG C of baking ovens；
3) it is taken out after toasting 4h, is punched into the disk of Φ 12mm, weighed, be denoted as m1=198.7mg；
4) 20 μm of aluminium foils are taken, the disk of same size is punched into, weighs, is denoted as m2=44.1mg.
2. assembling button electricity
9 μm of copper foils are taken, the disk of same size is punched into, the negative electrode tab as button electricity；The positive plate weighed with step 1
It is assembled into CR2016 type in glove box and buckles electricity.
3. detaining electrical testing and dismantling
After CR2016 type made from step 2 buckles electricity standing 6-12h, 3.8V constant-voltage charge is carried out in new prestige test cabinet, is cut
Only electric current 0.01C；Dismantling button electricity, takes negative copper foil to test after charging.
4. iron content is tested
1) the resulting negative copper foil of step 3 is dissolved by heating with 10mL top grade pure hydrochloric acid, keeps slightly boiled 30min；
2) it filters to 100mL volumetric flask, constant volume；
3) with the iron content in Atomic Absorption Spectrometry examination solution, it is denoted as c1=0.33mg/L；
4) copper foil for being punched into Φ 12mm separately is taken, repeated the above steps, tested as blank control, experimental result is denoted as c2
=0.26mg/L.
It is calculated according to following formula, the content of fe is 56.6ppm in LiFePO4.
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to case study on implementation, and described herein one
As principle be applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementation cases here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (3)
1. the detection method of simple substance iron content in a kind of LiFePO4, which comprises the following steps:
(1) 8:1:1 in mass ratio weighs iron phosphate powder, conductive agent, binder, is mixed and made into slurry, after being dispersed with solvent
It is coated on aluminum foil current collector surface, 2-6h is toasted at a temperature of 85 DEG C, is punched into disk, weighs, is denoted as m1；Aluminium foil is taken, is punched
At the disk of same size, weighing is denoted as m2；
It (2) is anode with the positive plate after toasting, copper foil is cathode, and CR2016 type is made and buckles electricity；
(3) CR2016 type obtained by is buckled after electricity carries out constant-voltage charge and is disassembled, and negative copper foil is retained；
(4) it by step (3) negative copper foil 10mL dissolving with hydrochloric acid, dissolves by heating and keeps slightly boiled 30min, filtering to 100mL capacity
Bottle, constant volume are denoted as c with the iron content in Atomic Absorption Spectrometry examination solution1；
(5) copper foil is separately taken, step (4) operation is repeated, is tested as blank control, in Atomic Absorption Spectrometry examination solution
Iron content is denoted as c2, the content of fe in LiFePO4 is calculated according to following formula:
With the iron content of Atomic Absorption Spectrometry examination copper foil surface, the content of fe as in LiFePO4.
2. the detection method of simple substance iron content in LiFePO4 according to claim 1, which is characterized in that the conductive agent
Selected from one of conductive black, electrically conductive graphite, carbon nanotube, carbon fiber, graphene or a variety of mixtures, binder is poly- inclined
Vinyl fluoride, solvent are N-Methyl pyrrolidone.
3. the detection method of simple substance iron content in LiFePO4 according to claim 1, which is characterized in that the step
(3) CR2016 type buckles electricity and carries out 3.8V constant-voltage charge, cut-off current 0.01C in.
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| CN113358714B (en) * | 2021-03-24 | 2024-03-19 | 厦门厦钨新能源材料股份有限公司 | Method for testing content of ferric iron in lithium iron phosphate |
| CN113567293B (en) * | 2021-07-21 | 2023-07-28 | 湖北亿纬动力有限公司 | Method for testing carbon nano tube content in carbon nano tube conductive paste |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779601A (en) * | 2013-12-19 | 2014-05-07 | 宁波维科电池股份有限公司 | Silicon cathode lithium ion battery and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779601A (en) * | 2013-12-19 | 2014-05-07 | 宁波维科电池股份有限公司 | Silicon cathode lithium ion battery and manufacturing method thereof |
Non-Patent Citations (3)
| Title |
|---|
| Failure Investigation of LiFePO4 Cells under Overcharge Conditions;Fan Xu等;《ECS Transactions》;20121231;第A678-A687页（参见摘要） * |
| 磷酸铁锂磁性杂质对电池自放电的影响;杨续来等;《电池》;20121231;第42卷(第6期);第314-317页 * |
| 锂离子电池新型电极材料的研究;王传宝;《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》;20130405;第C042-332页（参见正文第2页、第25页） * |
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