CN103456990A - PEO-based gel polymer electrolyte and preparation method thereof - Google Patents
PEO-based gel polymer electrolyte and preparation method thereof Download PDFInfo
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- CN103456990A CN103456990A CN2012101766606A CN201210176660A CN103456990A CN 103456990 A CN103456990 A CN 103456990A CN 2012101766606 A CN2012101766606 A CN 2012101766606A CN 201210176660 A CN201210176660 A CN 201210176660A CN 103456990 A CN103456990 A CN 103456990A
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Abstract
The invention belongs to the field of electrolytes and discloses a PEO-based gel polymer electrolyte and a preparation method thereof. The PEO-based gel polymer electrolyte comprises a PEO matrix, a lithium dicyanoamine/EC+DMC lithium salt and a metal oxide, wherein a mole ratio of lithium dicyanoamine to the metal oxide is 1: 0.001 to 1: 0.05. The metal oxide can react with H<+> of acid impurities in a dicyanoamine salt ionic liquid so that acid corrosion on aluminum foil of a double-layer capacitor is prevented and stability of the double-layer capacitor adopting the PEO-based gel polymer electrolyte is greatly improved. In the double-layer capacitor, the PEO-based gel polymer electrolyte does not leak, has good safety and greatly improves stability of the double-layer capacitor adopting the PEO-based gel polymer electrolyte containing lithium dicyanoamine.
Description
Technical field
The present invention relates to the electrolyte field, relate in particular to a kind of PEO matrix gel polymer dielectric and preparation method thereof.
Background technology
Safety problem is the bottleneck of the large capacity of restriction, high power lithium ion cell application.The burning that leakage, electrolyte oxidation decomposition and the thermal runaway etc. that now widely used liquid electrolyte produces cause, blast are the main potential safety hazards of battery.The studied persons of advantage such as gel polymer electrolyte lithium-ion battery is safe because having, nothing is leaked, leakage current is little pay attention to.And gel polymer electrolyte is a kind of novel functional high molecule material, can makes the battery thin type simultaneously as barrier film and electrolyte, thereby improve the flexibility of battery shape-designing.
The advantages such as PEO has the easy processing of solid electrolyte, and thermoplasticity is good, be applicable to doing the electrolyte matrix material,
Trifluoroacetic acid lithium (LiCF
3cO
2) because cost of material is low, and good with the compatibility of organic polymer, it is one of lithium salts for gel electrolyte relatively had DEVELOPMENT PROSPECT, yet, PEO base gel polymer electrolyte containing the trifluoroacetic acid lithium inevitably can contain impurity (water) in the process of preparation, and in the electrochemistry cyclic process, water will participate in electrode reaction and generate acid, thereby the aluminium foil of corrosion double electric layer capacitor, cause using containing LiCF
3cO
2the PEO base gel polymer electrolyte stability of making electrolytical double electric layer capacitor reduce.
Summary of the invention
Based on the problems referred to above, problem to be solved by this invention is to provide a kind of PEO matrix gel polymer dielectric
Technical scheme of the present invention is as follows:
A kind of PEO matrix gel polymer dielectric, comprise PEO matrix, dicyanogen methyl isophorone amine lithium/EC+DMC lithium salts and metal oxide; Wherein, the mol ratio of dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.001 ~ 1:0.05, PEO: dicyanogen methyl isophorone amine lithium: EC+DMC(means the mixed electrolytic solution of EC and DMC) mass ratio be 1:0.8:5.
Described PEO matrix gel polymer dielectric, wherein, the mol ratio of described dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.02 ~ 1:0.05.
Described PEO matrix gel polymer dielectric, wherein, the molar concentration of described dicyanogen methyl isophorone amine lithium/EC+DMC lithium salts is 1mol/L; And the EC(ethyl carbonate) with the DMC(dimethyl carbonate) volume ratio be 1:2.
Described PEO matrix gel polymer dielectric, wherein, described metal oxide is selected from Al
2o
3, MgO or BaO.
The present invention also provides a kind of PEO matrix gel method for preparing polymer electrolytes, comprises the steps:
S1, in PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium/EC+DMC and nanometer Al
2o
3, and be dissolved in acetone, continue to stir, obtain mixed solution; Wherein, the mol ratio of dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.001 ~ 1:0.05;
S2, mixed solution is cast on clean flat board, then after drying, obtain described PEO base gel polymer electrolyte under 80 ℃, 0.01MPa vacuum.
Described PEO matrix gel method for preparing polymer electrolytes, in step S1, the mol ratio of described dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.02 ~ 1:0.05.
Described PEO matrix gel method for preparing polymer electrolytes, in step S1, in step S1, the molar concentration of described dicyanogen methyl isophorone amine lithium/EC+DMC lithium salt solution is 1mol/L; And the EC(ethyl carbonate) with the DMC(dimethyl carbonate) volume ratio be 1:2.
Described PEO matrix gel method for preparing polymer electrolytes, in step S1, in step S1, described metal oxide is selected from Al
2o
3, MgO or BaO.
PEO matrix gel polymer dielectric provided by the invention, its metal oxide can with dicyanogen methyl isophorone amine salt class ionic liquid in acids impurity in H
+react, avoid the aluminium foil of acid corrosion double layer capacitor, can greatly improve the stability of using the present invention to do electrolytical double layer capacitor; And the invention belongs to PEO base gel polymer electrolyte, its for double layer capacitor after, without leaking, security performance is good, and can greatly improve and use the stability of making electrolytical double electric layer capacitor containing the PEO base gel polymer electrolyte of dicyanogen methyl isophorone amine lithium.
The accompanying drawing explanation
Preparation technology's flow chart that Fig. 1 is PEO matrix gel polymer dielectric of the present invention;
The double electric layer capacitor of the PEO matrix gel polymer dielectric that Fig. 2 makes from Comparative Examples 1 for the PEO matrix gel polymer dielectric that uses embodiment 1 to make respectively under different cycle-indexes than capacitance relation figure; Wherein, abscissa is cycle-index, and ordinate is than capacitance (F/g).
Embodiment
PEO matrix gel polymer dielectric provided by the invention, comprise PEO matrix, dicyanogen methyl isophorone amine lithium/EC+DMC lithium salts and metal oxide; Wherein, the mol ratio of dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.001 ~ 1:0.05, PEO: dicyanogen methyl isophorone amine lithium: EC+DMC(means the mixed electrolytic solution of EC and DMC) mass ratio be 1:0.8:5, EC and DMC are mixed electrolytic solution, play the effect of plasticizer, metal oxide is additive.
Described PEO matrix gel polymer dielectric, wherein, the mol ratio of described dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.02 ~ 1:0.05.
Described PEO matrix gel polymer dielectric, wherein, the molar concentration of described dicyanogen methyl isophorone amine lithium/EC+DMC lithium salts is 1mol/L; And the EC(ethyl carbonate) with the DMC(dimethyl carbonate) volume ratio be 1:2.
Described PEO matrix gel polymer dielectric, wherein, described metal oxide is selected from Al
2o
3, MgO or BaO.
Above-mentioned PEO matrix gel method for preparing polymer electrolytes, as shown in Figure 1, comprise the steps:
S1, in PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium/EC+DMC and nanometer Al
2o
3, and be dissolved in acetone, continue to stir, obtain mixed solution; Wherein, the mol ratio of dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.001 ~ 1:0.05;
S2, mixed solution is cast on clean flat board, then after drying, obtain described PEO base gel polymer electrolyte under 80 ℃, 0.01MPa vacuum.
Described PEO matrix gel method for preparing polymer electrolytes, in step S1, the mol ratio of described dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.02 ~ 1:0.05.
Described PEO matrix gel method for preparing polymer electrolytes, in step S1, in step S 1, the molar concentration of described dicyanogen methyl isophorone amine lithium/EC+DMC lithium salt solution is 1mol/L; And the EC(ethyl carbonate) with the DMC(dimethyl carbonate) volume ratio be 1:2.
Described PEO matrix gel method for preparing polymer electrolytes, in step S1, in step S 1, described metal oxide is selected from Al
2o
3, MgO or BaO.
PEO matrix gel polymer dielectric provided by the invention, its metal oxide can with dicyanogen methyl isophorone amine salt class ionic liquid in acids impurity in H
+react, avoid the aluminium foil of acid corrosion double layer capacitor, can greatly improve the stability of using the present invention to do electrolytical double layer capacitor; And the invention belongs to PEO base gel polymer electrolyte, its for double layer capacitor after, without leaking, security performance is good, and can greatly improve and use the stability of making electrolytical double electric layer capacitor containing the PEO base gel polymer electrolyte of dicyanogen methyl isophorone amine lithium.
Below preferred embodiment of the present invention is described in further detail.
In following each embodiment and Comparative Examples, the stability of double electric layer capacitor is with meaning than electric capacity conservation rate after 200 circulations, its test is specially: using active carbon as electrode material, take each embodiment as electrolyte, be assembled into button cell, utilize the CHI660A electrochemical workstation to carry out the constant current charge-discharge test to it, record it than electric capacity conservation rate, under 30 degrees celsius, in the 0-2v window ranges, with the ratio electric capacity and the ratio of first charge-discharge than electric capacity after 200 circulations of constant current repeated charge of 1A/g.
Embodiment 1
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO (polymer), dicyanogen methyl isophorone amine lithium (lithium salts), EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 10 and 20ml) quality be 0.5g, 0.4g, 2.5g, add nanometer Al
2o
3; Wherein, dicyanogen methyl isophorone amine lithium and Al
2o
3mol ratio be 1:0.05, be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, then after drying, obtain having added Al under 80 ℃, 0.01MPa vacuum
2o
3pEO base gel polymer electrolyte.
Embodiment 2
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium, EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 5 and 10ml) quality be 0.1g, 0.08g, 0.5g, add nano-MgO (wherein, dicyanogen methyl isophorone amine lithium: the mol ratio of MgO is 1:0.04), be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, then after drying, obtain having added the PEO base gel polymer electrolyte of MgO under 80 ℃, 0.01MPa vacuum.
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium, EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 8 and 16ml) quality be respectively 0.8g, 0.64g and 4g, add nanometer BaO (wherein, dicyanogen methyl isophorone amine lithium: the mol ratio of BaO is 1:0.02), be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, after drying, obtain having added the PEO base gel polymer electrolyte of BaO again under 80 ℃, 0.01MPa vacuum.
Embodiment 4
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium, EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 15 and 30ml) quality be respectively 0.6g, 0.48g and 3g, add nanometer Al
2o
3(wherein, dicyanogen methyl isophorone amine lithium: Al
2o
3mol ratio be 1:0.01), be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, then after drying, obtain having added Al under 80 ℃, 0.01MPa vacuum
2o
3pEO base gel polymer electrolyte.
Embodiment 5
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium, EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 17 and 34ml) quality be respectively 1g, 0.8g and 5g, add nano-MgO (wherein, dicyanogen methyl isophorone amine lithium: the mol ratio of MgO is 1:0.005), be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, after drying, obtain having added the PEO base gel polymer electrolyte of MgO again under 80 ℃, 0.01MPa vacuum.
Embodiment 6
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium, EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 20 and 40ml) quality be respectively 1.5g, 1.2g and 7.5g, add nanometer BaO (wherein, dicyanogen methyl isophorone amine lithium: the mol ratio of BaO is 1:0.01), be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, after drying, obtain having added the PEO base gel polymer electrolyte of BaO again under 80 ℃, 0.01MPa vacuum.
Comparative Examples 1
In PEO: dicyanogen methyl isophorone amine lithium: the ratio that EC+DMC is 1:0.8:5 (mass ratio) takes PEO, dicyanogen methyl isophorone amine lithium, EC+DMC(EC and DMC volume ratio 1:2; The volume number be respectively 10 and 20ml) quality be respectively 0.5g, 0.4g and 2.5g, be dissolved in appropriate acetone, after continuing to stir, it is cast on clean glass plate, then after drying, obtain PEO base gel polymer electrolyte under 80 ℃, 0.01MPa vacuum.
The double electric layer capacitor of the PEO matrix gel polymer dielectric that Fig. 2 makes from Comparative Examples 1 for the PEO matrix gel polymer dielectric that uses embodiment 1 to make respectively under different cycle-indexes than capacitance relation figure; Wherein, abscissa is cycle-index, and ordinate is than capacitance (F/g).
As can be seen from Figure 2, using the first charge-discharge of the electrolytical double layer capacitor in embodiment 1 is 52.0F/g than electric capacity, and the ratio electric capacity circulated after 200 times is 42.1F/g, and its conservation rate is 81.4%; And use the first charge-discharge of the electrolytical double layer capacitor in Comparative Examples 1, than electric capacity, be 51.7F/g, the ratio electric capacity circulated after 200 times is 36.5F/g, and its conservation rate is 70.6%; That uses electrolytical double layer capacitor in embodiment 1 has exceeded 10.8% than what use electrolytical double layer capacitor in Comparative Examples 1 than electric capacity conservation rate than electric capacity conservation rate, illustrate that the electrolytical double layer capacitor used in embodiment 1 is than the good stability of the electrolytical double layer capacitor in use Comparative Examples 1.
The ratio electric capacity conservation rate test result of the PEO matrix gel polymer dielectric that following table is embodiment 1 ~ 6 and Comparative Examples 1 preparation.
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | Comparative Examples 1 |
| Than electric capacity conservation rate | 81.4% | 80.8% | 79.9% | 78.1% | 76.0% | 73.2% | 70.6% |
Find by Data Comparison, add the conductivity that metal oxide can improve PEO base gel polymer electrolyte greatly.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (8)
1. a PEO matrix gel polymer dielectric, is characterized in that, comprises PEO matrix, dicyanogen methyl isophorone amine lithium/EC+DMC lithium salts and metal oxide; Wherein, the mol ratio of dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.001 ~ 1:0.05, PEO: dicyanogen methyl isophorone amine lithium: the mass ratio of EC+DMC is 1:0.8:5.
2. PEO matrix gel polymer dielectric according to claim 1, is characterized in that, the mol ratio of described dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.02 ~ 1:0.05.
3. PEO matrix gel polymer dielectric according to claim 1 and 2, is characterized in that, the molar concentration of described dicyanogen methyl isophorone amine lithium/EC+DMC lithium salts is 1mol/L; And the volume ratio of EC and DMC is 1:2.
4. PEO matrix gel polymer dielectric according to claim 1 and 2, is characterized in that, described metal oxide is selected from Al
2o
3, MgO or BaO.
5. a PEO matrix gel method for preparing polymer electrolytes, is characterized in that, comprises the steps:
S1, by PEO: dicyanogen methyl isophorone amine lithium: the mass ratio that metal oxide is 1:0.8:5 takes PEO, dicyanogen methyl isophorone amine lithium/EC+DMC and nanometer Al
2o
3, and be dissolved in acetone, continue to stir, obtain mixed solution; Wherein, the mol ratio of dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.001 ~ 1:0.05, PEO: dicyanogen methyl isophorone amine lithium: the mass ratio of EC+DMC is 1:0.8:5;
S2, mixed solution is cast on clean flat board, then after drying, obtain described PEO base gel polymer electrolyte under 80 ℃, 0.01MPa vacuum.
6. PEO matrix gel method for preparing polymer electrolytes according to claim 5, is characterized in that, in step S 1, the mol ratio of described dicyanogen methyl isophorone amine lithium and metal oxide is 1:0.02 ~ 1:0.05.
7. PEO matrix gel method for preparing polymer electrolytes according to claim 5, is characterized in that, in step S1, the molar concentration of described dicyanogen methyl isophorone amine lithium/EC+DMC lithium salt solution is 1mol/L; And the volume ratio of EC and DMC is 1:2.
8. according to the described PEO matrix gel of claim 5 or 6 method for preparing polymer electrolytes, it is characterized in that, in step S1, described metal oxide is selected from Al
2o
3, MgO or BaO.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107785614A (en) * | 2017-07-02 | 2018-03-09 | 江汉大学 | The preparation method of super corsslinking molecular gel composite electrolyte membrane based on PEO |
-
2012
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107785614A (en) * | 2017-07-02 | 2018-03-09 | 江汉大学 | The preparation method of super corsslinking molecular gel composite electrolyte membrane based on PEO |
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Application publication date: 20131218 |