CN100413137C - Solid electrolyte and uses thereof - Google Patents

Solid electrolyte and uses thereof Download PDF

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CN100413137C
CN100413137C CNB031376665A CN03137666A CN100413137C CN 100413137 C CN100413137 C CN 100413137C CN B031376665 A CNB031376665 A CN B031376665A CN 03137666 A CN03137666 A CN 03137666A CN 100413137 C CN100413137 C CN 100413137C
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solid electrolyte
anhydrous
iodate
electrolyte
compound
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CN1567484A (en
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孟庆波
王红霞
胡永胜
黄学杰
薛其坤
陈立泉
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Institute of Physics of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
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Abstract

The present invention relates to a solid electrolyte and an application thereof. The electrolyte is a compound which is generated by that a nitrile alcohol class organic solvent of which a molecule simultaneously has a hydroxyl group-OH and a nitrile grouping-CN, reacts with halogenating multialkali metal salt, or the electrolyte is formed by that at least one of simple substance iodine, crystallization rate control agents and a cuprous salt compound is added on the compound. The solid electrolyte has the advantages of high conductivity, small volatility, high stability, etc. The electrolyte can be applied to the fields of solar cells, fuel cells, etc.

Description

A kind of solid electrolyte and application thereof
Technical field
The present invention relates to a kind of electrolyte and application thereof that can be used for fields such as solar cell, fuel cell, particularly a kind of solid electrolyte and the application in organic solar batteries thereof.
Background technology
The electrolyte of high conductivity, stable performance has a wide range of applications.They can be applied in all kinds of batteries as requested.The common inorganic polycrystalline solid electrolyte or the ion migration rate of glassy polymers material are slow, and conductance is all lower, and liquid electrolyte exists the leakage and the encapsulation technology difficult problem of electrolyte.These effects limit the efficient of battery improve.Therefore, the searching solid electrolyte that volatility is little, conductivity is high and the research of fused salt electrolysis matter have caused people's extensive interest.B.Schoch in 1986, E.Hartmann, W.Weppner at " solid ionic " [referring to Solid State Ionics, 18 ﹠amp; 19 (1986), 529]; W.Weppner, W.Wlzel R.Kniep and A.Rabenau, " German applied chemistry " is [referring to Angew, Chem.Int.Ed.Engl.25,1087 (1986)] reported lithium salts halide (LiX on, X=Cl, Br, I) compound that reaction generates with alcohols has quite high conductivity, subsequently, (Ran Yujun, Chen Guanxiong, Chen Liquan such as Chen Liquan, Sichuan University's journal (natural science edition) 25 volumes, 4 phases, 450 (1988) further investigate this, measure the electrical properties and the crystal structure of this compounds.But the conductivity of the simple alcohols additive compound of this class has only 10 -4Scm -1, do not satisfy requirement of actual application.And, another shortcoming of this class alcohols additive compound is that crystalline rate is too fast, formed acicular crystal reaches the hundreds of micron to the millimeter magnitude, causes the contact of intergranule and electrolyte very poor with contacting of electrode, and this is the key factor that influences dielectric efficient and battery efficiency.Therefore, research high conductivity, volatility is little and the electrolyte of suitable fusing point has important practical value in field of batteries.
Summary of the invention
Technical problem to be solved by this invention provides a kind of solid electrolyte with high conductivity and suitable fusing point, can be applicable to fields such as solar cell, fuel cell.
Solid electrolyte of the present invention can be summarised as with following formula:
M 1 xM 2 yM 3 zM 4 vN·(A) w+aI 2+bB+cC，
Be that its composition comprises M 1 xM 2 yM 3 zM 4 vY (A) w, I 2, B and C, wherein, M 1, M 2, M 3, M 4Be selected from a kind of among alkali metal Li, Na, K, Ru, the Cs respectively, wherein x, y, z, v are the atom umber, 0≤(x, y, z, v)≤1 and x+y+z+v=1; Y is selected from least a among halogen F, Cl, Br, the I; A is nitrile alcohols and derivative thereof, and available general formula is expressed as HO-R n-CN (R is straight chain and branched paraffin, and n is the carbon atom number that R comprises), M 1 xM 2 yM 3 zM 4 vY (A) wBe nitrile alcohol A and alkali halide M 1 xM 2 yM 3 zM 4 vThe not isosteric compound that Y forms, wherein w=0.5～4; B is selected from and can suppresses M 1 xM 2 yM 3 zM 4 vY (A) wAt least a in the material of crystalline rate; C is cuprous salt Compound C uX, and wherein X is selected from least a among F, Cl, Br, I, SCN, the CN; A=0～0.2mol; B=0～0.2mol; C=0～0.2mol, i.e. M 1 xM 2 yM 3 zM 4 vY (A) w, I 2, B, C mol ratio be 1: (0～0.2): (0～0.2): (0～0.2).
Be example with n=2 (3-hydroxypropionitrile) among the described A, w=0.5,1,2,3,4.
Described B is selected from ceramic powders TiO 2, ZnO, ZrO 2, Al 2O 3, γ-LiAlO 2, MgO, SiO 2, SnO 2In at least a.
This solid electrolyte is preferably Li βM 1-βI (A) w+ aI 2+ bB+cC; Wherein M is selected from a kind of among alkali metal Li, Na, K, Ru, the Cs, and β is the atom umber, 0≤β≤1; A is a nitrile alcohols or derivatives thereof, w=0.5～4; B is selected from and can suppresses Li βM 1-βI (A) wThe material of crystalline rate at least a; C is cuprous salt Compound C uX, and wherein X is selected from least a among F, Cl, Br, I, SCN, the CN; A=0～0.2mol; B=0～0.2mol; C=0～0.2mol.
The preparation method of solid dielectric of the present invention is that promptly respectively by w: the mol ratio of a: b: c takes by weighing A, iodine, B and C, and iodine, B and C are added among the A, stirs and makes it abundant mixing; A certain amount of anhydrous iodate M of weighing in addition 1, anhydrous iodate M 2, anhydrous iodate M 3, anhydrous iodate M 4In at least a; By alleged anhydrous iodate M 1, anhydrous iodate M 2, anhydrous iodate M 3, anhydrous iodate M 4Amount, measure the required A mixed solution that contains iodine, B and C again; Said mixture is slowly added anhydrous iodate M 1, anhydrous iodate M 2, anhydrous iodate M 3, anhydrous iodate M 4In, anhydrous iodate M 1, anhydrous iodate M 2, anhydrous iodate M 3, anhydrous iodate M 4Be dissolved in gradually in the said mixture, chemical reaction take place and emit heat, generate solid electrolyte.
This solid electrolyte can be applicable to the field that solar cell, fuel cell etc. are had relatively high expectations to the solid electrolyte conductivity.
The electrolytical stable performance of solid composite of the present invention can steady in a long-termly be preserved in dry environment; Conductivity height, fusing point are suitable; By adjusting the proportioning of heterogeneity, can effectively regulate electrolytical physico-chemical property such as fusing point, conductivity etc., thereby make this solid electrolyte have application widely.
Embodiment
1, following form with form specifies the composition form of solid electrolyte of the present invention.
The general formula of the compound that nitrile alcohol organic solvent of the present invention and the reaction of halogenation polyamine/alkali salt generate is M 1 xM 2 yM 3 zM 4 vY (A) w, M in the formula 1, M 2, M 3, M 4Be selected from alkali metal Li respectively, Na, K, Ru, a kind of among the Cs, x wherein, y, z, v are the atom umber, 0≤(x, y, z, v)≤1 and x+y+z+v=1; Y is selected from least a among halogen F, Cl, Br, the I; A is nitrile alcohol or derivatives thereof, wherein w=0.5～4.Embodiment sees Table the embodiment 1 and 2 in 1.
For improving electrolytical conductivity, the nitrile alcohols organic salt compound that adopts nitrile alcohol type organic and halogenation polyamine/alkali salt to generate is doped with the composite solid electrolyte of elemental iodine.Its general formula is:
M 1 xM 2 yM 3 zM 4 vY·(A) w+aI 2
M in the formula 1, M 2, M 3, M 4Be selected from a kind of among alkali metal Li, Na, K, Ru, the Cs respectively, x wherein, y, z, v are the atom umber, 0≤(x, y, z, v)≤1 and x+y+z+v=1; Y is selected from least a among halogen F, Cl, Br, the I; A is nitrile alcohol or derivatives thereof, wherein w=0.5～4; A=0～0.2mol.Increase the defective of electrolyte crystal by the introducing iodine, thereby realize increasing the electrolyte ion conductivity.Embodiment sees Table the embodiment 3,4 and 5 in 1, and its conductivity is respectively 3.1 * 10 -3S/cm, 1.8 * 10 -3S/cm and 1.5 * 10 -3S/cm obviously is superior to the electrolytical conductivity of alcohols additive compound of the prior art.Other embodiment see Table 2-table 10.
The present invention is by at nitrile alcohols salt compound or be doped with in the nitrile alcohols salt compound of elemental iodine and add controlling agent B again, control electrolytical crystallization speed, the crystalline rate of solid electrolyte is reduced greatly, realize the nanometer crystallization, with fully contacting of further raising solid electrolyte and porous electrode interface.The general formula of the solid electrolyte of this interpolation controlling agent B is:
M 1 xM 2 yM 3 zM 4 vY (A) w+ bB; And
M 1 xM 2 yM 3 zM 4 vY·(A) w+aI 2+bB
M in the formula 1, M 2, M 3, M 4Be selected from a kind of among alkali metal Li, Na, K, Ru, the Cs respectively, x wherein, y, z, v are the atom umber, 0≤(x, y, z, v)≤1 and x+y+z+v=1; Y is selected from least a among halogen F, Cl, Br, the I; A is nitrile alcohol or derivatives thereof, wherein w=0.5～4; B is selected from and can suppresses M 1 xM 2 yM 3 zM 4 vY (A) wThe material of crystalline rate at least a a=0～0.2mol; B=0～0.2mol.M 1 xM 2 yM 3 zM 4 vY (A) wThe electrolytical embodiment of+bB sees Table 6 in 1,7 and 8.M 1 xM 2 yM 3 zM 4 vY (A) w+ aI 2The electrolytical embodiment of+bB sees Table 12 in 1,13 and 14, and its conductivity is respectively 1.3 * 10 -3S/cm, 2.3 * 10 -3S/cm, 3.2 * 10 -3S/cm.Other embodiment see Table 2-table 10.
Composite solid electrolyte for the more high conductivity of realizing stable performance, the present invention nitrile alcohols salt compound, be doped with elemental iodine nitrile alcohols salt compound, add the nitrile alcohols salt compound of controlling agent B and add controlling agent B and be doped with in the nitrile alcohols additive compound of elemental iodine and add the cuprous salt compound respectively, in the hope of by different cationic synergies, reach the electrolytical electric conductivity of further improvement.Its general formula is respectively:
M 1 xM 2 yM 3 zM 4 vY·(A) w+cC；
M 1 xM 2 yM 3 zM 4 vY·(A) w+aI 2+cC；
M 1 xM 2 yM 3 zM 4 vY (A) w+ bB+cC; And
M 1 xM 2 yM 3 zM 4 vY·(A) w+aI 2+bB+cC
M in the formula 1, M 2, M 3, M 4Be selected from a kind of among alkali metal Li, Na, K, Ru, the Cs respectively, x wherein, y, z, v are the atom umber, 0≤(x, y, z, v)≤1 and x+y+z+v=1; Y is selected from least a among halogen F, Cl, Br, the I; A is nitrile alcohols or derivatives thereof, wherein w=0.5～4; B is selected from and can suppresses M 1 xM 2 yM 3 zM 4 vY (A) wThe material of crystalline rate at least a; C is cuprous salt Compound C uX, and wherein x is selected from least a among F, Cl, Br, I, SCN, the CN; A=0～0.2mol; B=0～0.2mol; C=0～0.2mol.
M 1 xM 2 yM 3 zM 4 vY (A) wThe embodiment of+cC composite electrolyte sees Table 1 embodiment 9,10 and 11; Its conductivity is followed successively by 9.1 * 10 -3S/cm, 7.7 * 10 -3S/cm and 6.8 * 10 -3S/cm.Other embodiment see Table 2-table 10.
M 1 xM 2 yM 3 zM 4 vY (A) w+ aI 2The embodiment of+cC composite solid electrolyte sees Table 1 embodiment 15,16 and 17; Its conductivity is followed successively by 6.3 * 10 -3S/cm, 7.5 * 10 -3S/cm and 8.2 * 10 -3S/cm.Other embodiment see Table 2-table 10.
M 1 xM 2 yM 3 zM 4 vY (A) wThe embodiment of+bB+cC composite solid electrolyte sees Table 1 embodiment 18,19 and 20; Its conductivity is followed successively by 4.3 * 10 -3S/cm, 3.7 * 10 -3S/cm and 3.2 * 10 -3S/cm.Other embodiment see Table 2-table 10.
M 1 xM 2 yM 3 zM 4 vY (A) w+ aI 2The embodiment of+bB+cC composite electrolyte sees Table 1 embodiment 21-26; The conductivity of embodiment 21-23 is followed successively by 5.3 * 10 -3S/cm, 4.5 * 10 -3S/cm and 4.2 * 10 -3S/cm; Embodiment 25 and 26 conductivity are followed successively by 3.7 * 10 -3S/cm and 3.2 * 10 -3S/cm.Other embodiment see Table 2-table 10.
Therefore, the adding of cuprous salt Compound C uX can significantly improve the conductivity of this composite solid electrolyte.
The M of each embodiment in the following table 1 1Be alkali metal Li, M 2Be alkali metal element K or Na, M 3 z, M 4 vIn z and v be 0, Y is iodine I, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=4, B are TiO 2, C is CuI; "-" is expressed as testing data in the table.
Table 1:
Figure C0313766600091
The M of each embodiment in the following table 2 1Be alkali metal Li, M 2 y, M 3 z, M 4 vIn v, z and v be 0, Y is iodine I, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=4, B are ZnO, C is CuBr; "-" is expressed as testing data in the table.
Table 2
Figure C0313766600101
The M of each embodiment in the following table 3 1Be alkali metal Li, M 2 y, M 3 z, M 4 vIn y, z and v be 0, Y is iodine I, A is 3-hydroxypropionitrile (nitrile alcohol, HO-R n-CN, n=2), w=4, B are Al 2O 3, C is CuSCN; "-" is expressed as testing data in the table.
Table 3
Figure C0313766600111
The M of each embodiment in the following table 4 1Be Li, M 2 y, M 3 z, M 4 vIn y, z and v be 0, Y is iodine I, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=3, B are TiO 2, C is CuI; "-" is expressed as testing data in the table.
Table 4:
Figure C0313766600121
The M of each embodiment in the following table 5 1Be alkali metal Li, M 2Be alkali metal Na, M 3 z, M 4 vIn z and v be 0, Y is iodine I, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=3, B are TiO 2, C is CuI; "-" is expressed as testing data in the table.
Table 5:
Figure C0313766600131
The M of each embodiment in the following table 6 1Be alkali metal Li, M 2 y, M 3 z, M 4 vIn y, z and v be 0, Y is halogen bromine Br, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=4, B are TiO 2, C is CuI; "-" is expressed as testing data in the table.
Table 6:
The M of each embodiment in the following table 7 1Be alkali metal Li, M 2 y, M 3 z, M 4 vIn y, z and v be 0, Y is halogen bromine Br, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=3, B are Al 2O 3, C is CuBr; "-" is expressed as testing data in the table.
Table 7
Figure C0313766600151
The M of each embodiment in the following table 8 1Be alkali metal Li, M 2 y, M 3 z, M 4 vIn y, z and v be 0, Y is halogen bromine Br, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=2, B are SiO 2, C is CuSCN; "-" is expressed as testing data in the table.
Table 8
Figure C0313766600161
The M of each embodiment in the following table 9 1Be alkali metal Li, M 2 y, M 3 z, M 4 vIn y, z and v be 0, Y is halogen bromine Br, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=2, B are TiO 2, C is CuI; "-" is expressed as testing data in the table.
Table 9:
Figure C0313766600171
The M of each embodiment in the following table 10 1Be alkali metal Li, M 2Be Na, M 3 z, M 4 vIn z and v be 0, Y is halogen bromine Br, A is 3-hydroxypropionitrile (nitrile alcohol HO-R n-CN, n=2), w=0.5, B are TiO 2, C is CuI; "-" is expressed as testing data in the table.
Table 10:
Figure C0313766600181
The conductivity that above embodiment surveyed is mostly 10 -3The S/cm order of magnitude, the wherein conductivity of part material even reach 10 -2The S/cm order of magnitude, and the melting temperature excursion of solid electrolyte is 41～142 ℃, and this specific character is better than the conductivity of the solid electrolyte of existing alcohols and other type, makes this kind electrolyte that application prospect widely be arranged.
2, preparation embodiment
Be example with embodiment 12 below, sketch the preparation process of solid electrolyte of the present invention: take by weighing iodine and titanium dioxide by 0.0005: 0.0025 mol ratio respectively, add in the 3-hydroxypropionitrile, stir and make it fully dissolving and disperse; A certain amount of anhydrous lithium iodide of weighing in addition; By the amount of alleged anhydrous lithium iodide, measure the required 3-hydroxypropionitrile mixture that contains iodine and titanium dioxide again; Said mixture is slowly added in the anhydrous lithium iodide, and lithium iodide is dissolved in the said mixture gradually, chemical reaction takes place and emit heat, generates the solid electrolyte of embodiment 12.Whole experimental implementation all is to carry out in being full of the glove box of high-purity argon gas.The solid electrolyte of other embodiment all adopts the preparation method of embodiment 12, only need adjust each desired substance and content thereof.

Claims (6)

1. solid electrolyte, the composition of this solid electrolyte comprise,
M 1 xM 2 yM 3 zM 4 vY (A) w, I 2, B and C, wherein, M 1, M 2, M 3, M 4Be selected from alkali metal Li respectively, Na, K, Ru, a kind of among the Cs, x, y, z, v are the atom umber, 0≤(x, y, z, v)≤1 and x+y+z+v=1; Y is selected from least a among halogen F, Cl, Br, the I; A is a nitrile alcohol or derivatives thereof, and general formula is HO-R n-CN, its R are straight or branched alkane, and n is the carbon atom number that R comprises, M 1 xM 2 yM 3 zM 4 vY (A) wBe nitrile alcohol A and alkali halide M 1 xM 2 yM 3 zM 4 vThe not isosteric compound that Y forms, w=0.5～4; B is selected from and suppresses M 1 xM 2 yM 3 zM 4 vY (A) wThe ceramic powders TiO of crystalline rate 2, ZnO, ZrO 2, Al 2O 3, γ-LiAlO 2, MgO, SiO 2, SnO 2In at least a; C is cuprous salt Compound C uX, and wherein X is selected from least a among F, Cl, Br, I, SCN, the CN; M 1 xM 2 yM 3 zM 4 vY (A) w, I 2, B, C mol ratio be 1: (0～0.2): (0～0.2): (0～0.2).
2. solid electrolyte as claimed in claim 1 is characterized in that, described compound M 1 xM 2 yM 3 zM 4 vY (A) wMiddle w=0.5,1,2,3,4, the fusing point of these compounds and conductivity are all different.
3. solid electrolyte as claimed in claim 1 is characterized in that this solid electrolyte consists of Li βM 1-βI (A) w, I 2, B, C; Wherein M is selected from alkali metal Li, Na, and K, Ru, a kind of among the Cs, β is the atom umber, 0≤β≤1; B is selected from and suppresses Li βM 1-βI (A) wThe ceramic powders TiO of crystalline rate 2, ZnO, ZrO 2, Al 2O 3, γ-LiAlO 2, MgO, SiO 2, SnO 2In at least a.
4. the described method for preparing solid electrolyte of claim 1 is characterized in that, respectively by (0.5～4): (0～0.2): (0～0.2): the mol ratio of (0～0.2) takes by weighing A, I 2, B and C, with I 2, B and C add among the A, stir and make it abundant mixing; Take by weighing anhydrous iodate M 1, anhydrous iodate M 2, anhydrous iodate M 3, anhydrous iodate M 4In at least a; According to alleged anhydrous iodate M 1, M 2, M 3, M 4Amount, measure the required A mixture that contains iodine, B and C again according to above-mentioned mol ratio; Said mixture is slowly added anhydrous iodate M 1, M 2, M 3, M 4In, anhydrous iodate M 1, M 2, M 3, M 4Be dissolved in gradually in the said mixture, chemical reaction take place and emit heat, generate solid electrolyte.
5. method for preparing solid electrolyte as claimed in claim 4 is characterized in that, whole process of preparation all is to carry out in being full of the glove box of dry argon gas.
6. the application of the described solid electrolyte of claim 1 is characterized in that, this solid electrolyte is applicable to solar cell, fuel cell field.
CNB031376665A 2003-06-19 2003-06-19 Solid electrolyte and uses thereof Expired - Fee Related CN100413137C (en)

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JPH07259189A (en) * 1994-03-24 1995-10-09 S Bai L Kk Unit housing and building method thereof
JP2002187892A (en) * 2000-12-18 2002-07-05 Central Glass Co Ltd Addition compound of ionic metal complex
CN1371141A (en) * 2001-02-27 2002-09-25 中国科学院物理研究所 Lithium ion electrolyte containing lithium addition compound

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07259189A (en) * 1994-03-24 1995-10-09 S Bai L Kk Unit housing and building method thereof
JP2002187892A (en) * 2000-12-18 2002-07-05 Central Glass Co Ltd Addition compound of ionic metal complex
CN1371141A (en) * 2001-02-27 2002-09-25 中国科学院物理研究所 Lithium ion electrolyte containing lithium addition compound

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