CN108470875A - A kind of inorganic solid electrolyte-cellulose composite diaphragm and preparation method thereof - Google Patents

A kind of inorganic solid electrolyte-cellulose composite diaphragm and preparation method thereof Download PDF

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Publication number
CN108470875A
CN108470875A CN201810332125.2A CN201810332125A CN108470875A CN 108470875 A CN108470875 A CN 108470875A CN 201810332125 A CN201810332125 A CN 201810332125A CN 108470875 A CN108470875 A CN 108470875A
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Prior art keywords
cellulose
solid electrolyte
preparation
composite diaphragm
inorganic solid
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Chinese (zh)
Inventor
刘丹宪
黄杰
俞会根
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Beijing WeLion New Energy Technology Co ltd
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Beijing WeLion New Energy Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/411—Organic material
    • H01M50/429—Natural polymers
    • H01M50/4295—Natural cotton, cellulose or wood
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/44—Fibrous material
    • 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
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Manufacturing & Machinery (AREA)
  • Cell Separators (AREA)
  • Conductive Materials (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a kind of inorganic solid electrolyte cellulose composite diaphragm and preparation method thereof, which includes：Cellulosic material is added in deionized water S10, impregnates, is then ground in pulper, obtains the cellulose slurries with microfibrillar structure；Inorganic solid electrolyte is added in deionized water and suspension is made by S20, and wet strength agent is added and is stirred with cellulose slurries, is uniformly mixed；S30 is formed a film the cellulose slurries copy paper containing solid electrolyte using copy paper technique, i.e. wet cellulose electrolyte composite diaphragm；S40, hygrometric state composite diaphragm is dried in an oven, that is, prepares required cellulose solids electrolyte composite diaphragm.The composite diaphragm pore size distribution$ of preparation is uniform, it is convenient to prepare, it is suitable for mass production, heat resistance is high simultaneously, and wellability is good, ionic conductivity is high, and breakdown characteristics are strong, suitable for lithium ion battery separator, composite inorganic solid electrolyte simultaneously, can also play the role of electrolyte, without in addition addition electrolyte.

Description

A kind of inorganic solid electrolyte-cellulose composite diaphragm and preparation method thereof
Technical field
The present invention relates to battery technology field more particularly to a kind of inorganic solid electrolyte-cellulose composite diaphragm and its Preparation method.
Background technology
Diaphragm is one of important component of lithium ion battery, have isolation positive/negative plate prevent short circuit and provide lithium from The effect of sub- transmission channel.It is the main of the following Study on Li-ion batteries to improve battery safety and reduce diaphragm production cost One of target.
Cellulose resource is abundant, environmental-friendly, at low cost and with excellent performance, has been widely used in each The wellability in field, the hydrophilic characteristic of cellulose itself, cellulosic separator is good, while cellulosic separator thermal stability is good, 300 DEG C It is not heat-shrinked below.But current cellulosic separator is too thick, bad mechanical strength and Kong Tai great, limits answering for it With.The insertion of solid electrolyte can reduce the thickness of diaphragm, enhance breakdown characteristics, reduce short circuit, while solid electrolyte Addition improve the ionic conductivity of composite diaphragm, the nano-particle reinforcement of the solid electrolyte wellability of composite diaphragm.
Invention content
The purpose of the present invention is to provide a kind of inorganic solid electrolyte-cellulose composite diaphragms and preparation method thereof.It should The cellulose with microfibrillar structure that method is beaten dispersion preparation by height is compound with inorganic solid electrolyte, passes through machine hand Hygrometric state paper is made in skill, and then drying prepares composite diaphragm.Solid electrolyte-cellulose composite diaphragm prepared by this method has thickness Spend that small, breakdown characteristics are strong, ionic conductivity is high.The good advantage of wellability.
For realization goal of the invention, the technical solution adopted in the present invention is：
In a first aspect, the present invention provides a kind of preparation method of inorganic solid electrolyte-cellulose composite diaphragm, it is described Preparation method includes：
Cellulosic material is added in deionized water S10, impregnates, is then ground in pulper, obtains having micro- The cellulose slurries of fine structure；
Inorganic solid electrolyte is added in deionized water and suspension is made by S20, and wet strength agent is added and is stirred with cellulose slurries It mixes, is uniformly mixed；
S30 is formed a film the cellulose slurries copy paper containing solid electrolyte using copy paper technique, i.e., wet cellulose is electrolysed Matter composite diaphragm；
S40, hygrometric state composite diaphragm is dried in an oven, that is, prepares required cellulose-solid electrolyte composite diaphragm.
Preferably, the cellulosic material includes one or more of wood pulp, jute pulp, cotton pulp or bamboo pulp mixed slurry.
Preferably, a diameter of 200-500nm of cellulose in cellulose slurries.
A concentration of 1wt%-50wt% of cellulose slurries being preferably made from.
Preferably, the inorganic solid electrolyte includes NASICON types structure, LISICON types structure, carbuncle type knot At least one of structure, perovskite structure and its compound.
Preferably, the inoganic solids matter is selected from Li1+xAlxGe2-x(PO4)3/Li3yLa2/3-yTiO3、LiZr2-zTiz (PO4)3、Li1+mAlmTi2-m(PO4)3、Li7-nLa3Zr2-nTanO12、Li7-nLa3Zr2-nNbnO12、Li7-2nLa3Zr2-nWnO12、 Li7-2nLa3Zr2-nTenO12、Li7-3nGenLa3Zr2O12And Li7-3nAlnLa3Zr2O12In it is one or more, wherein 0≤r≤1, 0≤x≤2,0≤y≤2/3,0≤z≤2,0≤m≤2,0≤n≤0.6.Preferably, suspension is made in inorganic solid electrolyte Liquid, wherein the mass percent concentration of inorganic solid electrolyte is 5%-50%.
Preferably, the particle diameter of inorganic solid electrolyte is 10-1000nm.
Preferably, the wet strength agent includes chitosan, dialdehyde starch, poly, Malaysia sweet tea/vinyl alcohol terpolymer And its at least one of compound.
Preferably, ingredient is in the composite diaphragm：45%-95% celluloses, 0.5%-50% solid electrolytes, 0.5%-4% wet strength agents.
Preferably, the thickness of the composite diaphragm is 10 μm -100 μm.
Second aspect, the present invention provides a kind of inorganic solid electrolyte-cellulose composite diaphragms, by such as first aspect institute The preparation method stated is prepared.
Compared with prior art, beneficial effects of the present invention are embodied in：
The composite diaphragm pore size distribution$ that through the invention prepared by preparation method is uniform, and prepares conveniently, is suitable for criticizing Amount production, while heat resistance is high, wellability is good, ionic conductivity is high, and breakdown characteristics are strong, is suitable for lithium ion battery separator, Composite inorganic solid electrolyte simultaneously, can also play the role of electrolyte, without in addition addition electrolyte.
Description of the drawings
Below by drawings and examples, the technical solution of the embodiment of the present invention is described in further detail.
Fig. 1 is a kind of preparation method stream for inorganic solid electrolyte-cellulose composite diaphragm that the embodiment of the present invention 1 provides Journey schematic diagram.
Specific implementation mode
With reference to embodiment, the present invention is further described in detail, but is not intended to the guarantor of the limitation present invention Protect range.
Embodiment 1
Fig. 1 is that the embodiment of the present invention 1 provides a kind of preparation method stream of inorganic solid electrolyte-cellulose composite diaphragm Journey schematic diagram, as shown in Figure 1, the preparation method includes：
Cellulosic material is added in deionized water S10, impregnates, is then ground in pulper, obtains having micro- The cellulose slurries of fine structure.
Specifically, the cellulosic material includes one or more of wood pulp, jute pulp, cotton pulp or bamboo pulp mixed slurry. Impregnate for 24 hours, then ground in pulper in deionized water, grinding rate be 1-2 ten thousand/turn, manufactured cellulose slurries are dense Degree is 1wt%-50wt%, and obtained cellulose slurries have microfibrillar structure, a diameter of 200-500nm of cellulose.
Inorganic solid electrolyte is added in deionized water and suspension is made by S20, and wet strength agent is added and is stirred with cellulose slurries It mixes, is uniformly mixed.
Suspension is made in inorganic solid electrolyte, wherein the mass percent concentration of inorganic solid electrolyte is 5%- 50%.Specifically, the inorganic solid electrolyte includes NASICON types structure, garnet type structure solid electrolyte, sulfide At least one of system solid electrolyte and its compound.Such as, LATP (titanium phosphate aluminium lithium), LAGP (phosphoric acid germanium aluminium lithium) etc..
In one example, the inoganic solids matter is selected from Li1+xAlxGe2-x(PO4)3/Li3yLa2/3-yTiO3、LiZr2- zTiz(PO4)3、Li1+mAlmTi2-m(PO4)3、Li7-nLa3Zr2-nTanO12、Li7-nLa3Zr2-nNbnO12、Li7-2nLa3Zr2-nWnO12、 Li7-2nLa3Zr2-nTenO12、Li7-3nGenLa3Zr2O12And Li7-3nAlnLa3Zr2O12In it is one or more, wherein 0≤r≤1, 0≤x≤2,0≤y≤2/3,0≤z≤2,0≤m≤2,0≤n≤0.6.
Further, wet strength agent is added in the intensity after being soaked by electrolyte for reinforcing fiber element diaphragm.The wet strength agent packet Include chitosan, dialdehyde starch, poly, Malaysia sweet tea/at least one of vinyl alcohol terpolymer and its compound
S30 is formed a film the cellulose slurries copy paper containing solid electrolyte using copy paper technique, i.e., wet cellulose is electrolysed Matter composite diaphragm.
S40, hygrometric state composite diaphragm is dried in an oven, that is, prepares required cellulose-solid electrolyte composite diaphragm.
Specifically, drying condition is 50 DEG C -100 DEG C, and ingredient is in the composite diaphragm：45%-95% celluloses, The thickness of 0.5%-50% solid electrolytes, 0.5%-4% wet strength agents, the composite diaphragm prepared is 10 μm of -100 μ m。
I.e. the preparation method of the embodiment of the present invention by height be beaten cellulose with microfibrillar structure prepared by dispersion and Inorganic solid electrolyte is compound, hygrometric state paper is made by copy paper technique, and then drying prepares composite diaphragm, prepares through the invention Composite diaphragm pore size distribution$ prepared by method is uniform, and prepares conveniently, is suitable for producing in batches, while heat resistance is high, fits For lithium ion battery separator, while composite inorganic solid electrolyte, electrolyte can also be played the role of, without in addition addition Electrolyte.
The preparation method that following example 2-3 is provided according to embodiment 1, carries out preparing inorganic solid electrolyte-cellulose The detailed description of composite diaphragm process.
Embodiment 2
The preparation method for inorganic solid electrolyte-cellulose composite diaphragm that the present embodiment 2 provides, includes the following steps：
1) 1L deionized waters are added in 10g Cotton Pulps, impregnate for 24 hours, is then ground in pulper, 20,000 turns of grinding/ Point, obtain the cotton pulp cellulose slurries of a concentration of 2wt%, a diameter of 500nm of cellulose.
2) suspension is made in 5g titanium phosphate aluminium lithium (LATP) inorganic solid electrolyte addition 500mL deionized waters, be added 0.5g chitosans stir strongly with cellulose slurries, are uniformly mixed；
3) utilize copy paper technique that the cellulose slurries copy paper containing solid electrolyte forms a film, i.e. wet cellulose electrolyte Composite diaphragm；
4) by the 80 DEG C of dryings in an oven of hygrometric state composite diaphragm, cellulose-solid electrolyte that thickness is 20 μm is prepared Composite diaphragm；
The diaphragm plays the role of diaphragm and electrolyte simultaneously, is not necessarily to additionally incorporate electrolyte in lithium ion battery.
Embodiment 3：
The preparation method for inorganic solid electrolyte-cellulose composite diaphragm that the present embodiment 3 provides, includes the following steps：
1) 1L deionized waters are added in 15g hemp dissolving pulps, impregnate for 24 hours, is then ground in pulper, grinding 1.5 ten thousand Rev/min, obtain the ramie pulp fiber element slurries of a concentration of 1.5wt%, a diameter of 200-500nm of cellulose.
2) suspension is made in 5g phosphoric acid germanium aluminium lithium (LAGP) inorganic solid electrolyte addition 500ML deionized waters, be added 0.6g chitosans stir strongly with cellulose slurries, are uniformly mixed；
3) utilize copy paper technique that the cellulose slurries copy paper containing solid electrolyte forms a film, i.e. wet cellulose electrolyte Composite diaphragm；
4) by composite diaphragm 50 DEG C of dryings in an oven, it is compound to prepare cellulose/solid electrolyte that thickness is 30 μm Diaphragm.
The diaphragm plays the role of diaphragm and electrolyte simultaneously, is not necessarily to additionally incorporate electrolyte in lithium ion battery.
Normal diaphragm intrinsic breakdown voltage value intrinsic breakdown voltage of composite diaphragm in 600-800V, the present embodiment exists 1000V or more.
Comparative example 1：
Cellulosic separator is prepared, compared with Example 3, inorganic solid electrolyte is not added only in difference, remaining raw material With processing mode with embodiment 3.
In the glove box full of argon gas, between the composite diaphragm in embodiment 3 is clipped in two stainless steel gaskets, assembling Symmetrical cells test AC impedance, and ionic conductivity is obtained according to formula (σ=d/R*S).Cellulosic separator is also done in comparative example 1 Identical processing, test result are as shown in table 1.As it can be seen from table 1 the ion-conductance of solid electrolyte/cellulose composite diaphragm Conductance is significantly improved relative to pure cellulose diaphragm.
Table 1
Title R(Ω) σ(S/cm)
3 composite diaphragm of embodiment 53.8 1.09×10-4
1 cellulosic separator of comparative example 87.6 6.67×10-5
The present invention is beaten cellulose with microfibrillar structure prepared by dispersion by height and inorganic solid electrolyte is compound, Hygrometric state paper is made by copy paper technique, and then drying prepares composite diaphragm, the composite diaphragm that through the invention prepared by preparation method Pore size distribution$ is uniform, and prepares convenient, is suitable for producing in batches, while heat resistance is high, and wellability is good, ionic conductivity Height, breakdown characteristics are strong, are suitable for lithium ion battery separator, while composite inorganic solid electrolyte, can also play electrolyte Effect.
Above-described specific implementation mode has carried out further the purpose of the present invention, technical solution and advantageous effect It is described in detail, it should be understood that the foregoing is merely the specific implementation mode of the present invention, is not intended to limit the present invention Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include Within protection scope of the present invention.

Claims (10)

1. a kind of preparation method of inorganic solid electrolyte-cellulose composite diaphragm, which is characterized in that the preparation method packet It includes：
Cellulosic material is added in deionized water S10, impregnates, is then ground, is obtained with fento knot in pulper The cellulose slurries of structure；
Inorganic solid electrolyte is added in deionized water and suspension is made by S20, and wet strength agent is added and is stirred with cellulose slurries, It is uniformly mixed；
S30 is formed a film the cellulose slurries copy paper containing solid electrolyte using copy paper technique, i.e., wet cellulose electrolyte is multiple Close diaphragm；
S40, hygrometric state composite diaphragm is dried in an oven, that is, prepares required cellulose-solid electrolyte composite diaphragm.
2. preparation method according to claim 1, which is characterized in that the cellulosic material includes wood pulp, jute pulp, cotton pulp Or one or more of bamboo pulp mixed slurry.
3. preparation method according to claim 1, which is characterized in that a diameter of 200- of cellulose in cellulose slurries 500nm。
4. preparation method according to claim 1, which is characterized in that manufactured a concentration of 1wt%- of cellulose slurries 50wt%.
5. preparation method according to claim 1, which is characterized in that the inorganic solid electrolyte includes NASICON types At least one of structure, LISICON types structure, garnet type structure, Ca-Ti ore type and its compound.
6. preparation method according to claim 1, which is characterized in that suspension is made in inorganic solid electrolyte, wherein The mass percent concentration of inorganic solid electrolyte is 5%-50%.
7. preparation method according to claim 1, which is characterized in that the wet strength agent includes chitosan, dialdehyde starch, gathers Maleic acid, Malaysia sweet tea/at least one of vinyl alcohol terpolymer and its compound.
8. preparation method according to claim 1, which is characterized in that ingredient is in the composite diaphragm：45%-95% is fine Dimension element, 0.5%-50% solid electrolytes, 0.5%-4% wet strength agents.
9. preparation method according to claim 1, which is characterized in that the thickness of the composite diaphragm is 10 μm -100 μm.
10. a kind of inorganic solid electrolyte/cellulose composite diaphragm, which is characterized in that the composite diaphragm is by claim 1-9 Preparation method described in any claim is prepared.
CN201810332125.2A 2018-04-13 2018-04-13 A kind of inorganic solid electrolyte-cellulose composite diaphragm and preparation method thereof Pending CN108470875A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109560235A (en) * 2018-12-05 2019-04-02 河北金力新能源科技股份有限公司 A kind of new type lithium ion battery aramid fiber diaphragm preparation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102522517A (en) * 2011-12-22 2012-06-27 中国科学院青岛生物能源与过程研究所 Cellulose/inorganic particle composite diaphragm for lithium secondary battery and preparation method thereof
CN107615553A (en) * 2015-06-08 2018-01-19 富士胶片株式会社 Solid electrolyte composition, solid state secondary battery electrode slice, solid state secondary battery and the manufacture method of solid state secondary battery electrode slice and solid state secondary battery
CN107681196A (en) * 2017-09-22 2018-02-09 山东森鑫环保科技有限公司 Without synthetic polymer flexible solid dielectric film and its preparation method and its application
CN107887554A (en) * 2017-10-23 2018-04-06 柔电（武汉）科技有限公司 A kind of preparation method of flexible 3 D solid electrolyte barrier film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102522517A (en) * 2011-12-22 2012-06-27 中国科学院青岛生物能源与过程研究所 Cellulose/inorganic particle composite diaphragm for lithium secondary battery and preparation method thereof
CN107615553A (en) * 2015-06-08 2018-01-19 富士胶片株式会社 Solid electrolyte composition, solid state secondary battery electrode slice, solid state secondary battery and the manufacture method of solid state secondary battery electrode slice and solid state secondary battery
CN107681196A (en) * 2017-09-22 2018-02-09 山东森鑫环保科技有限公司 Without synthetic polymer flexible solid dielectric film and its preparation method and its application
CN107887554A (en) * 2017-10-23 2018-04-06 柔电（武汉）科技有限公司 A kind of preparation method of flexible 3 D solid electrolyte barrier film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109560235A (en) * 2018-12-05 2019-04-02 河北金力新能源科技股份有限公司 A kind of new type lithium ion battery aramid fiber diaphragm preparation method

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