CN109781756A - A kind of battery and its assemble method for in-situ TiC particles test - Google Patents
A kind of battery and its assemble method for in-situ TiC particles test Download PDFInfo
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- CN109781756A CN109781756A CN201910152425.7A CN201910152425A CN109781756A CN 109781756 A CN109781756 A CN 109781756A CN 201910152425 A CN201910152425 A CN 201910152425A CN 109781756 A CN109781756 A CN 109781756A
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Abstract
The invention belongs to battery in-situ tests, electrochemical field, more particularly, to a kind of battery and its assemble method for in-situ TiC particles test.The characteristics of sufficiently combining the test of existing battery in-situ TiC particles and demand, specific aim redesigns the in-situ TiC particles test process of battery electrode material, accordingly propose a kind of new battery assembly method for in-situ TiC particles test, the window material for replacing traditional metallic beryllium to test as electrode material in-situ TiC particles using carbon paper, it is applied in the test of battery electrode material in-situ TiC particles, the variation of battery electrode material product and phase in charge and discharge process is measured, in more cheap and environmental-friendly method convenient for studying the reaction mechanism of battery charge and discharge process.Thus solve it is existing carried out with beryllium window die expensive existing for in-situ TiC particles test, exist to environment and pollute, the complicated difficult technical problem of assembling steps.
Description
Technical field
The invention belongs to battery in-situ test, electrochemical field, more particularly, to a kind of for in-situ TiC particles test
Battery and its assemble method.
Background technique
X-ray powder diffraction (XRD) is a kind of quick analytical technology, is mainly used for the identification of phases of crystalline material, and can mention
For the information in relation to unit cell dimension.It by the material fine gtinding of analysis, homogenizes, and measures average ontology composition.X-ray powder
Diffraction (XRD) is most widely used for identifying unknown crystalline material (such as minerals, inorganic compound).Moreover, X-ray powder
Last diffraction (XRD) can also be used in the characterization of crystalline material, and identification is difficult to carry out fine mineral (such as clay and mixing of optical measurement
Layer clay), measure unit cell dimension and sample purity.
In the charge and discharge process of battery, crystalline types, crystal parameter of electrode material etc. can change, for determination
The specific variation that electrode material occurs in charge and discharge process, researchers generally use in-situ TiC particles and carry out in fact to electrode material
When observation.So as to deduce the intermediate product generated in electrochemical reaction process, pass through these intermediate product energy
Enough deduce the mechanism of reaction.A kind of derivative means of testing of the in-situ TiC particles as XRD, in li-ion electrode materials test
Good utilization is arrived, it can detect the variation of product and phase of the battery during charge and discharge, and energy in real time
Mechanism enough for lithium ion battery charge and discharge provides foundation.In short, in-situ TiC particles is effective electric with that can greatly improve research
The efficiency of pole material electrochemical reaction mechanism is the effective of variation of the research lithium ion battery electrode material in charge and discharge process
Means.
Currently, the mold for being mainly used for in-situ TiC particles test in the market is beryllium window die.In all metals, beryllium is saturating
The ability for crossing X-ray is most strong, there is the title of glassy metal, so beryllium is the material for manufacturing X-ray tube wicket and not replacing.So
And beryllium and its compound have severe toxicity, and carcinogenic, will cause pollution to environment.And metallic beryllium is expensive, surveys every time
Higher cost required for trying.Due to its difficulty of test is big, equipment installs complexity, test condition harshness etc., it is not
It is widely used.So we urgently develop a kind of in-situ TiC particles test method of environmental protection and economy, for studying battery electrode
The variation of product and phase of the material in charge and discharge process.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of electricity for in-situ TiC particles test
The characteristics of pond and its assemble method, the sufficiently test of combination existing battery in-situ TiC particles and demand, specific aim is to battery electrode material
In-situ TiC particles test process is redesigned, and a kind of new battery assembly method for in-situ TiC particles test is accordingly proposed,
It is applied in the test of battery electrode material in-situ TiC particles, battery electricity can be measured in more cheap and environmental-friendly method
The variation of pole material product and phase in charge and discharge process, convenient for studying the reaction mechanism of battery charge and discharge process.Thus it solves
It is existing to be carried out with beryllium window die expensive existing for in-situ TiC particles test, exist to environment and pollute, assembling steps complexity is tired
Difficult technical problem.
To achieve the above object, according to one aspect of the present invention, a kind of battery pack for in-situ TiC particles test is provided
Dress method, includes the following steps:
(1) cell negative electrode material is coated in the window material for being used for X-ray and penetrating using binder bonding, is born
It is loaded with the window material of cell negative electrode material；And the window material is conductive materials, and being capable of exclusion of water and oxygen；
(2) cell positive material and diaphragm are stacked gradually, electrolyte is added dropwise on diaphragm；
(3) window material that load has cell negative electrode material is covered on the diaphragm, and load has battery cathode material
The side of material is in contact with the diaphragm；The cell positive material, diaphragm, electrolyte and cell negative electrode material constitute battery master
Body structure；
(4) side that the battery main body structure is encapsulated using encapsulating material, is allowed to exclusion of water and oxygen, obtains for original
The assembled battery of position XRD test.
Preferably, the window material is carbon paper.
Preferably, the cell positive material and the window material are separately connected conducting wire and draw, for connecting battery
Test equipment.
Preferably, the encapsulating material by weight, including 60~70 parts of ultraviolet curing prepolymers, 20~35 parts
Reactive diluent monomer and 5~15 parts of photoinitiator.
Preferably, the ultraviolet curing prepolymer is urethane acrylate or epoxy acrylate；
The reactive diluent monomer is selected from tripropylene glycol, 1,6 hexanediol diacrylate and methacrylic acid-
Beta-hydroxy ethyl ester；
The photoinitiator is selected from 2,4,6- trimethylbenzoy-dipheny phosphine oxide, 1- hydroxycyclohexylphenyl first
Ketone and 2- hydroxy-2-methyl -1- phenylacetone.
Preferably, the encapsulation specifically: the encapsulating material is added dropwise on the side of the battery main body structure,
Exposed under UV light is to encapsulate the side of the battery main body structure.
Preferably, the substrate platform center for assembling the battery has groove, and the battery main body structure is assembled
After, liquid encapsulating material is added dropwise in the groove, so that the surrounding of the battery main body structure is immersed in encapsulating material,
Then ultraviolet light is used, the encapsulating material solidifies after exposure, realizes the isolation water oxygen of battery surrounding side.
Other side according to the invention provides the in-situ TiC particles that are used for that assemble method described in one kind obtains and tests
Assembled battery, from bottom to top include cell positive material, diaphragm, cell negative electrode material, membrane surface dropwise addition has electrolysis
Liquid；
The cell negative electrode material is carried on the window material penetrated for X-ray, and the window material it is conductive and
It being capable of exclusion of water and oxygen；
The battery is the battery after being encapsulated using encapsulating material, being capable of exclusion of water and oxygen.
Preferably, the window material is carbon paper.
Preferably, the battery is lithium ion battery or sodium-ion battery.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect:
(1) the present invention provides it is a kind of for in-situ TiC particles test battery assembly method, by select suitably with for
The window material that X-ray passes through cooperates suitable battery packaging material and packaging method, enables battery in normal charge and discharge
While carry out the XRD test of cell negative electrode material in situ.
(2) present invention by by ultraviolet curing prepolymer, reactive diluent monomer and photoinitiator according to a certain percentage
It is mixed to get ultraviolet light solidification presoma, which is used as the battery packaging material tested for in-situ TiC particles, and existing
Metal material encapsulating material it is different, be plastic material, be it is colorless and transparent, be convenient for X-ray transparent.Compared to common beryllium
Window test, have it is low in cost, assembling steps are simple to operation, and material therefor belongs to environmentally friendly.
(3) present invention is coated into cell negative electrode material using carbon paper, using carbon paper as window material, cooperated specific solid
Change the in-situ TiC particles test that glue encapsulation technology is applied to lithium ion battery electrode material, there is cure package technique in preparation process
Simply, low in cost, the advantages that design easy to process.
(4) present invention is surveyed using the in-situ TiC particles that the battery that carbon paper coating, solidification glue encapsulate carries out electrode material
Examination, obtained in-situ TiC particles data are fully aware of complete, can satisfy the change to electrode material product and phase in charge and discharge process
Change, convenient for studying the reaction mechanism of battery charge and discharge process.
Detailed description of the invention
Fig. 1 is the process flow diagram prepared in the embodiment of the present invention.
Fig. 2 is the pictorial diagram of used material before the assembling that the preparation process of the embodiment of the present invention obtains.
Fig. 3 is the pictorial diagram after the assembling that the preparation process of the embodiment of the present invention obtains.
Fig. 4 is the in-situ TiC particles figure for the battery for in-situ TiC particles test that the preparation process of the embodiment of the present invention obtains.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
The present invention provides a kind of battery assembly methods for in-situ TiC particles test, include the following steps:
(1) cell negative electrode material is coated in the window material for being used for X-ray and penetrating using binder bonding, is born
It is loaded with the window material of cell negative electrode material；And the window material is conductive and being capable of exclusion of water and oxygen；
(2) cell positive material and diaphragm are stacked gradually, electrolyte is added dropwise on diaphragm；
(3) window material that load has cell negative electrode material is covered on the diaphragm, and load has battery cathode material
The side of material is in contact with the diaphragm；The cell positive material, diaphragm, electrolyte and cell negative electrode material constitute battery master
Body structure；
(4) side that the battery main body structure is encapsulated using encapsulating material, is allowed to exclusion of water and oxygen, obtains for original
The assembled battery of position XRD test.
In battery assembly method of the present invention for in-situ TiC particles test, suitable penetrate for X-ray, substitution is found
The window material of the metallic beryllium of the prior art is most important, is not only required to penetrate X-ray, but also its XRD diffraction maximum
It is preferably able to distinguish with the diffraction maximum of cell negative electrode material, to avoid to cell negative electrode material X-ray diffraction analysis result
Interference.In addition, the window material is also required to exclusion of water and oxygen, just can guarantee in this way when battery carries out XRD test,
Battery can normal charge and discharge, make it possible in-situ TiC particles test.A variety of window materials have been attempted in experimentation, such as
Macromolecule polypropylene film (BOPP) and Kapton (PI), however, it was found that cannot be guaranteed the normal of XRD in-situ test
It carries out.Window material described in some embodiments of the present invention is carbon paper.Carbon paper surface is smooth, fine and close, and X-ray can penetrate,
And it derives peak angle degree at 25 °, angle where the derivative peak of surveyed cell negative electrode material is 28 ° and 38.5 ° or so, will not interfere electricity
The X-ray diffraction analysis of pond negative electrode material.
The present invention selects carbon paper to replace traditional metallic beryllium as the window material for electrode original position XRD test.Carbon paper
It is a kind of a kind of material being combined by carbon nano-fiber, there is good electric conductivity and flexibility.The present invention as
Window material finds the carrier that it is a kind of very excellent electrode material, and the X-ray diffraction peak of carbon paper is at 25 °, no
It can overlap, experimental result will not be impacted with the X-ray diffraction peak for the electrode material surveyed.The carbon paper of common model
It is able to satisfy the requirement of XRD in-situ test of the present invention.Common carbon paper model has SpectraCarb 2050A, CeTech
GDS090, Toray Carbon Paper120 etc..The carbon paper model JL-121 selected in some embodiments of the invention (passes through
It is commercially available to obtain), surface is smooth and fine and close, can exclusion of water and oxygen, test request can be met well.
The present invention is for its cell positive material in the battery assembly method of in-situ TiC particles test and window material difference
Connecting wire is drawn, for connecting blue electrical measurement test system CT2001A.In some embodiments of the invention, by taking glass slide as an example
The assembling of above-mentioned battery is carried out in substrate platform, and the substrate platform center has the groove of a 2 × 2cm.Carrying out battery
Before assembling, EQ-PLiB-ATC aluminium pole ears are first pasted in substrate platform, then according to the method described above successively by anode material
After the battery pack that material, diaphragm, electrolyte and negative electrode material are constituted installs, on window material surface, such as carbon paper surface stickup is led
Electric glue, then extraction wire, the assembled battery and blue electrical measurement test system CT2001A is connected.
The present invention will carry out the in-situ test of XRD, it is desirable that the battery in XRD test process can normal charge and discharge, this
Sample requires the battery of assembling to allow for exclusion of water and oxygen, this just needs to select suitable encapsulating material, and the encapsulating material is only
For encapsulating the surrounding of the assembled battery.
In some embodiments, the encapsulation specifically: the encapsulating material is added dropwise to the side of the battery main body structure
On face, exposed under ultraviolet light to encapsulate the side of the battery main body structure.
In some embodiments, the time for exposure is 180~400s, preferably 320s.
In some embodiments, after above-mentioned battery main body structure is assembled, due to the substrate platform for assembled battery
Center has groove, liquid encapsulating material is added dropwise in the groove, so that the surrounding of the battery main body structure stacked gradually is soaked
Then bubble uses ultraviolet light in encapsulating material, the encapsulating material solidifies after exposure, realizes the isolation of battery surrounding side
Water oxygen.The selection of suitable encapsulating material is also critically important.In some embodiments, the encapsulating material by weight, including 60
~70 parts of ultraviolet curing prepolymer, 20~35 parts of reactive diluent monomer and 5~15 parts of photoinitiator.Wherein light is solid
Change the main component that performed polymer is Polymeric encapsulation, reactive diluent monomer is crosslinking agent and solvent in solidifying, and photoinitiator exists
It is generated free radicals when illumination, carries out solidification process quickly.
In some embodiments, the ultraviolet curing prepolymer is urethane acrylate (PUA) or epoxy acrylate
(EA), preferably urethane acrylate.PUA and EA photocuring performed polymer and diaphragm and electrode material are in charge and discharge process
Other side reactions such as redox will not occur, there is preferable compatibility, and the adhesive after solidify is with polyurethane
High-wearing feature, adhesion strength, flexibility, high-peeling strength and excellent resistance to low temperature and polyacrylate brilliance optics
Performance and weatherability.
In some embodiments, reactive diluent monomer is selected from tripropylene glycol (TPGDA), 1,6- hexanediyl
Ester (HDDA) and methacrylic acid-beta-hydroxy ethyl ester (HEMA), preferably tripropylene glycol, with high activity and low-shrinkage
The advantages that.
In some embodiments, the photoinitiator be selected from 2,4,6- trimethylbenzoy-dipheny phosphine oxides (TPO),
1- hydroxycyclohexyl phenyl ketone (184) and 2- hydroxy-2-methyl -1- phenylacetone (1173), preferably 2,4,6- trimethyls
Benzoyl-diphenyl phosphine oxide, space charge force with higher, good heat stability, to cause wavelength relatively broad etc.
Advantage.
The present invention provides it is a kind of for in-situ TiC particles test assembled battery, from bottom to top include cell positive material, every
Film, cell negative electrode material, the membrane surface dropwise addition have electrolyte；
The cell negative electrode material is carried on the window material penetrated for X-ray, and window material surface light
It is sliding and fine and close, it being capable of exclusion of water and oxygen；
The battery is the battery after being encapsulated using encapsulating material, being capable of exclusion of water and oxygen.
In some preferred embodiments, the window material is carbon paper.
Battery and its assemble method proposed by the present invention for in-situ TiC particles test is suitable for various batteries or half-cell,
Such as including lithium ion battery or sodium-ion battery.
In some embodiments, battery is lithium ion battery, and anode material for lithium-ion batteries is circular high-purity lithium piece.
In some embodiments, the battery diaphragm is 2300 diaphragm of celgard, electrolyte 1molL-1LiPF6 carbon
Sour ethyl: diethyl carbonate (V:V=1:1).
In some embodiments, the cell negative electrode material be it is powdered, can obtain as follows: by active material,
Carbon black (Super P) and Kynoar (PVDF) 85~95:5 in mass ratio~10:5~10 mixing, instill 6-10 drop N- first
Base pyrrolidones (NMP) grinds 10-15min, negative for lithium ion battery on the carbon paper after grinding uniformly coated in 2cm ﹡ 2cm
Pole material, PVDF acts as the effect of binder here.
The present invention loads battery cathode material as the window material passed through for X-ray, and using carbon paper coating using carbon paper
Material, cooperation ultraviolet cured adhesive encapsulation, proposes a kind of battery and its assemble method for in-situ TiC particles test.It will need to survey
The electrode material slurry of examination is coated on carbon paper, then in intermediate reeded glass slide over-assemble battery, finally with a kind of purple
Outer optic-solidified adhesive solidification is packaged.Compared to traditional in-situ TiC particles test method, which does not need to use expensive
Beryllium window die, it is only necessary to some simple materials, it is low in cost；On the other hand, carbon paper can effectively starvation and water, together
When X-ray can be radiated at the electrode material coated on carbon paper through carbon paper, and assembling steps are simple to operation；It finally will be quasi-
The electrode test material got ready is directly used in in-situ TiC particles test, and X-ray can be radiated on electrode material through carbon paper, thus
Chemical reaction in detailed characterizations charge and discharge process, is conducive to study and produces in various batteries such as lithium ion battery charge and discharge process
The variation of object and phase.
In some embodiments, a kind of lithium ion assembled battery for in-situ TiC particles test provided by the invention, such as Fig. 1 institute
Show, by assembling sequence, including objective table, conducting wire, positive electrode, diaphragm, electrolyte coats window material (its of negative electrode material
It is covered on the surface of assembled battery, also referred to as cover plate), conducting wire, optic-solidified adhesive presoma.
Wherein, objective table can be normal transparent glass slide or center is the glass slide of square groove.Preferably, the load
It is the glass slide of square groove centered on object platform.The conducting wire is copper conductive adhesive or aluminium electrode.Preferably, the positive wire is
Aluminium electrode.The positive electrode is lithium piece or cobalt acid lithium.Preferably, the positive electrode is high-purity lithium piece.The diaphragm is
2300 diaphragm of celgard.The electrolyte is 1molL-1LiPF6Ethylene carbonate: dimethyl carbonate (V:V=1:1).
The window material of the coating negative electrode material is carbon paper.The cathode conductor is copper conductive adhesive, the later spot welding on copper conductive adhesive
Connect a conducting wire.Optic-solidified adhesive presoma includes that performed polymer is urethane acrylate (PUA), and reactive diluent monomer is two
Contracting tripropylene glycol (TPGDA), initiator 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO).As in Fig. 2 from a left side
Center objective table with groove, EQ-PLiB-ATC aluminium pole ears, carbon paper JL-121, conducting wire, copper conductive adhesive, coating are followed successively by the right side
There is the carbon paper of negative electrode material.
The following are embodiments:
A kind of carbon paper coating active material ultraviolet light cure package battery is present embodiments provided for the survey of battery in-situ TiC particles
The method of examination, comprising the following steps:
(1) PUA is ultraviolet curing prepolymer, TPGDA is reactive diluent monomer, TPO is photoinitiator, according to 60:
The percent mass of 30:10 obtains photocuring presoma than mixing；
(2) celgard 2300 is diaphragm；
(3) high-purity lithium piece is anode slice of lithium ion battery；
(4) active material, carbon black (Super P) and Kynoar (PVDF) 80:10:10 in mass ratio are mixed, drop
Enter 6-8 drop N-Methyl pyrrolidone (NMP), after mixing on the carbon paper coated in 2cm ﹡ 2cm, obtains negative electrode of lithium ion battery
Material；
(5) anode slice of lithium ion battery, diaphragm being stacked gradually on glass slide, 5 drop electrolyte are added dropwise in diaphragms,
Then the negative electrode material of stacking carbon paper coating, is added dropwise appropriate photocuring presoma, and make this in the groove at glass slide center
Battery structure surrounding after stacking gradually is immersed in the presoma, is then 5mW/cm in light intensity2, wavelength be 365nm it is ultraviolet
320s is irradiated under light, obtains battery of the carbon paper coating for in-situ TiC particles test.
Above-mentioned encapsulating material is applied to prepare the battery of in-situ test, process flow diagram figure is as shown in Figure 1, obtain
Carbon paper as shown in Figures 2 and 3 coats active material ultraviolet light cure package battery.It is detected, is prepared for in-situ TiC particles
The battery of test, sealing effect is preferable, and X-ray is easy to be radiated on active material through carbon paper, and obtained XRD diagram picture is such as
Fig. 4, image very complete display, it is sufficient to for studying the variation of product and phase of the battery electrode material in charge and discharge process.
In Fig. 4, angle where derivative peak is 28 ° and 38.5 °, during the charge and discharge cycles that the 0th circle is enclosed to 130,28 ° and 38.5 °
The intensity of place's diffraction maximum is gradually reduced, this shows mutually to be changed with the progress of charge and discharge process, negative electrode material, this is
It is lithium/sodium ion insertion abjection process, meeting in-situ TiC particles test needs purpose to be achieved.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of battery assembly method for in-situ TiC particles test, which comprises the steps of:
(1) cell negative electrode material is coated in the window material for being used for X-ray and penetrating using binder bonding, obtaining load has
The window material of cell negative electrode material；And the window material is conductive materials, and being capable of exclusion of water and oxygen；
(2) cell positive material and diaphragm are stacked gradually, electrolyte is added dropwise on diaphragm；
(3) window material that load has cell negative electrode material is covered on the diaphragm, and load has cell negative electrode material
Side is in contact with the diaphragm；The cell positive material, diaphragm, electrolyte and cell negative electrode material constitute battery main body knot
Structure；
(4) side that the battery main body structure is encapsulated using encapsulating material, is allowed to exclusion of water and oxygen, obtains in situ
The assembled battery of XRD test.
2. assemble method as described in claim 1, which is characterized in that the window material is carbon paper.
3. assemble method as described in claim 1, which is characterized in that the cell positive material and window material difference
Connecting wire is simultaneously drawn, for connecting battery test apparatus.
4. assemble method as described in claim 1, which is characterized in that the encapsulating material by weight, including 60~70
The ultraviolet curing prepolymer, 20~35 parts of reactive diluent monomer and 5~15 parts of photoinitiator of part.
5. assemble method as described in claim 1, which is characterized in that the ultraviolet curing prepolymer is polyurethane acroleic acid
Ester or epoxy acrylate；
The reactive diluent monomer is selected from tripropylene glycol, 1,6 hexanediol diacrylate and methacrylic acid-β-hydroxyl
Ethyl ester；
The photoinitiator be selected from 2,4,6- trimethylbenzoy-dipheny phosphine oxide, 1- hydroxycyclohexyl phenyl ketone and
2- hydroxy-2-methyl -1- phenylacetone.
6. assemble method as described in claim 1, which is characterized in that the encapsulation specifically: the encapsulating material to be added dropwise
To the side of the battery main body structure, exposed under ultraviolet light to encapsulate the side of the battery main body structure.
7. assemble method as described in claim 1, which is characterized in that the substrate platform center for assembling the battery has recessed
Liquid encapsulating material is added dropwise in the groove by slot after assembling the battery main body structure, so that the battery main body
The surrounding of structure is immersed in encapsulating material, then uses ultraviolet light, and the encapsulating material solidifies after exposure, realizes battery four
The isolation water oxygen of all sides.
8. the assembled battery for in-situ TiC particles test that assemble method as described in any one of claim 1 to 7 obtains, special
Sign is, from bottom to top includes cell positive material, diaphragm, cell negative electrode material, and the membrane surface dropwise addition has electrolyte；
The cell negative electrode material is carried on the window material penetrated for X-ray, and the window material is conductive and can
Exclusion of water and oxygen；
The battery is the battery after being encapsulated using encapsulating material, being capable of exclusion of water and oxygen.
9. assembled battery as claimed in claim 8, which is characterized in that the window material is carbon paper.
10. assembled battery as claimed in claim 8, which is characterized in that the battery is lithium ion battery or sodium-ion battery.
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| CN111948237A (en) * | 2020-08-06 | 2020-11-17 | 厦门厦钨新能源材料股份有限公司 | Soft package-like battery device for in-situ X-ray diffraction test and assembling method |
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