CN110473754B - Preparation optimization method of X-ray film window electrode and X-ray film window electrode obtained by same - Google Patents

Preparation optimization method of X-ray film window electrode and X-ray film window electrode obtained by same Download PDF

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CN110473754B
CN110473754B CN201910618474.5A CN201910618474A CN110473754B CN 110473754 B CN110473754 B CN 110473754B CN 201910618474 A CN201910618474 A CN 201910618474A CN 110473754 B CN110473754 B CN 110473754B
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CN110473754A (en
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于鹏飞
刘啸嵩
郑顺
任国玺
张念
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Shanghai Institute of Microsystem and Information Technology of CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J35/00—X-ray tubes
    • H01J35/02—Details
    • H01J35/04—Electrodes ; Mutual position thereof; Constructional adaptations therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems

Abstract

The invention relates to a preparation optimization method of an X-ray film window electrode, which comprises the following steps: determining an X-ray energy range from the electrode material; determining at least one substrate layer based on the X-ray transmission capability within a specific energy range; determining at least one conductive layer based on the X-ray penetration capability within a specific energy range; obtaining at least one composite layer with a conductive layer covering the substrate layer; according to O of the composite layer2And H2O transmittance defining at least one composite layer; determining the optimal material and the optimal thickness of the composite layer by combining with a spectroscopy signal test of a standard electrode material; and forming an electrode layer on the composite layer to obtain the X-ray thin film window electrode. The invention also relates to an X-ray film window electrode which comprises a three-layer composite structure formed by sequentially compounding the substrate layer, the conducting layer and the electrode layer. The invention simultaneously considers electrochemical and spectroscopy test factors, provides a high-efficiency window electrode composite structure, and formulates a rational optimization scheme of the window electrode.

Description

Preparation optimization method of X-ray film window electrode and X-ray film window electrode obtained by same
Technical Field
The invention relates to the field of X-ray testing of batteries, in particular to a preparation optimization method of an X-ray thin film window electrode and the X-ray thin film window electrode obtained by the same.
Background
With the increasing demand for energy storage, a large number of ion battery technologies have been developed, including lithium ion batteries, sodium ion batteries, and multivalent ion batteries. The cognition of the ion storage process is the basis for further improving the performance indexes of the battery systems: the recognition of charge compensation in the reaction process can promote the increase of the battery capacity; understanding the reaction kinetics is helpful for improving the rate performance of the battery; the interpretation of the irreversible reaction process helps to improve the cycle life of the battery. Abundant X-ray technology is a powerful tool to resolve the ion storage mechanism of battery systems: x-ray diffraction and scattering methods can understand the reaction process from the perspective of the long-range order of the structure; the X-ray absorption spectroscopy method can resolve the reaction process from the perspective of local structures or electronic structures. The X-ray test, namely the in-situ X-ray test, is carried out in real time in the working process of the battery, so that the analysis precision and accuracy of the reaction process can be improved on one hand, and the kinetic study of the reaction process can be carried out on the other hand.
The key of the in-situ X-ray testing technology lies in the design of an in-situ reaction tank, and in the center, the design of a reaction tank window is adopted, because the X-ray is incident through the window to acquire the chemical reaction information within the window. In order to ensure the smooth operation of the in-situ test, on one hand, the window needs to reduce the attenuation of the X-ray as much as possible, and the smooth operation of the X-ray test is ensured; on the other hand, sufficient chemical and electrochemical inertness is maintained in contact with the electrolyte, while blocking O2And H2And the smooth electrochemical reaction is ensured by the entering of O. Research reports that metal Be can Be used as a window, the X-ray transmittance is high, and O can Be isolated2And H2O, less interference with the spectrum in X-ray testing. Be, however, is extremely toxic and not easy to operate; meanwhile, Be has poor electrochemical stability, BeO is easily formed in the reaction process, and the interference of BeO on an X-ray spectrum is large; moreover, the price of Be is high. In CN102435625A, the inventors performed in situ XRD tests using polymeric material as window material. However, the polymer material may swell when contacting with the organic electrolyte, which affects the sealing performance; while ensuring effective isolation of O2And H2O, the thickness of the polymer material tends to be large (10. about.0mm). In CN103540131B and US8498381B2, the inventors prepared a composite film of polymer/carbon-based material as a window material, which improves the mechanical strength and O-exclusion of the window2And H2The capacity of O. In CN107487064A, the inventors prepared a polymer layer/metal layer composite film as a window material, which also enhances the mechanical strength and O isolation of the window2And H2The capacity of O. However, the above in-situ window design schemes do not consider the influence of the electrode, on one hand, the current collector will cause the attenuation of the X-ray, and in addition, the window parameter rational optimization is lacked,this makes the above-mentioned in-situ windows mostly only suitable for high-energy X-ray techniques with strong penetration capability; on the other hand, the relation between the window and the electrode is neglected, the relevance of electrochemistry and spectroscopy testing is weakened, and the deviation between the in-situ electrochemical reaction in the testing area and the normal reaction is easy to be larger. Since in the flexible and soft X-ray field, the penetration ability of X-rays decreases as their energy decreases, higher demands are made on the design of in-situ windows: on one hand, the window design is optimized to avoid the attenuation of X-rays to the maximum extent, and the optimal X-ray test signal is obtained; on the other hand, to ensure that the in-situ electrochemical reaction is consistent with the actual cell.
Disclosure of Invention
In order to solve the problem that the in-situ window design scheme in the prior art does not consider the influence of the electrode, the invention aims to provide an X-ray film window electrode preparation optimization method and an X-ray film window electrode obtained by the method.
The preparation optimization method of the X-ray film window electrode comprises the following steps: s1, determining the X-ray energy range according to the electrode material; s2, determining a first material and a first thickness of at least one matrix layer according to the absorption length in the X-ray energy range; s3, determining a second material and a second thickness of the at least one conductive layer based on the absorption length in the X-ray energy range; s4, growing a second material on the first material by using a vapor deposition method to obtain at least one composite layer with a conductive layer covering the substrate layer; s5, determining a final composite layer by combining a spectrum signal test of a standard electrode material; and S6, forming an electrode layer on the second material of the final composite layer by using a spin coating method, a blade coating method or a vapor deposition method, thereby obtaining the X-ray film window electrode.
Preferably, the X-ray energy range is 50eV to 20000 eV. In a preferred embodiment, the electrode material is Mo6S8And the X-ray energy range is 2000eV-3000 eV.
Preferably, the step S2 is specifically: determining a first candidate material and a first candidate thickness for the plurality of base layers based on the absorption length in the X-ray energy range; according to the first candidate material inAnd further determining a plurality of base material layers according to the evolution of the light transmittance at different X-ray energies along with the first candidate thickness. In a preferred embodiment, the first matrix layer candidate is Si with a photon absorption length of about 1-3 μm3N4Its thickness is less than 1.5 μm; the second candidate matrix layer is PP with photon absorption length of about 30-100 μm, and the thickness of the second candidate matrix layer is less than 50 μm; the third candidate matrix layer is PI with photon absorption length of about 13-42 μm, and the thickness of the third candidate matrix layer is less than 20 μm; the fourth candidate matrix layer is PTFE with a photon absorption length of about 4-13 μm, and a thickness of less than 6.5 μm. In a preferred embodiment, the first substrate layer is Si with a thickness of less than 250nm3N4(ii) a The second matrix layer is PP with the thickness of less than 25 mu m; the third matrix layer is PI with the thickness of less than 12 mu m.
Preferably, the step S2 further includes: according to the O of the base layer material2And H2O permeability to define a plurality of matrix layers. In a preferred embodiment, O of PI2And H2O having a permeability greater than that of PP2And H2And O transmittance. In the most preferred embodiment, the matrix layer is PI with a thickness of less than 12 μm.
Preferably, the first thickness is 50nm to 2 mm.
Preferably, the step S3 further includes: the plurality of conductive layers is determined according to a reaction potential of the electrode material, conductivity of the conductive layer material, and electrochemical stability of the conductive layer material. In a preferred embodiment, the electrode material is Mo6S8The reaction potential is 1.0-3.0V, the first conductive layer is Cu, and the second conductive layer is Al.
Preferably, the step S3 is specifically: determining a second candidate material and a second candidate thickness for the plurality of conductive layers based on the absorption length in the X-ray energy range; and further determining the plurality of conductive layers according to the evolution of the light transmittance of the second candidate material under different X-ray energies along with the thickness of the second candidate. In a preferred embodiment, the first candidate conductive layer is Cu with a thickness of less than 500 nm; the second candidate conductive layer is Al with a thickness of less than 1.7 μm. In a preferred embodiment, the conductive layer is Al with a thickness of less than 250 nm.
Preferably, the second thickness is 50nm to 2 mm.
Preferably, the vapor deposition methods include Chemical Vapor Deposition (CVD) and physical vapor deposition (magnetron sputtering and pulsed laser deposition). In a preferred embodiment, Al is grown on the PI surface using a magnetron sputtering method. In a particularly preferred embodiment, the final composite layer is a composite structure of 6 μm PI and 100nm Al.
Preferably, the electrode layer has a film surface density in the range of 0.1ug/cm2To 30mg/cm2. In a preferred embodiment, the surface density of the coated surface is 0.5mg/cm2Left and right.
Preferably, the preparation optimization method further comprises a step S7 of assembling the X-ray thin film window electrode into an in-situ battery for electrochemical performance test, and performing inspection by combining an X-ray test method.
Preferably, the X-ray testing method comprises one or more of X-ray absorption, X-ray diffraction and X-ray scattering.
The X-ray film window electrode comprises a three-layer composite structure formed by sequentially compounding a substrate layer, a conducting layer and an electrode layer.
Preferably, the matrix layer is 3, 4- (methylenedioxy) cinnamic acid (Mylar, C)10H8O4) Polycarbonate (PC, C)16H14O3) Polymethyl methacrylate (PMMA, C)5H8O2) Polyimide (PI, C)22H10N2O5) Polypropylene (PP, C)3H6) Polytetrafluoroethylene (PTFE, C)2F4) Silicon nitride (Si)3N4) And Boron Nitride (BN).
Preferably, the conductive layer is at least one of Au, Ag, Al, Cu, and C.
Preferably, the electrode layers are positive and negative electrode materials, including layered electrodes (e.g., L iCoO)2、LiNi0.8Co0.1Mn0.1O2Graphite, etc.), polyanionic electrodes (e.g., L iFePO4) Lithium-rich layered electrodes (e.g. L i)2MnO3And L i2RuO3) Spinel electrodes (e.g. L)i2MnO4And L i4Ti5O12) And an oxide conversion electrode.
The invention determines the X-ray energy range according to the electrode material; determining at least one substrate layer based on the X-ray transmission capability within a specific energy range; determining at least one conductive layer based on the X-ray penetration capability within a specific energy range; obtaining at least one composite layer with a conductive layer covering the substrate layer; according to O of the composite layer2And H2O transmittance defining at least one composite layer; determining the optimal material and the optimal thickness of the composite layer by combining with a spectroscopy signal test of a standard electrode material; and forming an electrode layer on the composite layer to obtain the X-ray thin film window electrode. The invention simultaneously considers electrochemical and spectroscopy test factors, provides a high-efficiency window electrode composite structure, and formulates a rational optimization scheme of the window electrode. After the optimization of the system, the window electrode can ensure that the electrochemical reaction of the detection area is highly consistent with the actual battery reaction on one hand, and can ensure that high-quality X-ray spectroscopy signals are obtained in the reaction process on the other hand, so that the window electrode is more suitable for the fields of flexibility and soft X-rays. The method is relatively simple to operate, low in price and suitable for batch preparation and application in-situ X-ray tests.
Drawings
FIG. 1 shows the variation of photon absorption length with the type of the substrate layer in the interval of 2000-3000 eV;
FIG. 2A shows PI, PP and Si3N4The light transmittance of the substrate layer evolves with the thickness under 2400 eV;
FIG. 2B shows PI, PP and Si3N4The light transmittance of the substrate layer evolves with the thickness at 2500 eV;
FIG. 2C shows PI, PP and Si3N4The evolution condition of the light transmittance of the substrate layer along with the thickness at 2600 eV;
FIG. 2D shows PI, PP and Si3N4The light transmittance of the substrate layer evolves with the thickness under 2700 eV;
FIG. 3 shows the variation of photon absorption length with the type of the conductive layer in the interval of 2000-3000 eV;
FIG. 4A shows the evolution of the light transmittance of the Al and Cu conductive layers with the thickness at 2400 eV;
FIG. 4B shows the evolution of the light transmittance of the Al and Cu conductive layers with the thickness at 2500 eV;
FIG. 4C shows the evolution of the light transmittance of the Al and Cu conductive layers with the thickness at 2600 eV;
FIG. 4D shows the evolution of the light transmittance of the Al and Cu conductive layers with the thickness at 2700 eV;
FIG. 5 is a standard MoS2S K edge absorption spectrum under the condition that the powder covers the window and directly exposes the cavity;
FIG. 6 is an optimized Mo6S8Comparing the discharge curves of the window electrode and the normal button cell;
FIG. 7 is an optimized Mo6S8Window electrode and Mo6S8Comparing S K side absorption spectrum signals of the conventional powder;
fig. 8 is a plot of the electrochemistry obtained from an in situ experiment conducted based on an optimized electrode window versus the corresponding spectroscopy.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
In-situ Mo test by flexible X-ray absorption spectrum technology6S8S K edge of electrode and Mo L2,3Absorption spectra Mo L due to the energy range at side S K being around 2470eV2,3The edges are near 2520eV and 2625eV, respectively, so the photon absorption length of several matrix layers in the range from 2000 to 3000eV is calculated to screen for suitable matrix layers. As shown in FIG. 1, Si3N4The photon absorption length of (a) is about 1 to 3 μm. For the organic polymer film, the maximum PP absorption length is about 30-100 mu m; the absorption length of PI is about 13-42 μm; the absorption length of PTFE is the smallest, about 4-13 μm. To obtain a good signal, the film thickness is smaller than the absorption length (the thickness of the material where the light intensity is reduced to 1/e). Because the experiment adopts a reflection mode for collecting fluorescence signals, the light propagation distance is actually 2 times of the thickness of the film, and therefore, Si3N4The thickness of the PP film is required to be less than 1.5 mu m, and the thickness of the PP film is required to be more than 50 mu mThe PI absorption length is 20 μm or less, and the PTFE is 6.5 μm or less. For organic films, commercially available thickness specifications are 3, 6, 12, 24 and 50 μm, while Si is3N4The thickness can be tailored between 100-500 nm. PTFE membranes were first excluded in view of membrane operability and the effect of subsequent conductive layers.
To further determine the kind and thickness of the window material, organic polymer matrix layers with thicknesses of 3, 6, 12, 24 and 50 μm and Si with thicknesses of 100, 200, 300, 400 and 500nm were calculated3N4Light transmittances at 2400, 2500, 2600, and 2700 eV. In practical experiments, 70% -80% of light transmittance is a guarantee condition for obtaining high signal-to-noise ratio, and about 50% of light transmittance is a minimum condition for obtaining good signal-to-noise ratio. As shown in FIGS. 2A-2D, Si3N4Within the range of 100-500nm, the light transmittance under different energies can reach more than 80 percent; after the pp thickness reaches 50 μm, the light transmittance still exceeds 50%; the light transmittance of PI at 24 μm is 45% or more. Therefore, theoretically, Si within 250nm3N4PP films within 25 μm and PI films within 12 μm can be used as candidate substrate layers for X-ray windows. Although Si3N4Best effect, but considering Si3N4The cost of the window is high and, unless necessary, the organic film substrate is generally preferred. Further, O is considered to be excellent in PI2Isolation capability and better H2O barrier capability (see table 1), PI films are preferred as candidate substrate layers.
TABLE 1O of PP and PI2And H2Transmittance of O
Figure GDA0002490177490000061
The type and thickness of the conductive layer then need to be selected using similar steps as described above. Mo6S8The reaction potential of the reservoir L i is 1.0 to 3.0V vs. (L i/L i.)+) In the meantime. Common electrode current collectors are Cu and Al. The electrochemical window for Cu is 0 to 3.6V, while for Al is 1.0 to 5.0V. Thus from the electrochemical stability point of viewAnd Cu and Al can be used as the conductive layer. Based on the photon absorption lengths of Cu and Al in the range of 2000 to 3000eV shown in fig. 3, it was preliminarily determined that both Cu below 500nm and Al below 1.7 μm are likely to satisfy the test requirements. To further determine the thickness of the conductive layer, fig. 4A-4D show the light transmission at 2400, 2500, 2600, and 2700eV for Al and Cu with thicknesses of 50, 100, 200, and 500nm, respectively. The light transmittance of Al is still kept above 90% within 200nm, and the light transmittance is still kept above 80% at 500 nm; the light transmittance of Cu at 500nm was 54%. In view of conductivity and maximum light transmittance, Al is the most suitable window coating material, and the thickness is preferably controlled to 250nm or less. And after determining the types and the thickness ranges of the substrate layer and the conducting layer, growing an Al layer on the surface of the PI by using a magnetron sputtering method. In experiments, the battery sealed by adopting the composite window of 6 mu m PI/100nm Al can maintain stable operation within 48h, and can be stable even for an insensitive system for 7 days.
Next, the standard MoS was tested2The powder is directly exposed to the S K side absorption spectrum of the cavity and the window of the covering film, and is used for verifying the influence of the window on the signal. As can be seen from FIG. 5, the MoS of the overlay window2The signal-to-noise ratio of the S K side absorption spectrum is good and not much different from the direct exposure. The difference is that after covering the window, the peak intensity of the characteristic peak in front of the side around 2470eV increases slightly, probably due to the X-ray absorption of the window. However, since the spectral shape changes under the same test conditions are compared in the research, the window coverage does not cause influence. From the above, it is considered that the composite window of 6 μm PI/100nm Al can effectively meet the requirements of operability, electrochemical stability, light transmittance, conductivity and sealing property, and is suitable for Mo6S8In situ flexible X-ray absorption spectroscopy studies.
The thickness of the absorption spectrum fluorescence reflection collection mode may be more than 1 μm. Therefore, the electrode preparation can select a simpler blade coating method to carry out Mo6S8PVDF and acetylene black AB in a ratio of 8: 1: 1, coating a film on a PI/Al window by mixing NMP, wherein the surface density of the coating film is 0.5mg/cm2Left and right. Assembling the prepared window electrodeForming an in-situ battery, and carrying out electrochemical performance test. As can be seen from fig. 6, the electrochemical reaction characteristics are very close to those of the actual button cell, and the polarization characteristics are also very close, indicating that the reaction process of the window electrode is very close to that of the actual cell. FIG. 7 shows Mo assembled as a window electrode and directly exposed cavity for in situ cell6S8S K side absorption spectra comparison. The signal-to-noise ratio of the in-situ window electrode is very good and is similar to MoS2In the case of the standard sample, the characteristic intensity of the side pre-peak is slightly increased, but the comparison of the in-situ electrode spectral evolution is not influenced. FIG. 8 shows Mo developed based on optimized electrode windows6S8Electrochemical vs. corresponding S K absorption spectrum curves obtained in situ experiments. It can be seen that the evolution process of the high-quality S K absorption spectrum is obtained in real time in the process of the electrochemical reaction, the edge pre-peak evolution trend and the electrochemical curve show clear corresponding relation, and Mo in the electrochemical reaction process is finely analyzed6S8The evolution of local structures and electronic structures lays the foundation.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.

Claims (10)

1. The preparation optimization method of the X-ray film window electrode is characterized by comprising the following steps of:
s1, determining the X-ray energy range according to the electrode material;
s2, determining a first material and a first thickness of at least one matrix layer according to the absorption length in the X-ray energy range;
s3, determining a second material and a second thickness of the at least one conductive layer based on the absorption length in the X-ray energy range;
s4, growing a second material on the first material by using a vapor deposition method to obtain at least one composite layer with a conductive layer covering the substrate layer;
s5, determining a final composite layer by combining a spectrum signal test of a standard electrode material;
and S6, forming an electrode layer on the second material of the final composite layer by using a spin coating method, a blade coating method or a vapor deposition method, thereby obtaining the X-ray film window electrode.
2. The production optimization method according to claim 1, wherein the X-ray energy is in a range of 50eV to 20000 eV.
3. The preparation optimization method according to claim 1, wherein the step S2 specifically comprises: determining a first candidate material and a first candidate thickness for the plurality of land layers based on the absorption length; and further determining a plurality of base layers according to the evolution of the light transmission rate of the first candidate material under different X-ray energies along with the thickness of the first candidate.
4. The production optimization method according to claim 1, wherein the step S3 further includes: the plurality of conductive layers is determined according to a reaction potential of the electrode material, conductivity of the conductive layer material, and electrochemical stability of the conductive layer material.
5. The preparation optimization method according to claim 1, wherein the step S3 specifically comprises: determining a second candidate material and a second candidate thickness for the plurality of conductive layers based on the absorption length; and further determining the plurality of conductive layers according to the evolution of the light transmittance of the second candidate material under different X-ray energies along with the thickness of the second candidate.
6. The manufacturing optimization method of claim 1, further comprising step S7, assembling the X-ray thin film window electrode into an in-situ battery for electrochemical performance testing, and performing the testing in combination with the X-ray testing method.
7. The production optimization method of claim 6, wherein the X-ray test method includes one or more of X-ray absorption, X-ray diffraction, and X-ray scattering.
8. An X-ray thin film window electrode obtained by the preparation optimization method according to any one of claims 1 to 7, which comprises a three-layer composite structure formed by sequentially compounding a substrate layer, a conductive layer and an electrode layer.
9. The X-ray film window electrode of claim 8 wherein the substrate layer is at least one of 3, 4- (methylenedioxy) cinnamic acid, polycarbonate, polymethylmethacrylate, polyimide, polypropylene, polytetrafluoroethylene, silicon nitride, and boron nitride.
10. The X-ray thin film window electrode of claim 8, wherein the conductive layer is at least one of Au, Ag, Al, Cu and C.
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