CN101771168A - Method for preparing miniature lithium battery - Google Patents
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- CN101771168A CN101771168A CN201010111609A CN201010111609A CN101771168A CN 101771168 A CN101771168 A CN 101771168A CN 201010111609 A CN201010111609 A CN 201010111609A CN 201010111609 A CN201010111609 A CN 201010111609A CN 101771168 A CN101771168 A CN 101771168A
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- 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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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for preparing a miniature lithium battery, relates to a lithium battery, and provides the method for preparing the miniature lithium battery, which is easy to implement and compatible with micro-processing technology. The miniature lithium battery consists of a substrate, a cathode current collector, a cathode film, a solid electrolyte film, an anode film, a lower-layer anode current collector and an upper-layer anode current collector. The method comprises the following steps of: depositing a layer of metal film on the substrate with a chemical deposition method or a physical deposition method serving as the cathode current collector and the lower-layer anode current collector; limiting a cathode graph on the cathode current collector with a photoresist, depositing a cathode thin film with the physical deposition method, removing the residual photoresist with an inert solvent stripping method to obtain the cathode thin film of the limited graph, and performing annealing treatment; limiting structures of the required solid electrolyte film and the anode film with the photoresist; limiting the structures of the solid electrolyte film and the anode film by using the photoresist as a sacrificial layer 4; preparing the solid electrolyte film, the anode film and the upper-layer anode current collector; and stripping the sacrificial layer to obtain the miniature lithium battery.
Description
Technical field
The present invention relates to a kind of lithium battery, especially relate to a kind of preparation method who adopts the full-solid-state minisize lithium cell of micro-processing technology preparation.
Background technology
In recent years, along with microelectromechanical systems (MEMS) technology rapid development, as: the fast development of microsensor, little gyro and Space Facilities microminiaturization, associated miniature energy technology also obtains people's attention more and more.Usually adopting external power supply is microelectromechanical systems (MEMS) power supply, can produce some defectives: as, reduced the design efficiency of MEMS; The noise that wiring point electric capacity produces; ([1] Koeneman P B, Busch-Vishniac I J, Wood K L.Journal of.Microelectromechanacal System.1997,6 (4): 355-362) such as interactive interference of supply lines and holding wire.Therefore, realize the microminiaturization of the energy, the integrated major issue that has become the solution of being badly in need of among the development MEMS with the defective that overcomes external power supply.In addition, very lagre scale integrated circuit (VLSIC) (VLSI) has also proposed similar requirement ([2] Minko B..SolarEnergy Materials﹠amp to power supply; Solar Cells, 2000,62:21-35).
In order to reduce the noise of power supply, reduce the consumption ease of electric energy in the dynamic random container (DRAMS) that high density is arranged, require in the actual production power supply and electronic equipment are connected as a single entity, realize the miniature localization of the energy, i.e. the minicell that quality of match is light, energy is high, the life-span is long on metal-oxide semiconductor (CMOS) storage piece.In the world the research of little energy is mainly contained several classes such as micro zinc-nickel battery, miniature lithium battery, miniature solar battery, miniature thermoelectric cell and micro fuel cell in recent years.
Full-solid-state minisize lithium cell occupies critical role because of its integrated preferably compatibility in all kinds of minicells, also be to realize MEMS, the microminiaturization of the VLSI energy, integrated better selection.
It mainly is cathodic coating, solid electrolyte film and anode film that the structure of full-solid-state minisize lithium cell is formed.Relating to configuration aspects has a variety of reports, and common structure can be described referring to U.S. Pat 5338625.Can be by deposition cathode current collector, cathodic coating, solid electrolyte film, anode film, anode current collector constitute successively on certain substrate (as monocrystalline silicon piece).The structure of battery has a variety of reports, and common structure such as U.S. Pat 5338625 are described.
The thin-film material that preparation constitutes micro cell mainly adopts micro-processing technology, as: methods such as magnetron sputtering, pulsed laser deposition, vacuum thermal evaporation deposition.
Because the reduction of thickness, electrolyte just can be with the poor lithium ion conductor-inorganic solid electrolytes of some ionic conductivities, employing rf magnetron sputtering Li under nitrogen atmosphere such as the Bates of U.S. Oak Ridge National Laboratory for example
3PO
4The method of target has prepared Li
3.3PO
3.9N
0.17(LiPON) film, conductivity at room temperature reach 2.3 (± 0.7) * 10
-6S/cm, electrochemical stability window is 5.5V, and it has been prepared Li/LiPON/LiCoO as solid electrolyte
2And Li/LiPON/V
2O
5Deng all solid-state thin-film lithium battery ([3] Wang B, Bates J B, Hart F X et al.J.Electrochem.Soc.1996,143:3203-3213).
The use of the solid-state inorganic electrolyte of electrochemical stability has improved the oxidation-reduction stability of battery greatly, just can consider with the high cathode material of some oxidation activities.Because the Li of solid-state inorganic electrolyte
+Ionic conductivity is low relatively, and the ratedeterming step of cell reaction may be that lithium ion is in electrolytical transmission course.So just do not have the very necessary electrode material that uses, increased the selection of electrode materials degree, make those amorphous state molybdenum of low lithium ion diffusion coefficient and sulfide and the oxide and the V of titanium be arranged especially with respect to its crystal structure form with high-lithium ion diffusion
2O
5Film becomes possibility.Reported the solid-state thin-film battery of multiple system in the document, for example Li/LiPON/LiCoO
2, SiTON/LiPON/LiCoO
2, SnN
x/ LiPON/LiCoO
2, Cu/LiPON/LiCoO
2And Li/LiPON/Li
xMn
2-yO
4Etc. system ([4] Bates J B, Dudney N J, Neudecher B et al.Solid State Ionics, 2000,135:33-45; [5] Neudecher B J, Dudney N J, Bates J B.J.Electrochem.Soc., 2000,147:517-523; [6] Neudecher B J, Zuhr R A, Bates J B.J.Power Sources, 1999,81:27-32; [7] Dudney N J, Bates J B, Zuhr R A et al.J.Electrochem.Soc., 1999,146:2455-2464; [8] Hart F X, Bates J B.J.App.Phys., 1998,83:7560-7566).
Lithium anode film commonly used mainly is to be deposited on the solid electrolyte with hot evaporation coating method under the environment of high vacuum.But in some integrated circuits (IC) manufacture craft, adopt reflow solder technique, in manufacturing process, IC is heated to 250～260 ℃ rapidly, because lithium has lower fusing point (180 ℃), therefore when temperature surpasses 250 ℃, can lithium battery be destroyed because of the anode fusing.In addition,, react with airborne oxygen and water vapour etc. easily, therefore need a kind of anode material of miniature lithium ion battery of alternative metals lithium because lithium metal is very active.Studies show that, various metal oxides (for example tin-oxide and based on the composite oxides of tin) are anode material ([9] Neudecker of a kind of miniature lithium ion battery of fine alternative metals lithium, B.J., R.A.Zuhr, et al. (1999) .Journal of Power Sources 82:27-32), its Heat stability is good, chemical property is more stable in air.The preparation method of metal-oxide film is easier, can be by a lot of methods magnetron sputtering for example, and thermal evaporation corresponding metal in oxygen atmosphere, the preparation of methods such as chemical vapour deposition (CVD).
In the technology of preparation battery, can use masks such as aluminium with special pattern, stainless steel to limit the shape of each component film of deposition micro cell, this mask technique is highly suitable for Centimeter Level or the more preparation of large scale battery, but rim effect can take place and can't obtain accurate figure in this mask method when preparation smaller szie micro cell, and there is pollution in mask in the deposit film process, also may scratch the film that has deposited and damages battery.Therefore, if micro cell will be applied on the various microdevices, its preparation technology must with microelectronics preparation technology compatibility.
Summary of the invention
The purpose of this invention is to provide a kind of easy realization, and with miniature lithium battery of micro-processing technology compatibility and preparation method thereof.
Miniature lithium battery of the present invention is made of substrate, cathode current collector, cathodic coating, solid electrolyte film, anode film, lower floor's anode collector and upper strata anode collector, substrate is monocrystalline silicon, quartz, pottery or polymer flexibility substrate, cathode current collector and lower floor's anode collector preparation are on substrate, cathodic coating is deposited on the cathode current collector, solid electrolyte film covers on the cathodic coating, separate by solid electrolyte film between cathodic coating and the anode film, and can the conductive lithium ion, described solid attitude electrolyte adopts LiPON or LiBO
2, anode film and upper strata anode collector are positioned on the solid electrolyte film.
Described cathodic coating can adopt the transition metal oxide cathodic coating.Described anode film can adopt the tin-oxide anode film.
The preparation method of miniature lithium battery of the present invention may further comprise the steps:
1) on substrate, deposits layer of metal film as cathode current collector and lower floor's anode collector by chemical deposition or physical deposition method;
2) limit cathode pattern with photoresist on cathode current collector, adopt physical deposition method deposition cathode film then, the method for peeling off with atent solvent is removed remaining photoresist again, obtains limiting the cathode thin film of figure, again annealing in process;
3) limit the structure of required solid electrolyte film and anode film with photoresist; Make the structure that limits solid electrolyte film and anode film with photoresist as sacrifice layer 4;
4) preparation solid electrolyte film, anode film and upper strata anode collector;
5) adopt wet method or dry method to peel off sacrifice layer (photoresist) at last, obtain the miniature lithium ion battery of complete structure.
In step 1), the material of described metal film can be Pt, Au, Ni or Al etc., and described substrate can be monocrystalline silicon, quartz, pottery or polymer flexibility substrate etc.
In step 2) in, the area of described cathode pattern can be 0.1～1mm
2, the thickness of described cathode thin film can be 0.1～1 μ m, and described cathode thin film can adopt LiCoO
2Film, LiMn
2O
4Film or V
2O
5Films etc., the area of described cathode thin film can be 0.1～1mm
2, described annealing in process preferably with cathode thin film in oxygen or air through 300～700 ℃ of annealing in process; Described physical deposition method can adopt methods such as magnetron sputtering or pulsed laser deposition; It is the photoresist of 5124E or AZ4620 that described photoresist can adopt existing product type.
In step 3), it is the photoresist of 5124E or AZ4620 that described photoresist can adopt existing product type.
In step 4), described solid electrolyte film can be selected LiPON film or LiBO for use
2Film, performance is a greater impact easily in the air because the LiPON film is exposed to, subsequent technique can avoid electrolytic thin-membrane to be exposed in the air, so described preparation solid electrolyte film, anode film and upper strata anode collector can adopt following method: according to the preparation method of cathode thin film, etch earlier the electrolyte thin film pattern with photoresist, then under the condition of not opening vacuum chamber, method successive sedimentation LiPON film and anode film with magnetron sputtering, deposit layer of metal again as the upper strata anode collector, described metal can adopt Pt, Au, Ni, Al or Cu etc.
Compared with the prior art, the present invention has outstanding advantage and effect:
1) preparation method and microelectronics preparation technology compatibility, product can be realized with microdevice integrated.
2) adopt the method for successive sedimentation to avoid solid electrolyte LiPON film to be exposed in the air.
3) in case miniature lithium battery form, can be by anode film, anode collector forms sealing to electrolyte and negative electrode, moves before miniature lithium battery uses like this to reach storage and can be effectively protected in air.
4) adopt metal oxide as anode material, perhaps in the initial charge process, on anode collector, generate lithium metal as anode, then can reduce the difficulty of technology, the inert environments that needs usually when avoiding using lithium metal and the requirement of high leakproofness as anode.
Description of drawings
Fig. 1 is the structural representation of embodiment of the invention substrate.
Fig. 2 has deposited the structural representation of cathodic metal collector and lower floor's anode collector for the embodiment of the invention.
Fig. 3 is deposited on the structural representation of the cathodic coating on the cathode current collector for the embodiment of the invention.
Fig. 4 is a structural representation of having photoresist before continuous sputter solid electrolyte of the embodiment of the invention and the anode film.
Fig. 5 is good solid electrolyte of the continuous sputter of the embodiment of the invention and anode film, the structural representation of anode collector layer.
Fig. 6 is the structural representation of the miniature lithium battery that discharges behind the embodiment of the invention stripping photoresist.
Electronic Speculum (SEM) photo of the miniature lithium battery product that Fig. 7 makes for the embodiment of the invention.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Shown in Fig. 1～7, miniature lithium battery of the present invention is by substrate 1, cathode current collector 2a, cathodic coating 3, solid electrolyte film 5, anode film 6, anode collector 2b of lower floor and upper strata anode collector 7 constitute, substrate 1 is a monocrystalline silicon, quartzy, pottery or polymer flexibility substrate, cathode current collector 2a and the anode collector 2b of lower floor preparation are on substrate 1, cathodic coating 3 is deposited on the cathode current collector 2a, solid electrolyte film 5 covers on the cathodic coating 3, separate by solid electrolyte film between cathodic coating 3 and the anode film 6, and can the conductive lithium ion, described solid attitude electrolyte adopts LiPON or LiBO
2, anode film 6 and upper strata anode collector 7 are positioned on the solid electrolyte film 5.
Described cathodic coating 3 can adopt the transition metal oxide cathodic coating.Described anode film 6 can adopt the tin-oxide anode film.
In Figure 4 and 5, mark 4 is sacrifice layer (adopting photoresist as sacrifice layer).
Below provide the concrete preparation method of described miniature lithium battery.
1) select substrate (structure is referring to Fig. 1) preparation cathode current collector and anode collector substrate 1 to adopt monocrystalline silicon substrate, adopt the dried wet oxygen method oxide layer of growing on substrate 1, oxide layer is as insulating barrier, and thickness is about 500nm.The cathode current collector that photoetching is good required and the structure graph of anode collector, the method of using direct current sputtering then splash-proofing sputtering metal Ti layer (thickness 20nm) successively on the substrate 1 of the good required collector figure of photoetching, metal Pt layer (thickness is 300nm), the metal Ti layer is as tack coat, and the metal Pt layer of deposition is as cathode current collector 2a and the anode collector 2b of lower floor (referring to Fig. 2).
2) LiCoO
2The preparation of cathodic coating
After the step 1), 5124E limits the cathode zone figure that needs the covered cathode film with photoresist on cathode current collector 2a, adopts the method deposition cathode film of rf magnetron sputtering then.Use diameter 100mmLiCoO
2Cavity air pressure is evacuated to 10～4Pa before the ceramic sputter targets, sputter, and sputtering atmosphere is the argon oxygen gas mixture, and volume ratio is Ar: O
2=3: 1, gas pressure is 1.3～3.0Pa, and sputtering power is 100W, and the temperature of substrate is a room temperature during deposition, and sedimentation time 1～2h can obtain LiCoO
2, cathodic coating 3 (referring to Fig. 3).Again with LiCoO
2 Cathodic coating 3 is heat-treated, at O
2In the atmosphere, rise to 600～700 ℃ with 5 ℃/min heating rate from room temperature, annealing in process 0.5～2h naturally cools to room temperature and takes out.Gained LiCoO
2The thickness of cathodic coating 3 is 200～400nm, and the area of cathode zone is 0.5 * 0.5mm
2
3) enclose photoresist before preparation solid electrolyte and the anode film
Step 2) after, limits the structure of required solid electrolyte film and anode film as sacrifice layer 4 (referring to Fig. 4) with the photoresist of model 5124E;
4) LiPON solid electrolyte film, SnO
xThe preparation of anode film and anode collector
After the step 3, use the Li of diameter 100mm
3PO
4Ceramic sputter targets, it is high-purity N that the preceding cavity air pressure of sputter is evacuated to 10～4Pa sputtering atmosphere
2, air pressure 1.3Pa, sputtering power 100～200W, sputtering time 2h can obtain the LiPON dielectric film 5 (referring to Fig. 5) of deposit thickness 400nm.Under the situation of not opening vacuum chamber, adopt the method for direct current sputtering to carry out continuous sputter, can deposit and obtain SnO
xAnode film 6 (referring to Fig. 5).Use the metal Sn sputtering target of diameter 100nm during preparation, sputtering atmosphere is Ar and O
2Gaseous mixture, volume ratio are Ar: O
2=2: 1, air pressure is 1.3Pa, sputtering power 50～200W, and sedimentation time is 10～60min, considers SnO
xThe irreversible capacity loss of first charge-discharge, its deposit thickness should with cathodic coating LiCoO
2Film is complementary, and LiCoO2 is 10: 1～20: 1 with the thickness ratio of SnOx, and the method plated metal Ni layer that continues then to adopt direct current sputtering is as upper strata anode collector 7 (referring to Fig. 5), and thickness is 200nm.
5) preparing product
Peel off sacrifice layer 4 with acetone as solvent at last, discharge final miniature lithium battery structure (referring to Fig. 6).The product of preparation as shown in Figure 7.
Embodiment 2
Similar to Example 1, its difference is:
In the step 1), substrate 1 is selected quartz substrate for use.Direct current sputtering plated metal Au layer (thickness is 300nm) is as cathode current collector 2a and the anode collector 2b of lower floor (referring to Fig. 2).
Step 2) in, sputtering power is 120W, and the temperature of substrate is 100 ℃ during deposition, and heating rate rises to 400 ℃ from room temperature, and the annealing in process time is 0.5～2h.
The anode of miniature lithium battery of the present invention is original position generation on anode collector Ni layer in the initial charge process.
Claims (10)
1. miniature lithium battery, it is characterized in that constituting by substrate, cathode current collector, cathodic coating, solid electrolyte film, anode film, lower floor's anode collector and upper strata anode collector, substrate is monocrystalline silicon, quartz, pottery or polymer flexibility substrate, cathode current collector and lower floor's anode collector preparation are on substrate, cathodic coating is deposited on the cathode current collector, solid electrolyte film covers on the cathodic coating, separated by solid electrolyte film between cathodic coating and the anode film, described solid attitude electrolyte adopts LiPON or LiBO
2, anode film and upper strata anode collector are positioned on the solid electrolyte film.
2. miniature lithium battery as claimed in claim 1 is characterized in that described cathodic coating is the transition metal oxide cathodic coating; Described anode film is the tin-oxide anode film.
3. the preparation method of miniature lithium battery as claimed in claim 1 is characterized in that may further comprise the steps:
1) on substrate, deposits layer of metal film as cathode current collector and lower floor's anode collector by chemical deposition or physical deposition method;
2) limit cathode pattern with photoresist on cathode current collector, adopt physical deposition method deposition cathode film then, the method for peeling off with atent solvent is removed remaining photoresist again, obtains limiting the cathode thin film of figure, again annealing in process;
3) limit the structure of required solid electrolyte film and anode film with photoresist; Make the structure that limits solid electrolyte film and anode film with photoresist as sacrifice layer 4;
4) preparation solid electrolyte film, anode film and upper strata anode collector;
5) adopt wet method or dry method to peel off sacrifice layer at last, obtain the miniature lithium ion battery of complete structure.
4. the preparation method of miniature lithium battery as claimed in claim 3 is characterized in that in step 1), and the material of described metal film is Pt, Au, Ni or Al, and described substrate is monocrystalline silicon, quartz, pottery or polymer flexibility substrate.
5. the preparation method of miniature lithium battery as claimed in claim 3 is characterized in that in step 2) in, the area of described cathode pattern is 0.1～1mm
2, the thickness of described cathode thin film is 0.1～1 μ m.
6. the preparation method of miniature lithium battery as claimed in claim 3 is characterized in that in step 2) in, described cathode thin film is LiCoO
2Film, LiMn
2O
4Film or V
2O
5Film, the area of described cathode thin film are 0.1～1mm
2
7. the preparation method of miniature lithium battery as claimed in claim 3 is characterized in that in step 2) in, described annealing in process be with cathode thin film in oxygen or air through 300～700 ℃ of annealing in process; Described physical deposition method adopts magnetron sputtering or pulsed laser deposition.
8. the preparation method of miniature lithium battery as claimed in claim 3 is characterized in that in step 2) and 3) in, described photoresist is that product type is the photoresist of 5124E or AZ4620.
9. the preparation method of miniature lithium battery as claimed in claim 3 is characterized in that in step 4), and described solid electrolyte film is LiPON film or LiBO
2Film.
10. the preparation method of miniature lithium battery as claimed in claim 3, it is characterized in that in step 4), described preparation solid electrolyte film, anode film and upper strata anode collector adopt following method: according to the preparation method of cathode thin film, etch earlier the electrolyte thin film pattern with photoresist, then under the condition of not opening vacuum chamber, method successive sedimentation LiPON film and anode film with magnetron sputtering, deposit layer of metal again as the upper strata anode collector, described metal is Pt, Au, Ni, Al or Cu.
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| CN102916200A (en) * | 2012-10-31 | 2013-02-06 | 武汉工程大学 | Method for preparing electrode of miniature film-free fuel cell |
| CN103636025A (en) * | 2011-06-17 | 2014-03-12 | 应用材料公司 | Mask-less fabrication of thin film batteries |
| CN104134816A (en) * | 2014-08-05 | 2014-11-05 | 厦门大学 | Three-dimensional all-solid-state mini thin-film lithium battery with inverted pyramid array structure |
| CN104302586A (en) * | 2012-03-09 | 2015-01-21 | 贝伦诺斯清洁电力控股有限公司 | V2O5-LiBO2, V2O5-NiO-LiBO2 glasses and their composites obtained by nitrogen doping and reduced graphite oxide blending as cathode active materials |
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