CN102623173A - Method for preparing alumina ordered nanopore structure-based capacitor - Google Patents
Method for preparing alumina ordered nanopore structure-based capacitor Download PDFInfo
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Abstract
The invention discloses a method for preparing an alumina ordered nanopore structure-based capacitor. The method comprises the following steps of: performing surface plasma treatment on a porous alumina base material; preparing a metal nanofilm serving as an electrode of the capacitor by using an atomic layer deposition method; preparing a conductive polymer composite nanofilm serving as a transitional material between a dielectric material and another electrode by using a chemical electrostatic self-assembly method; and preparing a metal nanofilm serving as an electrode material by using the atomic layer deposition method, so that a metal-insulator-polymer semiconductor-metal capacitor structure is obtained in the porous alumina nanostructure. The capacitor prepared by the method has a nano layer structure, so that the capacitor has high energy density and is easily arrayed. Meanwhile, the capacitor preparing technology overcomes defects of the prior art; and the preparation method is reasonable, simple, and easy to implement.
Description
Technical field
The present invention relates to the Electronic Material and Element field, be specifically related to preparation method based on the capacitor of ordered porous alumina nano material.
Background technology
Capacitor is as using energy storage device the most widely, also received stern challenge with the development of energy resource system demand.Traditional electrostatic condenser, its working mechanism is based on positive and negative electrode stored charge and electric charge release fast, so capacitor has higher power density.But owing to have only surface charge to be used for whole capacitor device charge stored, therefore the energy density density of this capacitor is not high.In recent ten years, the development of ultracapacitor (also being electrochemical capacitor) is swift and violent, and electric chemical super capacitor makes to have bigger energy density on the electrode interface through electric double layer (or Faraday effect) stored charge.But, compare traditional electrostatic condenser and yet have a certain distance because the migration (or oxidation-reduction process of electrode interface) of the need of work ion of capacitor makes that the power density of electrochemical capacitor is lower.Therefore, the energy storage capacitor that exploitation has high power density and high-energy-density characteristics concurrently is the emphasis direction of energy-storage system development of future generation, also is the key technology that improves China's energy development level and energy utilization rate.
Along with social development of science and technology to demand efficient, clean energy resource, exploitation long circulation life, the energy storage device of high energy storage density are the focuses that the numerous areas researcher pays close attention to always.Energy storage device is as the parts that occupy maximum ratio weight and volume in the energy resource system, and the raising of its energy storage density is significant, and the development of novel energy-storing device is being supported energy resource system to miniaturization, lightweight development.Compare with electrochemical capacitor, the present energy density of electrostatic condenser is lower, is that working mechanism has limited its energy density and further improves on the one hand, is owing to lack the capacitor arrangement that effective assembling means are difficult to obtain height ratio capacity on the other hand.At present; High power density is the intrinsic advantage of electrostatic condenser; But the lower big limitations of energy density the development and the scope of application of conventional electrostatic capacitor; The Gonna breakthrough electrostatic condenser scope of application also obtains better development, must improve the energy density of capacitor, satisfies various energy resource systems to the requirement of high-performance energy storage device through the raising of energy density.Therefore, on the basis of intrinsic advantage, how improving the energy density of capacitor through combining with new material and device architecture technology, is conventional electrostatic capacitor development letter problem to be solved, also for its development opportunity is provided simultaneously.
Development with nanometer technology; Present energy-storage system of future generation is more and more urgent to the demand of micro-/ nano yardstick energy storage device; The development of this inevitable requirement can provide the nano cell or the capacitor of the energy for MEMS and nanoelectronic circuit, and present nanometer energy storage capacitor reaches requirement far away on size and energy storage density.Over nearly 10 years with the development of nanometer technology; Various novel nano materials as: the electronic material of novelties such as CNT, Graphene is applied in the high performance energy storage device; Because this type nano material has bigger specific area and high surface, interfacial activity; The interfacial structure through ultra-thinization and the microminiaturization of device architecture have improved the performance of energy storage capacitor (especially ultracapacitor) greatly, and the use of these nano materials simultaneously also provides the important techniques support for the energy storage capacitor of constructing nanoscale.But the research that at present relevant nano structural material is applied to capacitor concentrates on the electrochemical capacitor aspect mostly, and the report aspect traditional electrostatic condenser is less.
Because nanostructure especially nano-porous structure has huge specific area, therefore a kind of effective method is to construct large-area ultra thin device structure in open nanostructure inside.Therefore to the micro-/ nanoization of electrostatic condenser, adopting the device architecture of high-density film and interface system is main probing direction.Construct the existing report of nano electrostatic capacitor with the nanostructure of oldered arrayization in recent years.People such as Shelimov have at first constructed the capacitor of metal-insulator-metal type (MIM) structure in the AAO template, capacitor volume has reached 13 μ F/cm
2People such as Sohn also adopt porous alumina formwork to prepare a kind of MIM capacitor device array structure, and adopt the electrode material of CNT as capacitor.People such as domestic Liu Ling have obtained polypyrrole (PPy)/TiO through in the AAO template, setting up conductive polymer electrodes
2/ PPy capacitor utilizes the quick oxidation-reduction process of conductive polymer nanometer structure to obtain the good capacitor of charge-discharge performance, can in the nanometer micro-electro-mechanical systems is unified the chemical power source of nanoelectronic line system, good prospects for application be arranged.
Recently, the people ALD deposition techniques such as Banerjee of University of Maryland prepare super thin metal-insulator-metal capacitor and array structure in the porous aluminum oxide nano structure.The array structure of this high-sequential has bigger ratio capacitor, the specific capacity of the nano electrostatic capacitor of having been reported before having substantially exceeded that in foraminous die plate, prepares.The condenser capacity maximum of being reported has reached about 100 μ F/cm2; Its power density (> 1 * 106 W kg-1) reached the level of electrostatic condenser; And energy density (0.7 Wh kg-1) is near the level of electric chemical super capacitor; This array of capacitors structure has the high energy density and the advantage of power density simultaneously, can be used as the high energy storage capacitor that discharges density of having of a kind of novelty.But present this nanometer capacitor array is because size is too little can't store more energy, and also there is certain problem in a plurality of array structures interconnected simultaneously, how to guarantee exaggerated scale simultaneously all capacitor operate as normal be still waiting further research.In addition, the contact resistance between electrode and dielectric layer is bigger at present, has influenced the equivalent series resistance (ESR) of capacitor, and the ESR value that how effectively to reduce capacitor also is such capacitor urgent problem.
In sum; Through combining with nano structural material; Utilize these characteristics of bigger serface of nano material; And the superthin structure of preparation large tracts of land, array improves the energy storage density of capacitor, just can obtain the nano electrostatic capacitor of high-energy-density, makes it have the characteristics of high power density and high-energy-density concurrently.At present; Structure to capacitor and array structure thereof also is in the starting stage; What work also was directed against mostly is the nano electrochemical capacitor of high-energy-density; And less to the report of traditional nano electrostatic capacitor, be still waiting deep, systematic research at aspects such as stable assembling of nano electrostatic capacitor and energy storage mechanism.The manufacturing that how to realize each Stability Analysis of Structures assembling of capacitor, steady operation and large tracts of land array remains urgent problem.Therefore based on the research of the capacitor of nano structural material and array technique high energy storage density device and energy-storage system being had the meaning of particular importance, is basic, the key exploration work to microelectronics nanometer energy resource system.Through exploring stable little/capacitor and array assemble method and studying it and electric property, can seek a kind of method of fitting general property for stable structure, the steady operation of little/capacitor and array thereof.
Summary of the invention
Problem to be solved by this invention is: the preparation method how a kind of capacitor is provided; The prepared capacitor based on nanostructure of this method has high energy density; The preparation process has overcome existing defective in the prior art, and the preparation method is rationally simple, easy operating.
Technical problem proposed by the invention is to solve like this: a kind of preparation method of the capacitor based on aluminium oxide ordered nano pore structure may further comprise the steps:
1. Woelm Alumina matrix material being carried out surface plasma handles;
2. adopt the method for ald on the Woelm Alumina matrix material of handling through surface plasma, to prepare the electrode of metal nanometer thin film as capacitor;
3. adopt Atomic layer deposition method at the dielectric material of metal nanometer thin film surface deposition dielectric nano thin-film as capacitor;
4. adopt chemical static self-assembling method to prepare the conducting polymer composite nano film on dielectric nano thin-film surface as dielectric material and another interelectrode transition material;
5. on conducting polymer composite nano film surface, adopt Atomic layer deposition method to prepare metal nanometer thin film, thereby in aluminum oxide porous nanostructure, obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal as electrode material.
Further, the metal nanometer thin film of step described in 2. is TiN or TaN nano thin-film.
Further, the dielectric nano thin-film of step described in 3. is Al
2O
3Or HfO
2Nano thin-film.
Further, the conducting polymer composite nano film of step described in 4. is polyaniline and kayexalate composite nano film.
Further, the metal nanometer thin film of step described in 5. is the TaN nano thin-film.
Further, specifically may further comprise the steps:
1. the Woelm Alumina material is put into the vacuum equipment cavity, carry out surface plasma and handle, the thickness of Woelm Alumina material is 30～50 μ m, the material intermediate pore size: length 20～30 μ m, diameter 60～80nm;
2. the Woelm Alumina material of surface plasma being handled is put into the atomic layer deposition apparatus cavity, adopts the method for ald to prepare the TiN metal nanometer thin film as electrode of capacitor;
The Woelm Alumina material that 3. will prepare metal electrode is put into the atomic layer deposition apparatus cavity, adopts the method deposition HfO of ald
2The dielectric nano thin-film is as capacitor dielectric material;
The Woelm Alumina material that 4. will prepare dielectric film is inserted polyaniline/N, in the dinethylformamide solution (mass ratio is 1:6) 15～20 minutes, takes out the back drying at room temperature 15～20 minutes, obtains the polyaniline nano film on the dielectric thin-film material surface;
The Woelm Alumina material that 5. will 4. obtain was inserted in the kayexalate aqueous solution (mass ratio is 1:3) 10～15 minutes, took out 80～100 ℃ of backs dry 15～20 minutes down, obtained the kayexalate nano thin-film on the polyaniline film surface;
6. repeating step is 4.～5. 8～10 times, thereby obtains polyaniline/polystyrene sodium sulfonate composite nano film as transition material on the dielectric material surface;
7. adopt Atomic layer deposition method to prepare the TiN nano thin-film on polyaniline/polystyrene sodium sulfonate composite nano film surface as another electrode of capacitor;
Thereby obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal.
The preparation method of capacitor provided by the present invention compared with prior art has following advantage:
The capacitor matrix material that adopts is Woelm Alumina (AAO); The nano-pore structure that wherein contains the length/diameter ratio of orderly arrangement; Guarantee that electrode has big surface, each capacitor film part is the nano thin-film structure simultaneously, has guaranteed the nanostructure of capacitor.This capacitor based on porous nanometer structure and nano thin-film structure can effectively improve the energy density of electrostatic condenser, and has the characteristics of rapid release, can satisfy the many-sided different needs of high energy storage density energy-storage system.In addition, introduce polymer semiconductor's nano thin-film structure between medium layer of the present invention and electrode film, can effectively reduce the contact resistance of electrode and dielectric material, reduced equivalent series resistance (ESR) value of capacitor.The preparation method is also rationally simple, easy operating.
Description of drawings
Fig. 1 is single capacitor arrangement schematic diagram.
Wherein Reference numeral is respectively: 1, Woelm Alumina matrix material; 2, orderly length/diameter ratio nano hole; 3, the metal electrode film of atomic deposition method preparation; 4, the dielectric nano thin-film of atomic deposition method preparation, 5, the composite nano-polymers film of chemical static self-assembling method preparation, 6, the metal electrode film of atomic deposition method preparation.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described:
The invention provides a kind of preparation method of the capacitor based on aluminium oxide ordered nano pore structure; At first the method through ald prepares metal nanometer thin film as electrode in nano-pore inside; Adopt Atomic layer deposition method on the metal electrode film, to prepare Nano dielectric film then as capacitor dielectric layer; Then Tonghua static self-assembling method prepares the conducting polymer composite nano film on dielectric film; Adopt Atomic layer deposition method to prepare metal nanometer thin film as another electrode at last, thereby obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal at the polymer nanocomposite film surface.Capacitor volume can be regulated and control through the orderly number of perforations of difference, hole depth and hole dimension.Key in this invention is a basis material for adopting the ordered nano porous structure of aluminium oxide, contains the nano-pore structure of length/diameter ratio in the material, and the cavernous structure of this length/diameter ratio has guaranteed the specific area that capacitor is bigger.Simultaneously, the electrode of capacitor and dielectric film adopt vacuum moulding machine and atomic deposition method, have guaranteed the nanostructure of film and device.In addition, this invention is introduced semiconducting polymer film as transition zone between Nano dielectric film and electrode film, effectively reduce the contact berrier of dielectric material and electrode, and then can reduce the capacitor equivalent series resistance.Therefore, the nano-pore through novelty combines with the device superthin structure, has guaranteed that the capacitor that obtains has high-energy-density, little equivalent series resistance.Two electrodes of capacitor are TiN, and metal nanometer thin films such as TaN, dielectric layer are Al
2O
3, HfO
2Deng the dielectric nano thin-film that adopts the atomic deposition method to obtain.In addition, through obtaining jumbo high energy density capacitor array structure with a plurality of Woelm Alumina capacitor substrates are interconnected, be easy to realize array.
The invention provides a kind of preparation method of the capacitor based on aluminium oxide ordered nano pore structure; At first the method through ald prepares metal nanometer thin film as electrode in nano-pore inside; Adopt Atomic layer deposition method on the metal electrode film, to prepare Nano dielectric film then as capacitor dielectric layer; Then Tonghua static self-assembling method prepares the conducting polymer composite nano film on dielectric film; Adopt Atomic layer deposition method to prepare metal nanometer thin film as another electrode at last, thereby obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal at the polymer nanocomposite film surface.Capacitor volume can be regulated and control through the orderly number of perforations of difference, hole depth and hole dimension.
Rely on good oxidation aluminium ordered nano hole structural material and ripe atomic layer level thin film deposition process and chemical static self-assembling method, the present invention can prepare the high energy density capacitor structure, and is easy to realize the large tracts of land array of structures.
Adopt some capacitor arrangements of the present invention's preparation to be exemplified below:
1. based on Al
2O
3The poroid capacitor arrangement of Nano dielectric film;
2. based on HfO
2The poroid capacitor arrangement of Nano dielectric film;
Below be specific embodiment of the present invention:
Embodiment 1
In Fig. 1; The Woelm Alumina material is carried out surface plasma to be handled; The Woelm Alumina material matrix material that surface plasma is handled is inserted in the atomic layer deposition apparatus cavity, and the method that adopts ald is at the electrode of metal nanometer thin films such as alumina nanohole (among Fig. 1 2) preparation TiN (among Fig. 1 3) as capacitor.
The Woelm Alumina material that has deposited the TiN electrode film is inserted in the atomic layer level thin film depositing device cavity, adopt the atomic deposition method in TiN film surface depositing Al
2O
3Etc. dielectric nano thin-film (among Fig. 1 4).
Adopt chemical static self-assembling method to continue at dielectric nano thin-film surface deposition polyaniline (PAn)/kayexalate (PSS) composite nano-polymers film (among Fig. 1 5).
Adopt the atomic deposition method at metal nanometer thin films such as composite nano-polymers film surface depositing TiNs as capacitor another one electrode, thereby in porous nanometer structure, obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal.
The preparation method is following:
1. the Woelm Alumina material is put into vacuum cavity, carry out surface plasma and handle, the thickness of Woelm Alumina material is 50 μ m, the material intermediate pore size: length 30 μ m, diameter 60nm;
2. the Woelm Alumina material of surface plasma being handled is put into the atomic layer deposition apparatus cavity, adopts the method for atomic deposition to prepare the TiN metal nanometer thin film as electrode of capacitor;
The Woelm Alumina material that 3. will prepare metal electrode is put into the atomic layer deposition apparatus cavity, adopts the method deposition HfO of ald
2The dielectric nano thin-film is as capacitor dielectric material;
The Woelm Alumina material that 4. will prepare dielectric film is inserted polyaniline/N, in the dinethylformamide solution (mass ratio is 1:6) 15 minutes, takes out the back drying at room temperature 15 minutes, obtains the polyaniline nano film on the dielectric thin-film material surface;
The Woelm Alumina material that 5. will 4. obtain was inserted in the kayexalate aqueous solution (mass ratio is 1:3) 15 minutes, take out back 100 ℃ dry 20 minutes down, obtain the kayexalate nano thin-film on the polyaniline film surface;
6. repeating step is 4.-5. 8 times, thereby obtains polyaniline/polystyrene sodium sulfonate composite nano film as transition material on the dielectric material surface;
7. adopt Atomic layer deposition method to prepare the TiN nano thin-film on polyaniline/polystyrene sodium sulfonate composite nano film surface as another electrode of capacitor;
Thereby obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal.
Thereby by 1.-7. obtaining a kind of TiN-HfO based on porous nanometer structure
2-PAn/PSS-TiN capacitor arrangement.
Embodiment 2
Like Fig. 1, capacitor dielectric nano thin-film is Al
2O
3
The preparation flow of capacitor is similar with execution mode one.Thereby obtained a kind of TiN-Al based on porous nanometer structure
2O
3The high energy density capacitor structure of-PAn/PSS-TiN.
Embodiment 3
Like Fig. 1, capacitor dielectric nano thin-film is HfO
2
Two electrode materials of capacitor are respectively the TaN metal nanometer thin film, and preparation flow is similar with execution mode one.Thereby obtained a kind of TaN-Al based on porous nanometer structure
2O
3The high energy density capacitor structure of-PAn/PSS-TaN.
Embodiment 4
Like Fig. 1, capacitor dielectric nano thin-film is Al
2O
3
Two electrode materials of capacitor are respectively TiN and TaN, and preparation flow is similar with execution mode one.Thereby obtained a kind of TiN-Al based on porous nanometer structure
2O
3The high energy density capacitor structure of-PAn/PSS-TaN.
Embodiment 5
Like Fig. 1, capacitor dielectric nano thin-film is HfO
2
Two electrode materials of capacitor are respectively TiN and TaN, and preparation flow is similar with execution mode one.Thereby obtained a kind of TiN-HfO based on porous nanometer structure
2The high energy density capacitor structure of-PAn/PSS-TaN.
Embodiment 6
Like Fig. 1, capacitor dielectric nano thin-film is HfO
2
Two electrode materials of capacitor are TaN, and preparation flow is similar with execution mode one.Thereby obtained a kind of TaN-HfO based on porous nanometer structure
2The high energy density capacitor structure of-PAn/PSS-TaN.
Claims (6)
1. the preparation method based on the capacitor of aluminium oxide ordered nano pore structure is characterized in that, may further comprise the steps:
1. Woelm Alumina matrix material being carried out surface plasma handles;
2. adopt the method for ald on the Woelm Alumina matrix material of handling through surface plasma, to prepare the electrode of metal nanometer thin film as capacitor;
3. adopt Atomic layer deposition method at the dielectric material of metal nanometer thin film surface deposition dielectric nano thin-film as capacitor;
4. adopt chemical static self-assembling method to prepare the conducting polymer composite nano film on dielectric nano thin-film surface as dielectric material and another interelectrode transition material;
5. on conducting polymer composite nano film surface, adopt Atomic layer deposition method to prepare metal nanometer thin film, thereby in aluminum oxide porous nanostructure, obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal as electrode material.
2. the preparation method of a kind of capacitor based on aluminium oxide ordered nano pore structure according to claim 1 is characterized in that, the metal nanometer thin film of step described in 2. is TiN or TaN nano thin-film.
3. the preparation method of a kind of capacitor based on aluminium oxide ordered nano pore structure according to claim 1 is characterized in that, the dielectric nano thin-film of step described in 3. is Al
2O
3Or HfO
2Nano thin-film.
4. the preparation method of a kind of capacitor based on aluminium oxide ordered nano pore structure according to claim 1 is characterized in that, the conducting polymer composite nano film of step described in 4. is polyaniline and kayexalate composite nano film.
5. the preparation method of a kind of capacitor based on aluminium oxide ordered nano pore structure according to claim 1 is characterized in that, the metal nanometer thin film of step described in 5. is the TaN nano thin-film.
6. according to the preparation method of each described a kind of capacitor based on aluminium oxide ordered nano pore structure of claim 1～5, it is characterized in that, specifically may further comprise the steps:
1. the Woelm Alumina material is put into the vacuum equipment cavity, carry out surface plasma and handle, the thickness of Woelm Alumina material is 30～50 μ m, the material intermediate pore size: length 20～30 μ m, diameter 60～80nm;
2. the Woelm Alumina material of surface plasma being handled is put into the atomic layer deposition apparatus cavity, adopts the method for ald to prepare the TiN metal nanometer thin film as electrode of capacitor;
The Woelm Alumina material that 3. will prepare metal electrode is put into the atomic layer deposition apparatus cavity, adopts the method deposition HfO of ald
2The dielectric nano thin-film is as capacitor dielectric material;
The Woelm Alumina material that 4. will prepare dielectric film is inserted the N of polyaniline; In the dinethylformamide solution 15～20 minutes, polyaniline and N, dinethylformamide mass ratio were 1:6; Took out the back drying at room temperature 15～20 minutes, and obtained the polyaniline nano film on the dielectric thin-film material surface;
The Woelm Alumina material that 5. will 4. obtain was inserted in the aqueous solution of kayexalate 10～15 minutes; The mass ratio of the kayexalate and the aqueous solution is 1:3; Took out 80～100 ℃ of backs dry 15～20 minutes down, and obtained the kayexalate nano thin-film on the polyaniline film surface;
6. repeating step is 4.～5. 8～10 times, thereby obtains polyaniline and kayexalate composite nano film as transition material on the dielectric material surface;
7. adopt Atomic layer deposition method to prepare the TiN nano thin-film at polyaniline and kayexalate composite nano film surface as another electrode of capacitor;
Thereby obtain the capacitor arrangement of a kind of metal-insulator-polymer semiconductor-metal.
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Granted publication date: 20140528 |