CN100457958C - Preparation method of metal oxide nano array-inverse thin film - Google Patents
Preparation method of metal oxide nano array-inverse thin film Download PDFInfo
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- CN100457958C CN100457958C CNB2006100218473A CN200610021847A CN100457958C CN 100457958 C CN100457958 C CN 100457958C CN B2006100218473 A CNB2006100218473 A CN B2006100218473A CN 200610021847 A CN200610021847 A CN 200610021847A CN 100457958 C CN100457958 C CN 100457958C
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Abstract
The invention relates the method for producing nanometer negative array film. The method comprises the following steps: dispersing the nanometer macromolecule colloid ball on the base-plate to form nanometer ball die plate, depositing metal-oxide film on the nanometer ball die plate with magnetron sputtering technology under oxygen environment, at the same time, etching macromolecule nanometer ball, and getting the product. The method uses different size macromolecule nanometer ball and control sputtering power and operating pressure, and the method can make different size products. The invention has the advantages of reducing devices, shortening making time and reducing cost. The metal-oxide nanometer negative array film can be used to make high density magnetic storage and sensing device.
Description
Technical field
The invention belongs to the material technology field, relate to a kind of method of utilizing nanometer colloid ball lithographic technique to prepare the nano-metal-oxide thin-film material.
Background technology
What nano science and technology were related is to have preparation and the sign of size in the structure of 1-100 nanometer range.The resolution limit of ordinary optical photoetching is 200nm, can not adapt to the preparation of nano material.The normal photoetching technique that adopts of structure of making nano-scale at present is beamwriter lithography (Electron-beam Lithography, EBL) and X-X-ray lithography X (X-ray Lithography, XRL) technology, wherein EBL is the serial processing pattern, ultimate precision is 1-2nm, because etching speed has only 1cm
-2/ s and be unfavorable for commercial utilization; The XRL precision is owing to be subjected to the influence of photoelectron distribution range and scattering effect, and precision is low slightly, is 20-50nm, but it has the ability of parallel processing; The precision of EBL and the parallel processing capability of XRL are combined, and people have developed the nanoimprinting technology based on scanning tunnel microscope (STM), but it is subjected to the restriction of serial processing equally.So exploitation is inexpensive and nanometer etching technology that have a parallel processing capability is one of research emphasis of nano science.
Scientist develops a kind of nanometer colloid ball lithographic technique (Nanosphere Lithography that is called recently, NSL) method is used to prepare nano-scale structure, this method is to use the nanometer colloid ball of narrow size distribution, as the polystyrene molecule, utilize " the self-assembly effect " of its height marshalling to make film, form with six side's closest packings on substrate is arranged in periodic structure, and can pass through the adjusting process parameter, as concentration ratio or rotating speed etc., can change the film number of plies and thickness.The characteristic of this method maximum just is that required plant and instrument is quite cheap, and technology is operated easily; Only need to change the particle diameter of different nano particle balls, just can on various substrates, obtain the large area periodic array structure of different nano-scales.
Utilize nanometer colloid ball lithographic technique,, can prepare positive array thin-film material of two dimension and array-inverse thin film material again in conjunction with other Micrometer-Nanometer Processing Technology.At present, the method key step of utilizing this technology to prepare two-dimentional anti-array is, as shown in Figure 5: (1). the high molecular nanometer colloidal spheres is dispersed in forms the nanometer ball template on the substrate, as shown in Figure 1; (2). under certain argon oxygen atmosphere, utilize reaction particle etching (reactive ion etching) equipment to reduce the diameter of macromolecule nanometer ball, and change sphere gap from, as shown in Figure 2; (3). deposit required film by evaporation or electro-plating method, as shown in Figure 3; (4). the stripping nano ball forms the anti-array of netted two-dimensional nano, as shown in Figure 4.
In the process of the anti-array of above-mentioned conventional preparation two-dimensional nano, need special reaction particle etching apparatus, strengthened the equipment input and prolonged the process time.
Summary of the invention
The present invention is intended to the weak point of utilizing nanometer colloid ball lithographic technique to prepare metal oxide nano array-inverse thin film at existing, and a kind of preparation method of metal oxide nano array-inverse thin film is provided.The mode that the present invention directly utilizes nanometer colloid ball lithographic technique and sputtering technology to combine prepares metal oxide nano array-inverse thin film.The present invention can reduce the equipment input of metal oxide nano array-inverse thin film preparation process, shortens preparation time, thereby reduces manufacturing cost.
The principle of its preparation is can form O when utilizing under the oxygen environment sputtering sedimentation metal oxide film
2-Negative ion carries out reverse sputtering to substrate, in deposit film, and O
2-Negative ion can carry out etching to the nanometer colloid ball, by suitably controlling sputtering atmosphere, just can obtain the regulatable metal oxide nano array-inverse thin film of cell size like this.
Technical solution of the present invention is:
A kind of preparation method of metal oxide nano array-inverse thin film may further comprise the steps, as shown in Figure 6:
Step 1. the substrate that is used to prepare metal oxide nano array-inverse thin film is carried out wetting ability handle.
Step 2. the high molecular nanometer colloidal spheres of certain size is scattered in the substrate surface of step 1 gained, forms the nanometer colloid ball template.
Step 3. the nanometer colloid ball template of step 2 gained is moved into magnetic control sputtering system, select corresponding sputtering target material according to the metal oxide nano array-inverse thin film of required preparation, adopt corresponding magnetron sputtering parameter and the sputtering sedimentation that carries out metal oxide film under the oxygen atmosphere is being arranged.
Step 4. the substrate behind the taking-up depositing metal oxide film, adopt conventional cleaning stripping nano ball, promptly get metal oxide nano array-inverse thin film.
In the technique scheme, described macromolecule nanometer ball can be the pipe/polyhenylethylene nano ball, also can be the polyisoprene nanometer ball.
Need to prove, step 3 when the depositing metal oxide film, the O that can form when utilizing reaction magnetocontrol sputtering
2-Negative ion carries out reverse sputtering to substrate the nanometer colloid ball is carried out etching, and what obtain is nano array-inverse thin film, rather than positive array film; By controlling suitable sputtering atmosphere, just can obtain the regulatable metal oxide nano array-inverse thin film of cell size.
The invention has the beneficial effects as follows: utilize O
2-The reverse sputtering corrasion of negative ion in reaction magnetocontrol sputtering, can directly utilize magnetically controlled sputter method to prepare the metal oxide array-inverse thin film, the step and the equipment of the special-purpose reaction particle etching nanometer colloid ball in the existing method have been saved, thereby reduce the equipment input of metal oxide nano array-inverse thin film preparation process, shorten preparation time, reduce manufacturing cost; The present invention can be used to prepare various metal oxide nano array-inverse thin films, can be applicable to the preparation of high-density magnetic storage, transmitter and based on the large-scale industrialization production of aspects such as the synthetic device performance optimization of cell size.
Description of drawings
The nanometer ball template synoptic diagram that Fig. 1 forms on the substrate for the nanometer colloid ball is dispersed in.
Fig. 2 be through the reaction particle etching apparatus change the diameter of nanometer colloid ball and sphere gap from after nanometer ball template synoptic diagram.
Fig. 3 has deposited the nanometer ball template synoptic diagram behind the metal oxide film.
Fig. 4 is the metal oxide nano array-inverse thin film synoptic diagram behind the stripping nano ball.
Fig. 5 is preparation method's schematic flow sheet of metal oxide nano array-inverse thin film in the prior art.
Fig. 6 is preparation method's schematic flow sheet of a kind of metal oxide nano array-inverse thin film of the present invention.
Fig. 7 is the atomic force microscope photo (spherical diameter is 500nm) of pipe/polyhenylethylene nano ball template.
Fig. 8 is the CoFe that utilizes the present invention to prepare
2O
4Oxide compound array-inverse thin film atomic force microscope photo.
Embodiment
The invention provides a kind of method of utilizing the nanometer ball template to prepare the controlled metal oxide nano array-inverse thin film of cell size.This method can form O when being based under the oxygen environment sputtering sedimentation sull
2-Negative ion carries out reverse sputtering to substrate, like this in deposit film, and O
2-Negative ion carries out etching to nanometer ball, by suitable control sputtering atmosphere, can obtain the regulatable metal oxide nano array-inverse thin film of cell size.By with different oxide film material preparation methods' combination, use present method and can prepare various metal oxide nano array-inverse thin films.Enumerating embodiment is below further specified the present invention.
Embodiment 1
1). with diameter is that 500nm polystyrene high score bulbec forms individual layer two-dimensional nano ball array template by self-assembly process on the silicon substrate of handling through wetting ability;
2). template is moved on to the rf magnetron sputtering vacuum chamber, take out back of the body end vacuum to 2 * 10
-7Mbar; Feed argon gas and oxygen then, wherein oxygen Ar Pressure ratio is 9: 1, and total operating air pressure (Ar Pressure and oxygen are pressed sum) is 7.74 * 10
-4Mbar, radio frequency power are 50W, and sputtering time is 2 minutes; Target is CoFe
2Alloy; Prepare CoFe by reactive sputtering
2O
4Film;
3) clean in toluene, peel off the pipe/polyhenylethylene nano ball template, polystyrene spheres is cleaned after this step, stays next CoFe
2O
4Oxidate nano antipoints battle array film is seen Fig. 2.Wherein antipoints battle array thickness is 20nm, and antipoints battle array size is 350nm.
Power and operating air pressure when macromolecule nanometer ball by adopting different size and control sputter can be prepared the metal oxide nano array-inverse thin film of different size.
Claims (3)
1, a kind of preparation method of metal oxide nano array-inverse thin film is characterized in that, may further comprise the steps:
Step 1. the substrate that is used to prepare metal oxide nano array-inverse thin film is carried out wetting ability handle;
Step 2. the macromolecule nanometer ball of certain size is scattered in the substrate surface of step 1 gained, forms the nanometer ball template;
Step 3. the nanometer ball template of step 2 gained is moved into magnetic control sputtering system, select corresponding sputtering target material according to the metal oxide nano array-inverse thin film of required preparation, adopt corresponding magnetron sputtering parameter and the deposition of carrying out metal oxide film under the oxygen atmosphere is being arranged;
Step 4. the nanometer ball template behind the taking-up depositing metal oxide film, adopt conventional cleaning stripping nano ball, promptly get metal oxide nano array-inverse thin film.
2, the preparation method of a kind of metal oxide nano array-inverse thin film according to claim 1 is characterized in that, described macromolecule nanometer ball is pipe/polyhenylethylene nano ball or polyisoprene nanometer ball.
3, the preparation method of a kind of metal oxide nano array-inverse thin film according to claim 1 is characterized in that, described macromolecule nanometer ball is the pipe/polyhenylethylene nano ball of 500nm; The described metal oxide that needs to prepare is CoFe
2O
4Oxide compound; Described sputtering target material is CoFe
2Alloy; Described magnetron sputtering parameter is: back of the body end vacuum is 2 * 10
-7Mbar, working gas are argon gas, and reactant gases is an oxygen, and oxygen argon ratio is 9: 1, and operating air pressure is 7.74 * 10
-4Mbar, radio frequency power are 50W, and sputtering time is 2 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101538008B (en) * | 2009-04-29 | 2010-12-01 | 北京大学 | Method for preparing nano-mesh film |
| CN102097208B (en) * | 2009-12-09 | 2013-12-18 | 吉林师范大学 | Preparation method of magnetic multilayer-film nano bowl monolayer array |
| CN102142362B (en) * | 2010-02-02 | 2012-10-10 | 中国科学院上海微***与信息技术研究所 | Method for photoetching by using electrophoretic deposition pattern of metallic compound |
| CN102148429B (en) * | 2010-02-06 | 2016-03-30 | 清华大学 | The manufacture method of nano-optical antenna array |
| CN102544366B (en) * | 2012-02-29 | 2013-11-13 | 天津大学 | Resistance switch based on cobalt ferrite nano-film and preparation method therefor |
| CN103626119A (en) * | 2013-12-08 | 2014-03-12 | 中国科学院光电技术研究所 | Preparation method for nano metal ball bowl array structure |
| CN104555910B (en) * | 2014-12-31 | 2016-05-18 | 吉林大学 | A kind of method of preparing film ordered micro structure based on reactive ion beam etching technique |
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| CN1588236A (en) * | 2004-10-13 | 2005-03-02 | 清华大学 | Method for preparing nano dot array of controllable unit size using nano ball template |
| US20060057388A1 (en) * | 2004-09-10 | 2006-03-16 | Sungho Jin | Aligned and open-ended nanotube structure and method for making the same |
| CN1769545A (en) * | 2004-11-02 | 2006-05-10 | 清华大学 | Method for developping directionally aligning zinc oxide nanometer rod array on silicon substrate |
| KR20060055575A (en) * | 2004-11-17 | 2006-05-23 | 삼성전기주식회사 | Fabrication method of field emitter electrode using nanosphere lithography |
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| US20060057388A1 (en) * | 2004-09-10 | 2006-03-16 | Sungho Jin | Aligned and open-ended nanotube structure and method for making the same |
| CN1588236A (en) * | 2004-10-13 | 2005-03-02 | 清华大学 | Method for preparing nano dot array of controllable unit size using nano ball template |
| CN1769545A (en) * | 2004-11-02 | 2006-05-10 | 清华大学 | Method for developping directionally aligning zinc oxide nanometer rod array on silicon substrate |
| KR20060055575A (en) * | 2004-11-17 | 2006-05-23 | 삼성전기주식회사 | Fabrication method of field emitter electrode using nanosphere lithography |
Non-Patent Citations (2)
| Title |
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| 纳米阵列结构功能材料的制备、性质及应用. 左娟，孙岚，林昌健.电子元件与材料，第22卷第12期. 2003 |
| 纳米阵列结构功能材料的制备、性质及应用. 左娟，孙岚，林昌健.电子元件与材料，第22卷第12期. 2003 * |
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