CN103233208B - Ion beam sputtering is utilized to prepare the method for micro nano structure film - Google Patents
Ion beam sputtering is utilized to prepare the method for micro nano structure film Download PDFInfo
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- CN103233208B CN103233208B CN201310146298.2A CN201310146298A CN103233208B CN 103233208 B CN103233208 B CN 103233208B CN 201310146298 A CN201310146298 A CN 201310146298A CN 103233208 B CN103233208 B CN 103233208B
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Abstract
The invention provides a kind of apparatus and method utilizing ion beam sputtering to prepare micro nano structure film, this device comprises ion beam sputtering device and collimation filtration unit, collimation filtration unit is connected with the specimen holder of ion beam sputtering device, collimation filtration unit comprises: disk, some filtering nets and multiple annulus, the lower surface of disk is connected with specimen holder, each annulus overlaps successively at disk upper surface, and filtering net is arranged between each annulus.The present invention effectively can improve the quality of micro nano structure film, has important using value in nanometer integrated circuit field.
Description
Technical field
The present invention relates to micro nano structure film preparing technology, particularly, relate to a kind of device and method utilizing ion beam sputtering to prepare micro nano structure film.
Background technology
The nearest more than ten years, along with developing rapidly of micro-nano processing technology, its minimum process yardstick strides forward to tens nanometers, and working accuracy also more and more higher (can reach several nanometer), and this has higher requirement to the film deposition techniques of micro nano structure.Such as, in the front line science researchs such as emerging nanophotonics, nanoelectronics, we often need to prepare the metallic film with certain micro nano structure.In the fundamental research in this field, evaporation coating technique (as hot evaporation, electron beam evaporation plating) due to the energy of the particle such as atom, elementide produced lower, it is less to the damage of photoresist material mask, is easy to demoulding, thus obtains at present applying comparatively widely.But adopt this deposition techniques film to there is certain problem, the problem such as such as film poor and utilization rate of raw materials relative to the bonding force of substrate is low, this will become the unavoidable problem of people in the industrialization process of following nanometer integrated circuit.
Sputter coating is a kind of important thin film deposition processes, and two kinds of important technologies of its construct physical vapor deposition together with evaporation, it plays very important effect in current suitability for industrialized production.Large area film depositing operation or MEMS (micro electro mechanical system) (Micro-Electro-MechanicalSystems, be called for short MEMS) in the graphic structure used generally more than several micron, physical vapor sputtered film deposition technique plays an important role in the scientific research and suitability for industrialized production in this field owing to saving starting material, film and to be combined the advantages such as firm and compactness is good with substrate.Although physical sputtering coating technique has the incomparable advantage of above-mentioned evaporation coating technique, in the fundamental research of the more and more less nano structured unit of preparation size, this technology is but hardly by people are adopted.As everyone knows, for evaporate process, the particle energys such as the atom in sputter coating process, elementide are approximately its tens times.When the dimension of picture prepared is more and more less, the thickness of its photoresist material mask also corresponding thinning (specifically, the thickness of photoresist material mask is no more than three times of dimension of picture).Therefore, high energy particle in physical sputtering coating process produces considerable damage effect by this relatively very thin photoresist material mask, particularly to the edge section of micro nano structure, it causes difficulty also to demoulding technique simultaneously, thus causes the quality of micro nano structure film to reduce rapidly.
If high-octane particle in sputtering technology can be reduced, to the destruction of photoresist material mask, just this sputter coating process can be used in the preparation process of micro nano structure film.Specifically, the main problem needing following two aspects of solution: first, reduce the energy of sputtering particle when deposit film; Secondly, strengthen the directivity of sputtering particle further, reduce the considerable damage that oblique incidence particle produces photoresist material edge.In the present invention, for ion beam sputtering deposition technology, by a set of collimation filtration unit of addition in this complete equipment, the quality of micro nano structure film can be significantly improved.This technology is simple and feasible, can not only improve the quality of micro nano structure film, and the physical sputtering equipment of current industrialization can be utilized to promote the process of industrialization of nanometer integrated circuit further.
Summary of the invention
For defect of the prior art, the object of this invention is to provide a kind of device and method utilizing ion beam sputtering to prepare micro nano structure film.
According to an aspect of the present invention, a kind of device utilizing ion beam sputtering to prepare micro nano structure film is provided, comprise ion beam sputtering device and collimation filtration unit, collimation filtration unit is connected with the specimen holder of ion beam sputtering device, collimation filtration unit comprises: disk, some filtering nets and multiple annulus, the lower surface of disk is connected with specimen holder, and each annulus overlaps successively at disk upper surface, and filtering net is arranged between each annulus.
Preferably, disk and annulus are provided with perforate, disk and annulus are solidly connected to specimen holder by perforate by screw.
Preferably, the quantity of filtering net is one, and the quantity of annulus is two; Or the quantity of filtering net is two, the quantity of annulus is three.
Preferably, the diameter of disk is 4 inches, and thickness is 3mm.
Preferably, filtering net is square, and its center mesh-portion is circular, and mesh is hexagonal structure.
Preferably, the thickness of filtering net is 50 μm, and the length of side is 50mm, and central network bore portion diameter is 42mm, and mesh aperture is 100 μm, and rib width is 40 ~ 50 μm.
Preferably, annulus external diameter is 4 inches, and internal diameter is 45mm, and thickness is 3mm.
Preferably, disk, filtering net and annulus all adopt stainless material to make.
According to another aspect of the present invention, a kind of method utilizing ion beam sputtering to prepare micro nano structure film is provided, comprises the following steps:
Step 1: preparation has the sample of photoresist material polymethylmethacrylate mask;
Step 2: the primary source opening ion beam sputtering equipment, is filled with nitrogen, opens vacuum chamber;
Step 3: sample step 1 prepared is fixed on the disk of collimation filtration unit, is clamped between annulus by filtering net, and specimen holder collimation filtration unit being fixed on ion beam sputtering device;
Step 4: water-cooling system and the mechanical pump power supply of opening vacuum chamber sample table successively, after vacuum tightness is higher than 1Pa, opens molecular pump; When vacuum chamber background vacuum reaches 2*10
-4after Pa, open ion beam sputter depositing equipment;
Step 5: after having sputtered, closure molecule pump and mechanical pump, be filled with nitrogen successively, take out sample, sample is placed in acetone reagent and soaks about 5 hours, remove PMMA electron beam resist, and use acetone, ethanol and washed with de-ionized water successively, finally dry up with nitrogen.
Preferably, in step 4, the processing parameter of ion beam sputtering is:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: O
2; 1.9*10
-2pa;
Depositing time: Cr is 20sec, Ag is 80sec;
Sputtering interval: often interval 5min after sputtering 60sec.
Compared with prior art, the present invention has following beneficial effect: the present invention collimates filtration unit by design and is arranged on the specimen holder of ion beam sputtering equipment, not only can effectively stop large-angle inclined projectile in suprabasil deposition, reduce the destruction that it produces photoresist material mask (particularly its boundary member), and the large size elementide produced after can stoping ion beam bombardment target etc. is in suprabasil deposition, thus effectively improve the micro nano structure film quality of preparation.For to expand with physical vapor sputtering technology be core, the application of coating process in micro nano structure element and following micro-nano integrated circuit is significant in the present invention.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is that the present invention utilizes ion beam sputtering to prepare the structural representation of the device of micro nano structure film;
Fig. 2 is the STRUCTURE DECOMPOSITION figure of the collimation filtration unit of the embodiment of the present invention;
Fig. 3 is the filter screen structure schematic diagram of the embodiment of the present invention;
Fig. 4 adopts scanning electronic microscope (SEM) shape appearance figure collimating the micro nano structure figure of the forward and backward preparation of filtration unit in the present invention to compare: (a) be not for adopt collimation filtration unit; B () is for adopting single layer filter net collimation filtration unit; C () is for adopting double-layer filtering net collimation filtration unit;
Fig. 5 utilizes in the present invention the optical morphology figure adopting double-layer filtering net to collimate the micro nano structure array of filtration unit deposition.
In figure: 1 is specimen holder, 2 is collimation filtration unit, and 3 is disk, and 4 is filtering net, and 5 is annulus.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
A kind of device utilizing ion beam sputtering to prepare micro nano structure film, comprise ion beam sputtering device and collimation filtration unit 2, collimation filtration unit 2 is connected with the specimen holder 1 of ion beam sputtering device, collimation filtration unit 2 comprises: disk 3, two filtering nets 4 and three annulus 5, the lower surface of disk 3 is connected with specimen holder 1, each annulus 5 overlaps the upper surface at disk 3 successively, and filtering net 4 is arranged between each annulus 3.
The lower surface of disk 3 is connected with specimen holder 1, and upper surface is used for placing and fixed sample, and the diameter of disk 3 is 4 inches, and thickness is 3mm.
As shown in Figure 3, it is the structural representation of filtering net.The size of filtering net 4 is slightly larger than the internal diameter size of annulus 5, and the profile of filtering net 4 is the square of length of side 50mm, and center is the filtering net of diameter 42mm, thickness is about 50 μm, mesh is hexagonal structure, and mesh aperture is about 100 μm, and rib width is about 40 μm ~ 50 μm.
Annulus 5 can not only be fixed on the specimen holder 1 of ion beam sputtering device together with disk 3, and can held tight filtering net 4 between each annulus 5.The external diameter of annulus 5 is 4 inches, and internal diameter is 45mm, and thickness is 3mm.
Further, annulus 5 and disk 3 have the perforate that three diameters are 3.5mm respectively, and three perforates are circumferentially evenly being distinguished, and annulus 5 and disk 3 can be fixed on specimen holder 1 with M3 screw.
More specifically, disk 3, filtering net 4 and annulus 5 all adopt stainless material to make.
In this example, have employed double-layer filtering net collimation filtration unit 2, comprise two filtering nets 4 and three annulus 5.But it should be noted that, the present invention does not limit concrete filtering net 4 and the quantity of annulus 5.In actual applications, selecting the structure of concrete collimation filtration unit 2 according to actual needs, can be double-layer filtering net, it can also be single layer filter net even bed filtration net, correspondingly, the quantity of filtering net 4 and annulus 5 can be a filtering net 4 and two annulus 5, or is multiple.Therefore, above employing double-layer filtering net collimation filtration unit 2 is an embodiment, is not intended to limit the present invention.
The present invention also provides a kind of method utilizing ion beam sputtering to prepare micro nano structure film, comprises the following steps:
Step 1: preparation has the sample of photoresist material polymethylmethacrylate (Poly (methylmethacrylate) is called for short PMMA) mask.
Step 2: the primary source opening ion beam sputtering equipment, is filled with nitrogen, opens vacuum chamber.
Step 3: sample step 1 prepared is fixed on the disk of collimation filtration unit, is clamped between annulus by filtering net, and specimen holder collimation filtration unit being fixed on ion beam sputtering device.
Step 4: water-cooling system and the mechanical pump power supply of opening vacuum chamber sample table successively, after vacuum tightness is higher than 1Pa, opens molecular pump; When vacuum chamber background vacuum reaches 2*10
-4after Pa, open ion beam sputter depositing equipment.
Particularly, the processing parameter of ion beam sputtering is:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: O
2; 1.9*10
-2pa;
Depositing time: Cr is 20sec, Ag is 80sec;
Sputtering interval: often interval 5min after sputtering 60sec.
Under above sputtering parameter, when not adopting collimation filtration unit, the sedimentation rate of film is 4nm/sec; After adding single layer filter net collimation filtration unit, the sedimentation rate of film is 2.6nm/sec; After adding double-layer filtering net collimation filtration unit, the sedimentation rate of film is 1.8nm/sec.Thus, adopting collimation filtration unit of the present invention, is the film of sediment-filled phase stack pile, needs to precalculate ion beam sputtering required time.
Step 5: after having sputtered, closure molecule pump and mechanical pump, be filled with nitrogen successively, take out sample, sample is placed in acetone reagent and soaks about 5 hours, remove PMMA electron beam resist, and with using acetone, ethanol and washed with de-ionized water successively, finally dry up with nitrogen.
For the above-mentioned technology utilizing ion beam sputtering device to deposit micro nano structure film, below for the indicia patterns in widely everybody the graphene nano electrode production process paid close attention to, illustrate how at SiO
2in (290nm thickness)/Si substrate, deposit thickness is about the micro nano structure Cr/Ag film of 40nm:
(1) SiO of 10mm is about in the length of side
2the electron beam resist of spin coating PMMA495 and 950 liang type successively in/Si substrate, its thickness is respectively 290nm and 230nm, and photoresist material mask total thickness is 520nm.
(2) utilize the exposure in this substrate with photoresist material mask described in (1) of ZeissUltra55 scanning electronic microscope and supporting electron beam diaphragm and graphicalphanumeric generator to be of a size of the indicia patterns of 500-1000nm, its exposure dose is 600.
(3) to develop successively in the developing solution and IPA stop bath of the mix reagent preparation of Virahol (IPA) and 4-methyl-2 pentanone (MIBK) 40 seconds and fixing 60 seconds, then dry up with nitrogen.The volume ratio of IPA and MIBK is 3:1.Development, fixing after, indicia patterns is transferred on PMMA photoresist material mask.
(4) open the primary source of ion beam sputtering equipment, be filled with nitrogen, open vacuum chamber.This ion beam sputtering equipment is the LDJ-2A-F100-100 series Dual ion beam sputtering deposition system that Beijing Institute of Advanced Ion Beam Technology produces.
(5) sample with photoresist material mask prepared in the step of above-mentioned (1) to (3) is fixed on the disk of collimation filtration unit, then (single-filtering net collimation filtration unit is namely adopted) between two annulus single filtering net being held on near-neighbor sample, or two filtering nets are held on successively between three annulus and (namely adopt two filtering net collimation filtration unit), finally this cover collimation filtration unit is fixed on the specimen holder of ion beam sputtering device.
(6) water-cooling system and the mechanical pump power supply of vacuum chamber sample table is opened successively.After vacuum tightness is higher than 1Pa, open molecular pump; When vacuum chamber background vacuum reaches 2*10
-4after Pa, open ion beam sputter depositing equipment.
Significant parameter in ion beam sputtering process is as follows:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: 1.9*10
-2the O of Pa
2;
Depositing time: Cr is 20sec, Ag is 80sec;
Sputtering interval: often interval 5min after sputtering 60sec.
(7) calculate sputtering time, after sputter procedure completes, closure molecule pump and mechanical pump, be filled with nitrogen successively, takes out sample.
(8) sample is placed in acetone reagent and soaks about 5 hours, remove PMMA electron beam resist, and with using acetone, ethanol and washed with de-ionized water successively, finally dry up with nitrogen.
The metallic film shape appearance figure utilizing SEM to observe above-mentioned ion beam sputtering equipment to prepare, compares the morphology change of the micro nano structure figure adopting the forward and backward preparation of collimation filtration unit, as shown in Figure 4.Can see, collimation filtration unit of the present invention obviously can improve the quality of the micro nano structure film utilizing ion beam sputtering equipment to deposit.The optical morphology of the micro nano structure indicia patterns array utilizing ion beam sputtering equipment and adopt double-layer filtering net collimation filtration unit to prepare as shown in Figure 5, can reach application requiring.
The present invention is by a set of collimation filtration unit of addition on the specimen holder of ion beam sputtering equipment, the large size elementides that the destruction that can effectively stop oblique incidence particle to produce mask (particularly boundary member) and stoping produces during ion beam bombardment target etc. are in suprabasil deposition, thus improve the quality of micro nano structure film, in nanometer integrated circuit field, there is important using value.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (1)
1. the method utilizing ion beam sputtering to prepare micro nano structure film, application ion beam sputtering device and collimation filtration unit, described collimation filtration unit is connected with the specimen holder of described ion beam sputtering device, described collimation filtration unit comprises: disk, some filtering nets and multiple annulus, the lower surface of described disk is connected with described specimen holder, described each annulus overlaps at described disk upper surface successively, and described filtering net is arranged between described each annulus; It is characterized in that, comprise the following steps:
Step 1: preparation has the sample of photoresist material polymethylmethacrylate mask;
Step 2: the primary source opening ion beam sputtering equipment, is filled with nitrogen, opens vacuum chamber;
Step 3: sample step 1 prepared is fixed on the disk of collimation filtration unit, is clamped between annulus by filtering net, and specimen holder collimation filtration unit being fixed on ion beam sputtering device;
Step 4: water-cooling system and the mechanical pump power supply of opening vacuum chamber sample table successively, after vacuum tightness is higher than 1Pa, opens molecular pump; When vacuum chamber background vacuum reaches 2 × 10
-4after Pa, open ion beam sputter depositing equipment, the processing parameter of ion beam sputtering is:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: O
2; 1.9 × 10
-2pa;
Depositing time: Cr is 20sec, Ag is 80sec;
Sputtering interval: often interval 5min after sputtering 60sec;
Step 5: after having sputtered, closure molecule pump and mechanical pump, be filled with nitrogen successively, take out sample, sample is placed in acetone reagent and soaks about 5 hours, remove PMMA electron beam resist, and use acetone, ethanol and washed with de-ionized water successively, finally dry up with nitrogen.
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| CN201310146298.2A CN103233208B (en) | 2013-04-24 | 2013-04-24 | Ion beam sputtering is utilized to prepare the method for micro nano structure film |
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| CN112475293A (en) * | 2020-12-08 | 2021-03-12 | 中北大学 | Preparation method of micro-nano lattice hole ultrathin stainless steel filter plate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5330628A (en) * | 1990-01-29 | 1994-07-19 | Varian Associates, Inc. | Collimated deposition apparatus and method |
| CN101307430A (en) * | 2008-07-04 | 2008-11-19 | 郑州大学 | Energy filtrated magnetron sputtering plating method and apparatus for applying the method |
| CN203295598U (en) * | 2013-04-24 | 2013-11-20 | 上海交通大学 | Device for preparing micro-nano structure thin film by utilizing ion beam sputtering method |
-
2013
- 2013-04-24 CN CN201310146298.2A patent/CN103233208B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5330628A (en) * | 1990-01-29 | 1994-07-19 | Varian Associates, Inc. | Collimated deposition apparatus and method |
| CN101307430A (en) * | 2008-07-04 | 2008-11-19 | 郑州大学 | Energy filtrated magnetron sputtering plating method and apparatus for applying the method |
| CN203295598U (en) * | 2013-04-24 | 2013-11-20 | 上海交通大学 | Device for preparing micro-nano structure thin film by utilizing ion beam sputtering method |
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