CN101041414A - Method for preparing silicon nanostructure based on nonaqueous etching and wet corrosion technique - Google Patents
Method for preparing silicon nanostructure based on nonaqueous etching and wet corrosion technique Download PDFInfo
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- CN101041414A CN101041414A CN200610040806.9A CN200610040806A CN101041414A CN 101041414 A CN101041414 A CN 101041414A CN 200610040806 A CN200610040806 A CN 200610040806A CN 101041414 A CN101041414 A CN 101041414A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 38
- 239000010703 silicon Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005530 etching Methods 0.000 title claims abstract description 19
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 13
- 238000005260 corrosion Methods 0.000 title claims description 18
- 230000007797 corrosion Effects 0.000 title claims description 18
- 238000001312 dry etching Methods 0.000 claims abstract description 22
- 238000001039 wet etching Methods 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 238000010894 electron beam technology Methods 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 238000000206 photolithography Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000011161 development Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 21
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000013461 design Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 7
- 229920002120 photoresistant polymer Polymers 0.000 claims description 6
- 238000010276 construction Methods 0.000 claims description 4
- 238000001259 photo etching Methods 0.000 claims description 4
- 239000002210 silicon-based material Substances 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 2
- 238000001020 plasma etching Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract 2
- 239000003292 glue Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 abstract 1
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 18
- 238000010586 diagram Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 101100460147 Sarcophaga bullata NEMS gene Proteins 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000000347 anisotropic wet etching Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005610 quantum mechanics Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 244000287680 Garcinia dulcis Species 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000329 molecular dynamics simulation Methods 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing silicon nanostructure by dry etching and wet etching process. (001) crystal direction common silicon wafer or SOI material is used as the substrate and an insulated layer deposited on the surface is used as the mask film. Nanometer hair stripe structure is prepared on electron beam resistant agent or photo resistance on the surface by electron-beam direct writing process or optical lithography. After development the dry etching is carried out to transfer the layout graphics to the surface layer silicon. The glue is eliminated by wet method and the surface layer silicon is eroded in anisotropy by wet method. As the etching depth and angle in dry etching and the temperature and the time of wet etching are changed, the nanometer structure with reversed cone support arm and inclined cantilever beam is prepared.
Description
Technical field
The present invention relates to the preparation of special nanostructured.In particular to a kind of method for preparing the special shape nanostructured in conjunction with dry etching and wet corrosion technique.
Background technology
The preparation of nanostructured is an important topic in the micro processing field always, especially little/receive in the Mechatronic Systems particularly important.Little/the Mechatronic Systems of receiving is to utilize the system of the micro-/ nano scale device of physical principles structures such as electromagnetic theory, classical mechanics, thermodynamics, quantum mechanics and molecular dynamics, promptly adds the ability of mechanical organs such as nano thin-film, beam, spring to realize environment is carried out perception, decision-making and control on circuit.With regard to MEMS (MEMS), products such as pressure sensor, accelerometer and micromechanical gyro have been arranged; Receive the critical size of system (NEMS) from several nanometers to the hundreds of nanometer, its character is subjected to the leading of microscopic theory such as quantum mechanics.Based on some the peculiar effects under the nanoscale, for example small-size effect and interfacial effect can be controlled its some fundamental characteristics (color, electric conductivity etc.) under the situation that does not change the material chemical composition.Therefore receive in the system research, the discovery of new property, new effect and utilization will be crucial, and new microfabrication manufacturing technology and processing method then are to realize preparing the basic premise of the system that receives.
The principle of anisotropic wet corrosion is that utilization corrosion rate of silicon in certain corrosive liquid depends on the crystal orientation that it is exposed to the surface in the corrosive liquid strongly, i.e. (100)＞＞(111).Yet the refinement of structure has the important meaning for little/further research of system received, for example the substrate design with cantilever beam is a triangle, also cantilever design can be the surface that is parallel to that tilt rather than single.
In the existing corrosion technology in the selection of etchant solution,, because the electrical conductance impurity of residual minim not, can be used as the anisotropic etchant of silicon chip in electron trade as the TMAH of the developer of important positive type photo-induced etching agent.TMAH has more advantage than the KOH anisotropic etchant.On corrosion rate, the corrosion Mean Speed of the TMAH of 90 ℃ of temperature (25%) can reach 900nm/min, near the corrosion rate of KOH; Simultaneously, TMAH is lower to the corrosion rate of SiO2 and Si3N4, and SiO2 and Si3N4 are good mask materials in the TMAH corrosion; The most important thing is that TMAH is metal ion not, good with the CMOS processing compatibility, meet development trend---the System on Chip/SoC (SOC) of MEMS/NEMS.In view of above advantage, TMAH just little by little replaces KOH.
Summary of the invention
The invention provides a kind of preparation method of a class nanostructured.The present invention is based on electron-beam direct writing technology and optical lithography, utilize the characteristics of anisotropic silicon wet etching, by the degree of depth of dry etch process etching and the preparation that angle realizes special nanostructured before the adjustment wet etching.
The preparation method of silicon nanostructure: the nanostructured that is used to prepare back draught support arm and angled cantilevered beams.Common silicon chip or SOI (Silicon on Insulator) material with (100) crystal orientation are substrate; Surface deposition one layer insulating is as mask; Electron-beam direct writing technology or optical lithography be preparation nanometer hachure structure on the electron sensitive resist on surface or photoresist; Carry out dry etching after the development, the domain figure is transferred on the surface silicon; Wet method is removed photoresist, and again surface silicon is carried out the anisotropic wet corrosion; In conjunction with the characteristics of anisotropic silicon wet etching, by the etching depth and the angle of change dry etching, and the temperature and time of wet etching can prepare the nanostructured of back draught support arm and angled cantilevered beams.
Described nanostructured be little/receive the supporting construction of Mechatronic Systems, as inverted triangle supporting construction and angled cantilevered beams structure.
Wherein substrate comprises common silicon chip and SOI material, and the crystal orientation requires to be (100).For the SOI substrate, the thickness of the further attenuate surface silicon of method that can be by thermal oxide and wet etching combination.
Wherein photoetching process comprises optical lithography and electron-beam direct writing.Select different photoetching processes according to the difference that concrete line thickness requires, live width generally adopts electron-beam direct writing technology in the structure of 0.5 micron following size.
Wherein dry etching is to adopt the ICP reactive ion etching, with CHF
3/ O
2Be reacting gas, simultaneously the angle that is etched by the angle control silicon materials of adjusting the substrate of the relative etching machine of substrate pallet.
Time by the change dry etching is controlled the degree of depth that silicon materials are etched, thereby changes some characteristic size of designed structure, as the vertical height of inverted triangle support arm and angled cantilevered beams.
Wherein wet etching adopts anisotropic wet corrosive liquid (for example TMAH corrosive liquid) to carry out at a certain temperature, by controlling some characteristic size of the temperature and time adjustment structure of corroding, for example sectional width of structure.
Little/preparation method of system architecture of receiving is different, and the present invention is in conjunction with basic fine process technology such as electron beam lithography, optical lithography, dry etching and wet etchings.Especially use the vertical stratification of the method etching high-aspect-ratio of dry etching, use the unsettled of anisotropic wet corroding method implementation structure.Wherein the principle of anisotropic wet corrosion is that utilization corrosion rate of silicon in certain corrosive liquid depends on the crystal orientation that it is exposed to the surface in the corrosive liquid strongly, i.e. (110)＞(100)＞＞(111).Yet the refinement of structure has the important meaning for little/further research of system received, for example the substrate design with cantilever beam is a triangle, also cantilever design can be the surface that is parallel to that tilt rather than single.
Characteristics of the present invention are: the preparation method who has proposed a class nanostructured.Make full use of characteristics, the preparation of the special nanostructured of realization that can be accurate and meticulous based on electron-beam direct writing technology and optical lithography and anisotropic silicon wet etching.
It is in order to disclose its essence that general introduction of the present invention and purpose are provided.By the following preferred embodiment of reference the present invention, in conjunction with the accompanying drawings, can understand the present invention more fully.
Description of drawings
Under Fig. 1 horizontal positioned substrate situation, in conjunction with the schematic diagram of dry etching and structure that wet etching forms
The SEM (SEM) of Fig. 2 inverted triangle support arm structure is observed photo
The schematic diagram of the structure that wet etching forms behind Fig. 3 small angle inclination placement substrate dry etching
The schematic diagram of the structure that wet etching forms behind Fig. 4 wide-angle tilt placement substrate dry etching
The SEM (SEM) of Fig. 5 small angle inclination cantilever design is observed photo
The specific embodiment
The preparation of special nanostructured is described in detail in detail below with reference to accompanying drawings, has been provided the exemplary embodiment of the inventive method in the accompanying drawing; From the more specifically description to preferred implementation of the present invention, with reference to above-mentioned accompanying drawing, aforementioned and other purpose, feature and advantage of the present invention will be clearly, and identical label is represented identical part in different figure.Accompanying drawing is not necessarily pro rata, and its emphasis is being explained on the method for the present invention on the contrary.In the accompanying drawings, for the sake of clarity, amplified the size and and the thickness in each layer and zone.
Fig. 1 is a process chart of realizing inverted triangle support arm structure among the present invention, mainly may further comprise the steps in the concrete technology: the meteorological deposit certain thickness of low pressure chemical silicon nitride film on (100) silicon chip substrate; The spin coating photoresist, optical lithography hachure structure, the direction of hachure are (110); The substrate horizontal positioned is carried out dry etching, and the difference of silicon etching degree of depth h has directly determined the vertical height of gusseted arm configuration; Under the high temperature in sulfuric acid and hydrogen peroxide wet method remove photoresist, (temperature is generally 60-90 degree centigrade) carries out the anisotropic wet etching process of silicon then at a certain temperature.Be divided into two structures that gable top links to each other up and down from the interface of silicon dry etching, the height of top del is the degree of depth of dry etching.Simultaneously by changing etching time (carry out as required, the speed of its corrosion is generally 0.1mm/10min).Can control gusseted the arm vertically depth d of corrosion, the i.e. sectional width of structure.The hypotenuse of triangular structure and the angle on plane promptly are the angles of (111) crystal face and (110) crystal face, are 54.7 °.Fig. 2 is SEM (SEM) schematic diagram of gusseted arm configuration.
Fig. 3 is a process chart of realizing the inclination cantilever design among the present invention, concrete technology and gusseted arm configuration are similar, when difference is dry etching the substrate tilting certain angle is placed, and the size of tilt angle alpha has determined the sectional width of anisotropic wet corrosion back final structure, the i.e. vertical width of this cantilever.As shown in Figure 3, when etching angle α greater than 54.7 °, because the difference of both sides etching depth makes B point and D point that certain altitude poor (degree of depth that B point etching depth h is ordered greater than D) be arranged, thereby between the two handstand triangles inclination cantilever design can appear behind the wet etching, because the anisotropic wet etching characteristic will be to launch along A-B and C-D direction from A point and C point in the incline structure; For the situation of etching angle α less than 54.7 °, as shown in Figure 4, incline structure will be to launch along B-A direction and C-D direction respectively from B point and C point, and the right half of degree of depth of launching is by the width decision of C-E, and promptly interfacial degree of depth h ' is comprehensively determined by etching angle and mask layer thickness.For very thin mask layer, then can ignore the C-E width, will be similar to the single inclination cantilever design of appearance.Certainly, the time of control wet etching can further change its sectional width equally, and the time with the TMAH wet etching is 5-10min in the present embodiment, and temperature is 70 degrees centigrade.The angle on cantilever and plane then is fixed as 54.7 °.Fig. 5 then is the SEM schematic diagram of the inclination cantilever design of low-angle lithographic method preparation on the silicon chip, illustration wherein is the inclination cantilever design of another sample, the architectural difference that brings behind the different and wet etching of the right and left etching depth under the low-angle etching condition as can be seen from wherein M point and N point.
Claims (9)
1, a kind of preparation method of silicon nanostructure is characterized in that common silicon chip or the SOI material with (100) crystal orientation is substrate; Surface deposition one layer insulating is as mask; Electron-beam direct writing technology or optical lithography be preparation nanometer hachure structure on the electron sensitive resist on surface or photoresist; Carry out dry etching after the development, the domain figure is transferred on the surface silicon; Wet method is removed photoresist, and again surface silicon is carried out the anisotropic wet corrosion; By the etching depth and the angle of change dry etching, and the temperature and time of wet etching prepares the nanostructured of back draught support arm and angled cantilevered beams.
2, according to the silicon nanostructure preparation method of claim 1, it is characterized in that nanostructured wherein mainly be little/receive the supporting construction of Mechatronic Systems, i.e. inverted triangle supporting construction and angled cantilevered beams structure.
3, according to the silicon nanostructure preparation method of claim 1, it is characterized in that wherein substrate comprises common silicon chip and SOI material, the crystal orientation requires to be (100); For the SOI substrate, and the thickness of the further attenuate surface silicon of method by thermal oxide and wet etching combination.
4,, it is characterized in that wherein photoetching process comprises optical lithography and/or electron-beam direct writing according to the silicon nanostructure preparation method of claim 1.Select different photoetching processes according to the difference that concrete line thickness requires, live width adopts electron-beam direct writing technology in the structure of 0.5 micron following size.
5,, it is characterized in that wherein dry etching is to adopt the ICP reactive ion etching, with CHF according to the silicon nanostructure preparation method of claim 1
3/ O
2Be reacting gas, control the angle that silicon materials are etched by the angle of adjusting the substrate of the relative etching machine of substrate pallet.
6, according to the silicon nanostructure preparation method of claim 1, it is characterized in that controlling the degree of depth that silicon materials are etched by the time that changes dry etching, thereby change some characteristic size of designed structure, for example the vertical height of inverted triangle support arm and angled cantilevered beams.
7, according to the silicon nanostructure preparation method of claim 1, it is characterized in that wherein wet etching adopts the anisotropic wet corrosive liquid to carry out at a certain temperature, by controlling some characteristic size of the temperature and time adjustment structure of corroding, for example sectional width of structure.
8,, it is characterized in that the size of tilt angle alpha has determined that anisotropic wet corrodes the sectional width of back final structure, the i.e. vertical width of this cantilever according to the silicon nanostructure preparation method of claim 5.
9, according to the silicon nanostructure preparation method of claim 5, it is characterized in that working as etching angle α greater than 54.7 °, behind the wet etching between the two handstand triangles inclination cantilever design can appear.
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| WO2017048671A1 (en) * | 2015-09-15 | 2017-03-23 | President And Fellows Of Harvard College | Wavelength selective optical nanostructures fabricated on the surface of bulk homogenous substrates |
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