CN100549836C - Production has the method for element of optical application of nanometer multilayer and the element of producing according to this method - Google Patents
Production has the method for element of optical application of nanometer multilayer and the element of producing according to this method Download PDFInfo
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- CN100549836C CN100549836C CNB2006800020704A CN200680002070A CN100549836C CN 100549836 C CN100549836 C CN 100549836C CN B2006800020704 A CNB2006800020704 A CN B2006800020704A CN 200680002070 A CN200680002070 A CN 200680002070A CN 100549836 C CN100549836 C CN 100549836C
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/28—Interference filters
- G02B5/283—Interference filters designed for the ultraviolet
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/28—Interference filters
- G02B5/285—Interference filters comprising deposited thin solid films
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
- G21K1/06—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
- G21K1/062—Devices having a multilayer structure
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Abstract
The present invention relates to prepare have a nanometer multilayer be used for the especially method of the element of X-ray optics system of optical application, element monocrystalline silicon preferably wherein, nanometer multilayer is by using the individual layer of the continuous paint of sol-gel-coating on it to prepare.The purpose of this invention is to provide the cost advantageous method, use this method particularly by aluminium oxide, to prepare nanometer multilayer only by a kind of material with the density adjustment that in multilayer, can be scheduled to.This purpose solves by following, wherein the layer structure of a plurality of continuous realizations of the same material of multilayer by having possible bed thickness minimum under every kind of situation realizes, each wherein continuous individual layer by element in sol-gel-pond short time dipping or with sol-gel-solution spraying on element, under predetermined temperature, prepare subsequently at air drying or annealing in process.
Description
Technical field
The present invention relates to produce and have being used for x-ray-optical system that optical application for example has hard and soft x ray, being used for vacuum-UV-radiation or being used for the analyzer-multilayer-grating of x ray fluorescence analysis and being used for element of nanometer multilayer in the different wavelength range radiation as the light filter that insulate, wherein this element is preferably monocrystalline silicon, is coated with the nanometer multilayer of the individual layer formation that is coated with continuously by sol-gel-coating (Sol-Gel-Beschichtung) method thereon.
Background technology
Traditional in the art optical element is to have a multi-component nanometer layer system (DE 198 23732 A1) by the material preparation that has density contrast under two or more the every kind situation between the individual layer.For different applications, knownly for example make by copper and carbon, chromium and scandium, nickel and titanium and vanadium and aluminium oxide.For the effect that realizes optical system is the bed thickness of very important individual layer, littler than incident light wavelength usually, because like this by interfering, can realize desirable optical effect.Yet the optical signature of this layer system is often owing to suffered damage by the material transfer of bluring between phase counterdiffusion between the interface and the individual layer that caused by crystallization when temperature heating that usually will be very low usually.This infringement can be for example by stoping diffusion to reduce (EP 1 394 815 Al, EP 1 384 234 A1) at interlayer.
Compare this system that only is made up of a kind of material with the layer system of this bi-component more stable.The variation of necessity of the refractive index in this multilayer realizes by the density of regulating between the individual layer.Thereby the multilayer system of this density adjustment does not have the chemical gradient that helps to spread guarantees himself stability when high temperature.Like this be, for example by Baranov, known pure carbon multilayer in " Kohlenstoff/Kohlenstoff-Multischichten hergestellt durch Laserablation " with different-thickness.Equally, it is the known individual layer with such density adjustment or has the multilayer of other phase composition of being made up of indium-Xi-oxide, zirconium sulfate or tin oxide.
Use now different vacuum coated methods in order to prepare this multilayer system, for example the vacuum coated method of physics or chemistry (PVD, CVD) or laser ablation.Make in this way to prepare optical layers, but at first they are because deposition is low and cost is very high with high homogeneity.
In principle, for the productive zone system, also have wet-chemical to be coated with from prior art is known, as sol-gel-method.Make in this way the layer system of preparation have necessary quality and reproducibility and obviously be that cost is favourable in addition.Thus, the colloidal suspension that is suspended in the inorganic particle of the nanometer range in suitable solvent such as water or the organic solvent is applied over nanometer potash (nanoskaligen) film that also forms necessity on the base material there.This film reinforces and forms the effective layer of uniform optics by annealing process.
Be used for the diverse ways that applies, particularly dip-coating, spraying or the spin coating of suspended matter from the feature according to base material and coating material known in the state of the art.So far, use this coating process preparation to have the layer system that is used for optical application of different materials combination.
Like this, in WO 2001/058681Al, described by base material to be coated is impregnated into and prepared the layer system of forming by cerium oxide and silicon oxide layer in the colloidal suspension.About astern speed and the receding angle that base material stretches from colloidal suspension with respect to the surface of colloidal suspension, thickness and the consistance that can regulate each layer, and the dip process duration is considered as no standard and can changes.By the thermal treatment of carrying out subsequently thereon, with the layer oxidation and the curing of deposition.Heat treatment period and temperature depend on whether be cured or at last whole layer system carried out whole processing before further coating process.Accordingly, thermal treatment can add up to up to 200 ℃ of a few minutes to one hour or in 450 ℃ of half an hour to two hour or under special circumstances also can the longer time.
Described the method for spraying in DE 198 40 525 A1, not only individual layer but also layer system can be by the multiple material preparations that applies continuously to use this method.The adjusting of Bi Yao inhomogeneity bed thickness is carried out according to the wet coating of the big octuple of desciccator diaphragm thickness (Factor acht) by preparation by different parameters and the opposing party of spray equipment on the one hand in the method.Thus, by in suspended matter, adding high boiling solvent equably and avoid compensating flow process and spray.The inorganic constituents of different metal oxides as suspended matter applied, because its structure size is transparent in nanometer range and in the end-state of solidifying.For example SiO like this
2, TiO
2, ZrO
2Or Al
2O
3
Find that particularly crystalline aluminium film or its amorphous variant are used for a lot of optics, electronics and protective finish.Use from B.E.Yoldas Ceramic Bulletin 54[3 in order to produce uniform aluminium film] the known favourable wet-chemical coating of cost in (1975) 289, use aluminium-alkali metal oxide as initial period.Also can use aluminium-colloidal suspension of making by inorganic salts, for example A1C13.6H2O.(Q.Fu，C-B.Cao，H.-S.Zhu，Thin?Solid?Films?348(1999)99)。Yet use the Sol-Gel-method so far, always realize unaccommodated too big bed thickness and uniform layer (N.Bahlawa-ne for the application purpose of enumerating, T.Watanabe, J.American Ceramic.Soc.80[12] (1997) 3213) and confirm to realize that the necessary homogeneity of the sedimentary deposit of wet-chemical in nanometer range is difficult.
Summary of the invention
Therefore, according to purpose of the present invention, realize that preparation has the optical application element that is used to the technology that begins to enumerate of nanometer multilayer, can cost advantageously use and use this method can be particularly have the multilayer that the density that can be scheduled to is adjusted in multilayer by the aluminium oxide preparation by a kind of material only.
This purpose solves by following the inventive method, i.e. preparation has the method for the element that is used for optical application of nanometer multilayer, nanometer multilayer prepares by the individual layer that sol-gel-coating process applies continuously on it, it is characterized by, the layer structure of a plurality of continuous realizations of the same material of multilayer by having minimum possible bed thickness separately realizes, each wherein continuous individual layer by element in sol-gel-pond short time dipping or with sol-gel-solution spraying on element, under predetermined temperature, in air, prepare subsequently by drying or annealing process.
The present invention relates to be used for the selectivity production method of the nanometer multilayer on the different substrate materials, this multilayer only is made up of a kind of material with the continuous individual layer that periodically overlaps each other, under every kind of situation of these individual layers by the interface of recently representing being separated from each other by density.Thereby the refractive index in the multilayer system also can be in the direction cyclical variation vertical with the interface.Density contrast as significance of the present invention is interpreted as in this interface upper density great-jump-forward variation.
The preparation of multilayer is carried out according to known sol-gel-method, wherein make to have and adjust deposition parameter targetedly, for example draw speed and and thus the predetermined temperature range that uses of the residence time in sol-gel-pond or spray parameters and allowing subsequently thermal treatment and therefore only by the deviation of material character between a kind of multilayer of material preparation.Because it is good at low-down expense expenditure, and make it approach described method of the present invention more in addition.
Show that like this individual layer in each deposition cycle preparation stacked has compares porous and therefore low-density thin list surface layer (top layer) with affiliated layer.This top layer has constituted the interface that has the density contrast in the multilayer by a kind of material preparation only.Simultaneously, use any independent drying or annealing in process to carry out to the slight curing of the individual layer that deposited.
In addition, can be according on purpose density adjustment of deposition parameter, because in sol-gel-method, not only the astern speed of Ying Yonging also has annealing or baking temperature to influence the thickness and the density of sol gel film.The temperature of drying or annealing process can be adjusted to the scope between 100 ℃～500 ℃, the scope between preferred 150 ℃～400 ℃.Like this, high astern speed causes the thick film of low average density, and this is owing to the porous of film.On purpose regulate the deposition parameter of adjusting about the density in the multilayer of forming by a kind of material, make its utilization become possibility for different optical application based on interference effect.
When another advantage of method of the present invention is high temperature in multilayer the stability of density adjustment and amorphous state.After thermal treatment in 1000 ℃ temperature air, can use the no crystallization phase of method proof of X-ray diffraction, because the crystallization phase of the growth formation by crystallite influences the rough interface degree conversely especially.
Use the method for the present invention can be particularly by Al
2O
3Equally by TiO
2Or SiO
2The preparation multilayer.
Description of drawings
The present invention will further specify according to following embodiment, and description of drawings is as follows:
Fig. 1 has the layer structure of the aluminium multilayer of different number of deposition cycles on silicon substrate
Aluminium lamination that Fig. 2 prepares in single deposition cycle uses astern speed as parameter, when the x-radiation exposure according to experiment with by the reflectivity of model determination.
The aluminium lamination density that Fig. 3 prepares in single deposition cycle is to the dependence of astern speed.
The aluminum layer thickness that Fig. 4 prepares in single deposition cycle is to the dependence of astern speed.
The aluminium lamination that Fig. 5 prepares in single deposition cycle depends on baking temperature, the relation of thickness and density
Aluminium lamination that Fig. 6 prepares in single deposition cycle uses baking temperature as parameter, when the x-radiation exposure according to experiment with by the reflectivity of model determination.
Fig. 7 aluminium multilayer uses 0 to 4 deposition cycle as parameter, when the x-radiation exposure according to experiment with by the reflectivity of model determination.
Fig. 8 a depends on number of deposition cycles, the dependence of the average gross density of aluminium multilayer.
Fig. 8 b depends on number of deposition cycles, the dependence of the individual layer average thickness of aluminium multilayer.
The dependence of the average gross density of Fig. 9 a.
The dependence of the average thickness in monolayer of Fig. 9 b
Fig. 9 c is 5 deposition cycle and in the surfaceness of the aluminium multilayer of 200 ℃ baking temperature preparation.
Wherein at Fig. 2,6,7 and 9a in the value that obtains by model according to the value and the dotted line representative of measuring of solid line representative.
Embodiment
Dull and stereotyped or the dish of making by silicon (thin slice) that in the element 1 of embodiment, relates to several centimetres of diameters with rectangle or circular contour.The thickness of element 1 is in millimeter scope or following.Its surface is that x light optics is smooth and have a roughness of 0.1 nanometer range.
In order to prepare sol-gel-pond, in an embodiment of the present invention at alkoxide-initial period as will have simultaneously before 98% purity aluminium isopropoxide adds, the divinyl propyl alcohol list ether of purity 98% is heated to 90 ℃ temperature.Add acetate in powerful mixing after 15 to 20 minutes.Once more 90 ℃ continue to mix 2 minutes after, with the colloidal suspension cools down to room temperature.The molar ratio of the alkoxide of organic solvent and acetate and initial period adds up to 40: 3: 1.
Before the at first dipping of element 1, in ultrasound wave electrolytic solution, used Ethanol Treatment about 2 minutes.On the silicon substrate of element 1, stay thin natural silicon oxide layer (following table is shown middle layer 2) with lower surfaceness.With element 1 last in above-mentioned colloidal suspension dipping and to pull out from sol-gel-pond to the predetermined speed of the scope of 4.14cm/min at 0.25cm/min.
After the impregnation steps, with the deposition film the definition temperature under (following is baking temperature) at air drying.
By aluminium oxide (Al
2O
3) graphic texture of the individual layer 3 that makes and different multilayers 5, use two, three, four, five and eight impregnation steps with final drying process (following be deposition cycle) to prepare, in Fig. 1, describe.The internal layer 2 that is made by monox at the element described in each described multilayer 51 covers.The overlapping in the above individual layer 3 that deposits, it is covered by top layer 4 under every kind of situation once more.The density of every kind of composition of multilayer 5 is the density of its dash area and for the thickness of its oblique line depth of section of density of the dash area under every kind of situation.
In each case only by the individual layer 3 of deposition cycle preparation, comprise the feature that under the baking temperature of different astern speeds and 200 ℃ and baking temperature, realizes of internal layer 2 and top layer 4, in following table 1, describe the astern speed of 0.56cm/min and 260 ℃.Wherein, as following table, t is bed thickness (nm), and σ is surfaceness (nm), and p is density (g/cm
3), v is that astern speed and T are baking temperatures.
Table 1
The individual layer 3 of multilayer 5, the feature of internal layer 2 and top layer 4 uses the astern speed of 0.56cm/min and 200 ℃ baking temperature to realize in two, three and four deposition cycle all the time, describes in table 2.The baking temperature of the astern speed of the feature of individual layer and 0.56cm/min and 200 ℃ or 260 ℃ is learnt from table 3 in five and eight deposition cycle.Because individual layer 3 and its are positioned at the feature of the top layer separately 4 under uppermost 3 layers, in table 2 and 3, summarized than multilayer overview preferably.In fact this mean, for example in four deposition cycle, produce four individual layers 3, enumerated the feature of the top layer 4 of uppermost individual layer 3, uppermost individual layer 3 itself from top to bottom, being the average characteristics of the top layer 4 and the second and the 3rd individual layer 3 itself of the second and the 3rd individual layer 3 then, is that the feature and the bottom of internal layer 2 is features of silicon cell 1 below.
Table 2
Table 3
The morphological structure of individual layer 3, especially bed thickness and density, the surface structure after use x ray reflection and the thermal treatment uses optical microscope to check.But Fig. 2 is illustrated in different astern speed v following Al by a deposition cycle preparation of every kind of situation
2O
3The reflectivity of-layer has been represented the influence of astern speed to individual layer 3.The representative of independent curve has the sol-Gel-coating process of the astern speed of increase under every kind of situation when the distance increase of curve and transverse axis.Astern speed is in the scope of 0.15-6.00cm/min, preferably in 0.25cm/min arrives the scope of 4.14cm/min.
All curves are all represented with so-called diffraction peak (Kiessig Fringes) order from big to small continuously, can determine bed thickness in accordance with known methods from its distance.Along with increasing minimum and maximum distance, astern speed reduces obviously to improve bed thickness.The pass that retreats temperature and bed thickness ties up among Fig. 4 to be described.
Cause lower average density in thicker layer at raising astern speed during the layer preparation, as from Fig. 3, inferring.Lower density represent prepared layer than porous.The pass of layer density and bed thickness ties up among Fig. 5 to be found out from the curve that descends.
Show, baking temperature to bed thickness as from Fig. 6 according to diffraction peak (kiessig Fringes) cycle that find out with further influence degree average density.In order to illustrate the influence degree of individual layer 3 has been described in Fig. 6 once more only by the reflectivity of the individual layer 3 of deposition cycle preparation.The baking temperature raising causes average density to improve like this, yet bed thickness reduces.For example be that dry temperature when 200 ℃ are brought up to 260 ℃, obtains Al
2O
3The bed thickness of-layer be in the time of 200 ℃ thickness arrive about 60%.In addition, the baking temperature raising causes surfaceness to improve.
Because the influence factor of bed thickness and layer density is known and can finely adjust, and can prepare the suitable comparable combination of features layer with different parameters thus, depend on for example base material or the influence on the internal layer 2 of the condition that further will consider under every kind of situation.
In order to prepare multilayer 5, in the above-mentioned dipping cycle, using at the table 2 and 3 according to embodiment is the astern speed and baking temperature always identical in the preparation process of multilayer 5 of 0.56cm/min all the time, repeats repeatedly.Explanation thus increases the average bed thickness reduction (Fig. 8 b) of individual layer 3 along with the continuous repeated deposition number of individual layer 3.The average thickness of individual layer 3 is because identical astern speed will be calculated from the merchant of total bed thickness and deposition cycle.Average bed thickness reduces owing to owing to the layer that will deposit at last subsequently is dry overlapping individual layer being solidified.Not only total bed thickness but also single monolayer thick can directly be measured by fast fourier transform (Fourriertransformation (FFT)) by advantageous method.FFT also provides for example layer transfer of generation in stacked of information about the reflex behavior of multilayer 5 in addition.
Simultaneously the gross density that increases multilayer 5 along with the repeat number of deposition increases that (Fig. 8 a).Can't cause apparent gross density to reduce yet above-mentioned consolidation effect is too little.Preferred this mainly owing to each in dipping and drying cycle, prepare stacked in individual layer 3 have and compare porous and so low-density thin list layer (top layer 4) with affiliated individual layer 3.The density of the top layer 4 of Chen Ji individual layer 3 has the density higher than the average density of film simultaneously at last, as individual layer preparation (Fig. 1).Feature with formation of low-density top layer 4 is interfaces reproducible and that therefore always cause density extra in each individual layer 3 to be adjusted for all aluminium films that use sol-gel-method to prepare.
Use the unbodied aluminium multilayer of the density adjustment of sol-gel process production to prove heat-staple.Its necessary thermal stability can realize in 300 ℃ to 1000 ℃ scope.The thermal stability check only obtains the result of the non-homogeneous curing of side, yet it is finished to 500 ℃ thermal treatment the time, as according in the measurement result of Fig. 9 a in the 9c, wherein described the thickness of average gross density, multilayer 5 and the surfaceness of multilayer 5 and depended on baking temperature.Compare with remainder layer, the thermal treatment that surpasses more than 500 ℃ at first causes density adjustment compensation and solidifies and increase simultaneously near the element 1 bed thickness at 1000 ℃.
Relevant literal is enumerated
1 element
2 internal layers
3 individual layers
4 top layers
5 multilayers
Claims (10)
1. preparation has the method for the element that is used for optical application of nanometer multilayer, nanometer multilayer prepares by the individual layer that sol-gel-coating process applies continuously on it, it is characterized by, the layer structure of a plurality of continuous realizations of the same material of multilayer by having minimum possible bed thickness separately realizes, each wherein continuous individual layer by element in sol-gel-pond short time dipping or with sol-gel-solution spraying on element, under predetermined temperature, in air, prepare subsequently by drying or annealing process.
2. preparation according to claim 1 has the method for the element that is used for optical application of nanometer multilayer, and it is characterized by described element is monocrystalline silicon.
3. preparation according to claim 1 has the method for the element that is used for optical application of nanometer multilayer, it is characterized by described element and is used to have the x-ray-optical system of hard and soft x ray and is used for vacuum-UV-radiation.
4. preparation according to claim 1 has the method for the element that is used for optical application of nanometer multilayer, it is characterized by analyzer-multilayer-grating that described element is used for the x ray fluorescence analysis.
5. preparation according to claim 1 has the method for the element that is used for optical application of nanometer multilayer, it is characterized by described element and is used for element in the different wavelength range radiation as the insulation light filter.
6. preparation according to claim 1 has the method for the element that is used for optical application of nanometer multilayer, it is characterized by, the astern speed of using when in the dip process of preparation individual layer element being pulled out from sol-gel-solution is different from the astern speed in the dip process of another individual layer that carries out subsequently.
7. method according to claim 1 is characterized by, use 0.25 and 4.14cm/min between astern speed element is pulled out the pond from sol-gel-solution impregnation.
8. according to claim 1 or 6 described methods, it is characterized by, with the adjustment of sol-gel-solution to about 20 ℃.
9. the described method of claim 1 is characterized by, and the drying of a plurality of individual layers or annealing process are carried out under identical or different temperature.
10. according to claim 1 or 6 described methods, it is characterized by and use Al
2O
3, TiO
2Or SiO
2Be coated with.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102005001232 | 2005-01-11 | ||
| DE102005001232.9 | 2005-01-11 |
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| Publication Number | Publication Date |
|---|---|
| CN101103313A CN101103313A (en) | 2008-01-09 |
| CN100549836C true CN100549836C (en) | 2009-10-14 |
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|---|---|---|---|
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Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP1839093A1 (en) |
| JP (1) | JP2008526480A (en) |
| CN (1) | CN100549836C (en) |
| DE (1) | DE112006000587A5 (en) |
| WO (1) | WO2006074642A1 (en) |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6409907B1 (en) * | 1999-02-11 | 2002-06-25 | Lucent Technologies Inc. | Electrochemical process for fabricating article exhibiting substantial three-dimensional order and resultant article |
| EP1152263A4 (en) * | 1999-09-30 | 2003-08-20 | Nikon Corp | Optical device with multilayer thin film and aligner with the device |
-
2006
- 2006-01-11 EP EP06705766A patent/EP1839093A1/en not_active Withdrawn
- 2006-01-11 JP JP2007549793A patent/JP2008526480A/en not_active Withdrawn
- 2006-01-11 CN CNB2006800020704A patent/CN100549836C/en not_active Expired - Fee Related
- 2006-01-11 DE DE112006000587T patent/DE112006000587A5/en not_active Withdrawn
- 2006-01-11 WO PCT/DE2006/000027 patent/WO2006074642A1/en active Application Filing
Also Published As
| Publication number | Publication date |
|---|---|
| CN101103313A (en) | 2008-01-09 |
| JP2008526480A (en) | 2008-07-24 |
| WO2006074642A1 (en) | 2006-07-20 |
| DE112006000587A5 (en) | 2007-12-27 |
| EP1839093A1 (en) | 2007-10-03 |
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