CN103901520A - Method for manufacturing triangular groove echelon gratings with 90-degree vertex angles - Google Patents
Method for manufacturing triangular groove echelon gratings with 90-degree vertex angles Download PDFInfo
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Abstract
The invention provides a method for manufacturing triangular groove echelon gratings with 90-degree vertex angles. Each triangular groove echelon grating is composed of a silicon grating structure (1), photoresist (3) and a metal film (4). A manufactured grating groove is a triangle with the vertex angle being 90 degrees, so that the diffraction efficiency higher than that of an echelon grating with the vertex angle being not 90 degrees can be achieved. Each grating structure is produced in an obliquely-cut monocrystalline wafer, the shining angles of the gratings are determined by an obliquely-cut angle for cutting each silicon wafer, and gratings with any blazing angles can be manufactured; according to the 90-degree vertex angles, grooves of silicon gratings with the vertex angles being not 90 degrees are filled with photoresist, then photoetching is conducted again, and the original silicon gratings with the vertex angles being not 90 degrees are converted into the triangular groove gratings with the vertex angles being 90 degrees. According to the manufactured grating structure, the shining face of each grating is a smooth monocrystal silicon <111> grate plane, scattering can be effectively lowered, and the diffraction efficiency of each grating is improved. The purpose that all the gratings have high diffraction efficiency on a broadband is achieved according to the fact that using wave bands can choose to be coated with various different reflecting film layers on the surfaces of the gratings.
Description
Technical field
The present invention relates to the dispersion element field using in a kind of spectral instrument, be specifically related to a kind of method for making of the echelon grating using to the echelle spectrograph of infrared band for visible ray.
Background technology
Fast-developing echelle spectrograph in recent years, utilize echelon grating for principal dispersion element, be aided with horizontal dispersion element and carry out level time separation, record the spectral line of wide spectral range (visible ray is to infrared) with area array CCD simultaneously, whole system volume is little, operating wavelength range is wide, and linear dispersion is high, and resolution is high.Echelon grating, as a kind of specific type of blazed grating, uses " minor face " of groove with the common blazed grating key distinction while being echelon grating work, blazing angle is greater than 45 ° conventionally.
For the spectral instrument taking grating as dispersion element, dispersive power and resolution are the important parameters that characterizes its optical characteristics.Linear dispersion:
Grating resolution:
Wherein, d is grating constant, and m is spectral order, and N is grating lines sums, f represents the focusing length of spectrometer, and β represents angle of diffraction, and the distance dl that wavelength X and λ+d λ two spectral lines separate on focal plane is larger, linear dispersion is larger, and resolution is higher, and spectrometer performance is better.In order to improve dispersive power and the resolution of spectrometer, one method is to reduce grating constant, expand area of raster to increase grid stroke number N, make the blazed grating of large area high linear density, this is echelon grating early stage of development common method, difficulty is large, and the raising of grid stroke density and area is limited.Other method is to use large period (being conventionally greater than 10 microns) blazed grating, i.e. echelon grating.Echelon grating can glitter at senior time (m) with larger angle of diffraction (β) at wide spectral range, and the grating cycle is made greatly and easily large-area optical grating construction (increase grating cutting and count N), and result will obtain higher linear dispersion and resolution.Therefore, echelon grating is in fact a kind of coarse grating, and incisure density is less than 100 lines per millimeters, has larger blazing angle, can, for very high order of interference, have high resolution.Common grating is to improve dispersive power by increasing focal distance f, and echelon grating is by increasing blazing angle β (50 °～70 °), utilizes high spectral order time m (40～120 grades) to improve linear dispersion.Current existing document: document 1:G.R.Harrison, " The Production of Diffraction Gratings:II.The Design of Echelle Gratings and Spectrographs; " J.Opt.Soc.Am.39,522-527 (1949). the design to echelon grating and use mechanical scratching are made echelon grating technology and are introduced.Document 2: the making of echelette diffraction grating and evaluation (U.U.Graf, D.T.Jaffe, E.J.Kim, J.H.Lacy, H.Ling, J.T.Moore, and G.Rebeiz, " fabrication and evaluation of an etched infrared diffration grating ", Applied Optics33,96-102 (1994)) to introduce use anisotropic wet etch made echelon grating in <100> silicon base, grating grooved is isosceles triangle, 55 ° of blazing angles, 70.53 ° of drift angles.Document 3: the infrasil prism (D.J.Mar that is manufactured with microstructure, J.P.Marsh, C.P.Deen, H.Ling, H.Choo, and D.T.Jaffe, " Micromachined silicon grisms for infrared optics, " Applied Optics48, 1016-1029 (2009) .) propose silicon to make prism as infrared band dispersion element, on one side of silicon prism, still use anisotropic wet etch in <100> silicon base, to make echelon grating structure, three kinds of blazing angles are obtained by different cutting angles: 6.16 °, 54.7 ° and 63.4 ° of echelon gratings, 70.53 ° of drift angles.Document 4: use echelon grating to TE and TM polarized light realize perfection glitter (Kleemann B H.Perfect blazing with echelle gratings in TE and TM polarization[J] .Optics letters, 37 (6): 1002-10042012.), introduce for echelon grating, realize perfect two necessary conditions of glittering: the drift angle of triangle grooved is 90 °, and the higher order of diffraction time of the order of diffraction while not existing than autocollimation incident.Echelon grating is the core parts of echelon grating spectrometer, and high-diffraction efficiency is the target of pursuing in echelon grating evolution.According to document 4, whether the drift angle of the echelon grating of triangle grooved is 90 ° will directly affect and whether can obtain perfection and glitter, as a of Fig. 1, b, shown in c, drift angle is that the diffraction efficiency of triangle grooved (as shown in the b of Fig. 1) at right angle is compared with the triangle grooved of 70.5 ° of drift angles (as shown in the c of Fig. 1) height.The mechanical scratching grating of introducing in document 1, grooved drift angle approximate right angle, but the face that glitters that delineation produces is coarse, and fabrication cycle is long.Document 2 is introduced on <100> silicon chip with document 3, make the echelon grating taking (111) lattice plane as the face of glittering, surfacing is smooth, reduce the scattering of light, but drift angle is not 90 ° of desirable angles, has limited the further raising of diffraction efficiency of grating.
Summary of the invention
Technology of the present invention is dealt with problems: overcome the deficiencies in the prior art, the method for making of 90 ° of vee gutter echelon gratings of a kind of drift angle is provided, to improve grating at the inferior diffraction efficiency 3%-19% of level that glitters; Manufacturing process is simple simultaneously.
Technical solution of the present invention;
Propose first to use photoetching technique in silicon echelon grating structure, produce the triangle echelon grating of 90 ° of drift angles, still with silicon (111) lattice plane of natural formation for the face of glittering, when blazing angle can be by cutting silicon chip, the angle of new surperficial original surface is cut drift angle and is controlled.Can obtain any blazing angle, and drift angle is the echelon grating of 90 °, will further improves grating in the diffraction efficiency for level time of glittering.
Operation steps of the present invention is as follows:
The monocrystalline silicon piece that the 1st step, preparation are cut sth. askew; Described can be common <110> or <100> monocrystalline silicon piece for the monocrystalline silicon piece of cutting sth. askew, and its surface is parallel with (110) lattice plane or (100) lattice plane respectively.The described monocrystalline silicon piece of cutting sth. askew refers to common <110> or <100> type monocrystalline silicon piece is cut, there is an angle on new surface with original surface (or the lattice plane paralleling with original surface), cuts drift angle.Cut drift angle according to monocrystalline silicon piece crystal orientation and made echelon grating flare angle θ
bdetermine.
The 2nd step, on monocrystalline silicon piece, be coated with 20-100nm silicon nitride (SiN cutting sth. askew
x) film;
The 3rd step, coating photoresist:
Use spin coating method on silicon nitride film, to be coated with the photoresist layer of 0.1-1 μ m thickness;
The 4th step, making photoresist mask graph:
Use has the mask of predetermined period (as 12.658 microns, corresponding grid stroke rod density 79 lines per millimeters) raster graphic, obtains photoresist grating figure by lithography steps such as exposure, development, oven dry;
The 5th step, etch silicon nitride:
Taking photoresist as mask, use reactive ion etching silicon nitride film layer, photoresist grating figure is translated into silicon nitride grating mask figure.
The 6th step, wet etching silicon:
Taking silicon nitride as mask, use the alkaline solutions such as potassium hydroxide solution (KOH) or TMAH, anisotropic etching silicon, forms silicon grating structure;
The 7th step, removal remaining nitride silicon layer:
Use hydrofluorite (HF) to soak and remove silicon nitride;
The 8th step, linear grating groove fill photoresist:
On silicon echelon grating, being coated with photoresist, is in linear grating groove, to fill up photoresist;
The 9th step, canted exposure:
The optical grating construction that groove is filled up to photoresist tilts to be placed in ultraviolet light field, and the inner point photoresist of part groove is exposed, exposure light and grating normal angle, and incident angle equals blaze of grating angle;
The 10th step, development:
After exposure, develop, use 0.5% sodium hydroxide solution to dissolve the photoresist being exposed, acquisition drift angle is the triangle grooved echelon grating structure of 90 °;
The 11st step, aluminize at grating surface, gold or other reflection horizon:
On echelon grating, be coated with aluminium, gold or other reflectance coating, Coating Materials uses wave band to determine according to grating.
Described silicon nitride film can pass through low pressure gas phase deposition; or plasma enhanced chemical vapor deposition (PECVD); also can make by magnetron sputtering; as the mask material of strong base solution etch silicon; thickness can protective covering cap part when ensureing wet etching silicon silicon be advisable, suggest thickness 20-100nm.
Described in step 2, photoresist can be positive photoresist (being called for short positive glue), can be also negative photoresist (being called for short negative glue), needs to determine according to figure on lay photoetching mask plate and making.The photoresist of filling described in step 7 is positive photoresist.
The condition of described etch silicon nitride: reactive ion beam etching (RIBE), reacting gas---carbon tetrafluoride, air pressure 0.5-1.5Pa, self-bias 100-200V, the time is more than or equal to 30 seconds.
The condition of described etch silicon: potassium hydroxide solution, concentration 50%, temperature is determined according to etch rate, 20 DEG C to 85 DEG C, 80 DEG C time at silicon wafer to <110> direction etch rate approximately 1.2 μ m/min, at silicon wafer to <100> direction etch rate approximately 1.4 μ m/min.Etching depth is definite according to grating cycle and blazing angle, to 79 lines/mm, and 55 ° of blazing angles, the degree of depth should be greater than 5.95 μ m, about 5 minutes of etching time.
Described removal silicon nitride condition: 10-39%HF solution, time 1-5 minute, also can select dry etching, as reactive ion etching (RIE) is removed silicon nitride.
Described canted exposure condition: after channel portions is filled photoresist, directly, in placement and ultraviolet light field, without mask, between incident ray and grating normal, angle is that angle of inclination equals blaze of grating angle.Time shutter determines according to exposure field energy density and photoresist thickness.
Described development conditions: make manufacturer provides with photoresist special developer solution or 0.5% NaOH (NaOH) aqueous solution carry out at normal temperatures development operation, developer endpoint is chosen in part photoresist to be removed (align glue, be exposed part) remove completely till.
Described plating reflectance coating condition: reflective film material, with aluminium or Jin Weizhu, in the normal aluminium of visible light wave range, is often selected gold at infrared band.Plated film mode is selected physical coating mode, comprises evaporation or sputter coating.
The present invention's useful technique effect is compared with prior art: the present invention uses ultraviolet photolithographic and wet etching silicon technology to make echelon grating, and method for making is ripe and simple, and fabrication cycle is short.The triangle grooved echelon grating of made, not only blaze of grating face is smooth silicon crystal lattice face, and easily obtain the triangular groove of 90 ° of drift angles, has met one of condition that echelon grating perfection glitters.The present invention and conventional art are different, make triangle grooved echelon grating although also utilized monocrystalline silicon, but filling gluing photoetching are again increased, having changed the echelon grating groove drift angle that in the past uses wet etching silicon technology to make is not all the present situation of 90 °, meet one of perfect condition of glittering of acquisition in document 4, to obtain than document 2 the high diffraction efficiency of triangle grooved grating of 70.5 ° of drift angles in document 3.Used in the present invention can be common <100> or <110> monocrystalline silicon piece for the monocrystalline silicon piece of cutting sth. askew, when cutting silicon wafer, select as required different inclination angle, can realize the echelon grating of any flare angle and make.
In a word, the optical grating construction that adopts made of the present invention, blaze of grating face is smooth monocrystalline silicon <111> lattice plane, can effectively reduce scattering, and realized the making of the vee gutter echelon grating of 90 ° of drift angles, will improve diffraction efficiency of grating.According to using wave band can select to be coated with variety classes reflective coating at grating surface, realize grating and all there is high-diffraction efficiency in broadband.
Brief description of the drawings
Fig. 1 calculates to obtain isosceles triangle grooved ladder and the inferior diffraction efficiency of blaze of grating level that drift angle is 70.5 ° of triangle grooved and the drift angles of 90 °; Wherein a is the triangle grooved of 90 °; , b is the isosceles triangle grooved ladder of 70.5 ° of drift angles, c is that drift angle is the isosceles triangle grooved echelon grating of 70.5 ° of the triangle grooved of 90 ° and the drift angles grade inferior diffraction efficiency of glittering;
Fig. 2 is echelon grating making step process flow diagram of the present invention;
Fig. 3 is the <110> silicon chip of cutting sth. askew used in the present invention, figure acceptance of the bid understands the relativeness of silicon chip new surface and inner (110) and (111) lattice plane after cutting sth. askew, and on new surface and (110) lattice plane angle α numerical value, equals 90 °-θ
b, θ
bfor blaze of grating angle.
Fig. 4 is plating silicon nitride (SiNx) film during the inventive method is made;
Fig. 5 is the coating photoresist during the inventive method is made;
Fig. 6 be the inventive method make in optical graving for photoresist grating mask graph;
Fig. 7 is the etch silicon nitride during the inventive method is made;
Fig. 8 be during the inventive method is made taking silicon nitride as mask, wet etching silicon, forms parallelogram grooved silicon grating;
Fig. 9 is the removal remaining silicon nitride during the inventive method is made;
Figure 10 is again coated with after photoresist during the inventive method is made on silicon grating, has been filled photoresist in groove;
Figure 11 is to filling up the optical grating construction of the photoresist uv-exposure that tilts in groove during the inventive method is made;
Figure 12 develops to silicon grating structure after canted exposure during the present invention makes, and obtains the triangle grooved optical grating construction of 90 ° of drift angles;
Figure 13 is the surface sweeping electron micrograph that the present invention makes the triangle grooved optical grating construction of 90 ° of drift angles of drift angle of acquisition;
Figure 14 be the inventive method make on 90 ° of drift angle triangle grooved optical grating constructions, be coated with reflection horizon, the kind in reflection horizon according to echelon grating use wave band determine.
Figure 15 is the silicon echelon grating diffraction efficiency comparison of 70.53 ° of the drift angles that uses the making of <100> monocrystalline silicon in 90 ° of drift angles and document 2, document 3 during the inventive method is made, 90 ° of drift angle diffraction efficiency of grating that the present invention makes, compared with 70.53 ° of high 6%-19% of drift angle grating, are measured wavelength 1.5-1.6 μ m.
Figure 16, for selecting the <100> monocrystalline silicon piece of cutting sth. askew, uses the schematic diagram of cutting drift angle and lattice plane of silicon chip in the inventive method making.
Figure 17 is for selecting the <100> monocrystalline silicon piece of cutting sth. askew, the inventive method make in taking silicon nitride as mask, wet etching silicon, forms the triangle grooved silicon grating of 70.53 ° of drift angles;
Figure 18 is for selecting the <100> monocrystalline silicon piece of cutting sth. askew, and the inventive method is removed remaining silicon nitride in making;
Figure 19 is for selecting the <100> monocrystalline silicon piece of cutting sth. askew, and the inventive method is again coated with after photoresist in making on silicon grating, has been filled photoresist in groove;
Figure 20 is for selecting the <100> monocrystalline silicon piece of cutting sth. askew, the inventive method make in to filling up the optical grating construction of the photoresist uv-exposure that tilts in groove;
Figure 21 is for selecting the <100> monocrystalline silicon piece of cutting sth. askew, and the present invention develops to silicon grating structure after canted exposure in making, and obtains the triangle grooved optical grating construction of 90 ° of drift angles;
Figure 22 is for selecting the <100> monocrystalline silicon piece of cutting sth. askew, and the inventive method is coated with reflection horizon in making on 90 ° of drift angle triangle grooved optical grating constructions, and the kind in reflection horizon is used wave band to determine according to echelon grating.
Figure 23 is during the inventive method is made, the use <110> monocrystalline silicon piece of cutting sth. askew, 70.53 ° of 90 ° of drift angles, the 76 ° of blazing angle echelon gratings of making and the drift angles that uses the making of <100> monocrystalline silicon, the silicon echelon grating diffraction efficiency comparison that blazing angle is 76 °, 90 ° of drift angle diffraction efficiency of grating that the present invention makes, compared with 70.53 ° of high 6%-14% of drift angle grating, are measured wavelength 1.5-1.6 μ m.
Figure 24 is during the inventive method is made, the use <100> monocrystalline silicon piece of cutting sth. askew, 90 ° of drift angles making, 54.47 ° of blazing angle echelon gratings and 70.53 ° of drift angles that use <100> monocrystalline silicon to make, the silicon echelon grating diffraction efficiency comparison of 54.47 ° ° of blazing angles, 90 ° of drift angle diffraction efficiency of grating that the present invention makes, compared with 70.53 ° of high 3%-11% of drift angle grating, are measured wavelength 1.5-1.6 μ m.
Figure 25 is during the inventive method is made, the use <100> monocrystalline silicon piece of cutting sth. askew, 90 ° of drift angles making, 76 ° of blazing angle echelon gratings and 70.53 ° of drift angles that use <100> monocrystalline silicon to make, the silicon echelon grating diffraction efficiency comparison of 76 ° of blazing angles, 90 ° of drift angle diffraction efficiency of grating that the present invention makes, compared with 70.53 ° of high 5%-17% of drift angle grating, are measured wavelength 1.5-1.6 μ m.
Embodiment
Before setting forth the present invention, relational language is described.
The <> using in the present invention is the symbol for representing crystal orientation, () is used for representing lattice plane, the direction (being crystal orientation) of a lattice plane refers to the normal direction of this lattice plane, as <110> refers to the normal direction of (110) lattice plane.
Below in conjunction with accompanying drawing, by embodiment, the invention will be further described.
Echelon grating preparation method comprises following operation steps, sees Fig. 2;
The <110> monocrystalline silicon piece 1 that selection is cut sth. askew, in order to make the echelon grating of 54.7 ° of blazing angles, cut silicon chip surface after cut sth. askew drift angle and the original surface of <110> monocrystalline silicon piece, (110) lattice plane angle α equals 35.3 °, sees Fig. 3;
Use low-pressure chemical vapor deposition (LPCVD) on silicon chip, to be coated with silicon nitride (SiNx) film 2 of thickness 50nm, see Fig. 4;
Use spin coating method on silicon nitride film, to be coated with the positive photoresist 3 of thickness 200nm, see Fig. 5, photoresist thickness is determined according to silicon nitride thickness, need to be greater than the thickness of silicon nitride film layer 2, selects 100-1000nm;
Use mask to expose on ultraviolet photolithographic machine, by developing, the steps necessary of a series of photoetching techniques such as oven dry obtains the photoresist relief pattern consistent with figure on mask, ensure to expose silicon nitride 2 between photoresist grating lines, see Fig. 6, on mask, there is cycles 12.658 μ m, line density 79 lines/mm, the grating lines chrome mask figure of spacing 10 μ m;
Carry out after photoresist mask graph, carry out reactive ion etching (RIE) silicon nitride film, reacting gas carbon tetrafluoride (CF4), 2 minutes time (etching condition: air pressure 0.5Pa, radio-frequency power 100W, bias voltage 100V), obtain the silicon nitride mask graph 2 that has residue photoresist to cover, see Fig. 7;
Use 50% potassium hydroxide (KOH) solution to soak, etch silicon 1, forms parallelogram channeled grating structure, has remaining silicon nitride 2 to cover on grating lines, sees Fig. 8.Soak time and solution concentration and temperature correlation, 80 DEG C of 50%KOH solution, the about 6min of etching time.
Use hydrofluorite (HF) solution: 39%HF, soak time 10min (silicon nitride thickness 50nm); Remove remaining silicon nitride 2, obtain silicon grating structure, see Fig. 9.
On silicon grating, be again coated with photoresist, make to fill up photoresist completely in linear grating groove, as Figure 10;
Then, to filling up the silicon grating structure canted exposure of photoresist in groove, on exposing light beam and grating normal angle numerical value, equal 54.7 °, blaze of grating angle, see Figure 11;
After canted exposure, develop, use 0.5% sodium hydrate aqueous solution, the photoresist that is exposed part is dissolved, obtain 54.7 ° of blazing angles, drift angle is the vee gutter echelon grating structure of 90 °, sees Figure 12 and Figure 13;
The last aluminium film 4 that plates thickness 100nm on silicon grating 1, as reflection horizon, is shown in Figure 14, improves diffraction efficiency of grating.Plated film mode: thermal evaporation is aluminized, thickness 200nm.
After aluminizing with document 2, document 3, use the silicon echelon grating diffraction efficiency comparison of 70.53 ° of the drift angles that <100> monocrystalline silicon makes, 90 ° of drift angle diffraction efficiency of grating that the present invention makes are compared with 70.53 ° of high 6%-19% of drift angle grating, measure wavelength 1.5-1.6 μ m, see Figure 15.
The <110> monocrystalline silicon piece 1 that selection is cut sth. askew, makes 76 ° of blazing angles, cuts silicon chip surface and original surface after cut sth. askew drift angle, and (110) lattice plane angle α equals 14 °, sees Fig. 3;
Use low-pressure chemical vapor deposition (LPCVD) on silicon chip, to be coated with silicon nitride (SiNx) film 2 of thickness 50nm, see Fig. 4;
Use spin coating method on silicon nitride film, to be coated with the positive photoresist 3 of thickness 100nm, see Fig. 5, photoresist thickness is determined according to silicon nitride thickness, need to be greater than the thickness of silicon nitride film layer 2, selects 100-1000nm;
Use mask to expose on ultraviolet photolithographic machine, by developing, the steps necessary of a series of photoetching techniques such as oven dry obtains the photoresist relief pattern consistent with figure on mask, ensure to expose silicon nitride 2 between photoresist grating lines, see Fig. 6, on mask, there is cycles 12.658 μ m, line density 79 lines/mm, the grating lines chrome mask figure of spacing 10 μ m;
Carry out after photoresist mask graph, carry out reactive ion etching (RIE) silicon nitride film, reacting gas carbon tetrafluoride (CF4), 2 minutes time (etching condition: air pressure 0.5Pa, radio-frequency power 100W, bias voltage 100V), obtain the silicon nitride mask graph 2 that has residue photoresist to cover, see Fig. 7;
Use 50% potassium hydroxide (KOH) solution to soak, etch silicon 1, forms parallelogram channeled grating structure, has remaining silicon nitride 2 to cover on grating lines, sees Fig. 8.Soak time and solution concentration and temperature correlation, 80 DEG C of 50%KOH solution, the about 6min of etching time.
Use hydrofluorite (HF) solution: 39%HF, soak time 10min (silicon nitride thickness 50nm); Remove remaining silicon nitride 2, obtain silicon grating structure, see Fig. 9.
On silicon grating, be again coated with photoresist, make to fill up photoresist completely in linear grating groove, as Figure 10;
Then, to filling up the silicon grating structure canted exposure of photoresist in groove, on exposing light beam and grating normal angle numerical value, equal 76 °, blaze of grating angle, see Figure 11;
After canted exposure, develop, use 0.5% sodium hydrate aqueous solution, the photoresist that is exposed part is dissolved, obtain 76 ° of blazing angles, drift angle is the vee gutter echelon grating structure of 90 °, sees Figure 12;
The last aluminium film 4 that plates thickness 100nm on silicon grating 1, as reflection horizon, is shown in Figure 14, improves diffraction efficiency of grating.Plated film mode: thermal evaporation is aluminized, thickness 200nm.
The inferior diffraction efficiency of autocollimation level after measurement is aluminized and the silicon echelon grating diffraction efficiency comparison of 70.53 ° of the drift angles that uses <100> monocrystalline silicon to make, 90 ° of drift angle diffraction efficiency of grating that the present invention makes are compared with 70.53 ° of high 6%-14% of drift angle grating, measure wavelength 1.5-1.6 μ m, see Figure 23.
Select <100> monocrystalline silicon piece 1, because <100> silicon chip surface equals 54.7 ° with (111) face angle α, cut drift angle cut sth. askew after new surface and the original surface of silicon chip, (100) lattice plane angle α equals 0 °, sees Figure 16;
Use low-pressure chemical vapor deposition (LPCVD) on silicon chip, to be coated with silicon nitride (SiNx) film 2 of thickness 50nm, see Fig. 4;
Use spin coating method on silicon nitride film, to be coated with the positive photoresist 3 of thickness 100nm, see Fig. 5, photoresist thickness is determined according to silicon nitride thickness, need to be greater than the thickness of silicon nitride film layer 2, selects 100-1000nm;
Use mask to expose on ultraviolet photolithographic machine, by developing, the steps necessary of a series of photoetching techniques such as oven dry obtains the photoresist relief pattern consistent with figure on mask, ensure to expose silicon nitride 2 between photoresist grating lines, see Fig. 6, on mask, there is cycles 12.658 μ m, line density 79 lines/mm, the grating lines chrome mask figure of spacing 10 μ m;
Carry out after photoresist mask graph, carry out reactive ion etching (RIE) silicon nitride film, reacting gas carbon tetrafluoride (CF4), 2 minutes time (etching condition: air pressure 0.5Pa, radio-frequency power 100W, bias voltage 100V), obtain the silicon nitride mask graph 2 that has residue photoresist to cover, see Fig. 7;
Use 50% potassium hydroxide (KOH) solution to soak, etch silicon 1, forms isosceles triangle channeled grating structure, and 70.53 ° of drift angles, have remaining silicon nitride 2 to cover on grating lines, see Figure 17.Soak time and solution concentration and temperature correlation, 80 DEG C of 50%KOH solution, the about 6min of etching time.
Use hydrofluorite (HF) solution: 39%HF, soak time 10min (silicon nitride thickness 50nm); Remove remaining silicon nitride 2, obtain silicon grating structure, see Figure 18.
On silicon grating, be again coated with photoresist, make to fill up photoresist completely in linear grating groove, as Figure 19;
Then, to filling up the silicon grating structure canted exposure of photoresist in groove, on exposing light beam and grating normal angle numerical value, equal 54.7 °, blaze of grating angle, see Figure 20;
After canted exposure, develop, use 0.5% sodium hydrate aqueous solution, the photoresist that is exposed part is dissolved, obtain 54.7 ° of blazing angles, drift angle is the vee gutter echelon grating structure of 90 °, sees Figure 21;
The last aluminium film 4 that plates thickness 100nm on silicon grating 1, as reflection horizon, is shown in Figure 22, improves diffraction efficiency of grating.Plated film mode: thermal evaporation is aluminized, thickness 200nm.
Autocollimation level after measurement is aluminized time diffraction efficiency, 90 ° of drift angle diffraction efficiency of grating that the present invention makes are compared with 70.53 ° of drift angles, and 54.7 ° of high 3%-11% of grating of blazing angle, measure wavelength 1.5-1.6 μ m, see Figure 24.
Select <100> monocrystalline silicon piece 1, because <100> silicon chip surface equals 54.7 ° with (111) face angle α, cut drift angle cut sth. askew after the new surface of silicon chip be that (100) lattice plane angle α equals 21.3 ° with original surface, see Figure 16;
Use low-pressure chemical vapor deposition (LPCVD) on silicon chip, to be coated with silicon nitride (SiNx) film 2 of thickness 50nm, see Fig. 4;
Use spin coating method on silicon nitride film, to be coated with the positive photoresist 3 of thickness 300nm, see Fig. 5, photoresist thickness is determined according to silicon nitride thickness, need to be greater than the thickness of silicon nitride film layer 2, selects 100-1000nm;
Use mask to expose on ultraviolet photolithographic machine, by developing, the steps necessary of a series of photoetching techniques such as oven dry obtains the photoresist relief pattern consistent with figure on mask, ensure to expose silicon nitride 2 between photoresist grating lines, see Fig. 6, on mask, there is cycles 12.658 μ m, line density 79 lines/mm, the grating lines chrome mask figure of spacing 10 μ m;
Carry out after photoresist mask graph, carry out reactive ion etching (RIE) silicon nitride film, reacting gas carbon tetrafluoride (CF4), 2 minutes time (etching condition: air pressure 0.5Pa, radio-frequency power 100W, bias voltage 100V), obtain the silicon nitride mask graph 2 that has residue photoresist to cover, see Fig. 7;
Use 50% potassium hydroxide (KOH) solution to soak, etch silicon 1, forms triangle grooved optical grating construction, and 70.53 ° of drift angles, have remaining silicon nitride 2 to cover on grating lines, see Figure 17.Soak time and solution concentration and temperature correlation, 80 DEG C of 50%KOH solution, the about 6min of etching time.
Remove remaining silicon nitride 2, obtain silicon grating structure, see Figure 18.Use hydrofluorite (HF) solution: 39%HF, soak time 10min (silicon nitride thickness 50nm);
On silicon grating, be again coated with photoresist, make to fill up photoresist completely in linear grating groove, as Figure 19;
Then, to filling up the silicon grating structure canted exposure of photoresist in groove, on exposing light beam and grating normal angle numerical value, equal 54.7 °, blaze of grating angle, see Figure 20;
After canted exposure, develop, use 0.5% sodium hydrate aqueous solution, the photoresist that is exposed part is dissolved, obtain 76 ° of blazing angles, drift angle is the vee gutter echelon grating structure of 90 °, sees Figure 21;
The last aluminium film 4 that plates thickness 100nm on silicon grating 1, as reflection horizon, is shown in Figure 22, improves diffraction efficiency of grating.Plated film mode: thermal evaporation is aluminized, thickness 200nm.
Autocollimation level after measurement is aluminized time diffraction efficiency, silicon echelon grating diffraction efficiency comparison with 70.53 ° of the drift angles that uses <100> monocrystalline silicon to make, 90 ° of drift angle diffraction efficiency of grating that the present invention makes are compared with 70.53 ° of drift angles, 76 ° of high 5%-17% of grating of blazing angle, measure wavelength 1.5-1.6 μ m, see Figure 25.
In a word, the present invention proposes the <110> or the <100> monocrystalline silicon piece that use inclined cut, by gluing again, canted exposure and development, the triangle grooved grating that making drift angle is right angle, and the face of glittering is silicon (111) lattice plane, surfacing is smooth, take into account the advantage of two kinds of main Types echelon gratings up to now, therefore the present invention is not increasing on the basis of manufacture difficulty, propose a kind of simple, novel and grating is in the high echelon grating method for making of diffraction efficiency of level time of glittering, on conventional monocrystalline silicon piece, realize echelon grating and obtained one of perfect condition of glittering---the triangle grooved that drift angle is 90 °.
Non-elaborated part of the present invention belongs to techniques well known.
The above; be only part embodiment of the present invention, but protection scope of the present invention is not limited to this, in the technical scope that any those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.
Claims (9)
1. a method for making for 90 ° of vee gutter echelon gratings of drift angle, is characterized in that step is as follows:
The monocrystalline silicon piece that the 1st step, preparation are cut sth. askew;
The 2nd step, on the described monocrystalline silicon piece of cutting sth. askew, be coated with 20-100nm silicon nitride (SiN
x) film;
The 3rd step, on described silicon nitride film, be coated with the photoresist layer of 100-1000nm thickness, the thickness of described photoresist layer is greater than silicon nitride (SiN
x) thickness of rete;
The 4th step, on the silicon chip of described coating photoresist layer, adopt and have the mask of predetermined period raster graphic, by lithographic process steps such as exposure, developments, in described photoresist layer, obtain photoresist grating figure;
The 5th step, taking described photoresist grating figure as mask, etch silicon nitride rete, translates into silicon nitride raster graphic by photoresist grating figure;
The 6th step, taking described silicon nitride raster graphic as mask, use potassium hydroxide solution (KOH) or TMAH alkaline solution, anisotropic etching silicon, forms the silicon grating structure that top has remaining silicon nitride to cover;
The 7th step, the silicon grating structure that has remaining silicon nitride to cover on described top are put into hydrofluorite (HF) solution, remove remaining silicon nitride, obtain silicon grating structure;
The 8th step, in described silicon grating structure, resist coating, fills linear grating groove, obtains the silicon grating structure of filling up photoresist in groove;
The 9th step, to described silicon grating structure canted exposure of filling up photoresist, on incident ray and grating normal angle numerical value, equal blazing angle, after developing, obtain the vee gutter optical grating construction of 90 ° of drift angles;
The 10th step, on described 90 ° of drift angle vee gutter optical grating constructions, plate thickness and be greater than 100nm metal film, obtain 90 ° of drift angle vee gutter echelon gratings.
2. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, it is characterized in that: in described the 1st step, be <110> or <100> monocrystalline silicon piece for the monocrystalline silicon piece of cutting sth. askew, its surface is parallel with (110) lattice plane or (100) lattice plane respectively; The described monocrystalline silicon piece of cutting sth. askew refers to common <110> or <100> type monocrystalline silicon piece is cut, the lattice plane that new surface parallels with original surface or with original surface has an angle, cuts drift angle; Cut drift angle according to monocrystalline silicon piece crystal orientation and made echelon grating flare angle θ
bdetermine.
3. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, is characterized in that: the photoresist in described the 3rd step is positive photoresist, or negative photoresist.
4. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, it is characterized in that: the condition of the etch silicon nitride rete in described the 5th step: adopt reactive ion etching (RIE), reacting gas carbon tetrafluoride (CF4), air pressure 0.1-1.5Pa, radio-frequency power 50-300W self-bias 100-200V, the time is more than or equal to 30 seconds.
5. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, it is characterized in that: the condition of the anisotropic etching silicon in described the 6th step is: adopt potassium hydroxide solution or TMAH solution, concentration 20%-60%, temperature is determined according to etch rate, 20 DEG C-85 DEG C, 80 DEG C time, silicon is at <110> direction etch rate approximately 1.2 μ m/min; Etching depth is definite according to grating cycle and blazing angle, to linear grating groove density 79 lines/mm, and 55 ° of blazing angles, the degree of depth should be greater than 5.95 μ m, etching time 5 minutes.
6. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, is characterized in that: the described removal silicon nitride condition in described the 7th step: 10%-40%HF solution, time 2-20 minute.
7. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, is characterized in that: the photoresist in described the 8th step is positive photoresist, and the thickness of the photoresist of filling equals the linear grating groove degree of depth.
8. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, it is characterized in that: in described the 9th step to described silicon grating structure canted exposure of filling up photoresist, do not need mask, directly use the uniform ultraviolet source exposure of light intensity.
9. the method for making of 90 ° of vee gutter echelon gratings of drift angle according to claim 1, is characterized in that: the reflectance coating being coated with in described the 10th step is determined according to echelon grating service band, uses aluminium film at visible light wave range, uses golden film at infrared band; The method that is coated with reflectance coating is thermal evaporation plated film or sputter coating.
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