CN109782384A - Novel critical angle transmission grating production method - Google Patents
Novel critical angle transmission grating production method Download PDFInfo
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- CN109782384A CN109782384A CN201811597429.8A CN201811597429A CN109782384A CN 109782384 A CN109782384 A CN 109782384A CN 201811597429 A CN201811597429 A CN 201811597429A CN 109782384 A CN109782384 A CN 109782384A
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Abstract
The invention discloses a kind of novel critical angle transmission grating production methods, comprising the following steps: S1, in monocrystal silicon substrate double-sided deposition silicon nitride layer, then in silicon nitride layer chrome-faced, two-sided spin coating photoresist again, after uv-exposure, development, wet etching chromium obtains benchmark grating；S2, in the two-sided spin coating photoresist of benchmark grating, obtain grating exposure mask after the exposure of scanning interferometer field exposure system, development；The silicon nitride layer of S3, then dry etching grating exposure mask, wet etching monocrystalline silicon remove silicon nitride layer finally to get transmission grating.Novel critical angle transmission grating production method of the invention makes monocrystalline silicon grating exposure mask by techniques such as two-sided chromium plating, two-sided spin coating photoresist, double-sided exposures.Then two-way simultaneous carries out wet etching to monocrystalline silicon using alkaline etch bath, can reduce grating stretching area, realizes the promotion of grating aperture opening ratio.
Description
Technical field
The present invention relates to grating preparation technical fields.It is more particularly related to a kind of novel critical angle transmission
Preparing grating method.
Background technique
The cosmic background radiations detecting devices such as China's existing " insight ", " realizing sky " and " day eye " are that have for detection
The astrophysics developments such as black hole, neutron star and the new pulsar of high-energy.Above equipment can be to the hard X ray of stronger energy
(20keV-250keV), gamma-rays (> 1240keV), high energy electron (5 × 107keV-1×1011KeV) and radio wave is visited
It surveys.But does not have and the full spectral coverage detectivity of high-resolution is carried out to the lower grenz ray of energy (0.2keV-2keV).Space
Contain the elemental characteristic spectral line largely with energy spectrum analysis value such as carbon, helium, oxygen, neon and iron in grenz ray, it is interspace to studying
Between and inner material composition, Celestial Objects and ambient substance composition, large scale structure of the universe variation and the astronomy such as baryon search
Important scientific problems have high scientific value.In order to improve the energy transmission and energy spectral resolution that grenz ray penetrates spectrometer, Europe
1 to the 4 generation soft X-ray telescope that Mei Deng state develops using grating as beam splitter, wherein 1,2 it is alternative be that glancing incidence is gold-plated
Reflecting grating, the IXO and Lynx for intending transmitting in 2021 and 2035 then use critical angle monocrystalline silicon transmission grating, and diffraction efficiency can
It is increased to 50% or so by original 15%, resolution ratio can be increased to 10000 by original 40.China carries out space grenz ray
High-resolution detection first has to solve to restrict the big depth-to-width ratio for carrying out the research, critical angle monocrystalline silicon transmission grating " bottleneck "
Problem.So it is significant to seek a kind of novel critical angle transmission grating production method.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of novel critical angle transmission grating production methods, pass through two-sided plating
The techniques such as chromium, two-sided spin coating photoresist, double-sided exposure make monocrystalline silicon grating exposure mask.Then two-way simultaneous utilizes alkaline etch bath
Wet etching is carried out to monocrystalline silicon, grating stretching area can be reduced, realizes the promotion of grating aperture opening ratio.
In order to realize these purposes and other advantages according to the present invention, a kind of novel critical angle transmission grating is provided
Production method, comprising the following steps:
S1, in monocrystal silicon substrate double-sided deposition silicon nitride layer, then in silicon nitride layer chrome-faced, then two-sided spin coating photoetching
Glue, after uv-exposure, development, wet etching chromium obtains benchmark grating；
S2, in the two-sided spin coating photoresist of benchmark grating, obtain grating after the exposure of scanning interferometer field exposure system, development and cover
Film；
The silicon nitride layer of S3, then dry etching grating exposure mask, wet etching monocrystalline silicon finally remove silicon nitride layer, i.e.,
Obtain transmission grating.
Preferably, the novel critical angle transmission grating production method, wet etching monocrystalline silicon is used in S3 carves
The KOH solution that liquid is mass fraction 40~50% is lost, etching temperature is 20~25 DEG C.
Preferably, it is living to be additionally added surface in S3 for the novel critical angle transmission grating production method in etching liquid
Property agent, the surfactant is at least one of IPA, TMDD and SDSS；Wherein, the additive amount of IPA is KOH solution matter
The additive amount of 3~6%, TMDD of amount is that the additive amount of 0.05~0.1%, SDSS of KOH solution quality is KOH solution quality
0.05~0.1%.
Preferably, the novel critical angle transmission grating production method is carried out when wet etching monocrystalline silicon in S3
Ultrasonic vibration, ultrasonic frequency is 80~120kHz, power is 250~350W.
Preferably, the novel critical angle transmission grating production method, in S1 using mass fraction be 25~
35% sulfuric acid solution etches chromium, and etching temperature is 18~22 DEG C.
Preferably, the novel critical angle transmission grating production method using mass fraction is 49% in S3
HF solution and 40% NH4The mixed solution of F solution removes silicon nitride layer, HF solution and NH4The mass ratio of F solution is 1:7.
Preferably, the novel critical angle transmission grating production method using mass fraction is 1 in S1, S2
~3 ‰ 40~50s of NaOH solution development.
Preferably, the novel critical angle transmission grating production method uses scanning interferometer field exposure system in S2
Before system exposure, the workbench of adjustment scanning interferometer field exposure system makes the crystal orientation direction of benchmark grating and the exposure of scanning interferometer field is
The workbench scanning direction of system is parallel.
Preferably, the novel critical angle transmission grating production method, scanning interferometer field exposure system in S2
Conditions of exposure are as follows: the wavelength of two beam interferometer light is 413.1nm, luminous intensity 4lux.
The present invention is include at least the following beneficial effects:
1, novel critical angle transmission grating production method of the invention, by two-sided chromium plating, two-sided spin coating photoresist, double
The techniques such as face exposure make monocrystalline silicon grating exposure mask.Then two-way simultaneous carries out wet process quarter to monocrystalline silicon using alkaline etch bath
Erosion, can reduce grating stretching area, realize the promotion of grating aperture opening ratio, by transmission grating prepared by technique of the invention,
It broadens area and is reduced into the 50% of traditional handicraft.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is the process flow of novel critical angle transmission grating production method of the present invention；
Fig. 2 is that scanning interferometer field of the present invention exposes architecture schematic diagram；
Fig. 3 is the structural schematic diagram for the grating that the method for the present invention is prepared.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be noted that in the description of the present invention, term " transverse direction ", " longitudinal direction ", "upper", "lower", "front", "rear",
The orientation or positional relationship of the instructions such as "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is based on attached drawing institute
The orientation or positional relationship shown, is merely for convenience of description of the present invention and simplification of the description, and is not the dress of indication or suggestion meaning
It sets or element must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as to limit of the invention
System.
Embodiment 1
As shown in Figures 1 to 3, a kind of novel critical angle transmission grating production method, comprising the following steps:
S1, in monocrystal silicon substrate double-sided deposition silicon nitride layer, then in silicon nitride layer chrome-faced, then two-sided spin coating photoetching
Glue, after uv-exposure, development, wet etching chromium obtains benchmark grating；
S2, in the two-sided spin coating photoresist of benchmark grating, obtain grating after the exposure of scanning interferometer field exposure system, development and cover
Film；
The silicon nitride layer of S3, then dry etching grating exposure mask, wet etching monocrystalline silicon finally remove silicon nitride layer, i.e.,
Obtain transmission grating.
As shown in Figure 1, in the equal chemical vapor deposition silicon nitride layer 11 of 1 upper and lower surface of monocrystal silicon substrate, then in silicon nitride
11 chrome-faced 12 of layer, after chromium surface spin coating photoresist 13, after uv-exposure, development, wet etching chromium obtains reference light
Grid, uv-exposure intensity are 4lux, time for exposure 25s, the 3 ‰ NaOH developer solutions that when development is, development using mass fraction
45s.Then in the two-sided spin coating photoresist of benchmark grating, obtaining the period after the exposure of scanning interferometer field exposure system, development is
The grating exposure mask of 5000gr/mm, the scanning interferometer field exposure system structure are as shown in Figure 2, wherein 21 be grating beam splitting device, 22
It is spectroscope for variable attenuator, 23,24 be polariscope, and 25 be reflecting mirror, and 26 be column reference mirror, and 27 is dry for phase-shifted measurement
Interferometer, 28 be phase interference mirror, and 29 be workbench, and 31 be spatial filter, and 32 be beam photospallation device, and 33 execute for phase-shifted
Device, 34 be controller, and 35 be phase error, and 36 be phase error signal, to work when which works
Platform exposes production grating along the step-scan of the direction X-Y.The benchmark grating for being coated with photoresist is placed on workbench in exposure,
30 be benchmark grating in figure, and the light beam of UV Laser emission is divided into two-beam through grating beam splitting device, and final two-beam is in photoresist
Surface interferes, and forms light and dark interference fringe and realizes exposure, that is, completes the exposure of benchmark grating one side, benchmark grating
The exposure method of another side is same as above, up to grating exposure mask after the benchmark grating development after exposure.Pass through scanning in exposure process
The supplementary means such as fringe locking, the phase-modulation of interference field exposure system improve scanning interferometer field exposure system stability, this is
System stability can achieve following parameter after improving: interference fringe PGC demodulation precision is less than 8.5nm, and interference fringe straightness is small
In 10nm, the small 10ppm of fringe period measurement accuracy, position lasting accuracy is less than 4 μm, and angle stabilization precision is less than 4 μ rad.
Then then dry etching silicon nitride, wet etching monocrystalline silicon remove silicon nitride layer to get transmission grating.Dry etching nitridation
When silicon, the etching gas that uses are as follows: fluoroform+oxygen, etching power are 600W, etch period 120s, and etching depth is
40nm。
The novel critical angle transmission grating production method, etching liquid used in wet etching monocrystalline silicon is quality in S3
The KOH solution of score 40%, etching temperature are 25 DEG C.
The novel critical angle transmission grating production method is additionally added surfactant in etching liquid in S3, described
Surfactant is IPA, and the additive amount of IPA is the 5% of KOH solution quality.The surfactant of addition can reduce bubble hydrogen with
Surface tension between silicon wafer.
The novel critical angle transmission grating production method carries out ultrasonic vibration when wet etching monocrystalline silicon in S3,
Ultrasound frequency be 80kHz, power 250W.
The novel critical angle transmission grating production method is carved using the sulfuric acid solution that mass fraction is 25% in S1
Chromium is lost, etching temperature is 18 DEG C.
The novel critical angle transmission grating production method, in S3 using mass fraction be 49% HF solution with
40% NH3The mixed solution of F solution removes silicon nitride layer, HF solution and NH3The mass ratio of F solution is 1:7.
The novel critical angle transmission grating production method, the NaOH for the use of mass fraction being 3 ‰ in S1, S2 are molten
Liquid development 45s.
The novel critical angle transmission grating production method, in S2 using the exposure of scanning interferometer field exposure system before,
The workbench of adjustment scanning interferometer field exposure system makes the crystal orientation direction of benchmark grating and the work of scanning interferometer field exposure system
Platform scanning direction is parallel.Before the exposure of scanning interferometer field exposure system, crystal orientation direction and the scanning for adjusting monocrystal silicon substrate are dry
The workbench scanning direction for relating to an exposure system is parallel.Before the exposure of scanning interferometer field exposure system, single-degree-of-freedom is first passed through
Corner adjustment carries out benchmark grating crystal orientation high-precision and is aligned, and adjusts workbench then to make the monocrystal silicon substrate of benchmark grating
Crystal orientation direction is parallel with workbench scanning direction (i.e. the Y direction in Fig. 2) of scanning interferometer field exposure system, to meet crystal orientation
Angle < 0.001 ° is directed to require.
The novel critical angle transmission grating production method, the conditions of exposure of scanning interferometer field exposure system in S2
Are as follows: the wavelength of two beam interferometer light is 413.1nm, luminous intensity 4lux.The obtained grating mask period after through exposure and development is
200nm。
By above-mentioned process conditions, the grating line density finally prepared is 5000gr/mm, account for it is wide than be 0.2, grid stroke
Depth-to-width ratio is 100:1.
B is transmission grating structure schematic diagram prepared by the present invention in Fig. 3, and a is that the structure of the grating of traditional handicraft preparation is shown
It is intended to.By transmission grating prepared by technique of the invention, broadening area is reduced into the 50% of traditional handicraft.
Embodiment 2
A kind of novel critical angle transmission grating production method, comprising the following steps:
S1, in monocrystal silicon substrate double-sided deposition silicon nitride layer, then in silicon nitride layer chrome-faced, then two-sided spin coating photoetching
Glue, after uv-exposure, development, wet etching chromium obtains benchmark grating；
S2, in the two-sided spin coating photoresist of benchmark grating, obtain grating after the exposure of scanning interferometer field exposure system, development and cover
Film；
The silicon nitride layer of S3, then dry etching grating exposure mask, wet etching monocrystalline silicon finally remove silicon nitride layer, i.e.,
Obtain transmission grating.
The novel critical angle transmission grating production method, etching liquid used in wet etching monocrystalline silicon is quality in S3
The KOH solution of score 45%, etching temperature are 20 DEG C.
The novel critical angle transmission grating production method is additionally added surfactant in etching liquid in S3, described
Surfactant is TMDD, and the additive amount of the surfactant is the 0.1% of KOH solution quality.The surfactant of addition
The surface tension between bubble hydrogen and silicon wafer can be reduced.
The novel critical angle transmission grating production method carries out ultrasonic vibration when wet etching monocrystalline silicon in S3,
Ultrasound frequency be 100kHz, power 300W.
The novel critical angle transmission grating production method is carved using the sulfuric acid solution that mass fraction is 30% in S1
Chromium is lost, etching temperature is 20 DEG C.
The novel critical angle transmission grating production method, in S3 using mass fraction be 49% HF solution with
40% NH4The mixed solution of F solution removes silicon nitride layer, HF solution and NH3The mass ratio of F solution is 1:7.
The novel critical angle transmission grating production method, the NaOH for the use of mass fraction being 1 ‰ in S1, S2 are molten
Liquid development 40s.
The novel critical angle transmission grating production method, in S2 using the exposure of scanning interferometer field exposure system before,
The workbench of adjustment scanning interferometer field exposure system makes the crystal orientation direction of benchmark grating and the work of scanning interferometer field exposure system
Platform scanning direction is parallel.
The novel critical angle transmission grating production method, the conditions of exposure of scanning interferometer field exposure system in S2
Are as follows: the wavelength of two beam interferometer light is 413.1nm, luminous intensity 4lux.The obtained grating mask period after through exposure and development is
200nm。
Embodiment 3
A kind of novel critical angle transmission grating production method, comprising the following steps:
S1, in monocrystal silicon substrate double-sided deposition silicon nitride layer, then in silicon nitride layer chrome-faced, then two-sided spin coating photoetching
Glue, after uv-exposure, development, wet etching chromium obtains benchmark grating；
S2, in the two-sided spin coating photoresist of benchmark grating, obtain grating after the exposure of scanning interferometer field exposure system, development and cover
Film；
The silicon nitride layer of S3, then dry etching grating exposure mask, wet etching monocrystalline silicon finally remove silicon nitride layer, i.e.,
Obtain transmission grating.
The novel critical angle transmission grating production method, etching liquid used in wet etching monocrystalline silicon is quality in S3
The KOH solution of score 50%, etching temperature are 22 DEG C.
The novel critical angle transmission grating production method is additionally added surfactant in etching liquid in S3, described
Surfactant is SDSS, and the additive amount of the surfactant is the 0.1% of KOH solution quality.The surfactant of addition
The surface tension between bubble hydrogen and silicon wafer can be reduced.
The novel critical angle transmission grating production method carries out ultrasonic vibration when wet etching monocrystalline silicon in S3,
Ultrasound frequency be 120kHz, power 350W.
The novel critical angle transmission grating production method is carved using the sulfuric acid solution that mass fraction is 35% in S1
Chromium is lost, etching temperature is 22 DEG C.
The novel critical angle transmission grating production method, in S3 using mass fraction be 49% HF solution with
40% NH4The mixed solution of F solution removes silicon nitride layer, HF solution and NH3The mass ratio of F solution is 1:7.
The novel critical angle transmission grating production method, the NaOH for the use of mass fraction being 2 ‰ in S1, S2 are molten
Liquid development 50s.
The novel critical angle transmission grating production method, in S2 using the exposure of scanning interferometer field exposure system before,
The workbench of adjustment scanning interferometer field exposure system makes the crystal orientation direction of benchmark grating and the work of scanning interferometer field exposure system
Platform scanning direction is parallel.
The novel critical angle transmission grating production method, the conditions of exposure of scanning interferometer field exposure system in S2
Are as follows: the wavelength of two beam interferometer light is 413.1nm, luminous intensity 4lux.The obtained grating mask period after through exposure and development is
200nm。
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (9)
1. a kind of novel critical angle transmission grating production method, which comprises the following steps:
S1, in monocrystal silicon substrate double-sided deposition silicon nitride layer, then in silicon nitride layer chrome-faced, then two-sided spin coating photoresist,
After uv-exposure, development, wet etching chromium obtains benchmark grating；
S2, in the two-sided spin coating photoresist of benchmark grating, obtain grating exposure mask after the exposure of scanning interferometer field exposure system, development；
The silicon nitride layer of S3, then dry etching grating exposure mask, wet etching monocrystalline silicon remove silicon nitride layer finally to get saturating
Penetrate grating.
2. novel critical angle transmission grating production method as described in claim 1, which is characterized in that wet etching list in S3
Etching liquid used in crystal silicon is the KOH solution of mass fraction 40~50%, and etching temperature is 20~25 DEG C.
3. novel critical angle transmission grating production method as claimed in claim 2, which is characterized in that in S3 in etching liquid also
Surfactant is added, the surfactant is at least one of IPA, TMDD and SDSS；Wherein, the additive amount of IPA
Additive amount for 3~6%, TMDD of KOH solution quality is that the additive amount of 0.05~0.1%, SDSS of KOH solution quality is
The 0.05~0.1% of KOH solution quality.
4. novel critical angle transmission grating production method as claimed in claim 2, which is characterized in that wet etching list in S3
Ultrasonic vibration is carried out when crystal silicon, ultrasonic frequency is 80~120kHz, power is 250~350W.
5. novel critical angle transmission grating production method as described in claim 1, which is characterized in that use quality point in S1
Number etches chromium for 25~35% sulfuric acid solution, and etching temperature is 18~22 DEG C.
6. novel critical angle transmission grating production method as described in claim 1, which is characterized in that use quality point in S3
Number is 49% HF solution and 40% NH4The mixed solution of F solution removes silicon nitride layer, HF solution and NH4The quality of F solution
Than for 1:7.
7. novel critical angle transmission grating production method as described in claim 1, which is characterized in that used in S1, S2
40~50s of NaOH solution development that mass fraction is 1~3 ‰.
8. novel critical angle transmission grating production method as described in claim 1, which is characterized in that dry using scanning in S2
Before relating to an exposure system exposure, the workbench of adjustment scanning interferometer field exposure system keeps the crystal orientation direction of benchmark grating and scanning dry
The workbench scanning direction for relating to an exposure system is parallel.
9. novel critical angle transmission grating production method as described in claim 1, which is characterized in that scanning interferometer field in S2
The conditions of exposure of exposure system are as follows: the wavelength of two beam interferometer light is 413.1nm, luminous intensity 4lux.
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Cited By (1)
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| CN111880254A (en) * | 2020-07-14 | 2020-11-03 | 浙江大学 | Preparation method of grating with continuously-changed diffraction efficiency |
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| CN109782384B (en) | 2020-07-03 |
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