CN109243662A - The preparation method of hanging thick golden zone plate lens without substrate supports - Google Patents
The preparation method of hanging thick golden zone plate lens without substrate supports Download PDFInfo
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Abstract
The invention belongs to inductively coupled plasma etching technical field, the preparation method of the hanging thick golden zone plate lens of specially a kind of no substrate supports.Its step includes: spin coating HSQ photoresist on a si substrate, the design configuration of zone plate lens is formed on a photoresist as the etching masking layer of zone plate silicon template using the method for electron beam lithography, then the zone plate silicon template that deep reaction ion etching forms large ratio of height to width is carried out in inductively coupled plasma etching system, and golden electroplating technique is combined to be electroplated in silicon template with certain thickness gold, it finally removes residual photoresist exposure mask and removes silicon structure remaining in substrate silicon and Au zone plate, to obtain the hanging golden zone plate of the large ratio of height to width applied to hard x-ray imaging field.The method of the present invention controllability is good, process stabilizing, and is suitable for the preparation of the metal structure of large ratio of height to width.
Description
Technical field
The invention belongs to inductively coupled plasma etching technical field, specially a kind of silicon substrate hollow out gold zone plate is saturating
The preparation method of mirror.
Background technique
Key focus and image-forming component of the Fresnel zone plate as synchrotron radiation X-ray whole audience imaging system, manufacture
It is horizontal that the progress of technology will directly influence X-ray microtechnic.In order to realize the imaging of high quality, zone plate absorber gold knot
The thickness of structure is usually tens microns of orders of magnitude.Thicker wavestrip chip architecture is needed for high X-ray energy, such thickness is used
To ensure the attenuation length of hard X ray.
For the technology of preparing of X-ray zone plate, the penetration capacity of electronics is limited and the approach effect of electron beam lithography
Limit its attainable depth-width ratio of institute.There is result of study to show that electron beam lithography production focuses 100 nm of 9keV X-ray
Its depth-width ratio limit of zone plate is 20.The zone plate made with electron beam lithography, thickness is substantially at 2 μm or less.
Solve the effective way of this problem first is that formed the template that there is certain thickness structure as zone plate from
And improve the thickness of zone plate.Due to silicon process technology maturation, it is suitable for the template of zone plate.
The method forms zone plate using inductively coupled plasma etching system and in conjunction with deep reaction ion etching
Silicon template, and electroplating technology is combined to prepare the hanging golden zone plate lens of no substrate supports, it may be implemented 200 ~ 300 nm points
Resolution, the hanging golden zone plate of 3 ~ 5 μ m-thicks.4 μ m thicks can be extrapolated according to attenuation length of the X-ray in Au material
Self-supporting Au zone plate can be used for the x-ray imaging of 20 keV, this has broken the imaging bottleneck of hard X ray.Hard X ray is compared
Grenz ray penetration power is stronger, can carry out the imaging of thick sample, and grenz ray is only applicable to sample surfaces imaging.
This technique is applicable not only to the preparation of X-ray focusing and image-forming component, can be also used for photon screen, laser target, light
Collimation lens etc. needs the field of large ratio of height to width silicon structure.
Summary of the invention
It is an object of the invention to propose it is a kind of simple, conveniently, high-precision production have large ratio of height to width without substrate supports
Hanging golden zone plate lens method.
The preparation method of the hanging golden zone plate lens of no substrate supports proposed by the present invention, is by electron beam lithography skill
Art, inductively coupled plasma etching and electroplating technology combine, and making has the outstanding without substrate supports of large ratio of height to width
Empty gold zone plate lens structure, the specific steps are as follows:
(1) spin coating HSQ photoresist on a silicon substrate, forms zone plate lens using the method for electron beam lithography on a photoresist
Photoetching offset plate figure；
(2) deep reaction ion etching is carried out in inductively coupled plasma etching system, forms the zone plate silicon of large ratio of height to width
Template；General depth-width ratio > 30:1, such as depth-width ratio are 30:1--60:1；
(3) metal conducting layer is prepared on the sample that step (2) obtains, material is Cr/Au composite membrane, as seed layer；
(4) Si is grown in the sample reverse side that step (3) obtains3N4Diaphragm；
(5) the sample front and back sides spin coating PMMA photoresist for obtaining step (4) then carries out overlay mark exposure, and in front
Open zone plate window；
(6) sample obtained to step (5) carries out plating Au；
(7) one Cr/Au composite membrane is grown using thermal evaporation to the sample reverse side that step (6) obtains, is marked as gold；
(8) the sample acetone obtained to step (7) removes front and back sides photoresist；
(9) sample reverse side step (8) obtained spin coating PMMA photoresist again, then in reverse side optics alignment to form zone plate logical
Light window；
(10) sample that step (9) is obtained, the Si exposed with the zone plate light passing window of reactive ion etching removal reverse side3N4
Diaphragm, and remove reverse side photoresist with acetone；
(11) KOH solution wet etching removes substrate silicon materials；
(12) HF solution wet etching removes HSQ remnants' exposure mask, then carries out inductively coupled plasma etching in front again and goes
Except the silicon materials in zone plate gap.
In step (1) of the present invention, photoresist is HSQ photoresist, with a thickness of the nm of 300 nm ~ 600.And it toasts and is allowed to hard
Change, baking temperature is between 150 DEG C ~ 180 DEG C, and the time is in the min of 10 min ~ 30.
In step (2) of the present invention, the deep reaction ion etching is using Bosch etching method；Bosch work is directed to when etching
Skill is regulated and controled: by passivation gas C4F8Be added in etch step and control lateral etching, by inaction period and etching period when
Between respectively reduce to 3-5s and 5-8 s, to guarantee low sidewall roughness；
Fixed following technological parameter: coil power 600W, pole plate power 20W, 25 DEG C of bottom crown cooling temperature, inaction period
In C4F8Gas flow is 85 sccm and air pressure is 19 mtorr, the SF in etching period6Gas flow be 175 sccm and
Air pressure is 35 mtorr, and etches and be fixed on 1 min, 30 s total time, carries out tracing analysis, finds optimal processing parameter model
It encloses, the thickness of zone plate silicon template is made to be increased to 4 μm.
In step (3) of the present invention, the seed layer is prepared using the method for thermal evaporation or physical vapor deposition, material
For Cr/Au composite membrane, Cr is with a thickness of 5 nm ~ 15 nm, Au with a thickness of the nm of 5 nm ~ 15.
In step (4) of the present invention, Si3N4Diaphragm is grown using PECVD, with a thickness of the nm of 100 nm ~ 300.
In step (5) of the present invention, the photoresist of spin coating is PMMA, with a thickness of the nm of 300 nm ~ 400.Front windowing is circle
Shape, diameter are the mm of 4 mm ~ 6.
In step (6) of the present invention, plated material is gold, and current density when plating is in 0.3 A/dm2~ 1A/dm2, voltage
For 10-21V, electroplating time is the min of 10 min ~ 30.Plating metal with a thickness of 3 μm ~ 5 μm.
In step (7) of the present invention, gold label is prepared using the method for thermal evaporation or physical vapor deposition, material Cr/
Au composite membrane, Cr is with a thickness of 5 nm ~ 15 nm, Au with a thickness of the nm of 100 nm ~ 110.
In step (9) of the present invention, the photoresist of spin coating is PMMA, with a thickness of the nm of 300 nm ~ 400.Reverse side opens light window
For circle, diameter is 85 μm ~ 120 μm, this window size makes the wave of etching exposing obtained by KOH wet etching angle calculation
Strap periphery guarantees have the gold of 5 μm ~ 15 μm of width to make peripheral support.
In step (10) of the present invention, the etching gas used in the RIE etching process of silicon nitride is CHF3And O2Mixing
Gas, CHF3Gas flow is 40 sccm ~ 60 sccm, O2Gas flow be the sccm of 5 sccm ~ 15, power be 200 W ~
300 W, time are the min of 1 min ~ 3.
Using KOH solution that substrate silicon material etch is clean in step (11) of the present invention, etching time is the h of 11 h ~ 14.
In step (12) of the present invention, remove the remaining HSQ photoresist exposure mask of sample after plating, minimizing technology is wet process quarter
Erosion, such as HF solution.Silicon materials in the removal zone plate gap of front using dry etching, using inductive coupling etc. from
Daughter etching removal.
The method of the present invention can be divided into four parts:
First part, i.e. step (1), form etch mask: spin coating photoresist on a silicon substrate utilizes the method for electron beam lithography
The photoetching offset plate figure of zone plate lens is formed on a photoresist；This figure is by the exposure mask as subsequent etch step.Specific packet
Include: one layer of HSQ photoresist of spin coating on a silicon substrate carries out front baking with a thickness of the nm of 300 nm ~ 600；HSQ photoresist will be had
Substrate be exposed under electron beam lithography machine；Develop to figure after exposure；
Second part, i.e. step (2), form deep silicon template: carried out in inductively coupled plasma etching system it is deep react from
Son etching forms the zone plate silicon template of large ratio of height to width, and deep reaction ion etching therein is using Bosch technique；
Part III, i.e. step (3) arrive step (6), the transfer of nano graph: one layer of metal conducting layer are first prepared, as seed
Layer, preparation method are thermal evaporation or physical vapor deposition, and material is Cr/Au composite membrane, and thickness is respectively the nm/5 of 5 nm ~ 15
nm~15 nm；This layer of seed layer and silicon substrate adhesiveness are good, prepare for subsequent plating Au；Zone plate window is opened then in front
The pattern transfer of silicon template is the figure of Au zone plate by the Au that electroplating thickness is 3 μm ~ 5 μm；
Part IV, i.e. step (7) arrive step (12), remove residual photoresist exposure mask and silicon removal: after plating
Sample is engraved in reverse side windowing using set, removes the Si of exposing3N4Diaphragm and KOH remove substrate silicon materials；Then molten in HF
Liquid uses inductively coupled plasma etching to remove the silicon in zone plate gap after removing remnants HSQ photoresist exposure mask.
In the present invention, the structure of this hanging golden zone plate does not need diaphragm support figure, supports wave using reinforcing rib structure
Strap annulus is hanging to ensure.Wherein, reinforcing rib is the radiation vertical element that each ring is connected along radial direction.For designed
The outermost ring width of 300 nm, diameter be 40 μm of zone plate, reinforcing rib number is 24, and width is 300 nm.
The number of area size and reinforcing rib that hanging fastness is reserved by alignment in control electroplating technology and width come
Control, by guaranteeing hanging fastness with external support inside zone plate.The zone plate of 2 microns or more thickness is not available electricity
Beamlet photoetching making, and the hard X ray that the hanging golden zone plate of this 4 micron thickness can be used for 20 keV focuses.
The method of the present invention controllability is good, process stabilizing, and is suitable for the preparation of the metal structure of large ratio of height to width.
The concrete operations process of the method for the present invention is as follows
(1) monocrystalline substrate is selected, substrate is cleaned；
(2) the HSQ photoresist that spin coating a layer thickness is the nm of 300 nm ~ 600 on substrate, carries out front baking processing；
(3) it selects suitable dosage to be exposed processing under electron beam lithography machine, develops to figure after exposure, form wave
The photoetching offset plate figure of strap lens；
(4) the zone plate silicon mould of large ratio of height to width is formed using Bosch etching technics in inductively coupled plasma etching system
Plate；
(5) one layer of metal conducting layer is prepared on obtained sample, as seed layer；
(6) Si is grown in sample reverse side3N4Diaphragm；
(7) then spin coating photoresist in sample front and back sides is subjected to front baking processing；
(8) it carries out overlay mark exposure and zone plate window is opened in front；
(9) plating Au is carried out to sample；Reverse side is using thermal evaporation growth layer of Au as gold label；
(10) remove front and back sides photoresist with acetone；
(11) reverse side spin coating photoresist again；
(12) zone plate light passing window is formed in reverse side optics alignment；
(13) Si that the zone plate light passing window of reactive ion etching removal reverse side exposes3N4Diaphragm；
(14) remove reverse side photoresist with acetone；
(15) KOH solution wet etching removes substrate silicon materials；
(16) HF solution wet etching removes HSQ remnants' exposure mask；
(17) silicon materials in inductively coupled plasma etching removal zone plate gap are carried out in front.
Detailed description of the invention
Fig. 1 is designed zone plate geometric graph and photoetching alignment mark figure.
Fig. 2 to Figure 18 is respectively corresponded in embodiment 1 in 17 steps according to the sequence of the above-mentioned making step of the present invention
The sectional view (reflect sample structure change situation) of 17 sample structures.
Fig. 2 corresponds to step 1: cleaning monocrystalline substrate.
Fig. 3 corresponds to step 2: spin coating HSQ photoresist on substrate.
Fig. 4 corresponds to the mask pattern for formation of developing after step 3:EBL exposes.
Fig. 5 corresponds to step 4: the large ratio of height to width silicon template formed after etching.
Fig. 6 corresponds to step 5: one layer of Cr/Au seed layer of thermal evaporation.
Fig. 7 corresponds to step 6: sample reverse side grows Si3N4Diaphragm.
Fig. 8 corresponds to step 7: front and back sides spin coating photoresist.
Fig. 9 corresponds to step 8: carrying out overlay mark exposure and zone plate window is opened in front.
Figure 10 corresponds to step 9: certain thickness Au is electroplated, reverse side is using thermal evaporation growth layer of Au as gold label.
Figure 11 corresponds to step 10: acetone removes front and back sides photoresist.
Figure 12 corresponds to step 11: reverse side spin coating photoresist again.
Figure 13 corresponds to step 12: forming zone plate light passing window in reverse side optics alignment.
Figure 14 corresponds to step 13: reactive ion etching removes the Si that reverse side exposes3N4Diaphragm.
Figure 15 corresponds to step 14: acetone removes reverse side photoresist.
Figure 16 corresponds to step 15:KOH solution wet etching removal substrate silicon materials.
Figure 17 corresponds to step 16:HF solution wet etching removal HSQ remnants' exposure mask.
Figure 18 corresponds to step 17: front carries out the silicon materials in inductively coupled plasma etching removal zone plate gap.
Figure 19 is the hanging golden zone plate schematic diagram that the present invention is realized.
Specific embodiment
Implementation of the invention is further described by way of example with reference to the accompanying drawing, but the present invention is not limited only to reality
Example.All technological parameters in embodiment have carried out simple change, belong within the scope of the present invention.
Embodiment 1: the hanging golden zone plate lens without substrate supports of large ratio of height to width are prepared:
(1)<100>crystal orientation is selected, resistivity is the n type single crystal silicon substrate of 1 ~ 10 Ω cm and cleans up substrate.First
Silicon wafer is put into acetone and is impregnated, this process combines ultrasonic treatment 10min.Then silicon substrate film is put into aqueous isopropanol and is soaked
Taking-up nitrogen gun dries up substrate slice after moistening 5 min, as a result as shown in Figure 2；
(2) the HSQ electron beam resist of 375 nm of spin coating thickness again after spin coating HMDS adhesion layer on a silicon substrate, and at 180 DEG C
It toasts 10 min in baking oven to be allowed to harden, as a result as shown in Figure 3；
(3) sample is exposed processing under electron beam lithography machine, exposure dose is 1700 μ C/cm2；
(4) TMAH/H for being 1:2.5 in the volume ratio that temperature is 50 DEG C23 min that develop in O mixed solution are later in H2It is fixed in O
30 s of shadow, as a result as shown in Figure 4；
(5) it is formed after HSQ exposure mask, big height is formed using Bosch etching technics in inductively coupled plasma etching system
The zone plate silicon template of wide ratio.The time of inaction period and etching period is respectively that 4 s and 5 s, bottom crown are cold in etching technics
But temperature is 25 DEG C, C4F8Gas flow is 85sccm and air pressure is 19 mtorr, and the air pressure in etching period is 35 mtorr,
And it also joined the C of 85sccm in etching period4F8, respectively 400 W and 35 W, SF of coil power and pole plate power6
Gas flow is 150 sccm, and etch period is 9 min, and the zone plate silicon template thickness of etching is 4.1 μm, and outer ring width is
220 nm.It is as shown in Figure 5 to etch result；
(6) the Cr/Au composite membrane that a layer thickness is respectively the nm of 5 nm/15 is deposited using thermal evaporation, as metal conducting layer,
As a result as shown in Figure 6；
(7) Si is grown using PECVD3N4Diaphragm, with a thickness of 100 nm, as a result as shown in Figure 7；
(8) front and back sides spin coating with a thickness of 300 nm PMMA photoresist, and in 180 DEG C of baking ovens toast 1h be allowed to harden, as a result
As shown in Figure 8；
(9) it carries out overlay mark exposure and zone plate window is opened in front, window is circle, and diameter is 4 mm, and zone plate is in
Window center position, as a result as shown in Figure 9；
(10) plating Au is carried out to sample, electroplating voltage is 50 V, in 0.5 A/dm2It is electroplated 3 min under current density, then
0.75 A/dm23 min are electroplated under current density, be electroplated Au with a thickness of 1.2 μm.One layer is grown using thermal evaporation in reverse side again
Au is Cr/Au composite membrane as gold label, material, and thickness is respectively the nm of 5 nm/100；The results are shown in Figure 10；
(11) remove front and back sides photoresist with acetone；As a result as shown in figure 11；
(12) reverse side again spin coating with a thickness of 300 nm PMMA photoresist, and in 180 DEG C of baking ovens toast 1h be allowed to harden,
As a result as shown in figure 12；
(13) zone plate light passing window is formed in reverse side optics alignment again, window is circle, and diameter, which is 100 μm, exposes etching
Zone plate periphery guarantee there is the gold of 10 μm of width to make peripheral support.As a result as shown in figure 13；
(14) Si that the zone plate light passing window of reactive ion etching removal reverse side exposes3N4Diaphragm；The etching gas used for
CHF3And O2Mixed gas, CHF3Gas flow is 50 sccm, O2Gas flow is 12sccm, and power is 300 W, time
For 1 min30 s.As a result as shown in figure 14；
(15) remove reverse side photoresist with acetone；As a result as shown in figure 15；
(16) wet process is carried out at 80 DEG C using the KOH solution (KOH of 500 g, the water of 1200 ml, 200 ml ethyl alcohol) of 30 %
Etching, 13 h of corrosion remove the substrate silicon materials of 500 μ m thicks.As a result as shown in figure 16；
(17) HF solution wet etching removes HSQ remnants' exposure mask, as a result as shown in figure 17；
(18) silicon materials in inductively coupled plasma etching removal zone plate gap are carried out in front；As a result such as Figure 18 institute
Show.
Embodiment 2: the preparation of the silicon nanometer column template applied to photon sieve with high height-width ratio:
The main distinction of this embodiment and upper example is: this HSQ photoresist mask pattern is round dot matrix.In addition, the portion of removing
Parameter used also has a little different outer step by step, other are identical as precedent.
(1)<100>crystal orientation is selected, resistivity is the n type single crystal silicon substrate of 1 ~ 10 Ω cm and cleans up substrate.
Silicon wafer is put into acetone first and is impregnated, this process combines ultrasonic treatment 10min.Then silicon substrate film is put into aqueous isopropanol
Taking-up dries up substrate slice with nitrogen gun after 5 min of middle infiltration, as a result as shown in Figure 2；
(2) the HSQ electron beam resist of 430 nm of spin coating thickness again after spin coating HMDS adhesion layer on a silicon substrate, and at 180 DEG C
It toasts 10 min in baking oven to be allowed to harden, as a result as shown in Figure 3；
(3) sample is exposed processing under electron beam lithography machine, exposure dose is 3000 μ C/cm2；
(4) TMAH/H for being 1:2.5 in the volume ratio that temperature is 50 DEG C21 min that develops in O mixed solution is later in H2It is fixed in O
30 s of shadow, as a result as shown in Figure 4；
(5) it is formed after HSQ exposure mask, big height is formed using Bosch etching technics in inductively coupled plasma etching system
The silicon nanometer column template of wide ratio.The time of inaction period and etching period is respectively that 4 s and 5 s, bottom crown are cold in etching technics
But temperature is 25 DEG C, C4F8Gas flow is 85sccm and air pressure is 19 mtorr, and the air pressure in etching period is 35 mtorr,
And it also joined the C of 85sccm in etching period4F8, respectively 400 W and 35 W, SF of coil power and pole plate power6
Gas flow is 150 sccm, and etch period is 25 min, and the silicon stem height of etching is 13.3 μm.Etch result such as Fig. 5 institute
Show；
(6) the Cr/Au composite membrane that a layer thickness is respectively the nm of 5 nm/15 is deposited using thermal evaporation, as metal conducting layer,
As a result as shown in Figure 6；
(7) Si is grown using PECVD3N4Diaphragm, with a thickness of 100 nm, as a result as shown in Figure 7；
(8) front and back sides spin coating with a thickness of 300 nm PMMA photoresist, and in 180 DEG C of baking ovens toast 1h be allowed to harden, as a result
As shown in Figure 8；
(9) it carries out overlay mark exposure and photon screen window is opened in front, window is circle, and diameter is 4 mm, and photon screen is in
Window center position, as a result as shown in Figure 9；
(10) plating Au is carried out to sample, electroplating voltage is 50 V, in 0.5 A/dm2It is electroplated 3 min under current density, then
0.75 A/dm23 min are electroplated under current density, be electroplated Au with a thickness of 1.2 μm.One layer is grown using thermal evaporation in reverse side again
Au is Cr/Au composite membrane as gold label, material, and thickness is respectively the nm of 5 nm/100；The results are shown in Figure 10；
(11) remove front and back sides photoresist with acetone；As a result as shown in figure 11；
(12) reverse side again spin coating with a thickness of 300 nm PMMA photoresist, and in 180 DEG C of baking ovens toast 1h be allowed to harden,
As a result as shown in figure 12；
(13) photon screen light passing window is formed in reverse side optics alignment again, window is circle, and diameter, which is 100 μm, exposes etching
Photon screen periphery guarantee there is the gold of 10 μm of width to make peripheral support.As a result as shown in figure 13；
(14) Si that the light passing window of reactive ion etching removal reverse side exposes3N4Diaphragm；The etching gas used is CHF3And O2
Mixed gas, CHF3Gas flow is 50 sccm, O2Gas flow is 12sccm, and power is 300 W, and the time is 1 min30
s.As a result as shown in figure 14；
(15) remove reverse side photoresist with acetone；As a result as shown in figure 15；
(16) wet process is carried out at 80 DEG C using the KOH solution (KOH of 500 g, the water of 1200 ml, 200 ml ethyl alcohol) of 30 %
Etching, 13 h of corrosion remove the substrate silicon materials of 500 μ m thicks；As a result as shown in figure 16；
(17) HF solution wet etching removes HSQ remnants' exposure mask, as a result as shown in figure 17；
(18) silicon materials in inductively coupled plasma etching removal photon screen gap are carried out in front.As a result such as Figure 18 institute
Show.
Claims (10)
1. a kind of preparation method of the hanging thick golden zone plate lens of no substrate supports, which is characterized in that specific step is as follows:
(1) spin coating HSQ photoresist on a silicon substrate, forms zone plate lens using the method for electron beam lithography on a photoresist
Photoetching offset plate figure；
(2) deep reaction ion etching is carried out in inductively coupled plasma etching system, forms the zone plate silicon of large ratio of height to width
Template；Depth-width ratio > 30:1；
(3) metal conducting layer is prepared on the sample that step (2) obtains, material is Cr/Au composite membrane, as seed layer；
(4) Si is grown in the sample reverse side that step (3) obtains3N4Diaphragm；
(5) the sample front and back sides spin coating PMMA photoresist for obtaining step (4) then carries out overlay mark exposure, and in front
Open zone plate window；
(6) sample obtained to step (5) carries out plating Au；
(7) one Cr/Au composite membrane is grown using thermal evaporation to the sample reverse side that step (6) obtains, is marked as gold；
(8) the sample acetone obtained to step (7) removes front and back sides photoresist；
(9) sample reverse side step (8) obtained spin coating PMMA photoresist again, then in reverse side optics alignment to form zone plate logical
Light window；
(10) sample that step (9) is obtained, the Si exposed with the zone plate light passing window of reactive ion etching removal reverse side3N4
Diaphragm, and remove reverse side photoresist with acetone；
(11) KOH solution wet etching removes substrate silicon materials；
(12) HF solution wet etching removes HSQ remnants' exposure mask, then carries out inductively coupled plasma etching in front again and goes
Except the silicon materials in zone plate gap.
2. preparation method according to claim 1, which is characterized in that in step (1), HSQ photoresist is with a thickness of 300
nm~600 nm；And toast and be allowed to harden, baking temperature is 150 DEG C to 180 DEG C, and the time is the min of 10 min ~ 30.
3. preparation method according to claim 1, which is characterized in that in step (2), the deep reaction ion etching is
Using Bosch etching method；Regulated and controled when etching for Bosch technique: by passivation gas C4F8It is added in etch step and controls
Lateral etching respectively reduces the time of inaction period and etching period to 3-5s and 5-8 s, to guarantee that low sidewall is coarse
Degree.
4. preparation method according to claim 1, which is characterized in that seed layer described in step (3) utilizes thermal evaporation
Or prepared by the method for physical vapor deposition, in Cr/Au composite membrane, Cr is with a thickness of 5 nm ~ 15 nm, Au with a thickness of 5 nm ~ 15
nm。
5. preparation method according to claim 1, which is characterized in that in step (4), Si3N4Diaphragm is raw using PECVD
It is long, with a thickness of the nm of 100 nm ~ 300.
6. preparation method according to claim 1, which is characterized in that in step (5), PMMA photoresist with a thickness of 300
nm~400 nm；Front windowing is circle, and diameter is the mm of 4 mm ~ 6.
7. preparation method according to claim 1, which is characterized in that in step (6), current density when plating is 0.3
A/dm2~ 1A/dm2, voltage is 10-21V, and electroplating time is the min of 10 min ~ 30；Electroplating gold with a thickness of 3 μm ~ 5 μm.
8. preparation method according to claim 1, which is characterized in that in step (7), gold label utilizes thermal evaporation or object
Prepared by the method for managing vapor deposition, in Cr/Au composite membrane, Cr is with a thickness of 5 nm ~ 15 nm, Au with a thickness of 100 nm ~ 110
nm。
9. preparation method according to claim 1, which is characterized in that in step (9), PMMA photoresist is with a thickness of 300
nm~400 nm；Reverse side opens light window as circle, and diameter is 85 μm ~ 120 μm, this window size is by KOH wet etching angle
Gained is calculated, the zone plate periphery for exposing etching guarantees have the gold of 5 μm ~ 15 μm of width to make peripheral support.
10. preparation method according to claim 1, which is characterized in that etched in the RIE of silicon nitride in step (10)
The etching gas used in journey is CHF3And O2Mixed gas, CHF3Gas flow is 40 sccm ~ 60 sccm, O2Gas stream
Amount is the sccm of 5 sccm ~ 15, and power is the W of 200 W ~ 300, and the time is the min of 1 min ~ 3.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113151801A (en) * | 2021-03-03 | 2021-07-23 | 电子科技大学 | Preparation method of self-supporting suspended carbon film |
| CN113707357A (en) * | 2021-07-08 | 2021-11-26 | 湖南大学 | Preparation method of high-aspect-ratio zone plate |
| CN113793714A (en) * | 2021-07-28 | 2021-12-14 | 湖南大学 | Preparation method for large-area soft X-ray zone plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111175861A (en) * | 2020-01-17 | 2020-05-19 | 中国科学院长春光学精密机械与物理研究所 | Design and preparation method of multi-focal-length curved fly-eye lens |
| CN111175861B (en) * | 2020-01-17 | 2021-06-15 | 中国科学院长春光学精密机械与物理研究所 | Design and preparation method of multi-focal-length curved fly-eye lens |
| CN113151801A (en) * | 2021-03-03 | 2021-07-23 | 电子科技大学 | Preparation method of self-supporting suspended carbon film |
| CN113151801B (en) * | 2021-03-03 | 2022-12-27 | 电子科技大学 | Preparation method of self-supporting suspended carbon film |
| CN113707357A (en) * | 2021-07-08 | 2021-11-26 | 湖南大学 | Preparation method of high-aspect-ratio zone plate |
| CN113793714A (en) * | 2021-07-28 | 2021-12-14 | 湖南大学 | Preparation method for large-area soft X-ray zone plate |
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