CN110286432B - Preparation method of X-ray gold transmission grating - Google Patents
Preparation method of X-ray gold transmission grating Download PDFInfo
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- CN110286432B CN110286432B CN201910555170.9A CN201910555170A CN110286432B CN 110286432 B CN110286432 B CN 110286432B CN 201910555170 A CN201910555170 A CN 201910555170A CN 110286432 B CN110286432 B CN 110286432B
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Abstract
The invention discloses a preparation method of an X-ray gold transmission grating, which comprises the steps of firstly using a metal catalytic etching technology to manufacture a silicon grating mask with large groove depth and steep and smooth side wall, then electroplating and depositing gold in a silicon grating mask groove, and finally removing the silicon grating mask to obtain the gold transmission grating with large groove depth and steep and smooth side wall. Compared with the prior art, the invention has the beneficial technical effects that: can manufacture the gold transmission grating with large groove depth, steep and smooth side wall.
Description
Technical Field
The invention belongs to the technical field of grating micro-nano processing, and particularly relates to a preparation method of an X-ray gold transmission grating.
Background
The gold transmission grating has simple structure, large solid angle and wide spectrum range, can be conveniently combined with a spatial resolution instrument at the same time, and is widely applied to the fields of laser inertial confinement nuclear fusion plasma diagnosis, X-ray celestial body physics and the like. At present, the use wave band of the gold transmission grating in the fields of plasma diagnosis and astrophysics is required to reach sub-kilo electron volts and even higher energy, and in order to realize high-energy X-ray energy spectrum resolution and obtain higher diffraction efficiency, the groove depth (the height of a gold grating line) is required to be increased to more than 500nm on the basis of improving the linear density of the grating, and the straightness and smoothness of the side wall of the grating line are required to be ensured.
In the prior art, two methods for manufacturing the X-ray gold transmission grating are provided, namely holographic photoetching-electroplating deposition and electron beam photoetching-electroplating deposition. The common point of the two process technologies is that a photoresist grating mask is firstly manufactured by photoetching, then gold is deposited in a mask grating groove, and finally the photoresist mask is removed to obtain a gold grating line. The height of the mask determines the groove depth of the finally manufactured gold grating, and the steepness and the roughness of the side wall of the grid line of the mask determines the steepness and the smoothness of the side wall of the gold grating obtained by electroplating, and finally influences the performance of the grating. However, the height of the photoresist mask for holographic lithography and electron beam lithography is limited, and especially for high linear density gratings, it is very difficult to produce a photoresist mask with a depth greater than 500nm, and the straightness and smoothness of the sidewalls of the lines of the mask grating for electroplating need to be improved.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art. Therefore, the invention provides a preparation method of an X-ray gold transmission grating, and aims to solve the problems that the gold transmission grating prepared by the prior art is small in groove depth, and the side wall of a grating line is not steep and smooth.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of an X-ray gold transmission grating comprises the following steps:
s1, taking an SOI silicon chip as a substrate, sequentially plating a gold film and a chromium film on the upper surface of the substrate, and plating a silicon nitride film on the lower surface of the substrate to form a substrate;
s2, respectively coating photoresist on the upper surface and the lower surface of the substrate, manufacturing a photoresist mask of a supporting structure on the upper surface of the substrate by utilizing ultraviolet lithography, and manufacturing a photoresist mask of a grating outer frame on the lower surface of the substrate;
s3, respectively removing the silicon nitride film and the chromium film in the non-mask areas on the upper surface and the lower surface of the substrate;
s4, removing the photoresist on the upper surface and the lower surface of the substrate;
s5, coating an anti-reflection film and a photoresist on the upper surface of the substrate in sequence;
s6, making a photoresist grating mask by holographic lithography, wherein the extension direction of the grating mask is vertical to the extension direction of the grating support structure;
s7, transferring the photoresist grating mask pattern into the antireflection film through reactive ion etching;
s8, transferring the photoresist grating mask pattern into the gold film through ion beam etching;
s9, removing the residual photoresist, antireflective film and chromium film on the upper surface of the substrate, and coating a protective adhesive on the lower surface;
s10, putting the substrate into etching liquid consisting of hydrofluoric acid and oxidant for metal catalytic etching;
s11, placing the substrate in a gold plating electrolyte, and electroplating and depositing gold on the upper surface;
s12, removing the protective glue on the lower surface of the substrate, and coating the protective glue on the upper surface of the substrate;
s13, etching the monocrystalline silicon in the non-mask area of the bottom layer;
s14, removing the protective glue on the upper surface;
s15, etching the top monocrystalline silicon;
s16, removing the silicon nitride and the middle SiO in the window2And cleaning and drying the layer to obtain the X-ray gold transmission grating.
And the gold film in the step S1 is deposited by adopting a magnetron sputtering, ion beam sputtering or electron beam evaporation coating method, and the film thickness is 15 nm-30 nm.
In the step S3, the silicon nitride film is etched on the lower surface of the substrate by using reactive ions, and the chromium film is etched on the upper surface by using a chromium removing solution.
And in the step S10, the oxidant is hydrogen peroxide, potassium permanganate or silver nitrate.
The concentration of the hydrofluoric acid in the step S10 is 4-6 mol/L, the concentration of the hydrogen peroxide is 0.2-0.3 mol/L, and the temperature of the etching solution is 5-15 ℃.
The structural parameters of the SOI silicon wafer are as follows: the top layer of monocrystalline silicon is<100>Crystal orientation, the middle layer is SiO2The underlying monocrystalline silicon is<100>And (4) crystal orientation.
The mask pattern of the grating support structure is a line array, the period is selected to be 10-20 microns, and the line width is 2-3 microns.
The mask image of the grating outer frame is an orthogonal grid, the width of the grid bars is 1-2 mm, and the interval of the grid bars is 4-6 mm.
The etching solution in the steps S13 and S15 adopts 25% KOH aqueous solution by mass, and the etching temperature is 85 ℃.
The invention has the beneficial effects that: the invention firstly uses the metal catalytic etching technology to manufacture the silicon grating mask with large groove depth and steep and smooth side wall, then the gold is electroplated and deposited in the silicon grating mask groove, and finally the silicon grating mask is removed to obtain the gold transmission grating with large groove depth and steep and smooth side wall. The etching direction of the metal catalytic etching is vertical to the surface of the silicon wafer and faces downwards, the side wall of the manufactured grating is steep, the etching depth is not limited, and the etching depth can be determined by the reaction time; the metal catalytic etching is a wet etching method, and the side wall of the grating is extremely smooth and can reach 1nm RMS magnitude. In general, compared with the prior art, the beneficial technical effects of the invention are as follows: can manufacture the gold transmission grating with large groove depth, steep and smooth side wall.
Drawings
The description includes the following figures, the contents shown are respectively:
FIG. 1 is a structural cross-sectional view of an SOI substrate provided by the present invention;
FIG. 2 is a cross-sectional view of the substrate with Au and Cr plated on the upper surface and silicon nitride plated on the lower surface;
FIG. 3 is a cross-sectional view of a structure of a photoresist mask with a support structure formed on the upper surface and a photoresist mask with a grating outer frame formed on the lower surface according to the present invention;
FIG. 4 is a cross-sectional view of the structure after etching a silicon nitride film on the lower surface and etching a Cr film on the upper surface according to the present invention;
FIG. 5 is a cross-sectional view of the structure after the photoresist has been removed according to the present invention;
FIG. 6 is a cross-sectional view of a structure in which an antireflective film and a photoresist are sequentially coated on an upper surface provided by the present invention;
FIG. 7 is a cross-sectional view of a structure of a photoresist grating mask produced by holographic lithography according to the present invention;
FIG. 8 is a cross-sectional view of the structure after transferring a photoresist grating mask to an antireflective film as provided by the present invention;
FIG. 9 is a cross-sectional view of the structure after transferring a photoresist grating mask to a gold film according to the present invention;
FIG. 10 is a cross-sectional view of the structure provided by the present invention with the photoresist, antireflective film and Cr film removed from the top surface;
FIG. 11 is a cross-sectional view of a structure of the present invention in which a protective adhesive is coated on a lower surface thereof;
FIG. 12 is a cross-sectional view of the structure after a top surface metal catalytic etching process provided by the present invention;
FIG. 13 is a cross-sectional view of the structure after gold is electroplated on the upper surface;
FIG. 14 is a cross-sectional view of the structure provided by the present invention, in which the protective adhesive is removed from the lower surface and the protective adhesive is coated on the upper surface;
FIG. 15 is a cross-sectional view of the structure provided by the present invention after etching of the bottom layer of monocrystalline silicon;
FIG. 16 is a cross-sectional view of the structure of the present invention with the protective glue removed from the top surface;
FIG. 17 is a cross-sectional view of the structure provided by the present invention after etching of the top layer of single crystal silicon on the upper surface;
FIG. 18 is a cross-sectional structural view of an X-ray gold transmission grating provided by the present invention after removal of the silicon nitride, intermediate SiO2 layer within the window.
Labeled as:
1. top layer monocrystalline silicon; 2. intermediate layer of SiO2(ii) a 3. Bottom layer monocrystalline silicon; 4. a SiN film; 5. an Au film; 6. a Cr film; 7. photoresist; 8. a antireflection film; 9. and (5) protective glue.
Detailed Description
The following detailed description of the embodiments of the present invention will be given with reference to the accompanying drawings for a purpose of helping those skilled in the art to more fully, accurately and deeply understand the concept and technical solution of the present invention and to facilitate its implementation. It should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
As shown in fig. 1 to 18, the present invention provides a method for preparing an X-ray gold transmission grating, which comprises the following steps:
and S1, taking the SOI silicon wafer as a substrate, sequentially plating a gold film and a chromium film on the upper surface of the substrate, and plating a silicon nitride film on the lower surface of the substrate to form the substrate.
As shown in FIG. 1, it is a structural cross-sectional view of an SOI silicon wafer composed of a top layer of single crystal silicon 1 and an intermediate layer of SiO 22 and a bottom layer of monocrystalline silicon 3. in the embodiment of the invention, the top layer of monocrystalline silicon can be<110>The crystal orientation,<111>Crystal orientation or<100>Crystal orientation of wherein<100>The top layer of the crystal orientation has the best effect, and the bottom layer of the crystal orientation can be monocrystalline silicon<110>Crystal orientation or<100>And (4) crystal orientation. The structural parameters of the SOI silicon wafer adopted in the embodiment of the invention are as follows: the top layer of monocrystalline silicon is<100>The crystal orientation is 2-10 microns thick; intermediate layer of SiO2The thickness of (A) is 1-2 microns; the bottom layer of monocrystalline silicon is<100>Crystal orientation, thickness of 300-500 micron, wherein, top layer monocrystalline silicon, middle layer SiO2And the thickness of the underlying single crystal silicon is designed based on the requirements of the product, SOI silicon is commercially available from Ultrasil Corporation, which can be customized to the customer's needs, with a silicon diameter of 4 inches being typically chosen.
FIG. 2 is a cross-sectional view of a substrate with an Au film 5 and a Cr film 6 plated on the upper surface and a SiN film 4 (silicon nitride film) plated on the lower surface, according to an embodiment of the present invention, wherein the Au film is deposited by magnetron sputtering, ion beam sputtering, or electron beam evaporation, and the thickness of the Au film is 15nm to 30 nm; because the Cr film is easy to be stripped from the SOI silicon wafer under the action of the Cr removing liquid, the Cr film is used as an intermediate layer of a transfer grating supporting structure, the Cr film is plated by adopting an electron beam evaporation or ion beam sputtering method, the thickness of the Cr film must be larger than that of the catalytic metal so as to protect the catalytic metal under the Cr film from being etched, and experiments prove that the requirement can be met when the thickness is larger than 100 nm; the silicon nitride film and the monocrystalline silicon have similar structures, so that the silicon nitride film and the monocrystalline silicon have strong adhesive force, the silicon nitride film and the monocrystalline silicon do not fall off in the later ultrasonic cleaning process, and the silicon nitride does not react with the potassium hydroxide etching solution for windowing the lower surface of the silicon wafer, so that the silicon nitride film is used as a protective layer for manufacturing the grating outer frame structure, and can be plated by adopting a PECVD (plasma enhanced chemical vapor deposition) method, and the thickness is more than 40 nm.
And S2, respectively coating photoresist on the upper surface and the lower surface of the substrate, manufacturing a photoresist mask of a supporting structure on the upper surface of the substrate by utilizing ultraviolet lithography, and manufacturing a photoresist mask of a grating outer frame on the lower surface of the substrate.
FIG. 3 is a structural cross-sectional view of a grating support structure mask made on the upper surface and a grating outer frame mask made on the lower surface, wherein the grating support structure mask is a line array, the period is preferably 10-20 micrometers, the line width is 2-3 micrometers, the grating outer frame mask image is an orthogonal grid, the width of the grid bars is 1-2 millimeters, and the interval of the grid bars is 4-6 millimeters.
The photoresist is a positive photoresist, such as AZ MIR-701, the coating thickness (500-1000) nm is preferred, the photoresist is coated by using a rotary coating method, and the thickness can be adjusted by adjusting the rotating speed and the proportion of a solvent in the photoresist according to the use instruction of the photoresist. The gluing process is as follows: coating the surface, and baking; then coating the lower surface, and then baking the glue. The baking condition can refer to the photoresist application instruction, and for the AZ MIR-701 photoresist, the single baking parameter is baking for 2 minutes at 90 ℃ of a hot table. The ultraviolet lithography uses a URE-2000/35 type ultraviolet lithography machine of photoelectric technology research institute of Chinese academy of sciences, and the specific process conditions can refer to the photoresist use instruction and the lithography machine use instruction. Because the selected positive photoresist is adopted, the pattern of the photoetching mask is consistent with the target pattern. The process of ultraviolet photoetching comprises the following steps: exposing the upper surface in a contact manner; lower surface contact exposure; and (6) developing.
S3, removing the silicon nitride film and the chromium film in the non-mask areas on the upper surface and the lower surface of the substrate respectively.
FIG. 4 is a cross-sectional view of a structure in which a silicon nitride film is etched on a lower surface and a Cr film is etched on an upper surface according to an embodiment of the present invention; for the etching of the silicon nitride film, an ICP-98A type induction coupling plasma etching machine developed by microelectronics of Chinese academy of sciences is used, the etching depth of the silicon nitride film is controlled by controlling the flow rate of reaction gas, the power of an excitation power supply, the power of a bias power supply and the etching time, and a large number of experiments prove that for the silicon nitride film with the thickness of 40nm, the adopted etching conditions are shown in Table 1:
TABLE 1 silicon nitride etch parameter Table
And (3) etching the Cr film by using a Cr removing liquid wet method, wherein the Cr removing liquid is prepared by mixing cerium ammonium nitrate: glacial acetic acid: water is mixed according to the mass ratio of 20:3: 100. Since the etching is isotropic, the etching time cannot be too long, otherwise the lateral undercutting effect will cause the Cr mask lines to disappear. The specific etching time can be obtained by experiment.
And S4, removing the photoresist on the upper surface and the lower surface of the substrate.
The photoresist on the upper surface and the lower surface is removed by acetone ultrasonic, and the structural cross-sectional view after the photoresist is removed is shown in fig. 5.
And S5, coating the antireflective film and the photoresist on the upper surface of the substrate in sequence.
FIG. 6 is a cross-sectional view of a structure with an antireflection film and a photoresist sequentially coated on the upper surface according to an embodiment of the present invention, in order to reduce the standing wave effect in holographic exposure, before coating the photoresist 7, an antireflection film 8 is coated on the prepared substrate, and the antireflection film is selected from Brewer Science, Inc
In series, AZ MIR-701 is selected as the positive photoresist. The thickness of the antireflective film is about 150nm, and the thickness of the photoresist is about 300 nm. The specific process conditions can refer to the application specifications of the antireflective film and the photoresist.
And S6, holographic photoetching is carried out to manufacture a photoresist grating mask, and the extension direction of the grating mask is vertical to the extension direction of the grating support structure.
Fig. 7 is a cross-sectional view of a structure of a grating mask manufactured by holographic lithography according to an embodiment of the present invention, which is obtained by performing holographic exposure on an exposure light path of a laemon lens, developing the exposure light path to obtain a photoresist grating mask, wherein an extending direction of the support structure mask is parallel to an optical platform during exposure, and an extending direction of interference fringes that generate a pattern of the photoresist grating mask is perpendicular to the optical platform, so that the photoresist grating mask obtained by development is naturally perpendicular to the support structure, and the holographic lithography is a conventional process means, and detailed description of a specific operation process is omitted.
S7, transferring the photoresist grating mask pattern into the antireflective film by reactive ion etching.
Fig. 8 is a cross-sectional view of the structure for transferring a photoresist grating mask to an antireflective film according to an embodiment of the present invention, in which an ICP-98A inductively coupled plasma etcher developed by microelectronics of the chinese academy of sciences is used, the etching depth of the antireflective film is controlled by controlling the flow rate of the reaction gas, the power of the excitation power supply, the power of the bias power supply, and the etching time, and finally the photoresist grating mask pattern is transferred to the antireflective film to form an antireflective film 8 of a grating structure, and for a 150nm ARC film, the etching conditions are as shown in table 2:
TABLE 2 ARC etch parameter Table
S8, transferring the photoresist grating mask pattern into the gold film by ion beam etching.
Fig. 9 is a cross-sectional view of the structure after transferring the photoresist grating mask to the gold film according to the embodiment of the present invention, in which the photoresist grating mask pattern is transferred to the gold film by using the conventional ion beam etching.
S9, removing the residual photoresist, antireflection film and chromium film on the upper surface of the substrate, and coating protective glue on the lower surface.
FIG. 10 shows an embodiment of the present inventionProviding a structural sectional view after removing the photoresist, the antireflective film and the Cr film; specifically, the photoresist and the antireflective coating (ARC) are removed by using an acetone ultrasonic method, and the Cr coating is removed by using a Cr removing liquid ultrasonic method. FIG. 11 is a cross-sectional view of a structure of a lower surface coated with a protective adhesive according to an embodiment of the present invention, wherein the protective adhesive 9 is selected from Brewer Science
And (5) protective glue. First coating
Primer, recoating
The specific process conditions can refer to the use specification.
S10, putting the substrate into etching liquid composed of hydrofluoric acid and oxidant to perform metal catalytic etching.
Fig. 12 is a cross-sectional view of the structure after the catalytic etching process of the upper surface metal provided by the present invention. The oxidant can be hydrogen peroxide, potassium permanganate or silver nitrate, the concentration and the etching temperature of each component of the specific etching solution can be obtained through a contrast experiment, the optimal target is to etch a grating structure with a smooth and steep side wall, the hydrogen peroxide is taken as the oxidant for example, the concentration of hydrofluoric acid in the etching solution is (4-6) mol/L, the concentration of hydrogen peroxide is (0.2-0.3) mol/L, when the temperature of the etching solution is (5-15) DEG C, the obtained grating structure is steep and the side wall is smooth, the roughness of the grating side wall is about 1nm, the etching time is determined by the etching depth and the etching rate, the etching depth is the thickness of the top silicon, and the etching rate can be measured through experiments.
S11, putting the substrate in the gold plating electrolyte, and electroplating and depositing gold on the upper surface. FIG. 13 is a cross-sectional view of the structure after gold is electroplated on the upper surface.
And S12, removing the protective glue on the lower surface of the substrate, and coating the protective glue on the upper surface of the substrate.
Removing alkali-resistant protective glue with Piranha solution, and removing in water bath at 80 deg.C for 30 minAnd 14, the structural cross-sectional view is provided after the protective adhesive is removed from the lower surface and coated on the upper surface. The protective adhesive 9 is prepared from Brewer Science
And (5) protective glue. First coating
Primer, recoating
The specific process conditions can refer to the use specification.
And S13, etching away the monocrystalline silicon in the non-mask area of the bottom layer.
Fig. 15 is a cross-sectional view of the structure after etching the lower surface single crystal silicon according to the embodiment of the present invention, in which a KOH aqueous solution with a mass fraction of 30% is used as an etching solution, the etching temperature is 80 ℃, and the etching time is longer than 6 hours. Etching to intermediate SiO2In the case of the layer, a smooth bottom surface is visible, at which point the etching can be stopped.
And S14, removing the protective glue on the upper surface.
The alkali-resistant protective glue is removed by using a Piranha solution, the alkali-resistant protective glue can be removed by water bath for 30 minutes at the water bath temperature of 80 ℃, and the structural cross-sectional view of the upper surface of the protective glue removed is shown in fig. 16.
S15, etching the top monocrystalline silicon;
fig. 17 is a cross-sectional view of the structure after etching the top-layer single-crystal silicon, which is provided by the embodiment of the present invention, and a KOH aqueous solution with a mass fraction of 30% is used as an etching solution, the etching temperature is 80 ℃, and the etching time is longer than 6 hours. Etching to intermediate SiO2In the case of the layer, a smooth bottom surface is visible, at which point the etching can be stopped.
S16, removing the silicon nitride and the middle SiO in the window2And cleaning and drying the layer to obtain the X-ray gold transmission grating.
Soaking in 48% hydrofluoric acid for 8 min to remove silicon nitride and SiO in the window2Layer, removal of silicon nitride and intermediate SiO2Structural section behind layerThe view is shown in fig. 18. And (3) cleaning with deionized water, and drying the sample by using a carbon dioxide critical point dryer so as to solve the problem of grating line adhesion caused by drying in the air. The dryer is a carbon dioxide critical point dryer of Quorum E3100 in UK, and the specific operation method can refer to the specification.
The invention firstly uses the metal catalytic etching technology to manufacture the silicon grating mask with large groove depth and steep and smooth side wall, then the gold is electroplated and deposited in the silicon grating mask groove, and finally the silicon grating mask is removed to obtain the gold transmission grating with large groove depth and steep and smooth side wall. The etching direction of the metal catalytic etching is vertical to the surface of the silicon wafer and faces downwards, the side wall of the manufactured grating is steep, the etching depth is not limited, and the etching depth can be determined by the reaction time; the metal catalytic etching is a wet etching method, and the side wall of the grating is extremely smooth and can reach 1nm RMS magnitude. In general, compared with the prior art, the beneficial technical effects of the invention are as follows: can manufacture the gold transmission grating with large groove depth, steep and smooth side wall.
The invention is described above with reference to the accompanying drawings. It is to be understood that the specific implementations of the invention are not limited in this respect. Various insubstantial improvements are made by adopting the method conception and the technical scheme of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.
Claims (9)
1. A preparation method of an X-ray gold transmission grating is characterized by comprising the following steps:
s1, taking an SOI silicon chip as a substrate, sequentially plating a gold film and a chromium film on the upper surface of the substrate, and plating a silicon nitride film on the lower surface of the substrate to form a substrate;
s2, respectively coating photoresist on the upper surface and the lower surface of the substrate, manufacturing a photoresist mask of a supporting structure on the upper surface of the substrate by utilizing ultraviolet lithography, and manufacturing a photoresist mask of a grating outer frame on the lower surface of the substrate;
s3, respectively removing the silicon nitride film and the chromium film in the non-mask areas on the upper surface and the lower surface of the substrate;
s4, removing the photoresist on the upper surface and the lower surface of the substrate;
s5, coating an anti-reflection film and a photoresist on the upper surface of the substrate in sequence;
s6, making a photoresist grating mask by holographic lithography, wherein the extension direction of the grating mask is vertical to the extension direction of the grating support structure;
s7, transferring the photoresist grating mask pattern into the antireflection film through reactive ion etching;
s8, transferring the photoresist grating mask pattern into the gold film through ion beam etching;
s9, removing the residual photoresist, antireflective film and chromium film on the upper surface of the substrate, and coating a protective adhesive on the lower surface;
s10, putting the substrate into etching liquid consisting of hydrofluoric acid and oxidant for metal catalytic etching;
s11, placing the substrate in a gold plating electrolyte, and electroplating and depositing gold on the upper surface;
s12, removing the protective glue on the lower surface of the substrate, and coating the protective glue on the upper surface of the substrate;
s13, etching the monocrystalline silicon in the non-mask area of the bottom layer;
s14, removing the protective glue on the upper surface;
s15, etching the top monocrystalline silicon;
s16, removing the silicon nitride and the middle SiO in the window2And cleaning and drying the layer to obtain the X-ray gold transmission grating.
2. The method for preparing an X-ray gold transmission grating as claimed in claim 1, wherein the gold film in step S1 is deposited by magnetron sputtering, ion beam sputtering or electron beam evaporation coating, and the thickness of the film is 15nm to 30 nm.
3. The method for manufacturing an X-ray gold transmission grating as claimed in claim 1, wherein in step S3, the silicon nitride film is etched on the lower surface of the substrate by using reactive ions, and the chrome film is etched on the upper surface by using a chrome removal solution.
4. The method for preparing an X-ray gold transmission grating as claimed in claim 1, wherein the oxidant in step S10 is hydrogen peroxide, potassium permanganate or silver nitrate.
5. The method for preparing an X-ray gold transmission grating as claimed in claim 4, wherein the concentration of hydrofluoric acid in the step S10 is 4mol/L to 6mol/L, the concentration of hydrogen peroxide is 0.2mol/L to 0.3mol/L, and the temperature of the etching solution is 5 ℃ to 15 ℃.
6. The method for preparing an X-ray gold transmission grating according to claim 1, wherein the structural parameters of the SOI silicon wafer are as follows: the top layer of monocrystalline silicon is<100>Crystal orientation, the middle layer is SiO2The underlying monocrystalline silicon is<100>And (4) crystal orientation.
7. The method of claim 1, wherein the mask pattern of the grating support structure is an array of lines with a period selected from 10-20 microns and a line width of 2-3 microns.
8. The method of claim 1, wherein the mask image of the outer frame of the grating is an orthogonal grid, the width of the grid bars is 1 mm to 2 mm, and the spacing between the grid bars is 4 mm to 6 mm.
9. The method for preparing an X-ray gold transmission grating as claimed in claim 1, wherein the etching solution in steps S13 and S15 is 25% KOH aqueous solution by mass, and the etching temperature is 85 ℃.
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