CN107403655B - X-ray neutral attenuation sheet and preparation method thereof - Google Patents
X-ray neutral attenuation sheet and preparation method thereof Download PDFInfo
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- CN107403655B CN107403655B CN201710684005.4A CN201710684005A CN107403655B CN 107403655 B CN107403655 B CN 107403655B CN 201710684005 A CN201710684005 A CN 201710684005A CN 107403655 B CN107403655 B CN 107403655B
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Abstract
The invention relates to an X-ray neutral attenuation sheet and a preparation method thereof, and relates to the field of quantitative measurement of soft X-ray radiation flow. The preparation method comprises the following steps: forming a first conductive metal layer on one side surface of the substrate; forming a photoresist layer on the surface of one side of the first conductive metal layer, which is far away from the substrate, forming a hole array on the photoresist layer after exposure and development, electroplating the photoresist layer with the hole array to form a second conductive metal layer, and removing the residual photoresist to obtain a sample with the hole array; and removing the substrate and the first conductive metal layer. The surface uniformity, the attenuation characteristic and the production efficiency of the X-ray neutral attenuation sheet are effectively improved. The X-ray neutral attenuation sheet prepared by the preparation method has the advantages that the aperture of each hole in the hole array is uniform, the side wall of each hole is steep, and the surface uniformity of the X-ray neutral attenuation sheet is good, so that the X-ray transmittance has high consistency, and the quantitative and accurate measurement of the soft X-ray radiation flow can be realized.
Description
Technical Field
The invention relates to the field of soft X-ray radiation flow quantitative measurement, in particular to an X-ray neutral attenuation sheet and a preparation method thereof.
Background
In the field of inertial confinement fusion, black cavity physics, radiation transport, radiation ablation, radio opacity, and implosion dynamics all require quantitative measurements of soft X-ray radiation flux. The measurement of radiation flux typically employs an X-ray flat response X-ray diode (XRD) detector. During the measurement process, fragments generated by laser targeting can adhere to the composite filter or penetrate through the filter, so that the measurement accuracy of the radiant flow is influenced; on the other hand, as the laser energy increases, the radiation flux increases causing the flat response detector to operate in a nonlinear region, beyond the detector operating range. Therefore, neutral attenuation plates are employed to eliminate debris effects and detector saturation problems.
the neutral attenuation sheet has the characteristic of attenuating X-rays, can uniformly attenuate the X-rays which pass through different wave bands, and ensures that light spots transmitted to the XRD detector have high uniformity.
The traditional neutral attenuation sheet adopts a laser drilling mode to realize a uniform hole array so as to achieve the attenuation effect on X rays, but has the following defects: (1) poor surface uniformity: the laser drilling method is to realize drilling by ablating the tantalum sheet by laser, and due to the limitation of light spots and the instability of thermal ablation, the aperture prepared by laser drilling is not uniform, and the surface uniformity of the attenuation sheet is poor (2) the phenomenon of taper hole: the hole prepared by the micro laser drilling mode is a taper hole due to long surface ablation time and short bottom ablation time, so that an X-ray transmittance curve has a certain slope, is not a fixed numerical value and cannot be regarded as a neutral attenuation sheet. (3) The preparation efficiency is low: the mode efficiency of laser drilling is lower, and along with effective area's increase, the number of holes sharply increases, leads to the time of punching to increase, has reduced production efficiency.
Disclosure of Invention
The invention aims to provide an X-ray neutral attenuation sheet which is provided with a uniform hole array, wherein the hole diameter of each hole in the hole array is uniform, the side wall of each hole is steep, the surface uniformity of the X-ray neutral attenuation sheet is good, the X-ray transmittance is highly consistent, and the quantitative and accurate measurement of soft X-ray radiation flow can be realized.
The invention also aims to provide a preparation method of the X-ray neutral attenuation sheet, which can effectively improve the surface uniformity, attenuation characteristics and production efficiency of the X-ray neutral attenuation sheet.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of an X-ray neutral attenuation sheet, which comprises the following steps:
A first conductive metal layer is formed on one side surface of the substrate.
And forming a photoresist layer on the surface of one side of the first conductive metal layer, which is far away from the substrate, forming a hole array on the photoresist layer after exposure and development, electroplating the photoresist layer with the hole array to form a second conductive metal layer, and removing the residual photoresist to obtain a sample with the hole array.
And removing the substrate and the first conductive metal layer.
The invention provides an X-ray neutral attenuation sheet prepared by the preparation method.
The X-ray neutral attenuation sheet and the preparation method thereof provided by the embodiment of the invention have the beneficial effects that:
By combining photoetching and micro-electroplating processes, the X-ray neutral attenuation sheet with the uniform hole array is prepared, the punching efficiency is effectively improved, the production efficiency is improved, the aperture of each hole is uniform, the surface uniformity of the attenuation sheet is good, the problem of the taper hole phenomenon is effectively solved, and finally the precision of the X-ray neutral attenuation sheet is improved.
The X-ray neutral attenuation sheet prepared by the method has a uniform hole array, the aperture of each hole in the hole array is uniform, the side wall of each hole is steep, the surface uniformity of the X-ray neutral attenuation sheet is good, the X-ray transmittance has high consistency, and the quantitative and accurate measurement of soft X-ray radiation flow can be realized.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic flow chart of a method for manufacturing an X-ray neutral attenuation sheet according to a preferred embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an X-ray neutral attenuator according to a preferred embodiment of the present invention;
FIG. 3 illustrates surface uniformity data for an X-ray neutral attenuator, according to a preferred embodiment of the present invention;
FIG. 4 is a surface micrograph of an X-ray neutral attenuator plate according to a preferred embodiment of the present invention;
FIG. 5 shows the X-ray transmittance of the X-ray neutral attenuator according to the preferred embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
the X-ray neutral attenuation sheet and the method for manufacturing the same according to the embodiments of the present invention will be specifically described below.
Referring to fig. 1, a method for preparing an X-ray neutral attenuation sheet includes:
a) a first conductive metal layer is formed on one side surface of the substrate.
b) And forming a photoresist layer on the surface of one side of the first conductive metal layer, which is far away from the substrate, exposing and developing to form a hole array on the photoresist layer, electroplating the photoresist layer with the hole array to form a second conductive metal layer, and removing the residual photoresist to obtain a sample with the hole array.
c) And removing the substrate and the first conductive metal layer in the sample.
Specifically, in the step a), the substrate is a silicon oxide wafer, so that subsequent removal is facilitated.
The first conductive metal layer is formed on the substrate through deposition of a magnetron sputtering process and serves as an electroplating seed layer, wherein the magnetron sputtering process can effectively improve the film coating efficiency, and meanwhile, the surface of the first conductive metal layer is smooth and easy to form.
The first conductive metal layer may be copper, gold, silver, or the like, for example, the first conductive metal layer may be copper or gold. The first conductive metal layer can be used as a corrosion barrier layer in the subsequent substrate corrosion process, so that the precision of a final product is effectively guaranteed, and the chemical property of gold is more stable, so that the first conductive metal layer is more preferably gold.
Meanwhile, the thickness of the first conductive metal layer is 20-50 nm; and/or the thickness of the second conductive metal layer is more than or equal to 20 mu m. That is, when the thickness of the first conductive metal layer is 20 to 50nm, for example, the thickness of the first conductive metal layer is 20nm, 25nm, 30nm, 40nm, 45nm, or 50nm, the thickness of the second conductive metal layer may be not less than 20 μm, or less than 20 μm.
The second conductive metal layer may be copper, gold, silver, or the like, for example, the second conductive metal layer may be copper or gold. Preferably, the second conductive metal layer is a final product, but stress exists inside the second conductive metal layer, so wrinkles are easily generated due to the stress in the production process, and the precision and the yield of the product are affected.
More preferably, the first conductive metal layer is made of gold, the second conductive metal layer is made of gold, the yield of the X-ray neutral attenuation sheet is effectively improved, the removal in the step d) is facilitated, meanwhile, the removed second conductive metal layer does not have metal infiltration, and the accuracy of the X-ray neutral attenuation sheet is effectively guaranteed.
In step b), the photoresist layer is pre-baked before exposure and is post-baked after exposure, so that the photoresist is effectively shaped. Preferably, in a preferred embodiment of the present invention, the pre-baking is: baking at 55-65 deg.C for 13-20min, and baking at 85-95 deg.C for 30-40 min; more preferably, the prebaking is: and after baking at 60 ℃ for 15min and baking at 90 ℃ for 35min, the solvent in the photoresist is effectively removed, meanwhile, the adhesiveness of the photoresist is enhanced, the stress in the photoresist film is released, and the photoresist is prevented from staining the equipment.
Preferably, in a preferred embodiment of the present invention, the post-baking is: baking at 65-75 deg.C for 13-20min, and baking at 85-95 deg.C for 45-55 min; more preferably, the postbaking is: and after the photoresist is baked at 65 ℃ for 15min and at 90 ℃ for 50min, the solvent in the photoresist is effectively evaporated, so that the photoresist is hardened and solidified, and the subsequent development and electroplating are facilitated.
Preferably the photoresist is at least 20 μm thick, i.e. the photoresist is a thick resist, so preferably uv lithography is used, more preferably the exposure is uv exposure for 20-30 s. Therefore, the photoresist is preferably SU-8 photoresist or AZ4620 photoresist, more preferably SU-8 photoresist, and the photoresist has better photoetching effect after the thick photoresist is formed.
specifically, the development time is 2.7-3.3min, and the performance of the finally prepared X-ray neutral attenuation sheet is prevented from being influenced by insufficient development, incomplete development and over development caused by overlong development time due to too short development time.
The developing solution corresponding to the photoresist, for example, a developing solution dedicated to SU-8 corresponding to SU-8 photoresist is used to perform development, that is, the soluble photoresist is dissolved away by the developing solution, and the hole array is formed in the photoresist layer. Wherein, the hole array is formed by uniformly forming an array by a plurality of columns. Preferably, each cylinder has a diameter of 30-40 μm; preferably, each cylinder has a diameter of 35 μm; and/or the distance between the axes of any two adjacent cylinders is 80-120 μm; more preferably, the distance between the axes of any two adjacent cylinders is 100 μm, so that the finally prepared X-ray neutral attenuation sheet has better light transmittance and effectively attenuates X-rays.
And electroplating the photoresist layer with the hole array to form a second conductive metal layer, wherein the electroplating rate is controlled to be 2.5-3.5 mu m/h, and more preferably, the electroplating rate is controlled to be 3 mu m/h, and the second conductive metal layer is uniformly electroplated, so that the second conductive metal layer has high forming rate and a smooth surface. Then, the remaining photoresist is removed to obtain a sample with an array of holes.
Where the array of holes on the sample is complementary to the array of holes on the photoresist layer to form a complete entity, i.e. each hole in the array of holes on the sample corresponds one-to-one to each cylinder in the array of holes on the photoresist layer. That is, in the hole array on the sample, the hole diameter of each hole is 30-40 μm; preferably, the pore size of each pore is 35 μm; and/or the hole spacing of any two adjacent holes is 80-120 mu m; preferably, the hole spacing between any two adjacent holes is 100 μm, so that the finally prepared X-ray neutral attenuation sheet has better light transmittance and effectively attenuates X-rays.
Preferably, the second conductive metal layer is electroplated and then soaked in an NMP solution, so that the remaining photoresist can be effectively removed, and the second conductive metal layer, the first metal material layer and the substrate are not affected.
In the preferred embodiment of the present invention, the X-ray neutral attenuator is used alone, and in order to ensure that the X-ray neutral attenuator can maintain a better accuracy for a long time, the sample is preferably annealed before the substrate and the first conductive metal layer are removed; more preferably, the annealing treatment is carried out at 145-160 ℃ for 2.5-4 h; more preferably, the annealing treatment is carried out at 150 ℃ for 3h, so as to effectively remove internal stress and keep the precision for a longer time.
And after annealing treatment, removing the substrate and the first conductive metal layer to obtain the X-ray neutral attenuation sheet.
In the preferred embodiment of the present invention, the substrate is removed by acid etching; preferably, the acid is prepared from a mixture of 2-7: 1, for example, a volume ratio of 2: 1. 3: 1. 4: 1. 5: 1. 6: 1 or 7:1, wherein the hydrofluoric acid is commercially available hydrofluoric acid, and the concentrated nitric acid is commercially available concentrated nitric acid, and the ratio is not limited herein. Meanwhile, when the substrate is removed through acid corrosion, the first conductive metal layer can be used as a corrosion barrier layer, and the second conductive metal layer is prevented from being corroded by acid to influence the precision of a final product.
And after removing the substrate, soaking the substrate in alcohol for ultrasonic cleaning for 10-23min, and removing the first conductive metal layer. Preferably, the first conductive metal layer is removed, and the X-ray neutral attenuation sheets with different specifications can be obtained by laser scribing.
Referring to fig. 2, the present invention further provides an X-ray neutral attenuation sheet manufactured by the above method, which has a uniform hole array, wherein the aperture of each hole in the hole array is uniform, the sidewall of the hole is steep, and the surface uniformity of the X-ray neutral attenuation sheet is good, such that the X-ray transmittance has high uniformity, and the quantitative and accurate measurement of the soft X-ray radiation flux can be achieved.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
An X-ray neutral attenuation sheet, which is prepared by the following method:
1) a first conductive metal layer of 40nm was deposited on a 2 inch silicon oxide wafer by a magnetron sputtering process.
2) And spin-coating SU-8 photoresist with the thickness of 35 μm on the surface of the first conductive metal layer, which is far away from the substrate, drying at 60 ℃ for 15min, drying at 90 ℃ for 35min, performing ultraviolet exposure for 24s, drying at 65 ℃ for 15min, drying at 90 ℃ for 50min, developing with SU-8 special developer for 3min, and forming a hole array consisting of cylinders on the photoresist layer.
3) after the photoresist layer with the hole array is electroplated with the second conductive metal layer with the thickness of 20 microns at the speed of 3 microns/h by adopting a pulse micro-electroplating process, the residual photoresist is removed by soaking in an NMP solution, and a sample with the hole array is obtained.
Wherein each well in the array of wells of the sample has an aperture diameter of 35 μm and the spacing between any two adjacent wells is 100 μm.
4) Keeping the temperature of a sample at 150 ℃ for 3h for annealing treatment, corroding the silicon wafer by using a mixed solution of hydrofluoric acid and concentrated nitric acid in a volume ratio of 4:1, placing the silicon wafer into alcohol for ultrasonic cleaning for 15min after the corrosion is automatically stopped on the first conductive metal material layer, removing the first conductive metal material layer, and performing laser scribing to obtain the X-ray neutral attenuation sheet.
The first conductive metal layer and the second conductive metal layer are gold layers.
Example 2
An X-ray neutral attenuation sheet, which is prepared by the following method:
1) A first conductive metal layer of 50nm was deposited on a 2 inch silicon oxide wafer by a magnetron sputtering process.
2) and spin-coating SU-8 photoresist with the thickness of 25 μm on the surface of the first conductive metal layer, which is far away from the substrate, drying at 55 ℃ for 13min, drying at 85 ℃ for 30min, performing ultraviolet exposure for 26s, drying at 65 ℃ for 16min, drying at 85 ℃ for 40min, developing with SU-8 special developer for 2.7min, and forming a hole array consisting of cylinders on the photoresist layer.
3) After a 25 mu m second conductive metal layer is electroplated on the photoresist layer with the hole array by adopting a pulse micro-electroplating process at the speed of 2.5 mu m/h, residual photoresist is removed by soaking in NMP solution, and a sample with the hole array is obtained.
Wherein the aperture of each well in the well array of the sample is 30 μm and the well spacing of any two adjacent wells is 84 μm.
4) Keeping the temperature of a sample at 145 ℃ for 4h for annealing treatment, corroding the silicon wafer by using a mixed solution of hydrofluoric acid and concentrated nitric acid in a volume ratio of 7:1, placing the silicon wafer into alcohol for ultrasonic cleaning for 15min after the corrosion is automatically stopped on the first conductive metal material layer, removing the first conductive metal material layer, and performing laser scribing to obtain the X-ray neutral attenuation sheet.
The first conductive metal layer and the second conductive metal layer are gold layers.
Example 3
An X-ray neutral attenuation sheet, which is prepared by the following method:
1) A first conductive metal layer of 20nm was deposited on a 2.5 inch silicon oxide wafer by a magnetron sputtering process.
2) and spin-coating SU-8 photoresist with the thickness of 40 μm on the surface of the first conductive metal layer, which is far away from the substrate, drying at 65 ℃ for 15min, drying at 95 ℃ for 30min, performing ultraviolet exposure for 27s, drying at 65 ℃ for 20min, drying at 90 ℃ for 52min, developing with SU-8 special developer for 3.4min, and forming a hole array consisting of cylinders on the photoresist layer.
3) After a 30 μm second conductive metal layer was electroplated on the photoresist layer having an array of holes consisting of cylinders using a pulse micro-electroplating process at a rate of 3.1 μm/h, the remaining photoresist was removed by soaking in an NMP solution to obtain a sample having an array of holes.
wherein the aperture of each well in the well array of the sample is 40 μm, and the well spacing of any two adjacent wells is 112 μm. The first conductive metal layer and the second conductive metal layer are both gold layers.
Test examples
The X-ray neutral attenuation sheet obtained by the invention is used for calibration measurement on a synchrotron radiation device of the institute of high-energy physics of the Chinese academy of sciences, and the surface uniformity of the X-ray neutral attenuation sheet in the energy region range of 70-1600eV is measured by utilizing a 4B7B beam line.
The specific measurement method comprises the following steps: and the X-ray neutral attenuation sheet moves in a direction vertical to the beam line according to fixed step length, and the photocurrents of different positions (sample 1# and sample 2#) on the surface of the X-ray neutral attenuation sheet are measured, so that the surface uniformity of the filter is characterized. The results are shown in FIG. 3. As can be seen from FIG. 3, the surface uniformity of the neutral damping sheet of the present invention is good, and the non-uniformity is within 1%.
The X-ray neutral attenuation sheet obtained by the invention is used for carrying out microscopic measurement on a transmission microscope, and a picture obtained by the measurement is shown in figure 4.
the X-ray neutral attenuation sheet obtained by the invention is used for calibration measurement on a synchrotron radiation device of the institute of high-energy physics of the Chinese academy of sciences, and the 4B7B beam is used for measuring the transmittance of the X-ray neutral attenuation sheet in the energy region range of 70-1600 eV.
The measuring method comprises the following steps: and (3) directly mounting the neutral attenuation sheet on a beam line for quantitative measurement, and comparing the intensity of the light source with the intensity of the light after penetrating through the neutral attenuation sheet to obtain the transmittance of the X-ray neutral attenuation sheet. The results are shown in FIG. 5.
as can be seen from FIG. 5, the X-ray neutral attenuation sheet provided by the invention has consistent attenuation characteristics to X-rays with different energies, and the transmittance of the X-ray neutral attenuation sheet in the energy region of 70-1600eV is 0.103 +/-0.002 (including the influence caused by instability of the light source).
In conclusion, the preparation method of the X-ray neutral attenuation sheet and the preparation method thereof provided by the invention have the advantages that the surface uniformity, the attenuation characteristic and the production efficiency of the X-ray neutral attenuation sheet are effectively improved, the surface uniformity of the prepared X-ray neutral attenuation sheet is good, the X-ray transmittance is highly consistent, and the quantitative and accurate measurement of the soft X-ray radiation flow can be realized.
the embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (17)
1. a method for preparing an X-ray neutral attenuation sheet is characterized by comprising the following steps:
Forming a first conductive metal layer on one side surface of the substrate;
Forming a photoresist layer on the surface of one side of the first conductive metal layer, which is far away from the substrate, forming a hole array on the photoresist layer after exposure and development, electroplating the photoresist layer with the hole array to form a second conductive metal layer, and removing the residual photoresist to obtain a sample with the hole array;
Removing the substrate and the first conductive metal layer;
The thickness of the photoresist layer is at least 20 μm;
The material of the first conductive metal layer is the same as that of the second conductive metal layer; and before removing the substrate and the first conductive metal layer, carrying out annealing treatment on the sample, wherein the annealing treatment is carried out at 145-160 ℃ for 2.5-4 h.
2. The method of claim 1, wherein the annealing treatment is carried out at 150 ℃ for 3 hours.
3. The method according to claim 1, wherein the first conductive metal layer is made of gold or copper; and/or the second conductive metal layer is made of gold or copper.
4. The method according to claim 1, wherein the first conductive metal layer is made of gold, and the second conductive metal layer is made of gold.
5. The production method according to claim 1, wherein the sample has an array of wells each having a pore diameter of 30 to 40 μm; and/or the hole spacing of any two adjacent holes is 80-120 μm.
6. The production method according to claim 5, wherein each of the pores has a pore diameter of 35 μm;
And/or the hole spacing between any two adjacent holes is 100 μm.
7. The production method according to claim 1,
and pre-baking the photoresist layer before exposure, and post-baking the photoresist layer after exposure.
8. the method of claim 7, wherein the pre-baking is: baking at 55-65 deg.C for 13-20min, and baking at 85-95 deg.C for 30-40 min.
9. The method of claim 7, wherein the post-baking is: baking at 65-75 deg.C for 13-20min, and baking at 85-95 deg.C for 45-55 min.
10. The method of claim 1, wherein the exposure is ultraviolet exposure for 20 to 30 seconds.
11. The production method according to claim 1, wherein the photoresist is SU-8 photoresist or AZ4620 photoresist.
12. the production method according to claim 1, wherein the thickness of the first conductive metal layer is 20 to 50 nm; and/or the presence of a gas in the gas,
The thickness of the second conductive metal layer is more than or equal to 20 mu m.
13. the method according to claim 1, wherein the second conductive metal layer is plated and then dipped in an NMP solution to remove the remaining photoresist.
14. The production method according to claim 1, wherein the substrate is removed by acid etching.
15. The method of claim 14, wherein the acid is prepared from a mixture of acids in a volume ratio of 2-7: 1 hydrofluoric acid and concentrated nitric acid.
16. The method of claim 14, wherein the first conductive metal layer is removed by immersing the substrate in alcohol and ultrasonically cleaning the substrate for 10 to 23 minutes.
17. An X-ray neutral attenuation sheet produced by the production method according to any one of claims 1 to 16.
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| CN107833820A (en) * | 2017-11-30 | 2018-03-23 | 中国工程物理研究院激光聚变研究中心 | A kind of new single channel x-ray diode detection system |
| CN111933327B (en) * | 2020-07-26 | 2022-10-25 | 同济大学 | Metal film filter disc with supporting structure and preparation thereof |
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