CN109827981B - Preparation method of X-ray all-optical solid ultrafast detection chip modulation grating and grating - Google Patents
Preparation method of X-ray all-optical solid ultrafast detection chip modulation grating and grating Download PDFInfo
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Abstract
The invention belongs to the field of ultrafast diagnosis, and provides a preparation method of an X-ray all-optical solid ultrafast detection chip modulation grating and a grating, which solve the problems that the modulation grating prepared by the prior art has a thin metal layer, is difficult to prepare a grating with a high depth-to-width ratio and cannot well realize the effect of blocking X-rays, and the method comprises the following steps: taking an epitaxial surface of an epitaxial wafer of an all-optical solid ultra-fast detection chip as a substrate of a grating material, and selecting a proper grating material, wherein the grating material is a metal material capable of effectively absorbing X-rays; step two, preparing a conductive metal module on the substrate to form a seed layer; preparing a glue film on the seed layer, and photoetching by using SU-8 glue to form a glue grating structure; step four, performing micro-electroplating on the substrate with the glue grating structure to form a metal grating structure; and step five, removing SU-8 glue to obtain the metal grating.
Description
Technical Field
The invention belongs to the field of ultrafast diagnosis, and particularly relates to a preparation method of an X-ray all-optical solid ultrafast detection chip modulation grating and a grating prepared by the method, which are applied to X-ray waveband ultrafast signal detection.
Background
The all-optical solid ultrafast diagnosis technology has ultrahigh time and spatial resolution, and refers to that an ultrafast semiconductor chip is adopted to detect a corresponding signal to be detected, so that light-light conversion is realized, when signal light is incident on the ultrafast detection chip, an unbalanced carrier is generated, the unbalanced carrier is modulated by a surface grating structure of the chip, an instantaneous refractive index spatial distribution pattern corresponding to the incident light is formed inside the detection chip, the spatial distribution pattern corresponds to the grating structure, and then probe light pulses are adopted to read out signal light information.
For an X-ray all-optical solid ultrafast detection chip, an X-ray modulation amplitude grating is prepared on the surface of a semiconductor ultrafast response material, when an X-ray is incident to the surface of the chip, a phase grating related to carrier concentration is formed in the semiconductor material due to the blocking of the grating on part of the X-ray, so that the modulation of probe light of incident light in the opposite direction is realized, a diffraction signal is generated, and the extraction of signal light information is completed. Therefore, the modulation grating on the surface of the chip is an important component of the X-ray all-optical solid ultrafast detection chip.
The modulation grating prepared by the process has a thin metal layer, is difficult to prepare the grating with a high depth-to-width ratio, and cannot well realize the blocking effect on X rays.
Disclosure of Invention
The invention aims to solve the problems that a metal layer of a modulation grating prepared by the prior art is thin, the grating with a high depth-to-width ratio is difficult to prepare, and the blocking effect on X-rays cannot be well realized, and provides a preparation method of an X-ray all-optical solid ultrafast detection chip modulation grating and a grating prepared by the method, which are applied to the ultrafast signal detection of an X-ray waveband.
The technical scheme of the invention is as follows: a preparation method of an X-ray all-optical solid ultrafast detection chip modulation grating is characterized by comprising the following steps:
step one, selecting grating material
Selecting a proper grating material by taking the epitaxial surface of the epitaxial wafer of the all-optical solid ultrafast detection chip as a substrate of the grating material, wherein the grating material is a metal material capable of effectively absorbing X-rays;
step two, preparing a seed layer
Preparing a conductive metal module on a substrate to form a seed layer;
step three, preparing the glue grating structure
Preparing a glue film on the seed layer, and photoetching by adopting SU-8 glue to form a glue grating structure;
step four, preparing the metal grating structure
Micro-electroplating the substrate with the glue grating structure to form a metal grating structure;
step five, removing the photoresist
And removing the SU-8 glue on the seed layer to obtain the metal grating.
Further, in the step one, in the grating material, the material of the grating material is Au, and the thickness of the material is 5 μm.
Further, in the step two, in the seed layer preparation, the metal module is made of Al, Cu or Au, and the thickness is 30-200 nm.
Further, the metal module is made of Cu and has a thickness of 100 nm.
Further, the seed layer preparation in the second step comprises the following specific steps:
growing a metal material on the substrate by adopting a magnetron sputtering film forming technology, preparing a metal module and forming a seed layer.
Further, the specific steps of preparing the metal grating structure in the fourth step are as follows:
the main salt is sodium gold sulfite NaAu (SO)3)2Electroplating solution with anhydrous sodium sulfite as main complexing agent to micro-electroplate the substrate with the glue grating structure to form a metal grating structure on the substrate;
the temperature of the electroplating solution is controlled to be 40-50 ℃, the PH value is controlled to be 8-10, and the pulse current density is 0.5A/dm2。
Further, the concentration of the main salt is 8-15 g/L, and the concentration of the main complexing agent is 120-140 g/L;
the electroplating solution also comprises auxiliary complexing agents, wherein the auxiliary complexing agents comprise potassium citrate with the concentration of 100-120 g/L, potassium chloride with the concentration of 15-25 g/L, dipotassium hydrogen phosphate with the concentration of 30-40 g/L and deionized water.
Further, the step five of removing the photoresist specifically comprises the following steps:
and (3) soaking by using SU-8 degumming liquid and soaking by using acetone to remove the SU-8 glue on the seed layer by ultrasonic waves to obtain the metal grating.
The invention also provides a grating prepared by the preparation method of the X-ray all-optical solid ultrafast detection chip modulation grating, which is characterized in that: the grating comprises a plurality of grating units;
each grating unit comprises a seed layer and an electroplated layer arranged on the seed layer, and a through groove penetrating to the surface of the seed layer is formed in the electroplated layer.
Furthermore, the structure of the grating unit is I-shaped, and the parameter of the grating unit is 70 lp/mm; the adjacent I-shaped grating units are vertically distributed.
Compared with the prior art, the invention has the following technical effects:
1. the preparation method of the surface amplitude type modulation grating of the X-ray all-optical solid ultrafast detection chip can effectively block incident X-rays, and the metal grating has a complete structure; meanwhile, the coating (seed layer preparation on the substrate) and the micro-plating technology are combined, so that high transmission of X-rays incident to the surface of the chip and high reflection of probe light are realized, the utilization rate of the incident light and the probe light is improved, and the process is simplified.
2. The grating material of the invention selects metal Au with the thickness of 5 μm, which can effectively absorb X-rays within the range of 1keV to 10 keV.
3. The seed layer is prepared on the surface of the substrate, the material can be Al, Cu or Au, the thickness is 30-200 nm, and the transmittance of incident light and the reflectivity of probe light can be met.
4. The invention prepares 100nm Cu material on the surface of the substrate as a seed layer, and can be used as a high-transmittance film for X-rays and a high-reflection film for probe light, and has good transmittance and reflectivity.
5. The grating prepared by the invention has a complete structure, can meet the requirement of high depth-to-width ratio, can realize effective blocking of incident X rays, and is suitable for the environment in which the chip is applied.
6. The grating units prepared by the invention are I-shaped, the parameters of the grating units are 70lp/mm, and the adjacent I-shaped grating units are vertically distributed, so that the problem of inconsistency of test data caused by rotation of a detection chip in the test process is solved.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the present invention;
FIG. 2 is a simulation curve of the incident depth of X-rays in a metallic Au material in a range of 1keV to 10 keV;
FIG. 3 is a schematic diagram of a grating profile prepared according to an embodiment of the present invention;
fig. 4 is a partial enlarged view of fig. 3 at point i.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments.
The chip test selects the X-ray with 4.5KeV incident signal light and 800nm probe light wavelength. In order to effectively modulate X-rays and block incident high-energy X-rays, Au with high atomic number is selected as a material of the X-ray modulation grating by the chip.
As shown in fig. 1, the method for preparing the modulation grating of the X-ray all-optical solid ultrafast detection chip provided by the invention comprises the following steps:
because the X-ray has extremely strong penetrating power, in order to effectively block partial X-ray, a metal material with high atomic number is needed, the invention adopts an Au material, as shown in figure 2, the incident depth of the X-ray in the range of 1keV to 10keV in the metal Au material is simulated, the relation between the incident depth of the X-ray in the semiconductor material and the thickness of the Au is obtained, and the Au with the thickness of 5 mu m is finally selected as a grating material through simulation calculation;
the micro-electroplating process is an expanded application of an electroplating process in the field of micro-nano processing, the principle of the micro-electroplating process is electrochemical deposition, the transmittance and the reflectivity of Al, Cu and Au materials to incident light and probe light respectively are calculated, and the comparison shows that:
1) the seed layer (Al film) prepared by adopting the Al material has a transmittance higher than 95% for X-rays in a 4.5KeV spectrum band when the thickness (film thickness) of the seed layer is less than 200 nm;
2) the seed layer (Cu film) prepared by using the Cu material has a transmittance higher than 95% for X-rays in a 4.5KeV spectrum band when the thickness (film thickness) of the seed layer is less than 200 nm;
3) the seed layer (Au film) prepared by the Au material has the transmittance higher than 80% for the X-ray of 4.5KeV spectral band when the thickness (film thickness) of the seed layer is less than 200 nm.
With this as a reference, the reflectivity of the probe light by the three metal material films with the thickness of less than 200nm is respectively compared as shown in table 1 below:
TABLE 1
By combining the X-ray transmittance and the probe light reflectance of each metal film, the X-ray transmittance of the Cu film is more than 95% and the probe light reflectance of the Cu film is better than 97% at the thickness of 100nm, so that the Cu film material with the thickness of 100nm is selected as a seed layer in the micro-electroplating process;
adopting a magnetron sputtering film forming technology to grow 100nmCu material on the epitaxial surface of the all-optical solid ultrafast detection chip epitaxial wafer to serve as a seed layer and serve as a high-transmittance film for incident light and a high-reflection film for probe light;
the Cu material with the thickness of 100nm prepared by the process has the X-ray transmittance of 95% and the light reflectance of 97.1% for the 800nm probe.
the thickness of the adhesive film in the process is 10 μm;
the process grating structure is designed to be an I-shaped rotating structure, as shown in fig. 3, the I-shaped rotating structure solves the problem of inconsistency of test data caused by rotation of the detection chip in the test process.
during the micro-electroplating of the chip with the grating adhesive film prepared by using the electroplating solution with main salt of sodium gold sulfite (NaAu (SO3)2) and anhydrous sodium sulfite as main complexing agents, wherein the main salt concentration is 8-15 g/L, the main complexing agent concentration is 120-140 g/L, potassium citrate 100-120 g/L is used as an auxiliary complexing agent, potassium chloride 15-25 g/L is used for improving the conductivity and cathode current density of the electroplating solution, dipotassium hydrogen phosphate 30-40 g/L is used as a conductive salt and a PH buffering agent, deionized water is added, the temperature of the electroplating solution is controlled to be 40-50 ℃, the PH value is controlled to be 8-10, and the pulse current density is 0.5A/dm 2.
And step 5, alternately soaking the SU-8 degumming solution and soaking the SU-8 degumming solution in acetone to remove the SU-8 degumming solution by ultrasound to obtain the metal grating.
The grating prepared by the method comprises a plurality of grating units, wherein each grating unit comprises a seed layer and an electroplated layer arranged on the seed layer, a through groove penetrating to the surface of the seed layer is formed in the electroplated layer, the structure of the grating unit is I-shaped, the parameter of the grating unit is 70lp/mm, the preferred material of the grating material is Au, the thickness is 5 mu m, and the thickness can be larger than 5 mu m under the grating structure of 70 lp/mm; the adjacent I-shaped grating units are vertically distributed, the grating structure is complete, the metal thickness is easy to control, the preparation of the metal grating with the high depth-to-width ratio can be realized, the partial blocking of incident X-rays is realized, and the modulation of probe light is finally realized.
Finally, it should be noted that: the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and it is obvious for a person skilled in the art to modify the specific technical solutions described in the foregoing embodiments or to substitute part of the technical features, and these modifications or substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions protected by the present invention.
Claims (7)
1. A preparation method of an X-ray all-optical solid ultrafast detection chip modulation grating is characterized by comprising the following steps:
step one, selecting grating material
The epitaxial surface of an epitaxial wafer of the all-optical solid ultra-fast detection chip is used as a substrate of a grating material, and the grating material is a metal material capable of effectively absorbing X-rays; the metal material is Au with the thickness of 5 mu m;
step two, preparing a seed layer
Preparing a conductive metal module on a substrate to form a seed layer, wherein the metal module is made of Cu and has the thickness of 100 nm;
step three, preparing the glue grating structure
Preparing a glue film on the seed layer, and photoetching by adopting SU-8 glue to form a glue grating structure;
step four, preparing the metal grating structure
Micro-electroplating the substrate with the glue grating structure to form a metal grating structure; the grating structure is an I-shaped rotating structure;
step five, removing the photoresist
And removing the SU-8 glue on the seed layer to obtain the metal grating.
2. The method for preparing the modulation grating of the X-ray all-optical solid ultrafast detection chip according to claim 1, wherein the step two of preparing the seed layer comprises the following specific steps:
growing a metal material on the substrate by adopting a magnetron sputtering film forming technology, preparing a metal module and forming a seed layer.
3. The method for preparing the modulating grating of the X-ray all-optical solid ultrafast detection chip according to claim 1, wherein the concrete steps for preparing the metal grating structure in the fourth step are as follows:
the main salt is sodium gold sulfite NaAu (SO)3)2The electroplating solution with the main complexing agent being anhydrous sodium sulfite is used for carrying out micro-electricity on the substrate with the glue grating structurePlating, namely forming a metal grating structure on the substrate;
the temperature of the electroplating solution is controlled to be 40-50 ℃, the PH value is controlled to be 8-10, and the pulse current density is 0.5A/dm2。
4. The method for preparing the modulating grating of the X-ray all-optical solid ultrafast detection chip as claimed in claim 3, wherein the concentration of the main salt is 8-15 g/L, and the concentration of the main complexing agent is 120-140 g/L;
the electroplating solution also comprises auxiliary complexing agents, wherein the auxiliary complexing agents comprise potassium citrate with the concentration of 100-120 g/L, potassium chloride with the concentration of 15-25 g/L, dipotassium hydrogen phosphate with the concentration of 30-40 g/L and deionized water.
5. The method for preparing the modulating grating of the X-ray all-optical solid ultrafast detection chip according to any one of claims 1 to 4, wherein the step five of removing photoresist specifically comprises the following steps:
and (3) soaking by using SU-8 degumming liquid and soaking by using acetone to remove the SU-8 glue on the seed layer by ultrasonic waves to obtain the metal grating.
6. The grating prepared by the preparation method of the X-ray all-optical solid ultrafast detection chip modulation grating, which is characterized by comprising the following steps of: the grating comprises a plurality of grating units;
each grating unit comprises a seed layer and an electroplated layer arranged on the seed layer, and a through groove penetrating to the surface of the seed layer is formed in the electroplated layer.
7. The grating prepared by the preparation method of the X-ray all-optical solid ultrafast detection chip modulation grating according to claim 6, which is characterized in that:
the structure of the grating unit is I-shaped, and the parameter of the grating unit is 70 lp/mm;
the adjacent I-shaped grating units are vertically distributed.
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| WO2012008120A1 (en) * | 2010-07-15 | 2012-01-19 | コニカミノルタエムジー株式会社 | Method for manufacturing metal grid, and metal grid |
| CN106094445A (en) * | 2016-06-12 | 2016-11-09 | 中国科学院微电子研究所 | The manufacture method of large ratio of height to width nano level metal structure |
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| CN102466967B (en) * | 2010-11-12 | 2014-03-26 | 中国科学院微电子研究所 | Manufacture method of diffractive optical element with large aspect ratio |
| CN102608863A (en) * | 2011-01-25 | 2012-07-25 | 中国科学院微电子研究所 | Method for preparing diffraction optical element with large aspect ratio |
| CN103913789B (en) * | 2014-04-03 | 2015-12-30 | 大连理工大学 | The method of high-aspect-ratio metal low-light grid prepared by metallic substrates |
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| WO2012008120A1 (en) * | 2010-07-15 | 2012-01-19 | コニカミノルタエムジー株式会社 | Method for manufacturing metal grid, and metal grid |
| CN106094445A (en) * | 2016-06-12 | 2016-11-09 | 中国科学院微电子研究所 | The manufacture method of large ratio of height to width nano level metal structure |
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