CN113215574B - Wet etching method for quantum chip of sapphire substrate aluminum-plated film - Google Patents

Wet etching method for quantum chip of sapphire substrate aluminum-plated film Download PDF

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CN113215574B
CN113215574B CN202110133690.8A CN202110133690A CN113215574B CN 113215574 B CN113215574 B CN 113215574B CN 202110133690 A CN202110133690 A CN 202110133690A CN 113215574 B CN113215574 B CN 113215574B
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于扬
宋树清
兰栋
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23F1/00—Etching metallic material by chemical means
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Abstract

The invention relates to a wet etching method for preparing an aluminized quantum chip with a sapphire substrate. Taking sapphire as a substrate, and cleaning the surface of the polished substrate; plating an aluminum film on the surface of the polished substrate, coating photoresist on the surface of the aluminum film, and exposing and developing to obtain a mask chip with a pattern; etching the hardened mask chip in tetramethyl ammonium hydroxide to remove the aluminum film corresponding to the pattern; removing all the residual photoresist to obtain a quantum chip; when the tetramethyl ammonium hydroxide is used for etching the aluminum film corresponding to the pattern, etching is carried out for multiple times, the etching time of each time is not more than 1 minute, and the next etching is carried out after the edge of the dissolved photoresist is solidified until the aluminum film is completely etched. The invention does not introduce extra ion pollution and saves the preparation cost of the microwave resonant cavity.

Description

Wet etching method for quantum chip of sapphire substrate aluminum-plated film
Technical Field
The invention belongs to the technical field of quantum chips, and particularly relates to a wet etching method for preparing a quantum chip with an aluminum film plated on a sapphire substrate, which is used for preparing a high-performance superconducting quantum bit microwave resonant cavity.
Background
In most cases, superconducting microwave resonators are fabricated from aluminum film on high purity sapphire substrates. Aluminum has a dense oxide layer and an ideal superconducting transition temperature, and sapphire has a low loss tangent of less than 10-9And the cavity is defined by lithography and etching, with losses determined by the amount of coupling to the two-level system (TLS). It is well known that TLS losses occur mainly at the interface between bulk medium and material.
The resonant cavity manufactured by using the traditional process is mainly prepared by a dry etching process or a wet etching process. Among them, dry etching is a technique of performing thin film etching using plasma. In dry etching of aluminum, plasma is generally generated by a glow process using argon gas, chlorine gas, and boron trichloride. The plasma gas has more active chemical property, can react with aluminum more quickly to realize the purpose of etching and removing, and can accelerate the plasma by using an electric field to ensure that the plasma has certain energy, and when the plasma bombards the surface of an etched object, atoms on the surface of the aluminum can be knocked out, so that the purpose of etching by using physical energy transfer is realized. Wet etching is a technique of immersing an etching material in an etching solution to perform etching. The aluminum film corrosion solution is a special corrosion solution for aluminum materials, and comprises the components of nitric acid (used for oxidizing aluminum), phosphoric acid (used for dissolving aluminum oxide on the surface), acetic acid (used for buffering) and water (used as a solvent).
However, both of the above two conventional schemes for manufacturing the resonant cavity have their drawbacks, so that the possibility of producing a high-quality superconducting microwave resonant cavity chip is significantly reduced. Specifically, the photoresist etched by the dry method is denatured and then difficult to remove due to the influence of the high-energy chloride ions, and the residual photoresist reduces the quality factor of the microwave resonant cavity. The aluminum film corrosive liquid used in the traditional wet etching brings extra acidic ions, generates extra ionic pollution and electromagnetic loss, and thus reduces the quality factor of the resonant cavity.
In the microwave resonant cavity, the etched interface of the aluminum and the substrate is ensured to be smooth, the fluctuation exceeding a hundred nanometers cannot occur, and the large fluctuation can cause extra electromagnetic loss and finally reduce the quality factor. If the tetramethyl ammonium hydroxide is directly used for etching, when the aluminum film is etched, the tetramethyl ammonium hydroxide not only etches the aluminum film, but also generates a huge etching effect on the photoresist serving as a mask, so that the photoresist close to the developing groove is etched, the good mask effect cannot be achieved, finally, the etched interface of the aluminum and the substrate generates large line width fluctuation, and high-quality factors cannot be achieved.
Disclosure of Invention
In order to solve the technical defects in the prior art, the invention provides a wet etching method for preparing a sapphire substrate aluminum-plated film quantum chip.
In order to solve the technical problem, the invention provides a wet etching method for preparing a sapphire substrate aluminum-plated film quantum chip, which comprises the following steps:
taking sapphire as a substrate, and cleaning the surface of the polished substrate;
plating an aluminum film on the surface of the polished substrate, coating a photoresist on the surface of the aluminum film,
obtaining a mask chip with a pattern through exposure and development;
etching the hardened mask chip in tetramethyl ammonium hydroxide to remove the aluminum film corresponding to the pattern;
removing all the residual photoresist to obtain a quantum chip;
when the tetramethyl ammonium hydroxide is used for etching the aluminum film corresponding to the pattern, etching is carried out for multiple times, the etching time of each time is not more than 1 minute, and the next etching is carried out after the edge of the dissolved photoresist is solidified until the aluminum film is completely etched.
Preferably, the flatness variation of the polished substrate surface is within 0.2 to 0.5 nm.
Preferably, the polished substrate surface is cleaned in an ultraviolet ozone or plasma stripper.
Preferably, the cleaned substrate is placed in an electron beam evaporator for evacuation under high vacuum (10)- 9mbar) environment.
Preferably, the thickness of the aluminum film is 80nm-120 nm.
Preferably, the mask chip is obtained by developing in a developing solution of tetramethylammonium hydroxide.
Preferably, the development time in the developer solution of tetramethylammonium hydroxide is 30 to 60 seconds.
Preferably, when the aluminum film is etched by using tetramethylammonium hydroxide, the interval between the two etching processes is more than 10 minutes until the dissolved photoresist is solidified.
Preferably, the masked chip is placed in acetone to remove the remaining photoresist.
Compared with the prior art, the invention has the remarkable advantages and beneficial effects that:
(1) in the invention, tetramethylammonium hydroxide is used as an etching solution, and the pattern is directly etched after development, so that extra ionic pollution is not introduced like an aluminum film etching solution;
(2) compared with a dry etching machine and an aluminum film corrosive liquid, the tetramethylammonium hydroxide has much lower cost, and the preparation cost of the microwave resonant cavity is greatly saved.
(3) The invention fully utilizes the principle that the developing rate of the photoresist is improved along with the reduction of the concentration of the photoresist, and the etching time does not exceed a certain time each time, thereby stopping the etching reaction before the developing rate of the photoresist is increased, generating a certain etching effect on the aluminum film, completing the etching of the aluminum film through multiple times of etching and not influencing the mask quality of the photoresist.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 is a schematic diagram of a superconducting microwave cavity process of the present invention.
FIG. 3 is an image under an optical microscope of a 10 qubit superconducting microwave cavity implemented in a coplanar waveguide geometry with a center frequency ω R/2 π in the range of 6.62-6.87 GHz.
Fig. 4 is a schematic diagram of a measuring device of a network analyzer, and the middle part of a wire frame is an equivalent circuit diagram of a superconducting qubit and a resonant cavity.
FIG. 5 is a schematic diagram of the S21 curves for 10 resonators as measured by a network analyzer.
Fig. 6 shows the fitted value of intrinsic quality factor at 270000 at high power.
Fig. 7 is a diagram showing the effect of TLS on the chip by comparing the intrinsic quality factor between low power and high power.
Detailed Description
It is easily understood that various embodiments of the present invention can be conceived by those skilled in the art according to the technical solution of the present invention without changing the essential spirit of the present invention. Therefore, the following detailed description and the accompanying drawings are merely illustrative of the technical aspects of the present invention, and should not be construed as all of the present invention or as limitations or limitations on the technical aspects of the present invention. The present invention may be embodied in various forms and the embodiments are not intended to limit the scope of the present invention. Rather, these embodiments are provided so that this disclosure will be thorough and complete. The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form a part hereof, and which together with the embodiments of the invention serve to explain the innovative concepts of the invention.
Example 1
In this embodiment, a wet etching method for preparing a sapphire substrate aluminum-plated film quantum chip performs the following steps in a dust-free environment with cleanliness superior to thousand levels:
step S1: selecting sapphire with the thickness of 0.4mm as a substrate, and requiring the fluctuation of the surface flatness of single-side polishing of the sapphire to be within 0.2-0.5 nm; the sapphire substrate is placed in a UV Ozone (ultraviolet light and Ozone) or a plasma degumming machine for cleaning, so that organic impurities on the surface of the sapphire substrate are removed, and dielectric loss caused by the sapphire substrate is reduced.
Step S2: placing the processed sapphire substrate in an electron beam evaporator, vacuumizing for more than 2 hours, and performing high vacuum (10)-9mbar) is plated to ensure the cleanliness of the microwave resonant cavity and the superconductivity of the aluminum film.
Step S3: uniformly coating the photoresist of S1805, S1813 or S1818 on the substrate coated with the aluminum film by using a photoresist homogenizer, using a 5mm writing head on a Heidelberg DWL66+ laser direct writer to develop a pattern to be exposed in a developing solution of tetramethylammonium hydroxide for 30 to 60 seconds, and obtaining the chip with the pattern mask. As shown in fig. 2 (a), the chip is exposed by laser direct writing, wherein 201 is a sapphire substrate, 202 is an aluminum film, 203 is an unexposed photoresist, and 204 is an exposed photoresist. As shown in fig. 2 (b), is a view of a sample with exposed photoresist 204 removed in a tetramethylammonium hydroxide developer while forming a pattern of the resonant cavity.
Step S4: and etching the microwave resonant cavity hardened at room temperature in a tetramethylammonium hydroxide developing solution to remove the aluminum film 202. The process of etching the aluminum film 202 by using the tetramethylammonium hydroxide developing solution is performed for multiple times, the etching time of each time is not more than 1 minute, otherwise, the etching rate of the photoresist is too high, so that the quality of the photoresist as a mask is affected, and then the photoresist is kept still for a certain time, such as 10 minutes or more, at room temperature, and the edge of the dissolved photoresist is solidified and then etched for the next time until the aluminum film is etched cleanly. And then removing the photoresist 203 in acetone to obtain the final wafer with the prepared superconducting microwave resonant cavity. As shown in fig. 2 (c), a chip is formed by etching aluminum film 202 using a tetramethylammonium hydroxide developer. Fig. 2 (d) shows the complete resonator after the protective glue 203 is removed.
Step S5: the wafer with the prepared superconducting microwave cavity was cut into 10x10mm squares, and finally the completed device was packaged into a sample box and measured in a dilution refrigerator at a temperature below about 20 mk.
Example 2
Referring to fig. 2, in this embodiment, another wet etching method for sapphire substrate aluminum-plated film quantum chip preparation is performed in a dust-free environment with cleanliness better than thousand levels
Step S1: selecting sapphire 201 with the thickness of 0.43mm as a substrate, and requiring the fluctuation of the surface flatness of the single-side polished surface of the sapphire 201 to be within 0.2-0.5 nm; the sapphire 201 substrate is placed in a UV Ozone (ultraviolet Ozone) or a plasma degumming machine for cleaning, so that organic impurities on the surface of the sapphire substrate are removed, and dielectric loss caused by the sapphire substrate is reduced.
Step S2: placing the processed sapphire substrate in an electron beam evaporator, vacuumizing for more than 2 hours, and performing high vacuum (10)-9mbar) is plated with an aluminum film 202 of 100nm thickness to ensure cleanliness of the microwave cavity and superconductivity of the aluminum film.
Step S3: the resist 203 was uniformly applied to the substrate coated with the aluminum film 202 by means of a spin coater in the form of S1805, S1813 or S1818, the pattern to be exposed was developed on a hexburg DWL66+ laser writer by using a 5mm writing head for 30 to 60 seconds in a tetramethylammonium hydroxide developer, and the chip with the pattern mask was obtained.
Step S4: and etching the microwave resonant cavity hardened at room temperature in a tetramethylammonium hydroxide developing solution to remove the aluminum film 202. The process of etching the aluminum film 202 by using the tetramethylammonium hydroxide developing solution is performed for multiple times, the etching time of each time is not more than 1 minute, otherwise, the etching rate of the photoresist is too high, so that the quality of the photoresist as a mask is affected, and then the photoresist is kept still for a certain time, such as 10 minutes or more, at room temperature, and the edge of the dissolved photoresist is solidified and then etched for the next time until the aluminum film is etched cleanly. And then removing the photoresist 203 in acetone to obtain the final wafer with the prepared superconducting microwave resonant cavity.
Step S5: the wafer with the prepared superconducting microwave cavity was cut into 10x10mm squares, and finally the completed device was packaged into a sample box and measured in a dilution refrigerator at a temperature below about 20 mk.
Example 3
With reference to fig. 2, in this embodiment, another wet etching method for preparing a sapphire substrate aluminum-plated quantum chip is performed in a dust-free environment with cleanliness better than thousand levels
Step 1: selecting sapphire 201 with the thickness of 0.5mm as a substrate, and requiring the fluctuation of the surface flatness of single-side polishing of the sapphire or 201 to be within 0.2-0.5 nm; the sapphire substrate is placed in a UV Ozone (ultraviolet light and Ozone) or a plasma degumming machine for cleaning, so that organic impurities on the surface of the sapphire substrate 201 are removed, and dielectric loss caused by the sapphire substrate is reduced.
Step 2: placing the processed sapphire substrate in an electron beam evaporator, vacuumizing for more than 2 hours, and performing high vacuum (10)-9mbar) is plated with an aluminum film 202 having a thickness of 120nm to ensure cleanliness of the microwave cavity and superconductivity of the aluminum film.
And step 3: the resist 203 was uniformly applied to the substrate coated with the aluminum film 202 by means of a spin coater in the form of S1805, S1813 or S1818, the pattern to be exposed was developed on a hexburg DWL66+ laser writer by using a 5mm writing head for 30 to 60 seconds in a tetramethylammonium hydroxide developer, and the chip with the pattern mask was obtained.
And 4, step 4: and etching the microwave resonant cavity hardened at room temperature in a tetramethylammonium hydroxide developing solution to remove the aluminum film 202. The process of etching the aluminum film 202 by using the tetramethylammonium hydroxide developing solution is performed for multiple times, the etching time of each time is not more than 1 minute, otherwise, the etching rate of the photoresist is too high, so that the quality of the photoresist as a mask is affected, and then the photoresist is kept still for a certain time, such as 10 minutes or more, at room temperature, and the edge of the dissolved photoresist is solidified and then etched for the next time until the aluminum film is etched cleanly. And then removing the photoresist 203 in acetone to obtain the final wafer with the prepared superconducting microwave resonant cavity.
And 5: the wafer with the prepared superconducting microwave cavity was cut into 10x10mm squares, and finally the completed device was packaged into a sample box and measured in a dilution refrigerator at a temperature below about 20 mk.
To further illustrate the beneficial effects of the present invention, the inventors examined the measurements as follows.
1. Network analyzer measurements
Fig. 3 shows a microscope image of a superconducting microwave cavity. The inventors coupled 10 λ/4 coplanar waveguide resonators on the readout transmission line. In connection with fig. 4, an attenuator is mounted on the microwave line to prevent thermal radiation from leaking into the cavity. After passing through the superconducting microwave resonant cavity, the signal is amplified by a low-temperature High Electron Mobility Transistor (HEMT) and a room-temperature amplifier. Finally, the amplitude and phase of the transmission signal S21 in fig. 6 were measured by a network analyzer to obtain the quality factor. At the resonant frequency, the quality factor of the resonant cavity can be fitted by equation (1):
Figure GDA0003359076410000061
wherein an intrinsic quality factor Q is usediAnd normalizing the quality factor Q* cDefines a normalized inverse transmission factor
Figure GDA0003359076410000062
2. Characterization and results
Loss angleThe method is a simple measurement parameter for calibrating the performance of the device, and Qi is a common measurement parameter for calibrating a high-performance device. The loss due to etching can be considered to be caused by coupling to a Two Level System (TLS). Since the interface between the superconductor and the substrate may be the largest source of TLS loss. According to TLS model, resonant cavity loss angle delta at constant temperatureTLSFollowing empirical formula (3):
Figure GDA0003359076410000063
the actual power on the sample is obtained by subtracting the attenuation on the line from the microwave power added to the system, N is a constant related to the number of characteristic photons of the delta saturation, so that delta is the higher the input powerTLSThe impact on the system is reduced, so the impact of TLS on the system can be measured by comparing the intrinsic quality factor between low power and high power.
As shown in fig. 7 (a), the inventors compared the difference in quality factors of the high power and the low power of 10 resonators, and as a result, showed that only a small amount of the two-level system was coupled to the quantum system during the etching. In order to determine whether the present invention can replace the dry etching and the wet etching using the etching solution of the aluminum film, the inventors used the sapphire substrate and the electron beam evaporated aluminum film subjected to the same process to control the parameters. On the basis of the above, the inventors fabricated 10 resonators and compared the three processes of dry etching, wet etching with aluminum film etching solution, and wet etching with tetramethylammonium hydroxide (ZJX-238). In fig. 7 (b), the horizontal axis is the ordinal number of the resonant cavity, the vertical axis is the intrinsic quality factor of the resonant cavity, the dry-etched photoresist is denatured and then difficult to remove after being affected by the high-energy chloride ions, and the residual photoresist can reduce the quality factor of the microwave resonant cavity. In the traditional wet etching, extra acidic ions and extra ionic pollution are brought by using an aluminum film corrosive liquid, extra electromagnetic loss is generated, and the quality factor of the resonant cavity is reduced, so that the quality factor of the resonant cavity etched by using tetramethylammonium hydroxide ZJX-238 is higher than those of the other two types of the resonant cavities. In addition, in the manufacturing process, tetramethyl ammonium hydroxide is used as an etching solution, so that the photoresist is not so strong in corrosivity, and the pattern is directly etched after development, so that extra ion pollution is not introduced, and the process time is shortened. More particularly, compared with a dry etching machine and an aluminum film corrosive liquid, the tetramethylammonium hydroxide has much lower cost, so the cost is reduced to a certain extent, the process period is shortened, and the novel etching method is more convenient.
The invention can be used for large-scale production only by using the same solution for development treatment after photoetching and etching. The invention also shows that the two-dimensional transport qubit made with tetramethylammonium hydroxide (ZJX-238) developer can have high quality and high yield, which also provides the possibility of starting the industrial fabrication of qubits.

Claims (9)

1. A wet etching method for preparing sapphire substrate aluminum-plated film quantum chips is characterized by comprising the following steps:
taking sapphire as a substrate, and cleaning the surface of the polished substrate;
plating an aluminum film on the surface of the polished substrate, coating a photoresist on the surface of the aluminum film,
obtaining a mask chip with a pattern through exposure and development;
etching the hardened mask chip in tetramethyl ammonium hydroxide to remove the aluminum film corresponding to the pattern;
removing all the residual photoresist to obtain a quantum chip;
wherein the content of the first and second substances,
when the tetramethyl ammonium hydroxide is used for etching the aluminum film corresponding to the pattern, etching is carried out for multiple times, the etching time of each time is not more than 1 minute, and the next etching is carried out after the edge of the dissolved photoresist is solidified until the aluminum film is completely etched.
2. The wet etching method as claimed in claim 1,
the fluctuation of the flatness of the polished substrate surface is within 0.2 to 0.5 nm.
3. The wet etching method as claimed in claim 1, wherein the polished surface of the substrate is cleaned in an ultraviolet ozone or plasma stripper.
4. The wet etching method as claimed in claim 1, wherein the cleaned substrate is subjected to a vacuum-pumping operation in an electron beam evaporator under a high vacuum 10-9And plating aluminum film in mbar environment.
5. The wet etching method as claimed in claim 1, wherein the aluminum film has a thickness of 80nm to 120 nm.
6. The wet etching method for a quantum chip as claimed in claim 1, wherein the mask chip is obtained by developing in a developer of tetramethylammonium hydroxide.
7. The wet etching method according to claim 6, wherein the developing time in the developer of tetramethylammonium hydroxide is 30 to 60 seconds.
8. The wet etching method of claim 1, wherein when the aluminum film is etched using tetramethylammonium hydroxide, the interval between the two etching processes is more than 10 minutes until the dissolved photoresist is solidified.
9. The wet etching method of claim 1, wherein the mask chip is placed in acetone to remove the remaining photoresist.
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