CN114976562B - Silicon-based microstrip circulator based on MEMS technology and application thereof - Google Patents
Silicon-based microstrip circulator based on MEMS technology and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 claims abstract description 4
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P11/00—Apparatus or processes specially adapted for manufacturing waveguides or resonators, lines, or other devices of the waveguide type
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/32—Non-reciprocal transmission devices
- H01P1/38—Circulators
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Micromachines (AREA)
- Drying Of Semiconductors (AREA)
Abstract
The invention relates to the field of IPC B81C1/00, in particular to a silicon-based micro-strip circulator based on an MEMS technology and application thereof. The preparation steps of the silicon-based microstrip circulator comprise: (1) etching a silicon wafer; (2) positive and negative magnetron sputtering coating; (3) etching to form a pattern; (4) secondary positive and negative magnetron sputtering coating; (5) Shaping and embedding magnetic materials to obtain a silicon-based microstrip circulator finished product; the thickness of the silicon wafer is 0.1-1mm. The silicon-based microstrip circulator is prepared by the MEMS process, and the obtained product has the advantages of high dimensional precision, small return loss and extreme temperature resistance, and can meet the working requirements of microwave radio frequency devices. The high-performance microwave radio frequency device can be obtained under a simple process flow through specific etching and coating process treatment, and has important significance for the actual production of large-scale high-precision silicon-based microstrip circulators.
Description
Technical Field
The invention relates to the field of IPC B81C1/00, in particular to a silicon-based micro-strip circulator based on an MEMS technology and application thereof.
Background
MEMS (Micro Electromechanical System) refers to a microstructure processing process that can be accurate to millimeter and nanometer dimensions. The existing MEMS technology has wide application and is related to the processing technology in various fields such as biological medicine, traffic technology, aerospace, national defense industry and the like. MEMS processes originally originated from semiconductor and microelectronic processes, and typically employed steps such as photolithography, epitaxy, thin film deposition, sputtering, evaporation, etching, etc. to produce complex, precise three-dimensional devices. With the rapid development of modern communication, the application of the MEMS technology to radio frequency or microwave wireless communication has become a research topic with great application prospect.
Chinese patent CN111180843a discloses a micro-strip circulator of MEMS and a method for manufacturing the same, CN104167584B discloses a thin film circulator of integrated micro-strip and a method for manufacturing the same, CN106829853a discloses a deep silicon etching method and a method for manufacturing a silicon-based MEMS motion sensor, and in the prior art, the working situation of a radio frequency communication device is accompanied with power consumption, and meanwhile, the problems of large working period, high driving voltage and the like are also present. The exploration of the existing MEMS technology in the technical field of microwave radio frequency devices still stays in a laboratory stage, and a great gap remains between the existing MEMS technology and the application of the existing MEMS technology in production practice. Based on the above, the research of a method for preparing a microstrip circulator by using MEMS which can be put into mass production application becomes a problem to be solved in the field.
Disclosure of Invention
The invention solves the problems of poor loss resistance, short service life and limited size precision of the traditional micro-strip circulator by providing the silicon-based micro-strip circulator based on the MEMS technology, and realizes the micro-strip circulator prepared based on the MEMS technology, which can be put into mass production and application.
In order to solve the above problems, a first aspect of the present invention provides a silicon-based microstrip circulator based on MEMS technology, the preparation steps of the silicon-based microstrip circulator include:
(1) Etching a silicon wafer;
(2) Performing positive and negative magnetron sputtering coating;
(3) Etching to form a pattern;
(4) Performing secondary positive and negative magnetron sputtering coating;
(5) Shaping and embedding magnetic materials to obtain the finished product of the silicon-based microstrip circulator.
The thickness of the silicon wafer is 0.1-1mm.
In some preferred embodiments, the step (1) specifically includes placing the silicon wafer in a high-density plasma etcher, sequentially performing passivation and etching operations to obtain a silicon wafer containing a cavity, and performing wet chemical cleaning on the silicon wafer containing the cavity to obtain a silicon substrate I.
In some preferred embodiments, the passivation and etching operations are repeated 5-20 times.
Still more preferably, C is used 4 F 8 Passivating the silicon wafer by using SF (sulfur hexafluoride) 6 ，C 4 F 8 And O 2 Etching the silicon wafer by the mixed gas; the passivation time is 4-25s, and the etching time is 5-10s; the pole plate power of the high-density plasma etching machine in the etching process is 10-20W.
Preferably, the method comprises the steps of,c in passivation process 4 F 8 The gas is introduced at a rate of 50-150mL/min.
Preferably, SF is used in the etching process 6 ，C 4 F 8 And O 2 The gas inlet speed is respectively 50-150mL/min,10-20mL/min and 4-10mL/min.
The invention discovers that the silicon wafer with the cavity and the smooth side wall and high etching verticality can be obtained by adopting a passivation and etching alternating operation method. In particular C 4 F 8 Passivation by gas using SF 6 ，C 4 F 8 And O 2 When the mixed gas is used for etching, the deposition and etching processes are easier to balance, the active F group formed by the passivation gas in a plasma state can uniformly act on the silicon wafer, the anisotropic effect of the deep silicon etching process is obvious due to the control of the specific gas inlet speed and equipment conditions, and the silicon wafer with the cavity, which has high smoothness and steepness, is obtained in a specific passivation-etching period.
In some preferred embodiments, the wet chemical cleaning step comprises sequentially placing the cavity-containing silicon wafer in a H-containing state 2 SO 4 H of (2) 2 O 2 Aqueous solution containing NH 4 H of OH 2 O 2 Aqueous solution, aqueous HF solution, H containing HCl 2 O 2 Cleaning in aqueous solution to remove organic matters and inorganic impurities; after each reagent is cleaned, the silicon wafer is cleaned by Milli Q water, and finally, after the cleaning is finished, the silicon wafer is washed by Milli Q water for 5-15min, then is placed in ethanol for ultrasonic cleaning for 2-10min, and is dried by nitrogen, so that a silicon substrate I is obtained.
The silicon wafer master batch is usually loaded with organic or inorganic impurities, and for a precise microstrip circulator, the existence of various impurities can cause interference to the transmission of information, and the service life of the silicon wafer is also easy to reduce. The invention discovers that the wet chemical cleaning method can effectively remove impurities from the etched silicon substrate, especially the H with specific acidity and alkalinity 2 O 2 The aqueous solution sequentially acts on the first silicon substrate, so that impurities in the first silicon substrate are effectively removed, meanwhile, the controllability of subsequent operation of the first silicon substrate can be improved, and the wet chemical cleaned silicon substrate is subjected to the wet chemical cleaningAnd the adhesive force between the microstrip circulator and the Ti target and the Au target is improved, so that an extremely thin Ti film layer and an extremely thin Au film layer can be formed, and the information transmission accuracy of the microstrip circulator is further improved.
In some preferred embodiments, the step (2) specifically comprises performing a positive and negative magnetron sputtering coating on the first silicon substrate, defining one surface of the first silicon substrate as a front surface, defining the other surface as a back surface, performing coating on the front surface by Ti, and performing coating on the back surface by Au to obtain the second silicon substrate.
Further preferably, the step (2) is specifically that the first silicon substrate is placed in an ultrahigh vacuum magnetron sputtering device, the front surface of the first silicon substrate is sputtered to form a film by using a Ti target, and mixed gas of high-purity helium and high-purity argon is continuously introduced at a speed of 12-25mL/min in the sputtering process, wherein the air pressure ratio of the high-purity helium to the high-purity argon is (3-7): 1, the air pressure value of the mixed gas is 0.1-1Pa; and then sputtering the back surface of the second silicon substrate to form a film by adopting an Au target, continuously introducing high-purity argon at a speed of 12-25mL/min in the sputtering process, wherein the sputtering power is 60-250W, and the air pressure value of the high-purity argon is 0.1Pa.
Further preferably, the Ti target in the step (2) is located at a distance of 5-12cm from the silicon substrate; the Au target is 16 cm to 22cm away from the silicon substrate.
In some preferred embodiments, the thickness of the coating on both the front and back sides is 2-16 μm.
In some preferred embodiments, the step (3) specifically includes sequentially performing primary photolithography, chemical etching, and secondary photolithography on the second silicon substrate, and forming a pattern on the opposite side of the second silicon substrate to obtain a third silicon substrate.
Preferably, the first photoetching and the second photoetching both adopt negative photoresist to act on the front surface of the second silicon substrate, and patterns are formed on the surface of the second silicon substrate through UV irradiation, development, etching and photoresist removal; the negative tone photoresist may be commercially available, for example, from Beijing Saima Laider trade Co., ltd., model number NR5-8000.
Preferably, the chemical etching is specifically that the silicon substrate II after primary photoetching is immersed in an acid mixed solution for 2-10min, taken out and flushed with Milli Q water for 1-3min, and purged with nitrogen.
In some preferred embodiments, the acid mixture comprises at least 2 of hydrofluoric acid, nitric acid, acetic acid, phosphoric acid, carbonic acid, oxalic acid, citric acid, and malic acid.
Further preferably, the acid mixture comprises hydrofluoric acid, nitric acid, acetic acid and water; the volume ratio of hydrofluoric acid, nitric acid, acetic acid and water is 40-60:1-3:0.1-1:0.5-2.
In some preferred embodiments, the step (4) specifically comprises performing secondary positive and negative magnetron sputtering coating on the third silicon substrate, wherein the front surface is coated with Ti, and the back surface is coated with Au, so as to obtain the fourth silicon substrate.
Further preferably, the step (4) is specifically that the third silicon substrate is placed in an ultrahigh vacuum magnetron sputtering device, the front surface of the third silicon substrate is sputtered to form a film by using a Ti target, and mixed gas of high-purity helium and high-purity argon is continuously introduced at a speed of 12-25mL/min in the sputtering process, wherein the air pressure ratio of the high-purity helium to the high-purity argon is (2-10): 1, the air pressure value of the mixed gas is 0.5-2Pa; then adopting an Au target to sputter and form a film on the back surface of the silicon substrate III, continuously introducing high-purity argon at a speed of 12-25mL/min in the sputtering process, wherein the sputtering power is 60-250W, and the air pressure value of the high-purity argon is 0.1-0.5Pa; and obtaining a silicon substrate IV.
Further preferably, the Ti target in the step (4) is three 5cm to 12cm away from the silicon substrate; the Au target is 16 cm to 22cm away from the silicon substrate III.
When the MEMS technology is used for processing the silicon substrate, various patterns can be formed on the surface of the silicon substrate by adopting photoetching or chemical etching, but tiny pores are easy to appear on the surface and the edge of the etched silicon substrate, and the conduction stability of the microstrip circulator is reduced. The invention adopts the secondary vacuum coating, can obviously reduce the fluctuation degree of the alloy coating, avoid the problems of rough, uneven and compact alloy coating, poor size precision of the micro-strip circulator and poor reliability of subsequent welding, and the prepared silicon substrate can maintain excellent reliability, endow the micro-strip circulator with extremely low return loss performance and prolong the service life of the silicon-based micro-strip circulator.
In some preferred embodiments, the step (5) specifically includes that 2 silicon substrates are aligned in an alignment machine, then transferred to a vacuum welding machine for welding, and cut and shaped by using a grinding wheel divider to obtain a silicon substrate five; and embedding the magnetic material into the cavity of the silicon substrate five to obtain a silicon-based microstrip circulator finished product.
Further preferably, the temperature of the welding is 250-420 ℃.
In some preferred embodiments, the magnetic material comprises at least one of silicon steel sheet, nickel base alloy, rare earth alloy, ferrite.
Further preferably, the magnetic material is ferrite.
The second aspect of the invention provides an application of a silicon-based microstrip circulator based on MEMS technology, which is applied to the technical field of microwave radio frequency devices.
The beneficial effects are that:
the silicon-based microstrip circulator is prepared by the MEMS process, and the obtained product has the advantages of high dimensional precision, small return loss and extreme temperature resistance, and can meet the working requirements of microwave radio frequency devices. The high-performance microwave radio frequency device can be obtained under a simple process flow through specific etching and coating process treatment, and has important significance for the actual production of large-scale high-precision silicon-based microstrip circulators.
Detailed Description
Example 1.
The embodiment provides a silicon-based microstrip circulator based on MEMS technology, and the preparation steps of the silicon-based microstrip circulator comprise:
(1) Etching a silicon wafer;
(2) Performing positive and negative magnetron sputtering coating;
(3) Etching to form a pattern;
(4) Performing secondary positive and negative magnetron sputtering coating;
(5) Shaping and embedding magnetic materials to obtain the finished product of the silicon-based microstrip circulator.
The silicon wafer was 2 inches in diameter and 0.5mm thick and was available from the source microelectronics technologies, inc. Hua Qin, su.
The step (1) is specifically that a silicon wafer is placed in a high-density plasma etching machine, passivation and etching operations are sequentially carried out, so that a silicon wafer containing a cavity is obtained, and wet chemical cleaning is carried out on the silicon wafer containing the cavity, so that a silicon substrate I is obtained.
The passivation and etching operations were repeated 5 times.
Specifically, C is adopted 4 F 8 Passivating the silicon wafer by using SF (sulfur hexafluoride) 6 ，C 4 F 8 And O 2 Etching the silicon wafer by the mixed gas; the passivation time is 15s, and the etching time is 8s; the power of the polar plate of the high-density plasma etching machine in the etching process is 15W.
C in passivation process 4 F 8 The gas feed rate was 90mL/min.
SF during etching 6 ，C 4 F 8 And O 2 The gas inlet speeds were 120mL/min,12mL/min and 7mL/min, respectively.
The wet chemical cleaning step comprises the steps of sequentially placing the silicon wafer containing the cavity into a wafer containing H 2 SO 4 H of (2) 2 O 2 Aqueous solution containing NH 4 H of OH 2 O 2 Aqueous solution, aqueous HF solution, H containing HCl 2 O 2 Cleaning in aqueous solution to remove organic matters and inorganic impurities; and after each reagent is cleaned, the silicon wafer is cleaned by Milli Q water, and finally, after the cleaning is finished, the silicon wafer is washed by Milli Q water for 10min, and then is placed in ethanol for ultrasonic cleaning for 5min, and is dried by using nitrogen gas, so that a silicon substrate I is obtained.
The H-containing 2 SO 4 H of (2) 2 O 2 H in aqueous solution 2 SO 4 ，H 2 O 2 And the volume ratio of water is 3:1:3, the cleaning temperature is 120 ℃, and the cleaning time is 18min.
The NH containing 4 H of OH 2 O 2 NH in aqueous solution 4 OH，H 2 O 2 And the volume ratio of water is 1:1:6, preparing a base material; the cleaning temperature was 68℃and the cleaning time was 4min.
The volume fraction of HF in the HF aqueous solution is 50%, the cleaning temperature is 27 ℃, and the cleaning time is 5min.
The H containing HCl 2 O 2 HCl, H in aqueous solution 2 O 2 And the volume ratio of water is 1:2:7, preparing a base material; the cleaning temperature was 62℃and the cleaning time was 13min.
And (2) performing positive and negative magnetron sputtering coating on the first silicon substrate, wherein one surface of the first silicon substrate is defined as the front surface, the other surface is defined as the back surface, ti is adopted for coating on the front surface, and Au is adopted for coating on the back surface, so that the second silicon substrate is obtained.
Specifically, placing a first silicon substrate in ultrahigh vacuum magnetron sputtering equipment, and sputtering the front surface of the first silicon substrate into a film by using a Ti target, wherein mixed gas of high-purity helium and high-purity argon is continuously introduced at a speed of 18mL/min in the sputtering process, and the air pressure ratio of the high-purity helium to the high-purity argon is 5:1, the air pressure value of the mixed gas is 0.8Pa; and then sputtering the back surface of the second silicon substrate to form a film by adopting an Au target, continuously introducing high-purity argon at the speed of 18mL/min in the sputtering process, wherein the sputtering power is 180W, and the air pressure value of the high-purity argon is 0.1Pa.
The Ti target in the step (2) is 10cm away from the silicon substrate; the Au target is 20cm away from the silicon substrate.
The thickness of the plating film on the front side and the back side is 5 mu m.
And (3) sequentially performing primary photoetching, chemical etching and secondary photoetching on the second silicon substrate, and forming a pattern on the back surface of the second silicon substrate to obtain a third silicon substrate.
The first photoetching and the second photoetching both adopt negative photoresist to act on the front surface of the second silicon substrate, and patterns are formed on the surface of the second silicon substrate through UV irradiation, development, etching and photoresist removal; the negative tone photoresist may be commercially available, for example, from Beijing Saima Laider trade Co., ltd., model number NR5-8000.
The chemical etching is specifically that a silicon substrate II subjected to primary photoetching is immersed in an acid mixed solution to react for 5min, taken out and washed with Milli Q water for 2min, and purged with nitrogen.
The acid mixed solution comprises hydrofluoric acid, nitric acid, acetic acid and water; the volume ratio of hydrofluoric acid, nitric acid, acetic acid and water is 52:2:0.6:1.2.
the step (4) is specifically that a third silicon substrate is placed in an ultrahigh vacuum magnetron sputtering device, a Ti target is used for sputtering and forming a film on the front surface of the third silicon substrate, mixed gas of high-purity helium and high-purity argon is continuously introduced at the speed of 18mL/min in the sputtering process, and the air pressure ratio of the high-purity helium to the high-purity argon is 5:1, the air pressure value of the mixed gas is 0.8Pa; then adopting an Au target to sputter and form a film on the back surface of the silicon substrate III, continuously introducing high-purity argon at the speed of 18mL/min in the sputtering process, wherein the sputtering power is 180W, and the air pressure value of the high-purity argon is 0.1Pa; and obtaining a silicon substrate IV.
The Ti target in the step (4) is three 10cm away from the silicon substrate; the Au target is three 20cm away from the silicon substrate.
Soaking a silicon substrate IV in acetone for 12min, taking out, flushing with Milli Q water for 2min, and purging with nitrogen; placing 2 silicon substrates four in an alignment machine, stacking and aligning with the front surface as a contact surface, transferring to a vacuum welding machine for welding, and cutting and shaping by using a grinding wheel divider to obtain a silicon substrate five; and embedding the magnetic material into the cavity of the silicon substrate five to obtain a silicon-based microstrip circulator finished product.
The temperature of the weld was 300 ℃.
The magnetic material is ferrite wafer, and is from Hua Qin Suzhou source microelectronics technologies.
Example 2.
The embodiment provides a silicon-based microstrip circulator based on MEMS technology, and the specific implementation mode is the same as that of embodiment 1; the difference is that SF is adopted 6 Etching the silicon wafer by gas and SF 6 The gas feed rate was 85mL/min.
Example 3.
The embodiment provides a silicon-based microstrip circulator based on MEMS technology, and the specific implementation mode is the same as that of embodiment 1; the difference is that C in the passivation process 4 F 8 The gas was introduced at a rate of 120mL/min and the passivation time was 10s.
Example 4.
The embodiment provides a silicon-based microstrip circulator based on MEMS technology, and the specific implementation mode is the same as that of embodiment 1; the difference is that in the step (2), the Ti target is used for sputtering and film forming the front surface of the silicon substrate I, and the mixed gas of high-purity helium and high-purity argon is continuously introduced at the speed of 28mL/min in the sputtering process, wherein the air pressure ratio of the high-purity helium to the high-purity argon is 5:1.
example 5.
The embodiment provides a silicon-based microstrip circulator based on MEMS technology, and the specific implementation mode is the same as that of embodiment 1; except that the Ti target was located at a distance of one 5cm from the silicon substrate in step (2).
Example 6.
The embodiment provides a silicon-based microstrip circulator based on MEMS technology, and the specific implementation mode is the same as that of embodiment 1; the difference is that the temperature of the weld is 375 ℃.
Performance test method
Return loss:
the silicon-based microstrip circulators of examples 1-6 were tested for return loss at 20 Ghz; each group of samples was averaged 5 times.
High temperature resistance:
placing the silicon-based microstrip circulator of examples 1-6 at 65deg.C for 24 hr, taking out, randomly taking 5 points on the substrate, measuring thickness, and calculating Relative Standard Deviation (RSD) of 5 points thickness result 1 The method comprises the steps of carrying out a first treatment on the surface of the Each group of samples was averaged 5 times.
Low temperature resistance:
placing the silicon-based microstrip circulator of examples 1-6 at-10deg.C for 24 hr, taking out, randomly taking 5 points on the substrate, measuring thickness, and calculating Relative Standard Deviation (RSD) of 5 points thickness result 2 The method comprises the steps of carrying out a first treatment on the surface of the Each group of samples was averaged 5 times.
Performance test data
TABLE 1 Performance test results
| Return loss dB | RSD 1 ％ | RSD 2 ％ | |
| Example 1 | 0.41 | 2.1 | 0.8 |
| Example 2 | 0.65 | 4.7 | 2.1 |
| Example 3 | 0.59 | 5.2 | 3.4 |
| Example 4 | 0.62 | 5.8 | 2.4 |
| Example 5 | 0.58 | 6.2 | 3 |
| Example 6 | 0.57 | 6.2 | 3.1 |
Claims (7)
1. The silicon-based microstrip circulator based on the MEMS technology is characterized by comprising the following preparation steps:
(1) Etching a silicon wafer;
(2) Performing positive and negative magnetron sputtering coating;
(3) Etching to form a pattern;
(4) Performing secondary positive and negative magnetron sputtering coating;
(5) Shaping and embedding magnetic materials to obtain a silicon-based microstrip circulator finished product;
the thickness of the silicon wafer is 0.1-1mm;
the step (2) is specifically that a first silicon substrate is subjected to positive and negative magnetron sputtering coating, one surface of the silicon substrate is defined as the front surface, the other surface is defined as the back surface, ti is adopted as the front surface for coating, and Au is adopted as the back surface for coating, so that a second silicon substrate is obtained;
the step (3) is specifically that the second silicon substrate is subjected to primary photoetching, chemical etching and secondary photoetching in sequence, and a pattern is formed on the back surface of the second silicon substrate to obtain a third silicon substrate;
and (4) performing secondary positive and negative magnetron sputtering coating on the silicon substrate III, wherein Ti is adopted for coating on the front surface, and Au is adopted for coating on the back surface, so as to obtain a silicon substrate IV.
2. The MEMS process-based silicon microstrip circulator of claim 1, wherein step (1) is specifically that a silicon wafer is placed in a high-density plasma etcher, passivation and etching operations are sequentially performed to obtain a silicon wafer containing a cavity, and wet chemical cleaning is performed on the silicon wafer containing the cavity to obtain a first silicon substrate.
3. A MEMS-technology based silicon-based microstrip circulator as claimed in claim 2, wherein said passivation and etching operations are repeated 5-20 times.
4. The MEMS-technology-based silicon-based microstrip circulator of claim 1, wherein the thickness of the plating film on the front and back surfaces is 2-16 μm.
5. The MEMS process-based silicon microstrip circulator of any one of claims 1 to 4, wherein the step (5) is specifically that 2 silicon substrates four are aligned in an alignment machine, then transferred to a vacuum welding machine for welding, and cut and shaped by a grinding wheel divider to obtain a silicon substrate five; and embedding the magnetic material into the cavity of the silicon substrate five to obtain a silicon-based microstrip circulator finished product.
6. The MEMS-technology-based silicon-based microstrip circulator of claim 5, wherein the magnetic material comprises at least one of a silicon steel sheet, a nickel-based alloy, a rare earth alloy, and ferrite.
7. The application of the silicon-based microstrip circulator based on the MEMS technology as claimed in claim 1, which is characterized by being applied to the technical field of microwave radio frequency devices.
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