CN114976562A - Silicon-based microstrip circulator based on MEMS (micro-electromechanical systems) process and application thereof - Google Patents
Silicon-based microstrip circulator based on MEMS (micro-electromechanical systems) process and application thereof Download PDFInfo
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- 239000010703 silicon Substances 0.000 title claims abstract description 159
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- 239000000696 magnetic material Substances 0.000 claims abstract description 11
- 238000007493 shaping process Methods 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 4
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- 229910000859 α-Fe Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
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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)
- Drying Of Semiconductors (AREA)
- Micromachines (AREA)
Abstract
The invention relates to the field of IPC B81C1/00, in particular to a silicon-based microstrip circulator based on an MEMS (micro-electromechanical system) process and application thereof. 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 a magnetic material to obtain a finished product of the silicon-based microstrip circulator; the thickness of the silicon wafer is 0.1-1 mm. The silicon-based microstrip circulator is prepared by the MEMS process, and the obtained product has the advantages of high size precision, low return loss and extreme temperature resistance, and can meet the working requirements of microwave radio-frequency devices. Through specific etching and coating process treatment, the high-performance microwave radio-frequency device can be obtained under a simple process flow, and the method has important significance for the actual production of large-batch 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 microstrip circulator based on an MEMS (micro-electromechanical system) process and application thereof.
Background
The mems (micro electro mechanical system) process refers to a micro-structure processing process capable of being precise to millimeter and nanometer dimensions. The existing MEMS process is widely applied and relates to processing technologies in various fields such as biomedicine, traffic technology, aerospace, national defense industry and the like. MEMS processes originally originated from semiconductor and microelectronic processes, and generally employ photolithography, epitaxy, film deposition, sputtering, evaporation, etching, and other steps to fabricate complex and precise three-dimensional devices. With the rapid development of modern communication, applying the MEMS technology to radio frequency or microwave wireless communication has become a research topic with great application prospects.
Chinese patent CN111180843A discloses an MEMS microstrip circulator and a method for making the same, CN104167584B discloses a microstrip integrated thin film circulator and a method for making the same, and CN106829853A discloses a deep silicon etching method and a method for making a silicon-based MEMS motion sensor. The existing MEMS technology still stays in a laboratory stage in the exploration in the technical field of microwave radio frequency devices, and has a large gap from the practical application of the technology in production. Based on the above, it is an urgent problem in the art to find a method for manufacturing a microstrip circulator by using MEMS, which can be put into mass production and application.
Disclosure of Invention
The invention provides the silicon-based micro-strip circulator based on the MEMS technology, solves the problems of poor loss resistance, short service life and limited size precision of the existing micro-strip circulator, and realizes the preparation of the micro-strip circulator 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 a MEMS process, the silicon-based microstrip circulator being fabricated by steps including:
(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) and (5) shaping, and embedding a magnetic material to obtain a finished product of the silicon-based microstrip circulator.
The thickness of the silicon wafer is 0.1-1 mm.
In some preferred embodiments, the step (1) is specifically to place the silicon wafer in a high-density plasma etcher, perform passivation and etching operations in sequence to obtain a silicon wafer containing a cavity, and perform wet chemical cleaning on the silicon wafer containing the cavity to obtain the first silicon substrate.
In some preferred embodiments, the passivation and etching operations are repeated 5-20 times.
Further preferably, C is used 4 F 8 Passivating the silicon wafer with gas by using SF 6 ，C 4 F 8 And O 2 Etching the silicon wafer by using the mixed gas; the passivation time is 4-25s, and the etching time is 5-10 s; the power of the polar plate of the high-density plasma etcher is 10-20W in the etching process.
Preferably, C in the passivation process 4 F 8 The gas is introduced at a rate of 50-150 mL/min.
Preferably, SF is used in the etching process 6 ，C 4 F 8 And O 2 The gas is introduced at the speed of 50-150mL/min, 10-20mL/min and 4-10mL/min respectively.
The invention discovers that the silicon chip containing the cavity with smooth side wall and high etching verticality can be obtained by adopting a passivation and etching alternative operation method. Especially with C 4 F 8 Passivating with gas using SF 6 ，C 4 F 8 And O 2 When the mixed gas is etched, the deposition and etching processes are more easily balanced, active F groups 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 remarkable by controlling the specific gas introduction speed and the equipment conditions, and the cavity-containing silicon wafer with high smoothness and steepness is obtained in a specific passivation-etching period.
In some preferred embodiments, the wet chemical cleaning step is to sequentially place the silicon wafer containing the cavity in the H-containing chamber 2 SO 4 H of (A) to (B) 2 O 2 Aqueous solution of NH 4 H of OH 2 O 2 Aqueous solution, aqueous HF solution, H containing HCl 2 O 2 Cleaning in water solution to remove organic matters and inorganic impurities; and cleaning the silicon wafer by using Milli Q water after each reagent is cleaned, washing the silicon wafer by using Milli Q water for 5-15min after the silicon wafer is cleaned, placing the silicon wafer in ethanol for ultrasonic cleaning for 2-10min, and drying the silicon wafer by using nitrogen to obtain the first silicon substrate.
The master batch of the silicon chip is usually loaded with organic or inorganic impurities, and for a precise microstrip circulator, the existence of various impurities can cause interference on information transmission and can also easily reduce the service life of the silicon chip. The invention discovers that the etched silicon substrate can be cleaned by adopting a wet chemical cleaning methodEffective impurity removal, especially by using specific acid-base H 2 O 2 The water solution acts on the first silicon substrate in sequence, so that impurities in the first silicon substrate are effectively removed, the controllability of subsequent operation of the first silicon substrate can be improved, the adhesive force between the first silicon substrate after wet chemical cleaning and the Ti target and the Au target is improved, extremely thin Ti film layers and Au film layers can be formed, and the information transmission accuracy of the microstrip circulator is further improved.
In some preferred embodiments, the step (2) is specifically to perform front-back magnetron sputtering coating on the first silicon substrate, defining one surface of the first silicon substrate as a front surface and the other surface as a back surface, and performing coating on the front surface by using Ti and performing coating on the back surface by using Au to obtain a second silicon substrate.
Further preferably, the step (2) is specifically that the first silicon substrate is placed in ultrahigh vacuum magnetron sputtering equipment, a Ti target is used for sputtering film formation on the front surface of the first silicon substrate, mixed gas of high-purity helium and high-purity argon is continuously introduced at a speed of 12-25mL/min in the sputtering process, and the gas pressure ratio of the high-purity helium to the high-purity argon is (3-7): 1, the pressure value of the mixed gas is 0.1-1 Pa; and then sputtering the reverse side of the second silicon substrate by using an Au target to form a film, wherein high-purity argon is continuously introduced at the speed of 12-25mL/min in the sputtering process, the sputtering power is 60-250W, and the air pressure value of the high-purity argon is 0.1 Pa.
Further preferably, the Ti target in the step (2) is 5-12cm away from the silicon substrate; the Au target is 16-22cm away from the silicon substrate.
In some preferred embodiments, the coating thickness of the front and back surfaces is 2 to 16 μm.
In some preferred embodiments, the step (3) is specifically to sequentially perform primary photolithography, chemical etching and secondary photolithography on the second silicon substrate, and form a pattern on the reverse side of the second silicon substrate, so as 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 photoresist may be commercially available, for example, from Nyquist, N.Y. model NR 5-8000.
Preferably, the chemical etching is specifically to immerse the silicon substrate II subjected to the primary photoetching in an acid mixed solution, react for 2-10min, take out, wash with Milli Q water for 1-3min, and purge with nitrogen.
In some preferred embodiments, the acid mixture includes 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 to nitric acid to acetic acid to water is 40-60: 1-3: 0.1-1: 0.5-2.
In some preferred embodiments, the step (4) is specifically to perform two times of front-back magnetron sputtering coating on the silicon substrate three, wherein the front surface is coated with Ti, and the back surface is coated with Au, so as to obtain the silicon substrate four.
Further preferably, the step (4) is specifically to place the third silicon substrate in ultrahigh vacuum magnetron sputtering equipment, perform sputtering film formation on the front surface of the third silicon substrate by using a Ti target, continuously introducing a mixed gas of high-purity helium and high-purity argon at a speed of 12-25mL/min during sputtering, wherein the gas pressure ratio of the high-purity helium to the high-purity argon is (2-10): 1, the pressure value of the mixed gas is 0.5-2 Pa; then sputtering the reverse side of the silicon substrate III by using an Au target to form a film, wherein high-purity argon is continuously introduced at the speed of 12-25mL/min in the sputtering process, the sputtering power is 60-250W, and the air pressure value of the high-purity argon is 0.1-0.5 Pa; and obtaining the silicon substrate IV.
Further preferably, the Ti target in the step (4) is three 5-12cm away from the silicon substrate; the Au target is 16-22cm away from the silicon substrate.
When the MEMS process 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 fine 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 secondary vacuum coating, can obviously reduce the fluctuation degree of the alloy coating, avoids the problems of rough, uneven and compact formed alloy coating, poor size precision of the microstrip circulator and poor reliability of subsequent welding, can keep excellent reliability of the prepared silicon substrate, endows the microstrip circulator with extremely low return loss performance, and prolongs the service life of the silicon substrate microstrip circulator.
In some preferred embodiments, the step (5) is specifically that 2 silicon substrates four are taken to be aligned in an alignment machine, then transferred to a vacuum welding machine for welding, and cut and shaped by using a grinding wheel cutter to obtain silicon substrates five; and embedding the magnetic material into the cavity of the silicon substrate V to obtain a finished product of the silicon-based microstrip circulator.
Further preferably, the temperature of the welding is 250-420 ℃.
In some preferred embodiments, the material of the magnetic material includes at least one of silicon steel sheet, nickel-based alloy, rare earth alloy, and ferrite.
Further preferably, the magnetic material is ferrite.
The invention provides an application of a silicon-based microstrip circulator based on an MEMS (micro-electromechanical system) process, which is applied to the technical field of microwave radio-frequency devices.
Has the advantages that:
the silicon-based microstrip circulator is prepared by the MEMS process, and the obtained product has the advantages of high size precision, low return loss and extreme temperature resistance, and can meet the working requirements of microwave radio-frequency devices. Through specific etching and coating process treatment, the high-performance microwave radio-frequency device can be obtained under a simple process flow, and the method has important significance for the actual production of large-batch high-precision silicon-based microstrip circulators.
Detailed Description
Example 1.
The embodiment provides a silicon-based microstrip circulator based on an MEMS (micro-electromechanical system) process, 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) and (5) shaping, and embedding a magnetic material to obtain a finished product of the silicon-based microstrip circulator.
The silicon wafers were 2 inches in diameter and 0.5mm thick and were from Suzhou wafer service source microelectronics technologies, Inc.
Specifically, the step (1) is to place the silicon wafer in a high-density plasma etching machine, sequentially perform passivation and etching operations to obtain a silicon wafer containing a cavity, and perform wet chemical cleaning on the silicon wafer containing the cavity to obtain a first silicon substrate.
The passivation and etching operations were repeated 5 times.
In particular, with C 4 F 8 Passivating the silicon wafer with gas by using SF 6 ，C 4 F 8 And O 2 Etching the silicon wafer by using the mixed gas; the passivation time is 15s, and the etching time is 8 s; the plate power of the high-density plasma etcher in the etching process is 15W.
In the passivation process C 4 F 8 The gas was introduced at a rate of 90 mL/min.
SF in etching process 6 ，C 4 F 8 And O 2 The gas was introduced at rates of 120mL/min, 12mL/min and 7mL/min, respectively.
The wet chemical cleaning step comprises sequentially placing silicon wafers containing cavities in a chamber containing H 2 SO 4 H of (A) to (B) 2 O 2 Aqueous solution of NH 4 H of OH 2 O 2 Aqueous solution, aqueous HF solution, H containing HCl 2 O 2 Cleaning in water solution to remove organic matters and inorganic impurities; and cleaning the silicon wafer by using Milli Q water after each reagent is cleaned, washing the silicon wafer by using Milli Q water for 10min after the cleaning is finished, placing the silicon wafer in ethanol for ultrasonic cleaning for 5min, and drying the silicon wafer by using nitrogen to obtain a first silicon substrate.
Said containing H 2 SO 4 H of (A) to (B) 2 O 2 H in aqueous solution 2 SO 4 ，H 2 O 2 And water in a volume ratio of 3: 1: 3, the cleaning temperature is 120 ℃, and the cleaning time is 18 min.
Said NH group 4 H of OH 2 O 2 NH in aqueous solution 4 OH，H 2 O 2 And water in a volume ratio of 1: 1: 6; the cleaning temperature is 68 deg.C, and the cleaning time is 4 min.
The volume fraction of HF in the HF aqueous solution is 50%, the cleaning temperature is 27 ℃, and the cleaning time is 5 min.
The HCl-containing H 2 O 2 HCl, H in aqueous solution 2 O 2 And water in a volume ratio of 1: 2: 7; the cleaning temperature was 62 ℃ and the cleaning time was 13 min.
And (2) performing positive and negative magnetron sputtering coating on the silicon substrate I, defining one surface of the silicon substrate as a front surface and the other surface as a back surface, coating the front surface with Ti, and coating the back surface with Au to obtain a silicon substrate II.
Specifically, a first silicon substrate is placed in ultrahigh vacuum magnetron sputtering equipment, a Ti target is used for sputtering and film forming on the front surface of the first 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 pressure ratio of the high-purity helium to the high-purity argon is 5: 1, the pressure value of the mixed gas is 0.8 Pa; and then sputtering the reverse side of the second silicon substrate by using an Au target to form a film, wherein high-purity argon is continuously introduced at the speed of 18mL/min in the sputtering process, the sputtering power is 180W, and the air pressure value of the high-purity argon is 0.1 Pa.
The distance between the Ti target in the step (2) and the silicon substrate is one 10 cm; the Au target was 20cm from the silicon substrate.
The thicknesses of the coating films on the front surface and the back surface are both 5 mu m.
And (3) specifically, carrying out primary photoetching, chemical etching and secondary photoetching on the second silicon substrate in sequence, and forming a pattern on the reverse side 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 side 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 photoresist may be commercially available, for example, from Nyquist, N.Y. model NR 5-8000.
And the chemical etching is specifically to immerse the silicon substrate II subjected to the primary photoetching in an acid mixed solution, react for 5min, take out, wash with Milli Q water for 2min, and purge with nitrogen.
The acid mixed solution comprises hydrofluoric acid, nitric acid, acetic acid and water; hydrofluoric acid, nitric acid, acetic acid and water in a volume ratio of 52: 2: 0.6: 1.2.
specifically, the silicon substrate III is placed in ultrahigh vacuum magnetron sputtering equipment, a Ti target is used for sputtering and film forming on the front surface of the silicon substrate III, 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 pressure ratio of the high-purity helium to the high-purity argon is 5: 1, the pressure value of the mixed gas is 0.8 Pa; then sputtering the reverse side of the silicon substrate III by using an Au target to form a film, wherein high-purity argon is continuously introduced at the speed of 18mL/min in the sputtering process, the sputtering power is 180W, and the air pressure value of the high-purity argon is 0.1 Pa; and obtaining the silicon substrate IV.
The distance between the Ti target and the silicon substrate in the step (4) is three 10 cm; the Au target was three 20cm from the silicon substrate.
Specifically, the silicon substrate IV is soaked in acetone for 12min, taken out, washed with Milli Q water for 2min, and purged with nitrogen; taking 2 silicon substrates four in an aligning machine, stacking and aligning by taking the front surfaces as contact surfaces, then transferring to a vacuum welding machine for welding, and cutting and shaping by using a grinding wheel cutter to obtain a silicon substrate five; and embedding the magnetic material into the cavity of the silicon substrate V to obtain a finished product of the silicon-based microstrip circulator.
The temperature of the welding was 300 ℃.
The magnetic material is ferrite wafer, and is from Suzhou Huawencheng source microelectronics technologies, Inc.
Example 2.
The embodiment provides a silicon-based microstrip circulator based on an MEMS (micro-electromechanical system) process, and the specific implementation manner is the same as that of embodiment 1; different from the above that SF is used 6 Etching a silicon wafer with gas, SF 6 The gas was introduced at a rate of 85 mL/min.
Example 3.
The embodiment provides a silicon-based microstrip circulator based on a MEMS (micro-electromechanical system) process, and the specific implementation manner is the same as that of the embodiment1; the difference is that C is in the passivation process 4 F 8 The gas was introduced at a rate of 120mL/min and the passivation time was 10 s.
Example 4.
The embodiment provides a silicon-based microstrip circulator based on an MEMS (micro-electromechanical system) process, and the specific implementation manner is the same as that of embodiment 1; the difference is that in the step (2), a Ti target is used for sputtering film formation on the front surface of the first silicon substrate, mixed gas of high-purity helium and high-purity argon is continuously introduced at a speed of 28mL/min in the sputtering process, and the 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 an MEMS (micro-electromechanical system) process, and the specific implementation manner is the same as that of embodiment 1; except that the Ti target was located one 5cm from the silicon substrate in the step (2).
Example 6.
The embodiment provides a silicon-based microstrip circulator based on an MEMS (micro-electromechanical system) process, and the specific implementation manner is the same as that of embodiment 1; except that the temperature of the weld was 375 deg.c.
Performance test method
Return loss:
the silicon-based microstrip circulators of examples 1-6 were tested for return loss under 20Ghz conditions; each set of samples was averaged 5 times in parallel.
High temperature resistance:
the silicon-based microstrip circulator of examples 1-6 was placed at 65 ℃ for 24h, and after being taken out, 5 points were randomly selected on the finished substrate to measure the thickness, and the relative standard deviation RSD of the 5 point thickness results was calculated 1 (ii) a Each set of samples was averaged 5 times in parallel.
Low temperature resistance:
the silicon-based microstrip circulator of the embodiment 1-6 is placed for 24h at the temperature of minus 10 ℃, 5 points are randomly selected on the finished substrate product after being taken out for testing the thickness, and the relative standard deviation RSD of the thickness result of the 5 points is calculated 2 (ii) a Each set of samples was averaged 5 times in parallel.
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 (10)
1. A silicon-based microstrip circulator based on MEMS technology is characterized in that the preparation step of the silicon-based microstrip circulator comprises the following 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 a magnetic material to obtain a finished product of the silicon-based microstrip circulator;
the thickness of the silicon wafer is 0.1-1 mm.
2. The silicon-based microstrip circulator of claim 1, wherein the 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. The silicon-based microstrip circulator of claim 2 wherein the passivation and etching operations are repeated between 5 and 20 times.
4. The silicon-based microstrip circulator as claimed in any one of claims 1 to 3, wherein step (2) is specifically to perform magnetron sputtering coating on the front and back sides of the first silicon substrate, defining one side of the first silicon substrate as the front side and the other side as the back side, and the front side is coated with Ti and the back side is coated with Au to obtain the second silicon substrate.
5. The silicon-based microstrip circulator of claim 4 wherein the front and back coating thickness is 2-16 μm.
6. The silicon-based microstrip circulator of any one of claims 1-5, wherein step (3) is specifically to sequentially perform a first photolithography, a chemical etching, and a second photolithography on the second silicon substrate, and form a pattern on the reverse side of the second silicon substrate to obtain a third silicon substrate.
7. The silicon-based microstrip circulator as claimed in any of claims 1 to 6, wherein step (4) is specifically to perform two magnetron sputtering coating on the third silicon substrate, and the front surface is coated with Ti and the back surface is coated with Au to obtain the fourth silicon substrate.
8. The silicon-based microstrip circulator of any one of claims 1 to 7, 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 cutter to obtain a silicon substrate five; and embedding the magnetic material into the cavity of the silicon substrate V to obtain a finished product of the silicon-based microstrip circulator.
9. The silicon-based microstrip circulator of claim 8 wherein the magnetic material comprises at least one of silicon steel, nickel-based alloy, rare earth alloy, and ferrite.
10. Use of a silicon-based microstrip circulator according to any of claims 1 to 9 in the field of microwave rf device technology.
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