CN114195092A - Glass fusion bonding-based vacuum leak hole packaging method with minimum leak rate - Google Patents

Glass fusion bonding-based vacuum leak hole packaging method with minimum leak rate Download PDF

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Publication number
CN114195092A
CN114195092A CN202111515859.2A CN202111515859A CN114195092A CN 114195092 A CN114195092 A CN 114195092A CN 202111515859 A CN202111515859 A CN 202111515859A CN 114195092 A CN114195092 A CN 114195092A
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glass tube
silicon wafer
vacuum
vacuum leak
leak hole
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CN202111515859.2A
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王旭迪
林文豫
毕海林
张俊
常仁超
党伟
黄昌俊
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Hefei University of Technology
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Hefei University of Technology
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Priority to CN202111515859.2A priority Critical patent/CN114195092A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C3/00—Assembling of devices or systems from individually processed components
    • B81C3/001—Bonding of two components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00261—Processes for packaging MEMS devices
    • B81C1/00325—Processes for packaging MEMS devices for reducing stress inside of the package structure

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Micromachines (AREA)

Abstract

The invention discloses a method for packaging a vacuum leak hole with minimum leak rate based on glass fusion bonding, which comprises the steps of firstly manufacturing a vacuum leak hole element with minimum leak rate by adopting an MEMS (micro electro mechanical system) ultraviolet lithography process and a silicon-silicon direct bonding technology, cleaning the vacuum leak hole element and a polished glass tube, aligning the vacuum leak hole element and the polished glass tube at room temperature, putting the vacuum leak hole element and the polished glass tube into a high-temperature furnace for heat treatment, leading the end surface of the polished glass tube to generate a fusion phenomenon along with the temperature rise, keeping the temperature at the highest temperature of the heat treatment for a certain time to ensure that a bonding interface of the end surface of the glass tube and the vacuum leak hole element generates enough material reflux, removing stress, annealing, eliminating internal stress generated by the heat treatment of the glass tube, cooling the glass tube to room temperature, taking out a bonding finished product, clamping the bonding finished product on a vacuum knife-edge flange with a clamping sleeve by using front and rear polytetrafluoroethylene clamping sleeves to complete the packaging of the vacuum leak hole, wherein the method has the minimum leak rate, the method can be applied to the packaging of ultrahigh vacuum and leakage holes with extremely low leakage rate.

Description

Glass fusion bonding-based vacuum leak hole packaging method with minimum leak rate
Technical Field
The invention relates to a manufacturing method and a packaging method of a vacuum leak with an extremely small leak rate, in particular to a packaging method of the vacuum leak with the extremely small leak rate based on glass fusion bonding.
Background
Fusion bonding is a technique for bonding specially treated materials at a specific temperature and pressure, and generally comprises two process steps: 1. pre-bonding at room temperature. 2. And (4) annealing at high temperature. The principle is that the viscosity of the material is reduced and the fluidity of the material is increased along with the increase of the temperature, a material flow is formed on a contact interface to fill a bonding gap, and the material flow is solidified again to play a role in connection after the temperature is reduced. One of the characteristics of fusion bonding is that no intermediate layer material and adhesive are needed, no extra electric field is needed, the steps are simple, the connection is reliable, and the bonding strength is high. Melt bonding has the additional feature of a wider choice of bonding materials and is therefore commonly used in mems packaging and IC production.
The vacuum leak hole is used as a key scale in the vacuum metering technology, can provide a constant known leak rate under a specific environmental condition, and is widely applied to the aspects of leak rate detection of a vacuum component, calibration of a measuring instrument and the like on the basis of the characteristic. The complete vacuum leak includes a vacuum leak element and a package component, and the vacuum leak can be generally classified into a penetration type vacuum leak and a channel type vacuum leak according to the difference of the leak mechanism. The permeation type vacuum leak hole is made according to the selective permeability of materials to gas, the gas leakage process comprises adsorption, permeation and desorption, the gas leakage in the channel type vacuum leak hole is a flow limiting channel passing through a leak hole element, and common flow limiting channels comprise a metal flat pressing pipe, a glass capillary pipe, a powder sintering channel and the like.
At present, the requirement for detection of the minimum leakage rate further reduces the size of a flow limiting channel of the channel type vacuum leak to the micro-nano level, which provides a challenge for the packaging of the minimum leakage rate vacuum leak and how to realize reliable connection of a micro channel and macro equipment to form a new problem. The current packaging method of the vacuum leak hole with the minimum leak rate mainly adopts vacuum glue sealing and a mechanical clamping structure, but the glue sealing has an air release phenomenon in a high vacuum environment, and the glue can block a flow limiting channel, which affects the practical use of the vacuum leak hole. The mechanical clamping structure directly applies pressure to the leak element during the packaging process, which causes the leak element made of brittle materials (such as silicon, glass, etc.) to be damaged with high probability. Therefore, there is a need for a method for packaging a vacuum leak with a minimum leak rate, which provides reliable micro-macro connection for the vacuum leak with the minimum leak rate and ensures the performance under high vacuum.
Disclosure of Invention
The invention provides a glass fusion bonding-based vacuum leak hole packaging method with a minimum leak rate, which is used for solving the problems.
A method for packaging a vacuum leak hole with minimum leak rate based on glass fusion bonding comprises fabricating a vacuum leak hole element with minimum leak rate by MEMS ultraviolet lithography and silicon-silicon direct bonding, cleaning the vacuum leak hole element and polished glass tube, aligning at room temperature, then the glass tube and the glass tube are put in a high temperature furnace for heat treatment, the polished end surface of the glass tube is firstly melted along with the temperature rise, keeping for a certain time at the highest temperature of the heat treatment to ensure that enough material backflow is generated on the bonding interface of the end face of the glass tube and the vacuum leak element, then performing stress relief annealing to eliminate the internal stress generated by the heat treatment of the glass tube, cooling to room temperature, and taking out the bonded product, and clamping the bonded product on a vacuum knife edge flange with a clamping sleeve by using a front polytetrafluoroethylene clamping sleeve and a rear polytetrafluoroethylene clamping sleeve to finish the packaging of the vacuum leak hole with the minimum leak rate.
As a preferred embodiment of the above method, the method operates as follows:
a. taking a new silicon wafer, wiping the surface with acetone to remove floating dust and particles on the surface, then placing the silicon wafer in a vacuum environment, and bombarding the silicon wafer with oxygen ions for 60min to activate the surface of the silicon wafer;
b. spinning AZ3740 photoresist on the surface of the silicon wafer treated in the step a, setting the rotating speed of a photoresist spinner to 800r/s for 8s, then entering 1500r/s for 35s, and then placing the silicon wafer into an oven to bake at 90 ℃ for 40min to cure the photoresist;
c. b, performing mask ultraviolet exposure on the silicon wafer on the basis of the step b, attaching the silicon wafer and the mask, horizontally placing the silicon wafer on a deep ultraviolet exposure platform, opening a mercury lamp to irradiate emitter ultraviolet light for 10s, then developing the silicon wafer in a developing solution for 90s, forming a photoresist pattern mask on the surface of the silicon wafer, and etching a groove shape with the depth of 100nm on the surface of the silicon wafer by using an RIE etching machine;
d. taking the other double polished silicon wafer as a cover plate, punching a hole at the center position by using laser to serve as an air outlet, and then putting the hole and the patterned silicon wafer in the step c into an H2SO4:H2O2(2:1) cleaning in the solution for 30min to remove surface impurities and residual photoresist, and then putting into NH4OH:H2O2:H2Heating in O (1:1:5) solution in water bath to 78 deg.C, and maintaining for 10 min;
e. d, washing the silicon wafer treated in the step d with deionized water, drying surface moisture by using nitrogen, aligning and attaching the cover plate silicon wafer and the pattern silicon wafer in an ethylene glycol solution at room temperature, taking out the silicon wafer, absorbing redundant ethylene glycol solution on the surface by using dust-free paper, heating the attached silicon wafer to 200 ℃, keeping the temperature for 120min, putting the silicon wafer into a high-temperature furnace after prebonding is completed, heating to 1100 ℃ and keeping the temperature for 30min, and cooling to room temperature to obtain the vacuum hole-leaking element with the minimum leak rate;
f. cutting the glass tube to a proper length by using a diamond cutting blade, polishing the end face of the glass tube by using polishing sand paper and grinding paste respectively, then soaking the glass tube into a 1% HF solution for ultrasonic cleaning for 20min, and removing wax and grinding particles on the surface of the glass tube;
g. f, using the glass tube treated in the step f as H2SO4:H2O2(2:1) cleaning the solution for 30min to remove organic impurities on the surface, washing the solution with deionized water, soaking the solution in absolute ethyl alcohol for 10min, taking out the solution, drying the solution with nitrogen, placing the cleaned glass tube in alignment with the vacuum leak hole element, and keeping the glass tube and the vacuum leak hole element to be dischargedAxial alignment of the ports;
h. putting the sample in the step g into a high-temperature furnace, heating to 780 ℃ and keeping for 5min, then cooling to 550 ℃ according to the cooling rate of 2 ℃/min and keeping for 60min, then cooling to 400 ℃ according to the cooling rate of 1 ℃/min, and then cooling to room temperature along with the furnace to obtain a fusion bonding sample of the glass tube and the vacuum leak element, wherein the air flow enters from the channels at the two sides of the vacuum leak element through the path of the sample, flows out from the central hole, and enters into external equipment through the glass tube;
i. and (4) selecting a polytetrafluoroethylene front clamping sleeve and a polytetrafluoroethylene rear clamping sleeve, clamping the sample obtained in the step h onto a vacuum knife edge flange with a clamping sleeve, and applying a certain torque to a torque wrench to tighten the clamping sleeve so as to finish the packaging of the vacuum leak hole with the minimum leak rate.
As a preferred embodiment of the above method, the spin-coated AZ3740 photoresist in step b is about 400nm thick.
As a preferred embodiment of the above method, the reticle pattern in step c is a linear grating having a period of 8um, a length of 15mm, a width of 1mm, and a total of 125 lines.
In a preferred embodiment of the above method, the diameter of the hole drilled at the center of step d is 2 mm.
As a preferred embodiment of the above method, the glass tube in step f is a high borosilicate glass tube having an outer diameter of 8mm, an inner diameter of 5mm, a cutting length of 30mm, and an end face polished surface roughness of less than 10 nm.
As a preferred embodiment of the above method, the torque for tightening the ferrule in step i is 2N · m.
Compared with the prior art, the beneficial technical effects of the invention are as follows:
1. the method has the advantages of simple and convenient operation, high bonding strength, reliable connection, high yield and capability of realizing batch production.
2. The difference of the thermal expansion coefficients of the high borosilicate glass and the silicon is small in a certain temperature range, and the high borosilicate glass and the silicon are not damaged due to the existence of excessive thermal stress in the fusion bonding.
3. The choice of 780 ℃/5min heat treatment parameters avoids complete melt bending of the high borosilicate glass tube while retaining sufficient mechanical strength to allow subsequent mechanical encapsulation.
4. The fused and bonded glass tube is used as a stress platform, so that the vacuum leak hole element is not stressed in the mechanical clamping process, and the vacuum leak hole element is prevented from being damaged.
5. The front and rear polytetrafluoroethylene clamping sleeves have self-lubricating property, are easy to deform and can ensure the sealing reliability.
6. The silicon-glass fusion bonding and the clamping and packaging of the clamping sleeve have enough sealing performance, the self-air-release rate of the selected material is extremely low, and any bonding agent is not needed in the packaging process, so that the silicon-glass fusion bonding and clamping sleeve can be used for packaging an extremely-low-leakage-rate vacuum leak hole and can be used in a high vacuum environment or even an ultrahigh vacuum environment.
Drawings
FIG. 1 is a flow chart of a process for preparing a vacuum leak hole element with a minimum leak rate and fusion bonding glass.
Fig. 2 is a schematic cross-sectional view of the flow direction of a micro-macro junction of a prepared melt-bonded sample gas.
FIG. 3 is a schematic cross-sectional view of the structure of the method for packaging a vacuum leak hole with a minimum leak rate based on glass fusion bonding according to the present invention.
Reference numbers in the figures: 1-silicon chip, 2-AZ3740 photoresist, 3-mask, 4-extreme ultraviolet light, 5-RIE etching gas, 6-glycol solution, 7-double polished silicon chip, 8-glass tube, 9-polytetrafluoroethylene front and rear cutting sleeve, 10-cutting sleeve and 11-vacuum knife edge flange.
Detailed Description
As shown in FIG. 3, the present example is a method for encapsulating a vacuum leak hole with a minimum leak rate based on glass fusion bonding, and the specific implementation mode is operated as follows:
1. as shown in fig. 1(a), a new silicon wafer 1 is taken, the surface of the silicon wafer is wiped by acetone to remove floating dust and particles on the surface, then the silicon wafer is placed in a vacuum environment, and the silicon wafer is bombarded by oxygen ions for 60min to activate the surface of the silicon wafer;
2. as shown in fig. 1(b), the surface of the silicon wafer 1 treated in the step 1 is spin-coated with AZ3740 photoresist 2, the rotating speed of a photoresist spinner is set to 800r/s for 8s, then the silicon wafer enters 1500r/s for 35s, and then the silicon wafer is placed into an oven to be baked at 90 ℃ for 40min to cure the photoresist;
3. carrying out mask ultraviolet exposure on the silicon wafer 1 and the AZ3740 photoresist 2 on the basis of the step 2, attaching the silicon wafer 1 coated with the AZ3740 photoresist 2 to a mask 3 as shown in a figure 1(c), horizontally placing the silicon wafer on a deep ultraviolet exposure platform, opening a mercury lamp, irradiating and exposing for 10s under extreme ultraviolet light 4, developing for 90s in a developing solution to form a photoresist mask on the surface of the silicon wafer 1, and etching a groove with the depth of 100nm on the silicon wafer 1 by using RIE etching gas 5 in an RIE etching machine as shown in a figure 1 (d);
4. taking the other double-polished silicon wafer 7 as a cover plate, punching a hole at the center position by using laser to serve as an air outlet, and then putting the hole and the silicon wafer 1 processed in the step (3) into a H2SO4:H2O2(2:1) cleaning in the solution for 30min to remove surface impurities and residual photoresist, as shown in FIG. 1(e), to obtain a clean silicon wafer surface, and then putting NH into the clean silicon wafer surface4OH:H2O2:H2Heating in O (1:1:5) solution in water bath to 78 deg.C, and maintaining for 10 min;
5. washing the treated silicon wafer 1 and the double polished silicon wafer 7 with deionized water, drying the surface moisture of the silicon wafer 1 with nitrogen, aligning and attaching the double polished silicon wafer 7 and the silicon wafer 1 in an ethylene glycol solution 6 at room temperature as shown in figure 1(f), taking out, absorbing the redundant ethylene glycol solution 6 on the surface with dust-free paper, heating the attached sample to 200 ℃, keeping for 120min, placing the pre-bonded silicon wafer into a high-temperature furnace, heating to 1100 ℃ and keeping for 30min, cooling to room temperature as shown in figure 1(g), and then bonding the silicon wafer 1 and the double polished silicon wafer 7 to obtain a vacuum hole-leaking element;
cutting the glass tube 8 to a proper length by using a diamond cutting blade, polishing the end face of the glass tube 8 by using polishing sand and grinding paste respectively, then soaking the glass tube into a 1% HF solution for ultrasonic cleaning for 20min, and removing wax and grinding particles on the surface of the glass tube 8;
7. h is used for the glass tube 8 treated in the step 62SO4:H2O2(2:1) cleaning with the solution for 30min to remove organic impurities on the surface, washing with deionized water, and soakingTaking out the glass tube 8 after being cleaned and drying the glass tube in the absolute ethyl alcohol for 10min, aligning the glass tube 8 with a vacuum leak hole element, and keeping the glass tube axially aligned with an air outlet of a double polished silicon wafer 7 as shown in figure 1 (h);
8. putting the sample in the step 7 into a high temperature furnace, heating to 780 ℃ and keeping for 5min, then cooling to 550 ℃ according to the cooling rate of 2 ℃/min and keeping for 60min, then cooling to 400 ℃ according to the cooling rate of 1 ℃/min, and then cooling to room temperature along with the furnace to obtain a fusion bonding sample of the glass tube 8 and the vacuum leak hole element, wherein as shown in fig. 2, the path of air flow passing through the sample is that the air flow enters from channels formed by sealing the silicon wafer 1 and the double polished silicon wafer 7 on two sides of the vacuum leak hole element, flows out from a central hole on the double polished silicon wafer 7, and enters external equipment through the glass tube 8;
9. as shown in fig. 3, a polytetrafluoroethylene front and rear clamping sleeve 9 is selected, the sample obtained in the step 8 is clamped on a vacuum knife edge flange 11 with a clamping sleeve 10, a certain torque is applied to a torque wrench to tighten the clamping sleeve 10, and the packaging of the vacuum leak hole with the minimum leak rate is completed.
The implementation method utilizes glass fusion bonding and a cutting sleeve structure to package the vacuum leak hole, and the packaging leak rate is lower than 10- 13Pa.m3.s-1The method meets the requirement of ultrahigh vacuum packaging and can be used for packaging vacuum leak holes with extremely low leak rate.

Claims (7)

1. A method for packaging a vacuum leak hole with minimum leak rate based on glass fusion bonding is characterized in that an MEMS ultraviolet photoetching process and a silicon-silicon direct bonding technology are firstly adopted to manufacture a vacuum leak hole element with minimum leak rate, then the vacuum leak hole element and a polished glass tube are cleaned and aligned at room temperature, then the glass tube and the glass tube are put in a high temperature furnace for heat treatment, the polished end surface of the glass tube is firstly melted along with the temperature rise, keeping for a certain time at the highest temperature of heat treatment to ensure that enough material backflow is generated on the bonding interface of the end face of the glass tube and the vacuum leak element, then removing internal stress generated by the heat treatment of the glass tube through stress relief annealing, cooling to room temperature, and taking out the bonded product, and clamping the bonded product on a vacuum knife edge flange with a clamping sleeve by using a front polytetrafluoroethylene clamping sleeve and a rear polytetrafluoroethylene clamping sleeve to finish the packaging of the vacuum leak hole with the minimum leak rate.
2. The method of claim 1 wherein the method comprises the steps of:
a. taking a new silicon wafer, wiping the surface with acetone to remove floating dust and particles on the surface, then placing the silicon wafer in a vacuum environment, and bombarding the silicon wafer with oxygen ions for 60min to activate the surface of the silicon wafer;
b. spinning AZ3740 photoresist on the surface of the silicon wafer treated in the step a, setting the rotating speed of a photoresist spinner to 800r/s for 8s, then entering 1500r/s for 35s, and then placing the silicon wafer into an oven to bake at 90 ℃ for 40min to cure the photoresist;
c. b, performing mask ultraviolet exposure on the silicon wafer on the basis of the step b, attaching the silicon wafer and the mask, horizontally placing the silicon wafer on a deep ultraviolet exposure table, starting a mercury lamp, performing extreme ultraviolet irradiation exposure for 10s, developing the silicon wafer in a developing solution for 90s, forming a photoresist pattern mask on the surface of the silicon wafer, and etching a groove shape with the depth of 100nm on the surface of the silicon wafer by using an RIE etching machine;
d. taking the other double polished silicon wafer as a cover plate, punching a hole at the center position by using laser to serve as an air outlet, and then putting the hole and the patterned silicon wafer in the step c into an H2SO4:H2O2(2:1) cleaning in the solution for 30min to remove surface impurities and residual photoresist, and then putting into NH4OH:H2O2:H2Heating in O (1:1:5) solution in water bath to 78 deg.C, and maintaining for 10 min;
e. d, washing the silicon wafer treated in the step d with deionized water, drying surface moisture by using nitrogen, aligning and attaching the cover plate silicon wafer and the pattern silicon wafer in an ethylene glycol solution at room temperature, taking out the silicon wafer, absorbing redundant ethylene glycol solution on the surface by using dust-free paper, heating the attached silicon wafer to 200 ℃, keeping the temperature for 120min, putting the silicon wafer into a high-temperature furnace after prebonding is completed, heating to 1100 ℃, keeping the temperature for 30min, and cooling to room temperature to obtain the vacuum leak hole element with the minimum leak rate;
f. cutting the glass tube to a proper length by using a diamond cutting blade, polishing the end face of the glass tube by using polishing sand paper and grinding paste respectively, then soaking the glass tube into a 1% HF solution for ultrasonic cleaning for 20min, and removing wax and grinding particles on the surface of the glass tube;
g. f, using the glass tube treated in the step f as H2SO4:H2O2(2:1) cleaning the solution for 30min to remove organic impurities on the surface, washing the solution with deionized water, soaking the solution in absolute ethyl alcohol for 10min, taking the solution out, drying the solution with nitrogen, placing the cleaned glass tube in alignment with a vacuum leak hole element, and keeping the glass tube in alignment with the axial direction of an air outlet of the vacuum leak hole element;
h. putting the sample in the step g into a high-temperature furnace, heating to 780 ℃ and keeping for 5min, then cooling to 550 ℃ according to the cooling rate of 2 ℃/min and keeping for 60min, then cooling to 400 ℃ according to the cooling rate of 1 ℃/min, and then cooling to room temperature along with the furnace to obtain a fusion bonding sample of the glass tube and the vacuum leak element;
i. and (4) selecting a polytetrafluoroethylene front clamping sleeve and a polytetrafluoroethylene rear clamping sleeve, clamping the fusion bonding sample obtained in the step h to a vacuum knife edge flange with a clamping sleeve, and applying a certain torque to a torque wrench to tighten the clamping sleeve so as to finish the packaging of the vacuum leak hole with the minimum leak rate.
3. The method as claimed in claim 2, wherein the spin-coated AZ3740 photoresist in step b has a thickness of about 400 nm.
4. The method of claim 2, wherein the reticle pattern in step c is a 125 line linear grating with a period of 8um, a length of 15mm and a width of 1 mm.
5. The method of claim 2 wherein the diameter of the hole drilled in the center of step d is 2 mm.
6. The method according to claim 2, wherein the glass tube in step f is a borosilicate glass tube having an outer diameter of 8mm, an inner diameter of 5mm, a cutting length of 30mm, and an end-face polished surface roughness of less than 10 nm.
7. The method of claim 2 wherein the torque to tighten the ferrule in step i is 2N · m.
CN202111515859.2A 2021-11-30 2021-11-30 Glass fusion bonding-based vacuum leak hole packaging method with minimum leak rate Pending CN114195092A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111515859.2A CN114195092A (en) 2021-11-30 2021-11-30 Glass fusion bonding-based vacuum leak hole packaging method with minimum leak rate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111515859.2A CN114195092A (en) 2021-11-30 2021-11-30 Glass fusion bonding-based vacuum leak hole packaging method with minimum leak rate

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CN114195092A true CN114195092A (en) 2022-03-18

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