WO2011072600A1 - 圆片级玻璃微腔的发泡成型制造方法 - Google Patents
圆片级玻璃微腔的发泡成型制造方法 Download PDFInfo
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- WO2011072600A1 WO2011072600A1 PCT/CN2010/079785 CN2010079785W WO2011072600A1 WO 2011072600 A1 WO2011072600 A1 WO 2011072600A1 CN 2010079785 W CN2010079785 W CN 2010079785W WO 2011072600 A1 WO2011072600 A1 WO 2011072600A1
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- temperature
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- microcavity
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/08—Other methods of shaping glass by foaming
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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
- 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
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00055—Grooves
- B81C1/00071—Channels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/0032—Packages or encapsulation
- B81B7/0045—Packages or encapsulation for reducing stress inside of the package structure
- B81B7/0051—Packages or encapsulation for reducing stress inside of the package structure between the package lid and the substrate
Definitions
- the present invention relates to a microsystem manufacturing technique, and more particularly to a foam molding manufacturing method for a wafer-level glass microcavity.
- Pyrex7740 glass (a glass containing alkaline ions, Pyrex is a product brand of Coming) is an important material with a thermal expansion coefficient similar to that of Si material, high transmittance and high strength, and By using a anodic bonding process to form a high strength bonding bond with the Si substrate, a strong Si-O covalent bond is produced on the bonding surface, which is even stronger than the Si material itself. Due to this feature, Pyrex7740 glass is widely used in MEMS packaging, microfluidics and MOEMS (micro-optical electromechanical systems). Currently, glass microcavities and microchannel systems are primarily used in the field of sensors and biochips.
- the current common method for the preparation of microchannels is to directly etch the microfluidic channel and the pattern structure of various fluid components on silicon, glass, PDMS (polydimethylsiloxane), and then bond the material to another plane.
- a MEMS microfluidic system is formed.
- Microfluidic glass thermoforming can be formed by vacuum forming and positive pressure forming.
- Negative pressure forming (China Patent 200710190226.2): Etching a pattern such as a flow path on silicon, anodic bonding silicon and glass in a vacuum, and then heating to a high temperature in air to form a negative pressure thermoforming inside and outside the chamber.
- This method can only be used with a vacuum bonding device, and thus the cost is high; in addition, the method uses negative pressure molding, so that the formed micro flow path is located on the back side of the glass wafer, so when the glass wafer is thick, the back surface
- the formed microchannel shape is uncontrollable and the flow channel is shallow; for forming a high glass microchannel, it is usually necessary to use a thick silicon wafer, and it is necessary to etch a deep silicon cavity (some even need to reach 900) Micron, Glass Blowing on a Wafer Level, JOURNAL OF MICROELECTROMECHANICAL SYSTEMS, VOL. 16, NO.
- the object of the present invention is to provide a wafer-level glass microparticle with low cost, high microcavity height and good arc shape. Foam molding manufacturing method of cavity.
- a foam molding manufacturing method for a wafer-level glass microcavity includes the following steps:
- the silicon trench is etched on the Si wafer by the Si micromachining process.
- the second step is to place an appropriate amount of high temperature release agent in the silicon tank.
- the Si wafer is anodic bonded to the Pyrex 7740 glass wafer to form the silicon cavity into a sealed cavity.
- the above-mentioned bonded wafer is heated to 810 ° C to 1000 ° C in air for 5 to 10 minutes, and the high-temperature release agent releases gas by heat, and generates a positive pressure so that the molten glass corresponding to the sealed cavity is sealed.
- the structure corresponding to the silicon groove is formed on the glass by deformation, and is cooled to obtain a wafer-level glass microchannel.
- the silicon trench is a specific silicon microchannel pattern or an array of mutually independent grooves. It is characterized in that the high temperature release agent is calcium carbonate powder or titanium hydride powder.
- the silicon trench etched in the first step has a depth of 10-300 microns.
- the two ends of the micro flow channel are removed by a laser dicing method.
- the specific steps of the laser dicing method are as follows: First, the dicing groove is laser etched on the silicon wafer, and then the bonded wafer is bent to make the wafer The wafer is broken by tension and the high temperature release agent residue is removed.
- the micromachining process on the shallow grooves on the Si wafer is a wet etching process.
- the anodic bonding process conditions of the Si wafer and the Pyrex 7740 glass are: temperature 400 ° C, voltage: 600V.
- the heating temperature in the fourth step is 840 ° C to 850 ° C.
- the microchannel obtained in the fourth step is thermally annealed under the following conditions: an annealing temperature in the range of 510 ° C to 560 ° C, an annealing time of 30 min, and then a slow air cooling to normal temperature.
- the bonding of the silicon to the glass wafer is carried out in air.
- the invention is based on a conventional MEMS processing process.
- a silicon trench structure processed on a Si wafer is filled with a high temperature gas release agent in a shallow groove, and then a Pyrex 7740 glass is covered on the shallow groove by an anodic bonding process to form a closed microcavity.
- Heating then causes the glass to melt, and the high temperature release agent releases the gas such that the circular or square (planar pattern;) has a spherical structure such that the rectangular silicon grooves form a narrow flow path structure.
- the glass is hemispherical in a circular arc shape to form a glass microchannel.
- the high-temperature release agent is used to provide a gas source for forming a glass microchannel, which has the advantages of low cost, simple method and high molding height (if a sufficient amount of high-temperature release agent is added, for a spherical cavity, it may be a cavity larger than a hemisphere;
- the micro-channel, the cross-section can be larger than the semi-circle, and the sphericity is good;
- the inner wall and the outer wall of the glass microcavity formed by thermoforming have high smoothness, the inner wall roughness can reach below 1 nm, and the outer wall roughness can be less than 10 nm. Therefore, it has a lower flow resistance for the micro flow passage; and has high light transmittance at the same time.
- the prior art etching a deep cavity having a relatively large depth and width requires a dry process, which usually takes several tens of hours, and the process cost is also high.
- the invention only needs to use a low-cost wet etching process to etch a shallow silicon trough on a silicon wafer, and to fill a high-temperature gas releasing agent in a part of the silicon trough, which has the advantages of simple method and low cost. 2.
- the contaminated area can be removed by the dicing process, and at the same time, the effect of opening the fluid inlet and outlet port is achieved.
- the invention only needs to place the high-temperature air release agent locally, and the generated gas can be used for the formation of the entire micro-flow passage, and the contamination of the MEMS micro-flow passage by the residue can be avoided.
- the anode bonding temperature is 400 degrees Celsius, so the standard temperature is 673K, the molding temperature is about 850 degrees Celsius, and the standard temperature is about 1123K.
- the amount of gas is constant, the expanded The volume is less than twice the original, which makes it necessary to etch deeper grooves.
- the present invention uses a wet process to etch silicon trenches on silicon at a lower cost.
- the prior art requires etching a deeper silicon cavity having a higher aspect ratio to provide sufficient gas. It is difficult to obtain a large aspect ratio by the wet etching process. When etching deeper microcavities, the cost is higher and takes longer.
- the wet process has lower cost and mature process, and has the advantages of low cost and high efficiency in etching shallow grooves.
- the invention does not require a large aspect ratio and does not require a large depth, and the wet process can reduce cost and improve efficiency.
- the high-temperature gas release agent of the invention uses calcium carbonate powder.
- the large decomposition temperature of the calcium carbonate powder is above 800 degrees Celsius, which has a good matching with the melting temperature of the glass.
- the calcium carbonate At less than 800 degrees Celsius, the calcium carbonate only There is a small amount of decomposition, so the glass cavity sealed before the glass is not formed will not be broken due to excessive gas pressure. Above 800 degrees Celsius, the calcium carbonate powder decomposes a large amount of carbon dioxide gas, thereby forming the glass.
- the present invention only requires a simple calculation based on the amount of decomposition of calcium carbonate, and the amount of calcium carbonate required to form a specific volume of the glass microcavity can be known. According to the correction formula of the reaction rate balance formula:
- the internal pressure can be controlled more accurately, so that the internal cross-section of the glass microchannel can be adjusted, and the self-regulation can be selected according to different flow rates. Therefore, the method is simple, reliable and has a wide application range.
- the high-temperature gas releasing agent of the invention uses titanium hydride powder, and a small amount of titanium hydride powder can release a large amount of gas, so the use of the titanium hydride powder can make the volume of the powder to be smaller and the technical difficulty is lowered.
- the invention mixes a small amount of powder into a large volume of water, acetone and the like to form a uniform mixed liquid, and then takes a specific volume and places it in the flow channel, thereby achieving the purpose of accurately controlling the volume of the powder, thereby facilitating the glass microcavity. Precise control of volume.
- the anodic bonding has the characteristics of high bonding strength and good airtightness.
- the present invention adopts anodic bonding to form a closed cavity, and the bonding region forms a Si-O bond, and the chemical bond still has high strength at a high temperature. It does not easily leak during heating and causes molding failure. Under the bonding conditions of temperature 400 ° C and voltage DC 600 V, anodic bonding can achieve better sealing effect.
- the annealing process in the fourth step can effectively eliminate the stress formed during the high temperature positive pressure forming process of Pyrex7740 glass, thus making it strong Degree of toughness is higher. Annealing under this condition can effectively retreat the stress and also make the shape of the microchannel cavity substantially unchanged.
- the present invention prepares Pyrex 7740 glass which is equivalent to the coefficient of thermal expansion of Si as a glass microchannel structure, and it is not easy to cause damage of the bonded wafer due to thermal mismatch in the preparation of the microcavity.
- FIG. 1 is a schematic transverse cross-sectional view of a bonding wafer with a microchannel shallow groove etched according to the present invention.
- FIG. 2 is a schematic cross-sectional view of the glass microchannel after the thermoforming of the present invention.
- FIG. 3 is a schematic longitudinal cross-sectional view of the glass microchannel after the thermoforming of the present invention.
- Figure 4 is a top plan view of the wafer-level glass microchannel of the present invention.
- Figure 5 is a schematic cross-sectional view of a wafer-level glass microcavity according to the present invention.
- Figure 6 shows the relationship between the mass of titanium hydride and the height of the glass microchannel under different opening half widths (half the width of the silicon groove) of the present invention (flow path length 3 cm, foaming temperature 1123 K, silicon etching depth 0.06 mm).
- Fig. 7 is a view showing the relationship between the mass of the titanium hydride and the glass microchannel under different opening radii (the opening of the silicon groove is round;); (foaming temperature 1123K, silicon etching depth 0.06mm;).
- FIG. 8 is a schematic view showing the structure of a spherical glass microcavity connected by a glass microchannel according to the present invention (Example
- a foam molding manufacturing method for a wafer-level glass microcavity includes the following steps:
- the silicon trench is etched on a Si wafer (such as a 4-inch wafer) by a Si micromachining process.
- the silicon wafer used may be a silicon wafer of standard thickness, or may be thinner (e.g., 300 micrometers) or thicker.
- Silicon wafer (600 microns) such as a 500 micron thick silicon wafer having a depth of 10-500 microns, such as 15 microns, 30 microns, 40 microns, 60 microns, 95 microns, 132 microns, 150 microns.
- the micromachining process of the pattern structure on the wafer is a wet etching process, or one of a dry inductively coupled plasma (ICP) etching process and a reactive ion etching, preferably a low-cost wet etching process, for example, using a TMAH solution.
- ICP dry inductively coupled plasma
- the pattern may be a square or circular groove array (for packaging MEMS device arrays;), the grooves are independent of each other, not connected; may also be a silicon flow channel having a certain size; or connected by a silicon flow channel Square slot Circular groove, a groove or a square groove width of the circular flow channel silicon may not be equal, or the size of a plurality of circular grooves square grooves may be unequal.
- an appropriate amount of high-temperature gas releasing agent is placed in the silicon tank, and the amount of the high-temperature releasing agent is determined according to the size of the micro-groove Calculate the volume of the inch, calculate the volume of the expected micro-cavity of the glass, and calculate the amount of the high-temperature release agent according to the amount of gas released from the high-temperature release agent.
- the high-temperature release agent refers to the release agent with an outgassing temperature higher than 500 degrees Celsius.
- a gas such as calcium carbonate (a chemically pure (99% by mass) calcium carbonate having a small particle size), magnesium carbonate, cesium carbonate, titanium hydride, zirconium hydride or the like can be used.
- the high-temperature air release agent can be mixed into a uniform mixture (such as water, alcohol, acetone or isopropanol;) into the silicon tank, and then dried; The mixed liquid is added to the silicon micro-tank, and dried after each addition until the amount of the high-temperature release agent meets the requirements.
- a uniform mixture such as water, alcohol, acetone or isopropanol
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding may be carried out in a vacuum, and the vacuum bonding may be carried out in an atmosphere of less than 1 Pa, for example, a pressure of 0.5 Pa, 0.2 Pa, O. lPa, 0.05 Pa, O.OlPa, O.OOlPa, on the Pyrex 7740 glass.
- the shallow groove forms a sealed cavity, and the bonding surface should maintain a high degree of cleanness and minimal surface roughness before bonding to meet the requirements of conventional bonding, and perform conventional cleaning according to the process requirements of anodic bonding or other bonding. And polished, it can also be bonded directly in the air.
- the above bonded wafer is heated to 810 ° C to 890 ° C under an atmospheric pressure, and kept at this temperature for 3 to 5 minutes, for example, the temperature can be selected as 820 ° C, 830 ° C, 840 ° C, 845 ° C, 850 ° C, 855 ° C, 860 ° C, 870 ° C, 880 ° C, 890 ° C, 2 ⁇ 10 min, the time can be selected as: 3.2 min, 3.5 min, 3.8 min, 4 min , 4.2min, 4.4min, 4.8min, 8 minutes, 9 minutes, the high-temperature gas release agent in the cavity releases gas, causing a pressure difference between the inside and the outside, so that the softened glass forms a spherical glass microcavity and is cooled to normal temperature, such as 20- At 25 ° C, for example, 22 ° C, the above-mentioned wafer is annealed under normal pressure to eliminate stress.
- the temperature can be selected as 820
- the atmospheric pressure refers to an atmospheric pressure
- silicon is removed to obtain a spherical glass microcavity for MEMS wafer-level packaging.
- the method of removing silicon can be etched by TMAH (10%) at 80 degrees Celsius or etched with potassium hydroxide.
- the surface bonding process of the Si wafer and the Pyrex 7740 glass is anodic bonding, and the process conditions are: temperature 400 ° C, voltage: 600V.
- the heating temperature in the third step is 840 ° C ⁇ 850 ° C to obtain a better effect, because the glass viscosity in this range is moderate, which is favorable for molding.
- the thermal annealing process conditions in the third step are as follows: the annealing temperature ranges from 510 ° C to 560 ° C, and the annealing temperature can be selected from 520 V, 530 ° C, 540 ° C, 550 ° C, and the annealing time is 30min, then slowly air-cooled to normal temperature (such as 25 ° C) 0
- the silicon wafer and the p yrex 7740 glass wafer were cleaned and polished according to the anodic bonding process requirements.
- the high temperature gas releasing agent is preferably calcium carbonate. Titanium hydride is also preferred as the high temperature gas release agent.
- the micromachining process of the shallow groove on the Si wafer is a wet etching process.
- the Si wafer and Pyrex7740 glass surface bonding process is anodic bonding, the process conditions are: temperature 400 ° C, voltage: 600V.
- the depth of the shallow groove etched in the first step is preferably 50-100 micrometers, for example 75 micrometers, 85 micrometers, and 90 micrometers. At this depth, the high-temperature air release agent is easily placed without causing contamination by the contact glass.
- the obtained wafer-level spherical glass microcavity array is aligned with a silicon wafer with a MEMS device, and bonded by an anodic bonding process to package the MEMS device.
- the process conditions are: temperature 400 ° C, voltage: 600 V .
- a foam molding manufacturing method for a wafer-level glass microcavity includes the following steps:
- the microfluidic shallow groove pattern is etched on a Si wafer (such as a 4-inch wafer;) using a Si micromachining process.
- the silicon wafer used may be a standard thickness silicon wafer, such as a 500 micron thick silicon wafer.
- the shallow groove has a depth of 10 to 200 ⁇ m, for example, 15 ⁇ m, 30 ⁇ m, 40 ⁇ m, 60 ⁇ m, 95 ⁇ m, 132 ⁇ m, 150 ⁇ m, 180 ⁇ m, and the aspect ratio is usually less than 2, for example, 1.5, 1, 0.8, 0.5, 0.2, 0.1, 0.05, 0.02,
- the micro-machining process of the pattern structure on the Si wafer is a wet etching process, or a dry inductively coupled plasma (ICP) etching process, reactive ion etching
- ICP dry inductively coupled plasma
- One of the etches preferably a wet etching process (lower cost;), such as etching with a TMAH solution, the pattern may be strip or serpentine, adjusted as needed.
- an appropriate amount of high-temperature gas releasing agent is placed at both ends of the microchannel shallow groove or other positions, and the amount of the high-temperature gas releasing agent is based on the size of the micro-groove and the total volume of gas in the micro-channel after molding, according to the high-temperature release.
- the amount of gas released from the gas is calculated by the amount of the high-temperature gas-releasing agent.
- the amount of the high-temperature gas-releasing agent is: The amount of gas released by the high-temperature gas-releasing agent is greater than or equal to the total volume of gas in the micro-flow channel after molding, for example, The total volume of gas in the microchannel is 5 ml, then the amount of high-temperature gas releasing agent capable of releasing 5 ml of gas is required; the high-temperature releasing agent refers to the releasing agent whose outgassing temperature is higher than 500 ° C, and gas is released when heated, for example Calcium carbonate (a chemically pure (99% by mass) calcium carbonate having a small particle size), one of magnesium carbonate, strontium carbonate, titanium hydride, zirconium hydride, etc., and the high-temperature gas-releasing agent has a small mesh size. It is suitable for being placed in a silicon microgroove, for example, a mesh size of 400 mesh or more, such as 600 mesh, 800 mesh, and the like.
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding may be carried out in a vacuum, and the vacuum bonding may be carried out in an atmosphere of less than 1 Pa, for example, a pressure of 0.5 Pa, 0.2 Pa, O. lPa, 0.05 Pa, O.OlPa, O.OOlPa, on the Pyrex 7740 glass.
- the above bonded wafer is heated to 810 ° C to 890 ° C under an atmospheric pressure, and kept at this temperature for 5 to 10 minutes, for example, the temperature can be selected as 820 ° C, 830 ° C, 840 ° C, 845°C, 850°C, 855°C, 860°C, 870°C, 880°C, 890°C, 5 ⁇ 10min, the time can be selected as: 5.5min, 6.5min, 6.0min, 7.0 Min, 8.0min, 8.5min, 9.0min, the high-temperature air release agent emits gas due to heat, and generates a positive pressure to deform the molten glass corresponding to the sealed cavity to form a micro-flow path corresponding to the shallow
- the glass forms a glass microchannel with a hemispherical cross section, and is cooled to a normal temperature, such as 20-25 ° C, for example, 22 ° C, and the above-mentioned wafer is annealed under normal pressure to eliminate stress, which is an atmospheric pressure.
- the dicing machine can be used to remove both ends of the microchannel to form the inlet and outlet ends of the fluid and to remove the high temperature release agent.
- a high temperature gassing agent is typically placed at both ends of the microchannel to remove the high temperature gassing agent while forming the inlet and outlet ends. This method is simpler and less expensive.
- the high temperature release agent is calcium carbonate powder.
- the two ends of the micro flow channel are removed by a laser dicing method.
- the specific steps of the laser dicing method are as follows: First, the dicing groove is laser etched on the silicon wafer, and then the bonded wafer is bent to make the wafer The wafer is broken and pulled to form the inlet and outlet of the microchannel while removing the high temperature release agent residue.
- the micromachining process on the shallow grooves on the Si wafer is a wet etching process.
- the anodic bonding process conditions of the Si wafer and Pyrex 7740 glass are: temperature 400 ° C, voltage: 600V.
- the heating temperature in the fourth step is 840 ° C to 850 ° C, for example, 845 ° C can be selected.
- the microchannel obtained in the fourth step is subjected to thermal annealing under the following conditions: the annealing temperature ranges from 510 ° C to 560 ° C, the annealing time is 30 min, and then the air is slowly cooled to room temperature.
- the silicon wafer and the Pyrex 7740 glass wafer were cleaned and polished as necessary in accordance with the anodic bonding process.
- the depth of the shallow groove etched in the first step is 50-100 microns.
- the bonding of the silicon to the glass wafer is carried out in air.
- the obtained micro-channel system can be directly used, and the two ends of the obtained wafer-level micro-channel can be cut away to remove the residue of the high-temperature gas-releasing agent, and the high-temperature gas-releasing agent of the micro-channel system with both ends open can also be obtained.
- Titanium hydride can be preferably used.
- the micromachining process of the shallow grooves on the Si wafer is a wet etching process.
- the Si wafer and the Pyrex 7740 glass surface bonding process are anodic bonding, and the process conditions are: temperature 400 ° C, voltage: 600V.
- the depth of the microchannel shallow groove etched in the first step is preferably 50-100 micrometers, for example, 75 micrometers, 85 micrometers, and 90 micrometers. At this depth, the high-temperature air release agent is easily placed without causing contamination by contact glass. .
- a foam molding manufacturing method for a wafer-level glass microcavity includes the following steps:
- the microchannel shallow groove is etched on the 4-inch Si wafer by the Si micromachining process.
- the silicon wafer used may be a standard thickness silicon wafer having a thickness of 500 micrometers, and the shallow trench has a depth of 60 micrometers.
- Runner The groove is a strip groove with a diameter of 2 mm and the groove length is 3 cm.
- the micro-machining process of the pattern structure on the Si wafer is a wet etching process, and the etching solution used is a TMAH solution with a concentration of 10% and a temperature of 80 degrees Celsius. .
- a chemically pure calcium carbonate powder having a particle size of 5 ⁇ m and a mass of 30 ⁇ g was placed in a shallow tank.
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding at 0.5Pa allows the shallow groove on the Pyrex 7740 glass to form a sealed cavity.
- the bonding surface should maintain a high degree of cleanness and minimal surface roughness before bonding to meet the requirements of conventional bonding, according to the anode bond. Conventional or other bonding processes require conventional cleaning and polishing.
- the anodic bonding process conditions are: temperature 400 ° C, voltage: 600V.
- the bonded wafer is heated to 850 ° C under an atmospheric pressure, and is kept at the temperature for 10 minutes.
- the pressure difference between the inside and the outside of the chamber causes the softened glass to form a structure corresponding to the microcavity pattern structure, and is cooled to At a normal temperature of 25 ° C, a microchannel is obtained, and atmospheric pressure (atmospheric pressure;) is annealed to eliminate stress, which is an atmospheric pressure.
- the area where the high-temperature release agent is placed at both ends of the micro-channel is diced by a dicing machine to form an inlet and an outlet end of the fluid.
- the thermal annealing process conditions in the fourth step are as follows: Annealing temperature range is 510 ° C ⁇ 560 ° C, annealing temperature can be selected as 520 ° C, 530 ° C, 540 ° C, 550 ° C, annealing holding time It is 30 min, then slowly air-cooled to normal temperature (such as 25 ° C;).
- a foam molding manufacturing method for a wafer-level glass microcavity includes the following steps:
- the microchannel shallow groove is etched on the 4-inch Si wafer by the Si micromachining process.
- the silicon wafer used may be a standard thickness silicon wafer having a thickness of 500 micrometers, and the shallow trench has a depth of 60 micrometers.
- the micro-machining process of the pattern structure on the Si wafer is a wet etching process, and the etching solution used is a TMAH solution having a concentration of 10% and a temperature of 80. Celsius.
- a titanium hydride powder having a particle size of less than 5 ⁇ m and a mass of 12 ⁇ g was placed in a shallow tank.
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding at 0.5Pa allows the shallow groove on the Pyrex 7740 glass to form a sealed cavity.
- the bonding surface should maintain a high degree of cleanness and minimal surface roughness before bonding to meet the requirements of conventional bonding, according to the anode bond. Conventional or other bonding processes require conventional cleaning and polishing.
- the anodic bonding process conditions are: temperature 400 ° C, voltage: 600V.
- the bonded wafer is heated to 850 ° C under an atmospheric pressure, and is kept at the temperature for 10 minutes.
- the pressure difference between the inside and the outside of the chamber causes the softened glass to form a structure corresponding to the microcavity pattern structure, and is cooled to At a normal temperature of 25 ° C, a microchannel is obtained, and atmospheric pressure (atmospheric pressure;) is annealed to eliminate stress, which is an atmospheric pressure.
- the area where the high-temperature release agent is placed at both ends of the micro-channel is diced by a dicing machine to form an inlet and an outlet end of the fluid.
- the thermal annealing process conditions in the fourth step are as follows: annealing temperature ranges from 510 ° C to 560 ° C, annealing time is 30 min, and then slowly air-cooled to room temperature (such as 25 ° C;).
- the height of the obtained microchannel (the height of the inner wall of the top of the runner, that is, the distance from the inner wall to the bottom of the glass) was 0.9 mm.
- a foam molding manufacturing method for a wafer-level glass microcavity includes the following steps:
- the microchannel shallow groove is etched on the 4-inch Si wafer by the Si micromachining process.
- the silicon wafer used may be a standard thickness silicon wafer having a thickness of 500 micrometers, and the shallow trench has a depth of 100 micrometers.
- An elongated groove having a groove width of 1 mm and a groove length of 2 cm.
- the micro-machining process of the pattern structure on the Si wafer is a wet etching process, and the etching solution used is a TMAH solution having a concentration of 10% and a temperature of 80. Celsius.
- titanium hydride was placed in a shallow tank with a powder size of 5 ⁇ m and a mass of 25 ⁇ g.
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding under air makes the shallow groove on the Pyrex7740 glass form a sealed cavity.
- the bonding surface should maintain a high degree of cleanness and minimal surface roughness before bonding to meet the requirements of conventional bonding, according to anodic bonding. Or other bonding processes require conventional cleaning and polishing.
- the anodic bonding process conditions are: temperature 400 ° C, voltage: 600V.
- the bonded wafer is heated to 850 ° C under an atmospheric pressure, and is kept at the temperature for 4 minutes.
- the pressure difference between the inside and the outside of the chamber causes the softened glass to form a structure corresponding to the microcavity pattern structure, and is cooled to room temperature.
- the above wafer was annealed at 25 ° C under normal pressure (one atmosphere;) to eliminate stress, which is an atmospheric pressure to obtain a glass microchannel.
- the area of the high-flow gas release meter placed at both ends of the micro-flow channel is removed by a dicing machine to form an inlet and an outlet end of the fluid.
- the thermal annealing process conditions in the fourth step are as follows: annealing temperature ranges from 510 ° C to 560 ° C, annealing temperature is 550 ° C, annealing holding time is 30 min, and then slowly air-cooled to 25 ° C.
- a method for manufacturing a wafer-level glass microcavity for MEMS packaging comprising the steps of: In the first step, the shallow trench is etched on the 4 inch Si wafer by the Si micromachining process.
- the silicon wafer used may be a standard thickness silicon wafer having a thickness of 500 micrometers, the shallow trench has a depth of 100 micrometers, and the microgroove is caliber.
- the micromachining process of the pattern structure on the Si wafer is a wet etching process, and the etching solution used is a TMAH solution having a concentration of 10% and a temperature of 80 degrees Celsius.
- titanium hydride was placed in a shallow tank, and the powder had a particle size of 5 ⁇ m and a mass of 5 ⁇ g.
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding under air makes the shallow groove on the Pyrex7740 glass form a sealed cavity.
- the bonding surface should maintain a high degree of cleanness and minimal surface roughness before bonding to meet the requirements of conventional bonding, according to anodic bonding. Or other bonding processes require conventional cleaning and polishing.
- the anodic bonding process conditions are: temperature 400 ° C, voltage: 600V.
- the bonded wafer is heated to 850 ° C under an atmospheric pressure, and is kept at the temperature for 4 minutes.
- the pressure difference between the inside and the outside of the chamber causes the softened glass to form a structure corresponding to the microcavity pattern structure, and is cooled to room temperature.
- the above wafer was annealed at atmospheric pressure (atmospheric pressure;) at 25 ° C to eliminate stress, which is an atmospheric pressure.
- the thermal annealing process conditions in the fourth step are as follows: annealing temperature ranges from 510 ° C to 560 ° C, annealing temperature is 550 ° C, annealing holding time is 30 min, and then slowly air-cooled to 25 ° C.
- the obtained glass microcavity was etched with TMAH (mass concentration 10%, water bath 80 ° C;) to remove the silicon to obtain a wafer-level glass microcavity array.
- TMAH mass concentration 10%, water bath 80 ° C;
- the obtained wafer-level spherical glass microcavity array is aligned with a silicon wafer with a MEMS device, and bonded by an anodic bonding process to package the MEMS device.
- the process conditions are: temperature 400 ° C, voltage: 600 V .
- a method for manufacturing a wafer-level glass microcavity for MEMS packaging comprising the steps of:
- the groove is etched on a 4-inch Si wafer by a Si micromachining process.
- the groove is composed of 10 circular grooves having a radius of 0.8 mm and a flow path connecting the ten circular grooves.
- the silicon wafer used is a standard thickness.
- the silicon wafer has a thickness of 500 ⁇ m and the shallow groove has a depth of 100 ⁇ m.
- the micro-machining process of the pattern structure on the Si wafer is a wet etching process, and the etching solution used is a TMAH solution at a concentration of 10%. It is 80 degrees Celsius.
- titanium hydride is placed in a circular groove, the powder has a particle size of 5 ⁇ m and the mass is 50 ⁇ g.
- Addition method Mix 1 mg of the powder in 4 ml of acetone and mix well, take 0.2 ml: Add 0.02 ⁇ l to the silicon tank. After the acetone is dried, add a second drop until 0.2 ml is added to the silicon tank. Medium.
- the above Si wafer and Pyrex 7740 glass wafer (a brand of borosilicate glass, manufactured by Corning-Coming, USA, commercially available, usually polished, the same size as the Si wafer)
- the anodic bonding under air makes the shallow groove on the Pyrex7740 glass form a sealed cavity.
- the bonding surface should maintain a high degree of cleanness and minimal surface roughness before bonding to meet the requirements of conventional bonding, according to anodic bonding. Or other bonding processes require conventional cleaning and polishing.
- the anodic bonding process conditions are: temperature 400 ° C, voltage: 600V.
- the bonded wafer is heated to 850 ° C under an atmospheric pressure, and is kept at the temperature for 4 minutes.
- the pressure difference between the inside and the outside of the chamber causes the softened glass to form a structure corresponding to the microcavity pattern structure, and is cooled to room temperature.
- the above wafer was annealed at atmospheric pressure (atmospheric pressure;) at 25 ° C to eliminate stress, which is an atmospheric pressure.
- the thermal annealing process conditions in the fourth step are as follows: annealing temperature ranges from 510 ° C to 560 ° C, annealing temperature is 550 ° C, annealing holding time is 30 min, and then slowly air-cooled to 25 ° C. A spherical glass microcavity structure connected by a glass microchannel is obtained.
- the obtained glass microcavity was etched with TMAH (mass concentration 10%, water bath 80 ° C;) to remove the silicon to obtain a wafer-level glass microcavity array.
- TMAH mass concentration 10%, water bath 80 ° C;
- the obtained wafer-level spherical glass microcavity array is aligned with a silicon wafer with a MEMS device, and bonded by an anodic bonding process to package the MEMS device.
- the process conditions are: temperature 400 ° C, voltage: 600 V .
- the invention adopts the MEMS processing and manufacturing technology: the anodic bonding process of the Si piece and the Pyrex 7740 glass, and then the heat treatment to produce the wafer-level Pyrex 7740 glass microcavity with the original polished surface roughness, and the process is simple and reliable.
- the glass microcavity obtained by the present invention can be packaged by other means such as bonding.
- the use of the present invention results in a wafer-level glass microcavity array glass wafer that can be bonded to a wafer with a wafer level MEMS device array to provide a wafer level packaged MEMS device.
- the invention can reserve the dicing groove on the above-mentioned wafer at the same time.
- each pattern can be diced along the dicing groove to obtain a plurality of different glass microcavities, thereby realizing the wafer-level fabrication of the microcavity. Reduce the cost of the process.
- Fig. 6 and Fig. 7 according to the thermal decomposition reaction kinetics of titanium hydride (the article published by the applicant on the decomposition kinetics of titanium hydride;), it is possible to calculate the forming height under the given conditions of other geometric and temperature conditions. The relationship between the quality of titanium hydride and thus the precise control of the size of the glass microcavity.
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Description
圆片级玻璃微腔的发泡成型制造方法
技术领域
本发明涉及一种微系统制造技术, 尤其涉及一种圆片级玻璃微腔的发泡成型 制造方法。
背景技术
Pyrex7740玻璃 (一种含有碱性离子的玻璃, Pyrex是 Coming公司的产品品 牌)是一种重要的材料, 它有着和 Si材料相近的热膨胀系数, 有着高透光率和较 高的强度, 并且可以通过使用阳极键合工艺与 Si衬底形成高强度的键合连接,在 键合表面产生了牢固的 Si-O共价键, 其强度甚至高于 Si材料本身。 由于这样的 特性, 使得 Pyrex7740玻璃广泛应用于 MEMS封装、 微流体和 MOEMS (微光学 机电系统) 等领域。 当前, 玻璃微腔和微流道系统主要应用于传感器和生物芯片 领域。 微流道的制备目前常用的手段是在硅, 玻璃, PDMS (聚二甲基硅氧烷) 上直接刻蚀出微流道和各种流体部件的图案结构, 然后于另一平面键合材料形成 MEMS微流体系统。 传统刻蚀形成的微流道系统, 微流道表面粗糙, 增加流体流 动阻力, 表面抛光技术还很难做到对 3D微流道系统的高效抛光。
微流道玻璃热成型可采用负压成型和正压成型。 负压成型(中国专利 200710190226.2): 在硅上刻蚀流道等图形, 将硅与玻璃在真空中阳极键合, 然后 在空气中加热至高温利用腔内外的负压热成型。 这种方法只能带有真空的键合设 备, 因而成本较高; 此外, 该方法采用负压成型, 因而形成的微流道位于玻璃圆 片的背面, 因而在玻璃圆片较厚时, 背面形成的微流道形状不可控, 且流道较浅; 对于形成较高的玻璃微流道时, 通常需要使用加厚的硅片, 而且需要刻蚀深的硅 腔 (有的甚至需要到 900微米, Glass Blowing on a Wafer Level, JOURNAL OF MICROELECTROMECHANICAL SYSTEMS, VOL. 16, NO. 2, APRIL 2007)和高 的深宽比以提供足够的气体, 使得玻璃气泡充分形成, 具有较高的高度, 以形成 较高的弧形; 有时甚至需要在另外一个硅圆片上刻蚀较大的孔, 再与带有通孔的 硅片键合, 从而提供足够的气体以成型高度较高, 弧形度较好的玻璃微流道, 通 常成本较高; 该方法的缺点还在于: 若用于形成复杂的微流体体系, 需要大面积 的湿法刻蚀, 成本较高, 而且在成型不同尺寸流道和腔的时, 由于难以在硅片上 用干法刻蚀不同深度的腔, 因此成型玻璃复杂结构面临着气源不足的问题。
发明内容
本发明的目的是提供一种成本低廉、 微腔高度高、 弧形度好的圆片级玻璃微
腔的发泡成型制造方法。
一种圆片级玻璃微腔的发泡成型制造方法, 包括以下步骤:
第一步, 利用 Si微加工工艺在 Si圆片上刻蚀硅槽,
第二步, 在硅槽内放置适量的高温释气剂,
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片进行阳极键合, 使上述硅槽形 成密封腔体,
第四步,将上述键合好的圆片在空气中加热至 810°C〜1000°C,保温 5〜10min, 高温释气剂因受热放出气体, 产生正压力使得密封腔体对应的熔融玻璃变形而在 玻璃上形成与硅槽对应的结构, 冷却, 获得圆片级玻璃微流道。
上述技术方案中, 硅槽为特定的硅微流道图案或者相互独立的槽的阵列。 其 特征在于高温释气剂为碳酸钙粉末或氢化钛粉末。 第一步刻蚀的硅槽的深度为 10-300微米。 将上述微流道的两端利用激光划片方法去除, 激光划片方法的具体 步骤为: 首先在硅片上用激光刻蚀划片槽, 然后再弯曲键合后的圆片使圆片因硅 片受拉而断裂, 去除高温释气剂残留物。所述 Si圆片上浅槽的微加工工艺为湿法 腐蚀工艺。 所述 Si圆片与 Pyrex7740玻璃的阳极键合工艺条件为: 温度 400°C, 电压: 600V。 第四步中的加热温度为 840°C〜850°C。 将第四步所得到的微流道进 行热退火,工艺条件为:退火温度范围在 510°C〜560°C中,退火保温时间为 30min, 然后缓慢风冷至常温。 第三步中硅与玻璃圆片的键合是在空气中进行的。
本发明获得如下效果:
1. 本发明基于传统 MEMS加工工艺, 首先在 Si片上加工的硅槽结构, 在浅槽中 填充高温释气剂, 再用阳极键合工艺将 Pyrex7740玻璃覆盖到该浅槽上形成密闭 微腔,然后加热使得玻璃融化, 高温释气剂释放出气体从而使得圆形或者方形 (平 面图形;)具有球形结构, 而使得长方形的硅槽形成狭长的流道结构。玻璃成半球圆 弧管状, 形成玻璃微流道。 采用高温释气剂释提供气源用于成型玻璃微流道, 具 有成本低, 方法简单, 成型高度高 (若加入足量的高温释气剂, 对于球形腔, 可 以为大于半球的腔; 对于微流道, 其截面可以是大于半圆), 球形度好的特点; 热成型形成的玻璃微腔内壁、 外壁光滑度较高, 内壁粗糙度可以达到 lnm以下, 外壁粗糙度可小于 10个纳米, 因此在用于微流道具有较低的流阻; 同时具有高 的透光性。 现有技术刻蚀深宽比较大的深腔需要采用干法工艺, 通常需要几十个 小时, 工艺成本也较高。 本发明仅需要采用成本低廉的湿法刻蚀工艺在硅片上刻 蚀浅的硅槽, 在硅槽的局部填充高温释气剂, 方法简单, 具有低成本的优点。
2. 本发明高温成型过后, 可通过划片工艺可以将污染的区域去除, 同时有起到了 开启流体进出端口的效果。 本发明仅需要在局部放置高温释气剂, 产生的气体可 用于整个微流道的成型, 可以避免残留物对 MEMS 微流道的污染。 通常阳极键 合的温度为 400摄氏度, 因而其标准温度为 673K, 成型温度为 850摄氏度左右, 标准温度为 1123K左右, 根据 PV=nRT, 根据现有技术, 如果气体的量不变, 膨 胀后的体积不足原来的两倍, 由此可见需要刻蚀较深的槽。
3. 本发明采用湿法工艺在硅上刻蚀硅槽, 其成本更低。现有技术需要刻蚀深宽比 较高的较深的硅腔以提供足够的气体。 湿法腐蚀工艺难以获得较大的深宽比。 在 刻蚀较深的微腔时, 其成本较高, 耗时较长。 但是湿法工艺成本较低, 工艺比较 成熟,在刻蚀浅槽方面具有低成本、高效率的优势。本发明不需要较大的深宽比, 也不需要大的深度, 采用湿法工艺即可降低成本、 提高效率。
4. 本发明高温释气剂选用碳酸钙粉末, 一方面, 碳酸钙粉末的大量分解温度在 800摄氏度以上, 与玻璃的熔化温度具有较好的匹配性, 在低于 800摄氏度时, 碳酸钙仅有少量分解, 因此玻璃未成型前密封的玻璃腔不会因为气体压力过大而 破裂。 高于 800摄氏度以后, 碳酸钙粉末大量分解出二氧化碳气体, 从而使得玻 璃成型。 本发明仅需要根据碳酸钙的分解量进行简单计算, 就可以知道成型特定 体积的玻璃微腔所需要的碳酸钙的量。 根据反应速率平衡公式的修正公式:
可以较为准确的控制内部压强, 从而可以调控玻璃微流道内部横截面的大小, 根 据不同的流速需要自行调控选择, 因而该方法简单, 可靠, 适用范围广。
5. 本发明高温释气剂选用氢化钛粉末, 很少量的氢化钛粉末可以释放出大量气 体, 因此使用氢化钛粉末可以使得放置粉末的体积更小, 降低技术难度。
6. 由于成型单个玻璃微腔所需要的氢化钛等粉末只有几十微克甚至几微克,因此 称量比较困难。 本发明将少量粉末混合于较大体积的水、 丙酮等液体中形成均匀 混合液, 然后再量取特定的体积, 放置于流道中, 从而达到精确控制粉末体积的 目的, 从而有利于玻璃微腔体积的精确控制。
7. 阳极键合具有键合强度高, 密闭性好的特点, 本发明采用阳极键合形成密闭空 腔, 键合区域形成 Si-O 键, 在高温时该化学键仍然具有较高的强度, 因而不会 在加热过程中不易发生泄漏而导致成型失败。 在温度 400°C, 电压直流 600V的 键合条件下, 阳极键合能够达到更好的密封效果。 采用的第四步中的退火工艺可 以有效的消除 Pyrex7740玻璃承受高温正压成型过程中形成的应力, 从而使其强
度靭性更高。 在该条件下退火, 既能有效退去应力, 还能够使得微流道腔的形状 基本无改变。
8. 本发明制备与 Si的热膨胀系数相当的 Pyrex7740玻璃作为玻璃微流道结构, 在制备微腔时不容易使键合好的圆片因热失配产生损坏。
附图说明
图 1 为本发明刻蚀有微流道浅槽的键合圆片横向截面示意图。
图 2 为本发明玻璃微流道热成型后横向截面示意图。
图 3 为本发明玻璃微流道热成型后纵向截面示意图。
图 4 为本发明圆片级玻璃微流道俯视图。
图 5 为本发明圆片级玻璃微腔剖视示意图。
图 6 为本发明不同的开口半宽度 (硅槽宽度的一半;)下氢化钛质量与玻璃微流 道高度关系 (流道长度 3 cm,发泡温度 1123K, 硅刻蚀深度 0.06mm)。
图 7 为本发明不同的开口半径 (硅槽开口为圆型;)下氢化钛质量与玻璃微流道 高度关系 (;发泡温度 1123K, 硅刻蚀深度 0.06mm;)。
图 8 为本发明得到的由玻璃微流道连接的球形玻璃微腔结构示意图 (实施例
7)。
具体实施方式
实施例 1
一种圆片级玻璃微腔的发泡成型制造方法, 包括以下步骤:
第一步,利用 Si微加工工艺在 Si圆片 (譬如 4英寸圆片)上刻蚀硅槽,所用硅 片可以是标准厚度的硅片, 也可以是较薄 (如 300微米)或较厚的硅片 (600微米), 譬如 500微米厚的硅片, 所述硅槽的深度为 10-500微米, 例如为 15微米, 30微 米, 40微米, 60微米, 95微米, 132微米, 150微米, 180微米, 250微米, 400 微米, 450微米, 优选 10-100微米, 刻蚀的深宽比任意, 例如可以选取为 1.5, 1, 0.8, 0.5, 0.2, 0.1, 0.05, 0.02, 所述 Si圆片上图案结构的微加工工艺为湿法腐 蚀工艺、 或者干法感应耦合等离子体 (ICP)刻蚀工艺、 反应离子刻蚀中的一种, 优 选低成本的湿法腐蚀工艺, 例如用 TMAH溶液腐蚀, 该图案可以是方形或圆形 槽阵列 (用于封装 MEMS器件阵列;), 槽之间互相独立, 不连通; 也可以是具有一 定尺寸的硅流道; 或者是由硅流道连接的方形槽或圆形槽, 方形槽或圆形槽与硅 流道的宽度尺寸可以不相等, 多个方形槽或圆形槽的尺寸也可以不相等。
第二步, 在硅槽中放置适量的高温释气剂, 高温释气剂的用量根据微槽的尺
寸计算其体积, 再计算预计玻璃微腔的体积, 再根据高温释气剂的释气量计算高 温释气剂的用量, 高温释气剂是指释气温度高于 500摄氏度的释气剂, 受热时放 出气体, 例如碳酸钙 (可以用粒度较小的化学纯 (质量百分比浓度为 99%)碳酸钙)、 碳酸镁、 碳酸锶、 氢化钛、 氢化锆等中的一种。 由于所取高温释气剂量较少, 为 微克, 因此可将高温释气剂配成均匀混合液 (如水、 酒精、 丙酮或异丙醇等;)体加 入硅槽中, 再干燥; 可以分多次将混合液体加入硅微槽, 每次加完后干燥, 直至 高温释气剂的量符合要求。
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 空气或者真空中进行阳极键合, 真空键合可以在小于 lPa的气氛下进行键合, 譬 如压力为 0.5Pa, 0.2Pa, O. lPa, 0.05Pa, O.OlPa, O.OOlPa, 使 Pyrex7740玻璃上 的上述浅槽形成密封腔体, 键合表面在键合前应该保持高度清洁和极小的表面粗 糙度, 以满足常规键合的要求, 按照阳极键合或其他键合的工艺要求进行常规清 洗和抛光, 也可以直接在空气中键合。
第四步, 将上述键合好的圆片在一个大气压下加热至 810°C〜890°C, 在该温 度下保温 3〜5min, 例如温度可以选取为 820°C, 830°C, 840°C, 845°C, 850°C, 855°C, 860°C, 870 °C , 880 °C , 890°C, 保温 2~10min, 时间可以选取为: 3.2min, 3.5min, 3.8min, 4min, 4.2min, 4.4min, 4.8min, 8分钟, 9分钟, 腔内高温释 气剂释放出气体, 使得内外产生压力差而使软化后的玻璃形成球形玻璃微腔, 冷 却到常温, 如 20-25°C, 譬如为 22°C, 将上述圆片在常压下退火消除应力, 该常 压是指一个大气压, 去除硅, 得到 MEMS 圆片级封装用球形玻璃微腔。 去除硅 的方法可用 TMAH (10%)在 80摄氏度下腐蚀去除硅, 也可以用氢氧化钾进行腐 蚀。
上述技术方案中,所述的 Si圆片与 Pyrex7740玻璃表面键合工艺为阳极键合, 工艺条件为: 温度 400°C, 电压: 600V。 第三步中的加热温度为 840°C〜850°C可 获得更好的效果, 因为在这个范围内玻璃黏度适中, 有利于成型。 第三步中所述 热退火的工艺条件为:退火温度范围在 510°C〜560°C中,退火温度可以选取为 520 V, 530°C, 540°C, 550°C, 退火保温时间为 30min, 然后缓慢风冷至常温 (;譬如 25°C)0第二步中硅圆片与 pyrex7740玻璃圆片按照阳极键合的工艺要求进行必要 的清洗和抛光。 上述技术方案中, 高温释气剂优选为碳酸钙。 高温释气剂也可优 选氢化钛。 所述 Si圆片上浅槽的微加工工艺为湿法腐蚀工艺。 所述的 Si圆片与
Pyrex7740玻璃表面键合工艺为阳极键合,工艺条件为:温度 400°C, 电压: 600V。 第一步刻蚀的浅槽的深度优选为 50-100微米, 例如 75微米, 85微米, 90微米, 在这个深度下, 高温释气剂容易放置, 又不至于因接触玻璃产生污染。 将所得到 的圆片级的球形玻璃微腔阵列与带有 MEMS 器件的硅圆片对准, 用阳极键合工 艺进行键合, 封装 MEMS器件, 工艺条件为: 温度 400°C, 电压: 600V。
实施例 2
一种圆片级玻璃微腔的发泡成型制造方法, 包括以下步骤:
第一步,利用 Si微加工工艺在 Si圆片 (;譬如 4英寸圆片;)上刻蚀微流道浅槽图 案, 所用硅片可以是标准厚度的硅片, 譬如 500微米厚的硅片, 所述浅槽的深度 为 10-200微米, 例如为 15微米, 30微米, 40微米, 60微米, 95微米, 132微 米, 150微米, 180微米, 深宽比通常小于 2, 例如可以选取为 1.5, 1, 0.8, 0.5, 0.2, 0.1, 0.05, 0.02, 所述 Si圆片上图案结构的微加工工艺为湿法腐蚀工艺、 或 者干法感应耦合等离子体 (ICP)刻蚀工艺、 反应离子刻蚀中的一种, 优选湿法腐蚀 工艺 (;成本较低;), 如用 TMAH溶液腐蚀, 该图案可以是条形或蛇形, 根据需要调 节。
第二步, 在微流道浅槽两端或其它位置中放置适量的高温释气剂, 高温释气 剂的用量根据微槽的尺寸和预计成型后微流道中气体体积总量, 根据高温释气剂 的释气量计算高温释气剂的用量, 所述的高温释气剂的用量的需求为: 高温释气 剂所放出的气体量大于等于预计成型后微流道中气体体积总量, 例如, 微流道中 气体总体积为 5毫升, 那么需要能够释放出 5毫升气体的高温释气剂的用量; 高 温释气剂是指释气温度高于 500摄氏度的释气剂, 受热时放出气体, 例如碳酸钙 (可以用粒度较小的化学纯 (质量百分比浓度为 99%)碳酸钙)、 碳酸镁、 碳酸锶、 氢化钛、氢化锆等中的一种, 高温释气剂的目数较小,适合放入硅微槽,例如 400 目以上的粒度, 如 600目, 800目等。
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 空气或者真空中进行阳极键合, 真空键合可以在小于 lPa的气氛下进行键合, 譬 如压力为 0.5Pa, 0.2Pa, O. lPa, 0.05Pa, O.OlPa, O.OOlPa, 使 Pyrex7740玻璃上 的上述浅槽形成密封腔体, 键合表面在键合前应该保持高度清洁和极小的表面粗 糙度, 以满足常规键合的要求, 按照阳极键合或其他键合的工艺要求进行常规清 洗和抛光。
第四步, 将上述键合好的圆片在一个大气压下加热至 810°C〜890°C, 在该温 度下保温 5〜10min, 例如温度可以选取为 820°C, 830°C, 840°C, 845°C, 850°C, 855°C, 860°C, 870°C, 880°C, 890°C, 保温 5~10min, 时间可以选取为: 5.5min, 6.5 min, 6.0min, 7.0min, 8.0min, 8.5 min, 9.0min, 高温释气剂因受热放出气体, 产生正压力使得密封腔体对应的熔融玻璃变形而在玻璃上形成与硅微流道浅槽 图案对应的微流道图案, 玻璃形成半球形截面的玻璃微流道, 冷却到常温, 如 20-25°C, 譬如为 22°C, 将上述圆片在常压下退火消除应力, 该常压是指一个大 气压。
最后还可利用划片机将微流道两端划去, 形成流体的入口和出口端, 并除去 高温释气剂。 通常将高温释气剂放置在微流道的两端, 在形成入口与出口端的同 时除去高温释气剂。 这种方法比较简单, 成本更低。
上述技术方案中, 高温释气剂为碳酸钙粉末。 将上述微流道的两端利用激光 划片方法去除, 激光划片方法的具体步骤为: 首先在硅片上用激光刻蚀划片槽, 然后再弯曲键合后的圆片使圆片因硅片受拉而断裂, 从而形成微流道的入口和出 口, 同时去除高温释气剂残留物。所述 Si圆片上浅槽的微加工工艺为湿法腐蚀工 艺。所述的 Si圆片与 Pyrex7740玻璃的阳极键合工艺条件为:温度 400°C, 电压: 600V。 第四步中的加热温度为 840°C〜850°C, 例如可以选取为 845 °C。 将第四步 所得到的微流道进行热退火, 工艺条件为: 退火温度范围在 510°C〜560°C中, 退 火保温时间为 30min, 然后缓慢风冷至常温。 第二步中硅圆片与 Pyrex7740玻璃 圆片按照阳极键合的工艺要求进行必要的清洗和抛光。 第一步刻蚀的浅槽的深度 为 50-100微米。第三步中硅与玻璃圆片的键合是在空气中进行的。得到的微流道 系统可直接使用, 也可将得到的圆片级微流道的两端划开, 去除高温释气剂的残 留物,得到两端开口的微流道系统高温释气剂也可优选为氢化钛。所述 Si圆片上 浅槽的微加工工艺为湿法腐蚀工艺。所述的 Si圆片与 Pyrex7740玻璃表面键合工 艺为阳极键合, 工艺条件为: 温度 400°C, 电压: 600V。 第一步刻蚀的微流道浅 槽的深度优选为 50-100微米, 例如 75微米, 85微米, 90微米, 在这个深度下, 高温释气剂容易放置, 又不至于因接触玻璃产生污染。
实施例 3
一种圆片级玻璃微腔的发泡成型制造方法, 包括以下步骤:
第一步, 利用 Si微加工工艺在 4英寸 Si圆片上刻蚀微流道浅槽, 所用硅片 可以是标准厚度的硅片, 厚度为 500微米, 所述浅槽的深度为 60微米, 微流道
槽为口径为 2毫米的条形槽,槽长 3厘米,所述 Si圆片上图案结构的微加工工艺 为湿法腐蚀工艺,所用的腐蚀液为 TMAH溶液,浓度为 10%,温度为 80摄氏度。
第二步, 在浅槽中放置化学纯碳酸钙粉末, 粉末粒径 5微米, 质量为 30微 克。
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 在 0.5Pa下阳极键合, 使 Pyrex7740玻璃上的上述浅槽形成密封腔体, 键合表面 在键合前应该保持高度清洁和极小的表面粗糙度, 以满足常规键合的要求, 按照 阳极键合或其他键合的工艺要求进行常规清洗和抛光, 所述的阳极键合工艺条件 为: 温度 400°C, 电压: 600V。
第四步, 将上述键合好的圆片在一个大气压下加热至 850°C, 在该温度下保 温 10min, 腔内外压力差使软化后的玻璃形成与上述微腔图案结构相应的结构, 冷却到常温 25°C, 得到微流道, 常压 (一个大气压;)下退火消除应力, 该常压是指 一个大气压。
第五步, 利用划片机将微流道两端放置高温释气剂的区域划去, 形成流体的 入口和出口端。 第四步中所述热退火的工艺条件为: 退火温度范围在 510°C〜560 °C中,退火温度可以选取为 520°C, 530°C, 540°C, 550°C,退火保温时间为 30min, 然后缓慢风冷至常温 (;譬如 25°C;)。
实施例 4
一种圆片级玻璃微腔的发泡成型制造方法, 包括以下步骤:
第一步, 利用 Si微加工工艺在 4英寸 Si圆片上刻蚀微流道浅槽, 所用硅片 可以是标准厚度的硅片, 厚度为 500微米, 所述浅槽的深度为 60微米, 微流道 槽宽度为 0.3mm的条形槽, 槽长 3厘米, 所述 Si圆片上图案结构的微加工工艺 为湿法腐蚀工艺,所用的腐蚀液为 TMAH溶液,浓度为 10%,温度为 80摄氏度。
第二步, 在浅槽中放置氢化钛粉末, 粉末粒径小于 5微米, 质量为 12微克。 第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 在 0.5Pa下阳极键合, 使 Pyrex7740玻璃上的上述浅槽形成密封腔体, 键合表面 在键合前应该保持高度清洁和极小的表面粗糙度, 以满足常规键合的要求, 按照 阳极键合或其他键合的工艺要求进行常规清洗和抛光, 所述的阳极键合工艺条件 为: 温度 400°C, 电压: 600V。
第四步, 将上述键合好的圆片在一个大气压下加热至 850°C, 在该温度下保 温 10min, 腔内外压力差使软化后的玻璃形成与上述微腔图案结构相应的结构, 冷却到常温 25°C, 得到微流道, 常压 (一个大气压;)下退火消除应力, 该常压是指 一个大气压。
第五步, 利用划片机将微流道两端放置高温释气剂的区域划去, 形成流体的 入口和出口端。 第四步中所述热退火的工艺条件为: 退火温度范围在 510°C〜560 °C中, 退火保温时间为 30min, 然后缓慢风冷至常温 (;譬如 25°C;)。 得到的微流道 的高度 (流道顶部内壁的高度, 即内壁到玻璃底面之间的距离;)为 0.9毫米。
实施例 5
一种圆片级玻璃微腔的发泡成型制造方法, 包括以下步骤:
第一步, 利用 Si微加工工艺在 4英寸 Si圆片上刻蚀微流道浅槽, 所用硅片 可以是标准厚度的硅片, 厚度为 500微米, 所述浅槽的深度为 100微米, 微槽宽 度为为 1毫米的长条形槽,槽长 2厘米,所述 Si圆片上图案结构的微加工工艺为 湿法腐蚀工艺, 所用的腐蚀液为 TMAH溶液, 浓度为 10%, 温度为 80摄氏度。
第二步, 在浅槽中放置氢化钛, 粉末粒径 5微米, 质量为 25微克。
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 在空气下阳极键合, 使 Pyrex7740玻璃上的上述浅槽形成密封腔体, 键合表面在 键合前应该保持高度清洁和极小的表面粗糙度, 以满足常规键合的要求, 按照阳 极键合或其他键合的工艺要求进行常规清洗和抛光, 所述的阳极键合工艺条件 为: 温度 400°C, 电压: 600V。
第四步, 将上述键合好的圆片在一个大气压下加热至 850°C, 在该温度下保 温 4min,腔内外压力差使软化后的玻璃形成与上述微腔图案结构相应结构,冷却 到常温 25°C, 将上述圆片在常压 (一个大气压;)下退火消除应力, 该常压是指一个 大气压, 得到玻璃微流道。
第五步, 利用划片机将微流道两端放置高温释气计的区域划去, 形成流体的 入口和出口端。
第四步中所述热退火的工艺条件为: 退火温度范围在 510°C〜560°C中, 退火 温度为 550°C, 退火保温时间为 30min, 然后缓慢风冷至 25°C。
实施例 6
一种 MEMS封装用圆片级玻璃微腔的制造方法, 包括以下步骤:
第一步, 利用 Si微加工工艺在 4英寸 Si圆片上刻蚀浅槽, 所用硅片可以是 标准厚度的硅片, 厚度为 500微米, 所述浅槽的深度为 100微米, 微槽为口径为 1毫米的圆形槽, 所述 Si圆片上图案结构的微加工工艺为湿法腐蚀工艺, 所用的 腐蚀液为 TMAH溶液, 浓度为 10%, 温度为 80摄氏度。
第二步, 在浅槽中放置氢化钛, 粉末粒径 5微米, 质量为 5微克。
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 在空气下阳极键合, 使 Pyrex7740玻璃上的上述浅槽形成密封腔体, 键合表面在 键合前应该保持高度清洁和极小的表面粗糙度, 以满足常规键合的要求, 按照阳 极键合或其他键合的工艺要求进行常规清洗和抛光, 所述的阳极键合工艺条件 为: 温度 400°C, 电压: 600V。
第四步, 将上述键合好的圆片在一个大气压下加热至 850°C, 在该温度下保 温 4min,腔内外压力差使软化后的玻璃形成与上述微腔图案结构相应结构,冷却 到常温 25°C, 将上述圆片在常压 (一个大气压;)下退火消除应力, 该常压是指一个 大气压。
第四步中所述热退火的工艺条件为: 退火温度范围在 510°C〜560°C中, 退火 温度为 550°C, 退火保温时间为 30min, 然后缓慢风冷至 25°C。
将得到的玻璃微腔用 TMAH (;质量浓度 10%, 水浴 80摄氏度;)腐蚀可去掉硅, 得到圆片级玻璃微腔阵列。将所得到的圆片级的球形玻璃微腔阵列与带有 MEMS 器件的硅圆片对准, 用阳极键合工艺进行键合, 封装 MEMS器件, 工艺条件为: 温度 400°C, 电压: 600V。
实施例 7
一种 MEMS封装用圆片级玻璃微腔的制造方法, 包括以下步骤:
第一步, 利用 Si微加工工艺在 4英寸 Si圆片上刻蚀槽, 槽由半径为 0.8毫 米的 10个圆形槽以及连接这十个圆形槽的流道组成, 所用硅片是标准厚度的硅 片, 厚度为 500微米, 所述浅槽的深度为 100微米, 所述 Si圆片上图案结构的微 加工工艺为湿法腐蚀工艺, 所用的腐蚀液为 TMAH溶液, 浓度为 10%, 温度为 80摄氏度。
第二步, 在圆形槽中放置氢化钛, 粉末粒径 5微米, 质量为 50微克, 加入 方法: 将 1毫克的粉末混匀在 4毫升的丙酮中搅拌均匀, 取 0.2毫升: 每次向硅 槽中加入 0.02微升, 待丙酮干燥后, 再滴加第二滴, 直至 0.2毫升全部加入硅槽
中。
第三步, 将上述 Si圆片与 Pyrex7740玻璃圆片 (;一种硼硅玻璃的品牌, 美国 康宁 -coming公司生产, 市场可购得, 通常已经经过抛光, 其尺寸与 Si圆片相同) 在空气下阳极键合, 使 Pyrex7740玻璃上的上述浅槽形成密封腔体, 键合表面在 键合前应该保持高度清洁和极小的表面粗糙度, 以满足常规键合的要求, 按照阳 极键合或其他键合的工艺要求进行常规清洗和抛光, 所述的阳极键合工艺条件 为: 温度 400°C, 电压: 600V。
第四步, 将上述键合好的圆片在一个大气压下加热至 850°C, 在该温度下保 温 4min,腔内外压力差使软化后的玻璃形成与上述微腔图案结构相应结构,冷却 到常温 25°C, 将上述圆片在常压 (一个大气压;)下退火消除应力, 该常压是指一个 大气压。
第四步中所述热退火的工艺条件为: 退火温度范围在 510°C〜560°C中, 退火 温度为 550°C, 退火保温时间为 30min, 然后缓慢风冷至 25°C。 得到由玻璃微流 道连接的球形玻璃微腔结构。
将得到的玻璃微腔用 TMAH (;质量浓度 10%, 水浴 80摄氏度;)腐蚀可去掉硅, 得到圆片级玻璃微腔阵列。将所得到的圆片级的球形玻璃微腔阵列与带有 MEMS 器件的硅圆片对准, 用阳极键合工艺进行键合, 封装 MEMS器件, 工艺条件为: 温度 400°C, 电压: 600V。
本发明通过 MEMS加工制造技术: Si片与 Pyrex7740玻璃的阳极键合工艺, 再利用热处理制造出具有原始抛光表面粗糙度的圆片级 Pyrex7740玻璃微腔, 工 艺简单、 可靠。 本发明获得的玻璃微腔可通过键合等方式对其它器件进行封装。 利用本发明获得带有的圆片级的玻璃微腔阵列玻璃圆片, 可与带有圆片级的 MEMS器件阵列的硅片进行键合, 从而得到圆片级封装的 MEMS器件。 本发明 可以在同时在上述圆片上预留划片槽, 在加工形成后, 可以沿划片槽将各图形划 片, 获得多个不同的玻璃微腔, 从而实现微腔的圆片级制作, 降低该工艺的成本。 如附图 6和附图 7, 根据氢化钛热分解反应动力学 (申请者已经发表的关于氢化钛 分解动力学的文章;),可以计算在其他几何与温度条件给定情况下,成型高度与氢 化钛质量的关系, 从而用于玻璃微腔尺寸的精确控制。
Claims
1. 一种圆片级玻璃微腔的发泡成型制造方法, 其特征在于, 包括以下步 骤:
第一步, 利用 Si微加工工艺在 Si圆片 (1)上刻蚀硅槽,
第二步, 在硅槽内放置适量的高温释气剂 (3 ),
第三步, 将上述 Si圆片 (1 ) 与 Pyrex7740玻璃圆片 (2) 在空气或者特 定的真空中进行阳极键合, 使上述硅槽形成密封腔体 (4),
第四步, 将上述键合好的圆片在空气中加热至 810 °C〜1000 °C, 保温 2〜10min, 高温释气剂因受热放出气体, 产生正压力使得密封腔体 (4) 对应 的熔融玻璃变形而在玻璃上形成与硅槽对应的结构, 冷却, 获得圆片级玻璃 微腔 (5 )。
2. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于, 硅槽为特定的硅微流道图案或者相互独立的槽的阵列或者由微流道连 接的较大开口尺寸的槽。
3. 根据权利要求 1或 2所述的圆片级玻璃微腔的发泡成型制造方法, 其 特征在于高温释气剂为碳酸钙粉末或氢化钛粉末。
4. 根据权利要求 3所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于第一步刻蚀的硅槽的深度为 10-300微米。
5. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于将上述微流道的两端利用激光划片方法去除, 激光划片方法的具体步骤 为: 首先在硅片上用激光刻蚀划片槽, 然后再弯曲键合后的圆片使圆片因硅 片受拉而断裂, 从而去除高温释气剂残留物。
6. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于所述 Si圆片上浅槽的微加工工艺为湿法腐蚀工艺。
7. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于所述 Si圆片与 Pyrex7740玻璃的阳极键合工艺条件为:温度 400°C,电压: 600V。
8. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于, 第四步中的加热温度为 840°C〜880°C。
9. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法, 其特征 在于将第四步所得到的玻璃微腔进行热退火, 工艺条件为: 退火温度范围在 510°C〜560°C中, 退火保温时间为 30min, 然后缓慢风冷至常温。
10. 根据权利要求 1所述的圆片级玻璃微腔的发泡成型制造方法,其特征 在于所述高温释气剂放置于硅槽中的方法是: 将高温释气剂配成均匀混合液 体加入硅槽中, 再干燥。
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