MICROELECTROMECHANICAL SYSTEM COMPONENT OR A MICROFLUIDIC COMPONENT COMPRISING A FREE-HANGING OR FREE-STANDING MICROCHANNEL
20220324701 · 2022-10-13
Inventors
- Wouter SPARREBOOM (Ruurlo, NL)
- Jarno GROENESTEIJN (Ruurlo, NL)
- Jack Herman VAN PUTTEN (Ruurlo, NL)
- Meint Jelle DE BOER (Ruurlo, NL)
- Remco John WIEGERINK (Ruurlo, NL)
- Henk-Willem VELTKAMP (Ruurlo, NL)
- Qihui YU (Ruurlo, NL)
- Mahdieh YARIESBOUEI (Ruurlo, NL)
- Miguel A. RODRIGUEZ OLGUIN (Ruurlo, NL)
- Joost Conrad LÖTTERS (Ruurlo, NL)
Cpc classification
B81C1/00119
PERFORMING OPERATIONS; TRANSPORTING
B81B2201/058
PERFORMING OPERATIONS; TRANSPORTING
G01N9/32
PHYSICS
B81B2201/0214
PERFORMING OPERATIONS; TRANSPORTING
International classification
B81C1/00
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The invention relates to a microelectromechanical system (MEMS) component or microfluidic component comprising a free-hanging or free-standing microchannel (1), as well as methods for manufacturing such a microchannel, as well as a flow sensor, e.g. a thermal flow sensor or a Coriolis flow sensor, pressure sensor or multi-parameter sensor, valve, pump or microheater, comprising such a microelectromechanical system component or microfluidic component. The MEMS component allows to increase the flow range and/or decrease the pressure drop of for instance a micro Coriolis mass flow meter by increasing the channel diameter, while maintaining its advantages.
Claims
1-18. (canceled)
19. A microelectromechanical system component or microfluidic component comprising a free-hanging or free-standing microchannel, wherein the microchannel has a substantially circular cross-section, wherein the diameter of the microchannel is at least 10 times the thickness of the microchannel wall and the diameter of the microchannel is at least 20 μm.
20. The microelectromechanical system component or microfluidic component according to claim 19, wherein the diameter of the microchannel is selected from at least 50 μm, at least 100 μm, at least 200 μm, at least 500 μm, and at least 1000 μm.
21. The microelectromechanical system component or microfluidic component according to claim 19, wherein the thickness of the microchannel wall is smaller than 10 μm.
22. A flow sensor comprising the microelectromechanical system component or microfluidic component according to claim 19.
23. The flow sensor according to claim 22, wherein the flow sensor is at least one of a thermal flow sensor, a Coriolis flow sensor, a pressure sensor, a density sensor, a viscosity sensor, a multi-parameter sensor, a valve, a pump and a microheater.
24. A method of manufacturing a free-hanging or free-standing microchannel using an electroplating method comprising the steps of: providing a conductive or non-conductive electroplating wire; when the electroplating wire is non-conductive: forming a conductive coating on the electroplating wire to form a cathode; electroplating a channel wall on the electroplating wire or the conductive coating; and removing the electroplating wire.
25. The method according to claim 24, wherein the microchannel has a substantially circular cross-section, wherein the diameter of the microchannel is at least 10 times the thickness of the microchannel wall and the diameter of the microchannel is at least 20 μm.
26. The method according to claim 24, wherein the electroplating wire is made of acrylonitrile-butadiene-styrene (ABS) or copper.
27. The method according to claim 24, wherein the conductive coating comprises silver.
28. The method according to claim 24, wherein the microchannel wall comprises nickel or copper and the electroplating step is carried out in a nickel or copper electroplating cell using an aqueous nickel or copper solution.
29. The method according to claim 24, wherein the microchannel is incorporated in a microelectromechanical system (MEMS) component or a microfluidic system.
30. The method according to claim 24, wherein the electroplating wire is pre-shaped to be a part of a MEMS system or a microfluidic system before the step of electroplating.
31. The method according to claim 30, wherein the pre-shaped electroplating wire is attached to a MEMS system or a microfluidic system before the step of electroplating.
32. A free-hanging or free-standing microchannel manufactured according to the method of claim 24.
33. A microfluidic system or a MEMS system, comprising the free-hanging or free-standing microchannel of claim 32.
34. A flow sensor, comprising the free-hanging or free-standing microchannel according to claim 32.
35. The flow sensor according to claim 34, wherein the flow sensor is at least one of a thermal flow sensor, a Coriolis flow sensor, a pressure sensor, a density sensor, a viscosity sensor, a multi-parameter sensor, a valve, a pump and a microheater.
36. A microfluidic density sensor comprising: the free-hanging or free-standing microchannel of claim 32; actuating means for vibrating the free-hanging or free-standing microchannel at its resonance frequency; and readout means for measuring and comparing the resonance frequency.
37. A method of manufacturing a free-hanging microchannel, comprising the steps of: (a) providing a substrate of a first material; (b) depositing a trench-etch protective layer on at least one of a front side and a back side of the substrate; (c) etching a trench in the first material through the trench-etch protective layer; (d) creating a channel-etch protective layer in the trench, covering a bottom wall and side walls of the trench; (e) etching the first material of the substrate through the channel-etch protective layer and the bottom wall of the trench to form a channel outline centering around the location of the etched-away bottom wall of the trench; (f) removing the trench-etch and channel-etch protective layers from the substrate; (g) depositing a wall-forming layer on the substrate, wherein the wall-forming layer forms a microchannel wall on the channel outline and closes the trench; (h) etching the substrate to remove the first material surrounding the microchannel wall, such that the microchannel becomes free-hanging.
38. The method according to claim 37, wherein the microchannel has a substantially circular cross-section, wherein the diameter of the microchannel is at least 10 times the thickness of the microchannel wall and the diameter of the microchannel is at least 20 μm.
39. The microelectromechanical system component or microfluidic component according to claim 19, wherein the free-hanging or free-standing microchannel is manufactured using a sol-gel method comprising the steps of: forming a mould with a circular channel; flushing the circular channel with a flushing fluid to create an oxidized inner channel wall; cleaning and drying the oxidized inner channel wall; flushing the circular channel with a sol-gel solution; initiating a gelation reaction until a desired microchannel wall thickness is achieved; flushing out the remaining sol-gel solution; and removing the mould material from around the microchannel wall.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0128] The invention will next be explained by means of the accompanying drawings and description of the figures.
[0129] In
[0130]
[0131]
[0132]
[0133]
[0134]
[0135]
[0136]
[0137]
[0138]
[0139]
[0140] In
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[0143]
[0144]
[0145]
[0146]
[0147] In
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DETAILED DESCRIPTION
First Method
[0152] As will be shown with respect to
[0153] However, as discussed in the foregoing, many applications, like liquid chromatography or “Lab-on-a-Chip” use higher flowrates while requiring the low volumes of microfluidic flowmeters. To be able to increase the flow-range and/or decrease the pressure drop of the micro Coriolis MFM the channel-diameter needs to be increased, while maintaining its advantages (fast, accurate, low volume, small form factor). However, inherent to the SCT process, the channels have a flat top and a maximum channel-wall thickness. Both of these limit the maximum size of the free-hanging channel and increase the sensitivity to pressure when the channel size increases.
[0154] The fabrication process shown in
Fabrication Outline
[0155] In
[0156] As shown in
[0157] As shown in
[0158] As shown in
[0159] The PECVD process is preferably not conformal, which means that virtually no SiO.sub.2 will be deposited inside the trenches 15, while a relatively thick layer is deposited on the surface of the wafer 2. A directional plasma etch may be used to remove the t-SiO.sub.2 at the bottom 16 of the trenches 15. Since the etch-rate of this process decreases heavily inside the trenches 15, the PECVD SiO.sub.2 layer 6 at the surface (front side 11) needs to be much thicker than the t-SiO.sub.2 layer at the bottom 16.
[0160] As shown in
[0161] As shown in
[0162] As shown in
[0163] As shown in
Fabrication Results
[0164] At the start of the etch, the silicon loading is very small and plenty of etchant can reach the silicon, while the reaction products can be removed. This results in a completely isotropic etch. However, when the channel diameter increases, the silicon load also increases while the trenches 15 through which the etchant and reaction products have to diffuse does not increase. As a result, the XeF.sub.2 concentration inside the channels will decrease, changing the etch kinetics, eventually resulting in a less desirable hexagonal cross-section.
Channel Wall
[0165] Previously, the channel wall 7 was made using a single silicon-rich silicon nitride layer (SiRN). Due to intrinsic stress in the layer available, the layer can only be 2 μm thick. This means that, when the channel 1 diameter increases, the strength and stiffness of the channel wall 7 may not increase with it. As a result, the mechanical behaviour of the free-hanging channel 1 will increasingly depend on external influences like applied pressure and temperature. To create free-hanging channels 1 with a thicker channel wall 7, preferably a layer stack is used where every layer has a function: The SiO.sub.2 protects the channel wall 7 during the XeF.sub.2 release etch.
[0166] SiO.sub.2 has a much better selectivity compared to SiRN which allows to release the complete channel 1.
[0167] The SiRN at the inside of the channel wall 7 results in a chemically inert fluid path. Due to intrinsic stress, the maximum thickness of these SiRN layers is approximately 2 μm and can thus not be used for the whole channel wall 7. It is also deposited at the outside of the channel wall 7 to make sure the stress in the channel wall 7 is mostly balanced.
[0168] The polySi can be deposited e.g. up to 10 μm while its stress can be tuned by annealing. As a result, this layer can be used to reach a specific wall thickness without influencing the stress inside the channel wall 7.
[0169]
[0170] In this case, the trench was only 10 μm wide, and it was completely closed during deposition of the polySi layer 27. As a result, the final SiRN layer 28 is only to be found on top of the wafer 2 and not at the inside of the channel wall 7.
Silicon Isotropic Wet Etching
[0171] Silicon isotropic wet etching, also known as HNA etching, is a chemical etching of silicon by a mixture of hydrofluoric acid (H), nitric acid (N) and acetic acid (A), while some researchers like to use water instead of acetic acid. It is proceeded by a sequential oxidation-followed-by-dissolution process. The complete reaction can be described as:
Si+2HNO.sub.3+6HF->H.sub.2SiF.sub.6+2NO.sub.2+2H.sub.2O
[0172] The factor that limits the etch rate is highly dependent on the composition of the mixture. When the concentration of nitric acid is low and hydrofluoric acid is high, the etch rate of process is limited by the oxidation step. When in the opposite situation, the limit is then the dissolution of SiO.sub.2.
[0173] With a sufficient supply of etchant, together with an ultrasonic bath to accelerate diffusion of etchant and etching product, the maximum diameter of etched channels 1 will be limited only by the depth of trench 15 and thickness of SiRN mask. From the earlier test, SiRN is a good material to serve as a mask for HNA solution, with an etch rate of approximately 23 nm per minute. However, a thicker layer of SiRN can stand longer during etching, as a trade-off, it also becomes more difficult to remove the layer at the bottom 16 of trenches 15. Thus an alternate material can also be considered to serve as mask for HNA solution.
Channel Release
[0174] Releasing the channels 1 “from the bulk” is done in three steps. First, the channel wall 7 layer stack 9, which is also deposited on the top/front side 11 of the wafer may be patterned with release windows next to the channels 1 using a directional plasma etch. To prevent the exposed polySi layer 27 from etching during the bulk etch, a new photoresist layer 3 is applied with smaller release windows. This photoresist requires excellent planarization properties to be able to fully cover the 10 μm step and also allow for accurate enough patterning for comb-fingers used for capacitive read-out. Next, e.g. 200 μm deep trenches may be etched through the release windows using a directional plasma etch. To remove the silicon underneath the channel 1, an isotropic XeF.sub.2 etch is done through these trenches.
[0175] To keep the silicon loading during this etch low (and thus the etch-rate relatively high), parallel channels 1 were made around the free-hanging channel 1 to act as an etch-stop. This is shown in
Actuation and Read-Out
[0176]
[0177] Thus, the Applicant has developed a fabrication process for the fabrication of relatively large, round free-hanging microchannels 1. The channels 1 can have a diameter up e.g. to 180 μm with a channel wall 7 thickness of e.g. up to 10 μm. Integrated metal electrodes 23 can be used for actuation and read-out of e.g. a microfluidic sensor, such as a high flow micro Coriolis mass flow sensor.
Second Method
[0178] A second method that may result in (almost perfectly) circular channels 1 with various diameters and channel wall 7 thicknesses comprises a so-called “sol-gel” method.
[0179]
[0180] Referring to
[0181] As shown in
[0182]
Third Method
[0183] A third method that can be used is electroplating. Plating can be performed on wires 34 (with a circular cross-section) of for instance Acrylonitrile-Butadiene-Styrene (ABS), which can afterwards be dissolved by e.g. acetone.
[0184] To produce an electrically conductive cathode the FDM-ABS wire 34 may be coated by silver conductive paint 35 and dried at room temperature. A volume of 1 litre aqueous copper solution preferably contains 0.1 kg copper salt, 0.11 litre 96% sulphuric acid, 0.15 ml 50% HCl, 10 ml HL11 starter and 0.25 ml HL13 grain refiner. DI water may be added to reach the required volume. The electroplating may be done e.g. at room temperature with a current density of 3 A/dm.sup.2 for 1 h. After electroplating, the substrate is rinsed with DI water to prevent oxidation of the electroplated copper 36. Next, the wire 34 may be immersed in e.g. a beaker of acetone for 12 hours to completely dissolve the ABS wire 34 inside. Instead of ABS, PA or PVA polymer could also be used which can be dissolved in hot water.
[0185] This plating method can be used to predictably manufacture microchannels with a very high degree of circularity, e.g., the channels 1 produced by the plating method have a high degree of rotational symmetry. Flat parts can be prevented by selecting a highly circular wire 34.
[0186] The method was repeatedly tested using ABS wires 34 with a diameter of 120 to 1000 μm. Table 1 shows examples of measured wall thicknesses for several different runs of nickel electroplating for every size of ABS wire 34. The thinnest wall thickness achieved was approximately 8 μm. The thickest walls were 60 μm, and thicker walls can be achieved if the electroplating step is permitted to continue even longer.
TABLE-US-00001 TABLE 1 Diameter of Thickness of the nickel coating the ABS wire (wall thickness) 120 μm 8 μm, 20 μm, 40 μm 128 μm-130 μm 8 μm, 10 μm, 20 μm, 40 μm, 50 μm, 60 μm 165 μm 8 μm, 10 μm, 20 μm, 40 μm, 50 μm 169 μm 10 μm, 20 μm, 40 μm, 50 μm, 60 μm 178 μm 10 μm, 20 μm, 30 μm, 233 μm 10 μm 20 μm, 30 μm, 43 μm 550 μm 10 μm, 20 μm, 40 μm, 50 μm, 60 μm 600 μm 10 μm, 20 μm, 40 μm, 50 μm, 60 μm 862 μm 10 μm, 15 μm, 20 μm, 30 μm, 40 μm, and 50 μm 866 μm 10 μm, 15 μm, 20 μm, 30 μm, 40 μm, and 50 μm 1000 μm 9 μm, 10 μm, 15 μm, 20 μm, 30 μm, 40 μm, and 50 μm
[0187] Thus the method can be used to manufacture channels with ratio of wall thickness to channel diameter from approximately 1:3 to 1:115. In addition, the channel walls were found to be highly uniform.
[0188] The plating method can be used to manufacture a microfluidic density sensor with low fabrication cost. Such a density sensor could preferably comprise a free-standing U-shaped channel, where the straight leg parts are connected to the straight middle part by rounded edges. In this case, the density sensor tube is made of nickel.
[0189] The channel is made using electroplating. Before immersion in the bath, a 600 μm diameter ABS wire is bent into the U-shape (optionally using a mould), deep coated with silver paint and dried. The anode of the electroplating cell is a 99.99% pure nickel bar, whereas the conductive or non-conductive electroplating wire forms the cathode. The electroplating is allowed to continue until the desired wall thickness of 20 μm was reached. Then the wire was removed from the electroplating bath and placed in an ABS-dissolving liquid consisting of acetone, and optionally heated. The resulting channel has a highly circular cross-section with a diameter of 600 μm and a wall thickness of 20 μm.
[0190] The U-shaped density sensor channel is 12*12 mm long and broad, and may be used in a set-up similar to those mentioned in aforementioned Groenesteijn, et al., 2012. The density sensor was further assembled by placing three external magnets parallel to the length of the channel, attaching the power supply and connecting the inlet to a fluid supply and the outlet to a drain. Preferably, a filter and a degasser are placed before the inlet. Alternating current is applied to the density sensor tube in the presence of an external magnetic field to vibrate the channel by Lorentz force. When the vibrating channel fills with fluid, the mass increases and this increase can be detected through change in (twist mode) resonance frequency. The mode of detection can change depending on the channel shape used. This density sensor has a spring constant of 1.56*10.sup.4 N/m and a of 3.78*10.sup.5 at atmospheric pressure and room temperature. The circular cross-section of the channel results in low dependency on gauge pressure.
LIST OF REFERENCE NUMERALS
[0191] 1. Microchannel [0192] 2. Substrate of first material (silicon) [0193] 3. Photoresist layer [0194] 4. First thermal SiO.sub.2 layer [0195] 5. LPCVD SiO.sub.2 layer [0196] 6. PECVD SiO.sub.2 layer [0197] 7. Channel wall [0198] 8. Metal layer [0199] 9. Wall-forming layer [0200] 10. Inlet [0201] 11. Front side [0202] 12. Back side [0203] 13. Inlet side wall [0204] 14. Inlet top wall [0205] 15. Trench [0206] 16. Trench bottom wall [0207] 17. Trench side wall [0208] 18. Second thermal SiO.sub.2 layer [0209] 19. Channel outline [0210] 20. Continuous flow channel [0211] 21. Closed channel etch-trench [0212] 22. Comb structure with comb fingers [0213] 23. Metal electrodes [0214] 24. Release hole [0215] 25. First wall-forming layer (thermal SiO.sub.2) [0216] 26. Second wall-forming layer (SiRN) [0217] 27. Third wall-forming layer (polySi) [0218] 28. Fourth wall-forming layer (SiRN) [0219] 29. Circular mould [0220] 30. Piranha solution [0221] 31. Hydroxyl group [0222] 32. Sol-gel mixture [0223] 33. Silicon dioxide layer [0224] 34. ABS wire [0225] 35. Silver layer [0226] 36. Copper layer [0227] 37. Circular channel of mould