CN116586126A - Piezoelectric type micro-fluid device, manufacturing method thereof and integrated chip - Google Patents
Piezoelectric type micro-fluid device, manufacturing method thereof and integrated chip Download PDFInfo
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- CN116586126A CN116586126A CN202310427550.0A CN202310427550A CN116586126A CN 116586126 A CN116586126 A CN 116586126A CN 202310427550 A CN202310427550 A CN 202310427550A CN 116586126 A CN116586126 A CN 116586126A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/50273—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the means or forces applied to move the fluids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502769—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements
- B01L3/502784—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements specially adapted for droplet or plug flow, e.g. digital microfluidics
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
- B01L2200/10—Integrating sample preparation and analysis in single entity, e.g. lab-on-a-chip concept
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/04—Moving fluids with specific forces or mechanical means
- B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
- B01L2400/0415—Moving fluids with specific forces or mechanical means specific forces electrical forces, e.g. electrokinetic
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Hematology (AREA)
- Clinical Laboratory Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Micromachines (AREA)
Abstract
The application provides a piezoelectric type micro-fluid device, a manufacturing method thereof and an integrated chip, wherein the piezoelectric type micro-fluid device comprises: the piezoelectric device comprises a substrate, a first electrode, a piezoelectric layer, a second electrode and an electroplated metal layer, wherein the first electrode, the piezoelectric layer, the second electrode and the electroplated metal layer are sequentially arranged on the upper surface of the substrate; the substrate is provided with a first hollow structure, and the first electrode and the first hollow structure are constructed to form a first cavity and a flow channel; the electroplated metal layer is provided with a second hollow structure, and a second cavity and a nozzle are formed by constructing the second electrode and the second hollow structure; the second electrode and the first electrode are both used for being connected with a power supply, and the first cavity and the second cavity are used for storing liquid; the first electrode, the piezoelectric layer and the second electrode form a piezoelectric resonator which vibrates when energized to enable ejection of liquid through the nozzle. The piezoelectric type micro-fluid device greatly improves the miniaturization, integration level, manufacturing precision and efficiency of the micro-fluid device, can realize the mass production of products, has lower manufacturing cost and has better applicability.
Description
Technical Field
The application relates to the technical field of microfluidic integrated chips, in particular to a piezoelectric microfluidic device, a manufacturing method thereof and an integrated chip.
Background
Microfluidic technology and devices are used in a wide range of applications, from subsurface research to space applications, for example, in the oil and gas industry to study the behavior of crude oil and brine through porous media, and microgravity examination at international space stations. At present, microfluidic technology and devices are becoming more and more widely used in the biological and medical fields, from drug research to drug delivery, from antibody research to antigen detection, from organ-chip to life detection, from gene sequencing to gene transfer, from single cell lysis to 3D printing of artificial organs, and so forth.
Microfluidic systems operate by using microelectromechanical (MEMS) devices, where different types of pumps accurately move liquids within the device at a rate of 1 μl/min to 10000 μl/min, where there are microfluidic channels to handle the liquids, such as mixing, chemical or physical reactions; the liquid may carry tiny particles, such as cells or nanoparticles; these particles can be driven by the microfluidic device to process, for example, capturing and collecting normal cells from the blood.
In the prior art, microfluidic devices based on MEMS technology have lengths or widths ranging from 1 cm to 10 cm and chip thicknesses ranging from about 0.5 mm to 5 mm. The microfluidic device has micro-channels inside, such as hairlines, which are connected to the outside through holes on the chip called inlet/outlet ports. MEMS devices are piezoelectric or made of thermoplastics such as quartz, piezoceramics, acrylic, glass, or PDMS, etc., with channels made by photolithography, hot stamping, injection molding, micromachining, or etching, depending on the choice of materials. However, in the prior art, there are still serious limitations in terms of minimum feature size, surface roughness, optical transparency, and choice of materials for microfluidic devices.
In summary, the present application provides a new piezoelectric microfluidic device and a method for manufacturing the same, so as to promote the development of miniaturization, high integration, high manufacturing precision and high efficiency, and further provides an integrated chip including the piezoelectric microfluidic device, so as to further promote the integration, miniaturization and multifunctional application of the chip.
Disclosure of Invention
Based on the above description, the present application provides a piezoelectric type microfluidic device, a manufacturing method thereof, and an integrated chip, so as to promote the development of miniaturization, high integration, high manufacturing precision and efficiency of the microfluidic device, and promote the integration, miniaturization and multifunctional application of the chip.
The technical scheme for solving the technical problems is as follows:
in a first aspect, the present application provides a piezoelectric microfluidic device comprising: the piezoelectric device comprises a substrate, a first electrode, a piezoelectric layer, a second electrode and an electroplated metal layer, wherein the first electrode, the piezoelectric layer, the second electrode and the electroplated metal layer are sequentially arranged on the upper surface of the substrate;
the substrate is provided with a first hollow structure, and the first electrode and the first hollow structure are constructed to form a first cavity and a flow channel; the electroplated metal layer is provided with a second hollow structure, and the second electrode and the second hollow structure are constructed to form a second cavity and a nozzle;
the second electrode and the first electrode are both used for being connected with a power supply, and the first cavity and the second cavity are used for storing liquid; the first electrode, the piezoelectric layer and the second electrode form a piezoelectric resonator; upon energization, the resonator vibrates to enable the liquid to be ejected through the nozzle.
On the basis of the technical scheme, the application can be improved as follows.
Further, the piezoelectric layer is provided with a through hole;
the through hole is used for communicating the first cavity and the second cavity.
Further, the piezoelectric microfluidic device further comprises a metal connector;
the metal connecting piece penetrates through the piezoelectric layer and is connected with the first electrode, and the first electrode is used for being connected with the power supply through the metal connecting piece.
Further, the piezoelectric microfluidic device further comprises a passivation layer and a first seed layer;
the passivation layer covers the upper surfaces of the second electrode, the piezoelectric layer and the metal connecting piece;
the first seed layer covers the upper surface of the passivation layer.
Further, the electroplated metal layer comprises a first metal layer and a second metal layer;
the first metal layer and the second metal layer are sequentially arranged on the upper surface of the first seed layer.
Further, the piezoelectric microfluidic device further comprises a second seed layer;
the second seed layer is arranged between the first metal layer and the second metal layer.
In a second aspect, the present application also provides a method for fabricating the piezoelectric microfluidic device according to any one of the first aspects, comprising:
depositing a metal material on the upper surface of the substrate with the sacrificial layer to manufacture a first electrode;
manufacturing a piezoelectric material on the upper surface of the first electrode to obtain a piezoelectric layer;
etching the sacrificial layer to obtain a first cavity;
sequentially carrying out photoresist treatment and metal material electroplating on the second electrode to manufacture an electroplated metal layer so as to form a second cavity and a nozzle;
etching the substrate at the bottom of the first cavity to manufacture a runner.
On the basis of the technical scheme, the application can be improved as follows.
Further, after obtaining the piezoelectric layer, the method further comprises:
depositing a metal material on a part of the area of the piezoelectric layer to manufacture a second electrode;
etching is carried out on the other partial area of the piezoelectric layer to obtain a connecting hole, and a metal connecting piece is used for penetrating the connecting hole to be in contact with the first electrode.
After the first cavity is obtained, the method further comprises:
passivating the upper surfaces of the second electrode, the piezoelectric layer and the metal connecting piece to manufacture a passivation layer;
electroplating the upper surface of the passivation layer to manufacture a first seed layer;
performing photoetching and electroplating processes on the first seed layer to form a first electroplated metal layer;
and manufacturing a second seed layer on the first electroplated metal layer, and carrying out a photoetching process and an electroplating process to form a second electroplated metal layer.
In a third aspect, the present application also provides an integrated chip comprising a piezoelectric microfluidic device as claimed in any of the first aspects and a CMOS control circuit provided on a substrate of the piezoelectric microfluidic device.
Compared with the prior art, the technical scheme of the application has the following beneficial technical effects:
the piezoelectric type micro-fluid device provided by the application is a micro-fluid system based on a piezoelectric material and a semiconductor manufacturing technology, so that the miniaturization, integration level, manufacturing precision and efficiency of the micro-fluid device are greatly improved, the large-scale production of products can be realized, and the manufacturing cost is lower;
when the piezoelectric type micro-fluid device is electrified, the upper part of the substrate of the piezoelectric type micro-fluid device forms a resonator, the two ends of a power supply are respectively communicated with the first electrode and the second electrode, voltage is applied to the piezoelectric layer, and the piezoelectric effect of the piezoelectric material converts electric energy into mechanical energy to cause the resonator to vibrate up and down, so that the liquid in the cavity can be sprayed out through the nozzle;
in droplet microfluidic applications, the piezoelectric microfluidic device is capable of producing tiny volumes of droplets, up to nanoliter (nL), femtoliter (fL), and even picoliter (pL) levels, which can be widely used in molecular biology, where droplets act as bioreactors, individual cells are trapped in droplets, undergo a series of reactions within the droplets, each of which can be analyzed individually; for microparticle synthesis, the droplets are typically made of hydrogels, which after generation are amenable to photo, chemical or thermal technology curing; in microbiological studies, microorganisms are encapsulated in droplets and can be used to analyze their response to various drug development reagents;
in conclusion, the piezoelectric type micro-fluidic device has high miniaturization degree, integration level, manufacturing precision and efficiency and good applicability.
Drawings
Fig. 1 is a schematic structural diagram of a piezoelectric microfluidic device according to an embodiment of the present application;
fig. 2 is a schematic diagram of a detailed structure of a piezoelectric microfluidic device according to an embodiment of the present application;
fig. 3 is a schematic diagram of an energizing operation of a piezoelectric microfluidic device according to an embodiment of the present application;
fig. 4 is a flowchart of a method for fabricating a piezoelectric microfluidic device according to an embodiment of the present application;
FIG. 5 is a schematic diagram of an arrangement of an integrated chip according to an embodiment of the present application;
FIG. 6 is a schematic diagram of a fabricated wafer according to an embodiment of the present application;
reference numerals:
1. a substrate; 2. a first electrode; 3. a piezoelectric layer; 4. a second electrode; 5. electroplating a metal layer; 51. a first metal layer; 52. a second metal layer; 6. a first cavity; 7. a second cavity; 8. a nozzle; 9. a flow passage; 10. a through hole; 11. a passivation layer; 12. a first seed layer; 13. a second seed layer; 14. a metal connector.
Detailed Description
In order that the application may be readily understood, a more complete description of the application will be rendered by reference to the appended drawings. Embodiments of the application are illustrated in the accompanying drawings. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It should be noted that the terms "first" and "second" are used herein for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Embodiments of the present application will be described in further detail with reference to the accompanying drawings and examples, which are provided to illustrate the present application, but are not intended to limit the scope of the present application.
Example 1
The embodiment of the application provides a piezoelectric type micro-fluidic device, as shown in fig. 1, which structurally comprises a substrate 1, and a first electrode 2, a piezoelectric layer 3, a second electrode 4 and an electroplated metal layer 5 which are sequentially arranged on the upper surface of the substrate 1, wherein the substrate 1 is provided with a first hollow structure, and a first cavity 6 and a flow channel 9 are formed by the first electrode 2 and the first hollow structure; the electroplated metal layer 5 is provided with a second hollow structure, the second electrode 4 and the second hollow structure are constructed to form a second cavity 7 and a nozzle 8, and the circulation function is to provide liquid in the cavity.
The substrate 1 may be silicon, sapphire, glass, or the like, and is preferably a silicon substrate 1.
The second electrode 4 and the first electrode 2 are both used for being connected with a power supply, and the first cavity 6 and the second cavity 7 are used for storing liquid; in the energized state, the piezoelectric layer 3 is able to vibrate the first cavity 6 and the second cavity 7 so that liquid can be ejected through the nozzle 8.
Wherein, as shown in fig. 2, the piezoelectric layer 3 is provided with a through hole 10; the through holes 10 serve to communicate the first cavity 6 and the second cavity 7 so that the liquid can communicate.
Further, in order to facilitate the connection of the first electrode 2 to the end of the power supply, the piezoelectric microfluidic device further comprises a metal connection 14, as shown in fig. 1; the metal connecting piece 14 penetrates through the piezoelectric layer 3 to be connected with the first electrode 2, and the first electrode 2 is used for being connected with a power supply through the metal connecting piece 14.
Furthermore, in order to achieve protection of the electrode, the piezoelectric layer 3 and the first cavity 6, the piezoelectric microfluidic device further comprises a passivation layer 11; the passivation layer 11 covers the upper surfaces of the second electrode 4, the piezoelectric layer 3 and the metal connection member 14. As shown in fig. 1, the passivation layer 11 is capable of isolating the second electrode 4 from the metal connection 14 to prevent the two from being in electrical communication.
Based on the above embodiments, the piezoelectric microfluidic device further comprises a first seed layer 12; the first seed layer 12 covers the upper surface of the passivation layer 11, and serves as a seed layer and a conductive layer for a subsequent electroplating process.
Further, the electroplated metal layer 5 comprises a first metal layer 501 and a second metal layer 502, and the piezoelectric type micro-fluidic device is further provided with a second seed layer 13; the first metal layer 501 and the second metal layer 502 are sequentially disposed on the upper surface of the first seed layer 12, and the second seed layer 13 is disposed between the first metal layer 501 and the second metal layer 502. By arranging two metal layers, a second cavity 7 with a corresponding shape and a nozzle 8 with a corresponding shape can be constructed according to the needs, the size of the nozzle 8 is smaller than that of the second cavity 7, the specific shape and the size of the nozzle are not limited, and the nozzle can be arranged according to the actual needs.
As shown in fig. 3, in the piezoelectric microfluidic device provided by the embodiment of the present application, under the condition that the piezoelectric microfluidic device is electrified, the upper structure of the substrate 1 of the piezoelectric microfluidic device forms a resonator, two ends of a power supply are respectively connected with the metal connecting piece 14 and the second electrode 4, so that the first electrode 2 and the second electrode 4 are electrically connected with the power supply, and thus voltage is applied to the piezoelectric layer 3, and due to the piezoelectric effect of the piezoelectric material, electric energy is converted into mechanical energy, so that the resonator vibrates up and down, and the resonator vibrates, so that liquid in the cavity can be ejected through the nozzle 8.
The piezoelectric microfluidic device can be applied to the field of microfluidics, and compared with the prior art, the piezoelectric microfluidic device can generate tiny-volume liquid drops, reaches nanoliter (nL), femto liter (fL) and even pico liter (pL) levels, can be widely applied to molecular biology, microparticle synthesis and microbiological research, wherein in the molecular biology, the liquid drops serve as bioreactors, single cells are trapped in the liquid drops, a series of reactions are carried out in the liquid drops, and each liquid drop can be independently analyzed; for microparticle synthesis, the droplets are typically made of hydrogels, which after generation are amenable to photo, chemical or thermal technology curing; in microbiological studies, microorganisms are encapsulated in droplets and can be used to analyze their response to various drug development reagents.
Example 2
The embodiment of the present application further provides a method for manufacturing the piezoelectric microfluidic device according to any one of the first aspect, as shown in fig. 4, including:
step S1: a metal material is deposited on the upper surface of the substrate 1 having the sacrificial layer to fabricate the first electrode 2.
Specifically, in this step, the substrate 1 is cleaned first, and the upper surface of the silicon substrate 1 is etched by using a photolithography method including photoresist coating, alignment, exposure and development, a groove having a depth of 2-5 μm is etched, and further photoresist removing and cleaning are performed to prepare a first cavity 6, i.e., a lower cavity, and in actual operation, the first cavity 6 may be circular, square, rectangular, etc., and this embodiment is described by taking a circular shape as an example, and as shown in fig. 2, the circular structure is provided with an externally protruded portion, and a plurality of tooth-like grooves are formed.
A thin film of silicon dioxide, phosphosilicate glass (PSG, phosphorus doped silicon dioxide) or the like is deposited on the upper surface of the silicon substrate 1, and this thin film is removed in a subsequent process, and is thus called a sacrificial layer. The thickness of the sacrificial layer is generally 3 to 8 μm depending on the etching depth, and the specific thickness is not limited herein and may be selected according to actual needs.
Further, the sacrificial layer is subjected to planarization treatment, and the wafer surface is planarized by using a CMP (chemical mechanical polishing) process, which comprises the following specific steps: the silicon substrate 1 is pressed against the polishing pad, global planarization is realized by coupling of polishing solution corrosion, particle friction, polishing pad friction and the like, the polishing pad is driven to rotate by the polishing disk, and real-time thickness measurement with resolution of 3-10 nm is realized by rubbing different materials and thicknesses through an advanced endpoint detection system to prevent over-polishing.
The surface polishing quality is achieved by optimizing the following process parameters: polishing pad materials, structures, hardness, polishing solution components, pH values, polishing pressure settings and the like. Alternatively, in order to reduce the polishing amount or the time of the CMP process, a two-step process may be performed: firstly, removing a sacrificial layer outside the cavity by using an etching method, including photoetching, etching (dry method or wet method), photoresist removing, cleaning and the like; a CMP planarization process is then performed.
Then, a metal material is deposited on the upper surface of the substrate 1 to manufacture the first electrode 2, where the electrode material may be molybdenum (Mo), gold (Au), titanium (Ti), aluminum (Al), tungsten (W), platinum (Pt), copper (Cu), tantalum (Ta), and the like, and the electrode may be manufactured in various manners, such as: metal evaporation, metal sputtering, chemical vapor deposition, etc., the manufacturing process is generally two kinds: metal Lift-off process (Metal Lift-off) and Metal Etch process (Metal Etch). The thickness of the electrode metal layer is dependent on the frequency of the resonator. The manufacturing mode, process and thickness of the electrode are not particularly limited, and can be selected by those skilled in the art according to actual requirements.
Step S2: a piezoelectric material is formed on the upper surface of the first electrode 2 to obtain a piezoelectric layer 3.
Specifically, in this step, the piezoelectric material may be AlN, gaN, PZT, znO, lithium tantalate, lithium niobate, etc., and may be monocrystalline or polycrystalline, doped or undoped. The thickness of the piezoelectric material is between 10nm and 5 mu m, and the specific thickness is determined by the working frequency of the device.
The method of manufacturing the piezoelectric material may be various depending on the kind of material and the thickness of the piezoelectric layer 3, such as sputtering (dispenser), metal Organic Compound (MOCVD), atomic Layer Deposition (ALD), and the like.
For some piezoelectric materials, such as AlN, the piezoelectric properties may be improved by doping. The doping element may be one of the following rare metals: scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), chromium (Cr), and the like.
After the piezoelectric film is manufactured, the piezoelectric layer 3 is manufactured into a required pattern through photoetching, etching, photoresist removing, cleaning and other processes.
Step S3: a metal material is deposited on a part of the area of the piezoelectric layer 3 to produce the second electrode 4.
Specifically, in this step, a metal material is deposited on the upper surface of the piezoelectric layer 3 to form the second electrode 4, i.e., the upper electrode, where the electrode material is molybdenum (Mo), gold (Au), titanium (Ti), aluminum (Al), tungsten (W), platinum (Pt), copper (Cu), tantalum (Ta), and the like, and the electrode is formed in various manners, such as: metal evaporation, metal sputtering, chemical vapor deposition, etc., the manufacturing process is generally two kinds: metal Lift-off process (Metal Lift-off) and Metal Etch process (Metal Etch). The second electrode 4 may be fabricated in the same manner as the first electrode 2 described above. Similarly, the thickness of the metal layer of the second electrode 4 is also dependent on the frequency of the resonator.
Step S4: etching is performed on the other partial region of the piezoelectric layer 3 to obtain a connection hole, and the connection hole is penetrated by a metal connecting piece 14 to be in contact with the first electrode 2.
Specifically, in this step, the piezoelectric layer 3 is etched to obtain the through-hole 10, and the metal connection member 14 can be connected to the first electrode 2 through the through-hole 10, and the process steps include gluing, alignment, development, etching, photoresist removal, cleaning, and the like.
The metal connection piece 14 may be a metal connection wire, which leads out the lower electrode: the metal connection line is generally made of a metal such as aluminum (Al), tungsten (W), copper (Cu), or gold (Au). Can be manufactured by CVD (chemical vapor deposition), PVD (physical vapor deposition), sputtering, evaporation or electroplating. The thickness is between 0.2 and 5 mu m.
The corresponding process steps comprise: metal deposition, gumming, alignment, development, metal etching, photoresist removal, cleaning and the like.
Step S5: the sacrificial layer is etched to obtain a first cavity 6.
Specifically, in this step, a through hole 10 is etched in the convex portion of the circular structure, through the piezoelectric layer 3, and in contact with the sacrificial layer. The etching process comprises the following steps: (1) The etching of the piezoelectric layer 3 can be performed by a wet etching method or a dry etching method; (2) etching the sacrificial layer.
Wherein, etching the sacrificial layer: etched silicon dioxide (SiO) 2 ) The buffer oxide etching solution is generally BOE (buffer oxide etch) etching solution, which is prepared by mixing hydrofluoric acid (49%) with water or ammonium fluoride with water, and is mainly hydrofluoric acid etching solution, NH 4 F is used as a buffer.
After the sacrificial layer is removed, a cavity is formed below the resonator as a lower cavity of the resonator, the first cavity 6.
Step S6: the upper surfaces of the second electrode 4, the piezoelectric layer 3 and the metal connection member 14 are subjected to passivation treatment to produce a passivation layer 11.
Specifically, in this step, after step S4 is completed, a passivation layer 11 is formed on the upper surface of the structure to serve as a protection layer, and the passivation layer 11 is formed to protect the resonator and the metal electrode.
The passivation layer 11 may be silicon carbide, silicon nitride or silicon oxide. The manufacturing method comprises CVD, PVD, thermal reaction method and the like. The thickness is 10-1000 nm.
Atomic Layer Deposition (ALD) may also be used to obtain thinner, more uniform passivation layers 11, up to 5-20 nm thick. The passivation layer 11 is manufactured according to actual needs.
Step S7: a plating process is performed on the upper surface of the passivation layer 11 to produce a first seed layer 12.
Specifically, in this step, a metal seed layer is formed, which can be used as a seed layer and a conductive layer for subsequent metal plating.
In practice, different seed layers are selected according to the electroplating process, for example, if copper is plated, the seed layers can be Ti/Cu, tiW/Cu and the like, wherein the thickness of Ti or TiW is 10-100 nm, and the thickness of Cu is 20-300 nm; if copper is plated, the seed layer may be Ti/Cu, tiW/Cu, etc., wherein the thickness of Ti or TiW is 10-50 nm, and the thickness of Cu is 20-300 nm; if nickel plating is performed, the seed layer may be Ti/Ni, tiW/Ni, etc., wherein the Ti or TiW has a thickness of 10 to 50nm and the Ni has a thickness of 20 to 300nm.
Step S8: a photoresist treatment and a metal material electroplating are sequentially performed on the second electrode 4 to manufacture a metal layer 5 to form a second cavity 7 and a nozzle 8.
Specifically, in this step, first, a first photoresist treatment, that is, photoresist coating, is performed: and selecting a positive adhesive or a negative adhesive, wherein the thickness of the positive adhesive or the negative adhesive is 20-100 mu m. The thickness is dependent on the application, and positive photoresist is used as an example; aligning the mark on the photomask with the mark on the wafer; exposing; developing: the photoresist is positive photoresist, and the exposed portions are dissolved by a developing solution, and the unexposed portions (intermediate portions) remain.
Then, the first metal layer 501 is fabricated to form a cavity, i.e., the second cavity 7 is fabricated. A thicker metal layer can be manufactured by adopting an electroplating process so as to meet the requirements of different thicknesses of the cavity; the thickness of the cavity is 20-100 μm according to different applications, and the metal layer can be nickel or copper and is manufactured by electroplating process.
Further, a second metal seed layer is manufactured and used as a seed layer and a conductive layer of a subsequent electroplating process. Different seed layers are selected according to different electroplating processes. The metal seed layer may be manufactured in the same manner as the first seed layer 12, and the desired morphology may be obtained by optimizing exposure parameters, such as exposure energy and time, and other process parameters, including post-baking temperature and time of the glue, which are not described herein.
Furthermore, the second photoresist treatment is performed on the upper surface of the second seed layer 13, and the photoresist treatment method can refer to the first photoresist treatment process described above, and will not be described herein.
Finally, the second metal layer 502 is fabricated to form the nozzle 8, and a thicker metal layer can be fabricated by electroplating to meet the requirements of the nozzle 8. The height of the nozzle 8 is in the range of 10 to 80. Mu.m, and the diameter is generally 10 to 60. Mu.m. The metal layer may be nickel or copper, and is fabricated by an electroplating process.
After the plating is completed, photoresist stripping is performed, and after the photoresist stripping, a cavity and a nozzle 8 are formed.
The stripping of the photoresist can be directly realized by adopting a mode of adding acetone and isopropanol, namely, the wafer is placed into a solution filled with acetone for soaking, and the corresponding soaking time is set according to the type and thickness of the photoresist.
In order to enhance the photoresist removing effect and reduce the soaking time, the acetone can be heated to 60 ℃, and after the acetone soaking is finished, the wafer is cleaned by the isopropyl alcohol, so that the residues are further removed.
Other photoresist stripping solutions with good photoresist stripping effect, such as N-methyl pyrrolidone (NMP), ethanolamine, diethylene glycol butyl ether and the like, can be used.
Step S9: the bottom of the first cavity 6 is etched to create a flow channel 9.
Specifically, in this step, the flow channel 9 is a channel through which liquid enters the lower cavity of the resonator, the lower cavity and the upper cavity are connected by the through hole 10, and the liquid flows into the lower cavity of the resonator through the flow channel 9 and then enters the upper cavity of the resonator through the through hole 10.
When the device is powered on by an external power source to apply a voltage to the resonator, the resonator vibrates due to the piezoelectric effect, and liquid can be ejected through the nozzle 8.
In practice, the flow channel 9 is manufactured in various ways, for example, laser drilling, wet etching, dry deep silicon etching, etc.
The process of the runner etching comprises the following steps:
1. sticking film: the already fabricated structure (wafer) is front-side attached to a blue film, UV film or other film. Alternatively, the wafer may be bonded to a carrier such as sapphire, glass, or another wafer by bonding.
2. Perforating the bottom of the substrate 1 by a laser perforation method, and communicating with the bottom of a second cavity 7 of the resonator; or adopting an etching method to manufacture the hollow structure with the required shape.
If an etching method can be adopted, the method comprises the following process steps:
2.1 photolithography processes including gumming, alignment, exposure, development, and the like. The alignment here is to align the position of the flow channel 9 with the lower cavity position of the resonator on the front side of the wafer.
2.2 etching of the runner 9, or back hole etching, may be wet process or dry etching, or a combination of wet and dry processes.
2.3 removing photoresist: after the etching is completed, the photoresist on the back side is removed.
3. The wafer is peeled from the blue film or separated from the carrier by a debonding process.
4. And (5) cleaning the wafer.
The cavity of the piezoelectric type micro-fluid device manufactured by the method is used for storing liquid, when the piezoelectric type micro-fluid device is connected with an external power supply, namely, the two ends of the power supply are respectively connected with the upper electrode and the lower electrode of the resonator, voltage is applied to the piezoelectric material of the resonator, and the electric energy is converted into mechanical energy due to the piezoelectric effect of the piezoelectric material, so that the resonator vibrates up and down. The vibration of the resonator ejects the liquid in the cavity through the nozzle 8. The size of the droplets is determined by the nozzle 8, and the frequency of the ejection is controlled by the power frequency. By varying the size of the nozzle 8 and the frequency of the power supply, different liquid volumes and ejection frequencies can be obtained, enabling various microfluidic and microfluidic applications.
Example 3
An embodiment of the present application further provides an integrated chip, as shown in fig. 5, which includes the piezoelectric microfluidic device according to the first aspect and a CMOS control circuit provided on a substrate 1 of the piezoelectric microfluidic device.
Specifically, the MEMS device and the CMOS control circuit are integrally manufactured on the same chip, so that the integration level of the device can be improved, the manufacturing cost can be reduced, and the multifunctional application of the device can be realized. As shown in fig. 5, in a specific example, the left part is a CMOS control circuit, the right part is a MEMS device, and the manufacturing sequence is not limited, and the positions can be replaced according to actual needs.
According to different physical principles and applications, the MEMS device is of various types, and the microfluidic device based on the MEMS device provided by the embodiment of the application can be applied to the fields of biological detection technology, medical equipment and life science research, and can also be applied to the application fields of commercial inkjet printing, industrial identification printing, 3D printing and the like.
The number of MEMS microfluidic devices may be one, two or more. The specific number is not limited. For example, as shown in fig. 5, is an integrated chip with a plurality of MEMS devices. Each MEMS device has CMOS circuitry to be independently controlled to achieve a variety of complex applications.
As shown in FIG. 6, each cell is a chip, and the chip can be square or rectangular, and the side length is in the range of 200 μm-3 cm. The number of devices per chip ranges from one, a few to tens, hundreds, and even thousands.
The MEMS device is manufactured by adopting a semiconductor process, and the resonator, the runner, the cavity and the nozzle are integrally manufactured on the same chip, so that the integration level, the reliability, the consistency and the uniformity of the chip are improved, the manufacturing process is simplified, the cost is reduced, and the large-scale production and the application are facilitated; further, the integrated circuit is integrated with a CMOS control circuit, and each MEMS device is manufactured on the same chip and is independently controlled by the CMOS control chip, so that the integration level of the chip, the performance and the function of the device are further improved.
In the description of the present specification, the description with reference to the term "particular example" or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the embodiments of the application. In this specification, particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and are not limiting; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present application.
Claims (10)
1. A piezoelectric microfluidic device, comprising: the piezoelectric device comprises a substrate, a first electrode, a piezoelectric layer, a second electrode and an electroplated metal layer, wherein the first electrode, the piezoelectric layer, the second electrode and the electroplated metal layer are sequentially arranged on the upper surface of the substrate;
the substrate is provided with a first hollow structure, and the first electrode and the first hollow structure are constructed to form a first cavity and a flow channel; the electroplated metal layer is provided with a second hollow structure, and the second electrode and the second hollow structure are constructed to form a second cavity and a nozzle;
the second electrode and the first electrode are both used for being connected with a power supply, and the first cavity and the second cavity are used for storing liquid; the first electrode, the piezoelectric layer and the second electrode form a piezoelectric resonator; upon energization, the resonator vibrates to enable the liquid to be ejected through the nozzle.
2. The piezoelectric microfluidic device according to claim 1, wherein the piezoelectric layer is provided with a through hole;
the through hole is used for communicating the first cavity and the second cavity.
3. The piezoelectric microfluidic device of claim 1, further comprising a metal connection;
the metal connecting piece penetrates through the piezoelectric layer and is connected with the first electrode, and the first electrode is used for being connected with the power supply through the metal connecting piece.
4. The piezoelectric microfluidic device of claim 3, further comprising a passivation layer and a first seed layer;
the passivation layer covers the upper surfaces of the second electrode, the piezoelectric layer and the metal connecting piece;
the first seed layer covers the upper surface of the passivation layer.
5. The piezoelectric microfluidic device of claim 4, wherein the electroplated metal layer comprises a first metal layer and a second metal layer;
the first metal layer and the second metal layer are sequentially arranged on the upper surface of the first seed layer.
6. The piezoelectric microfluidic device of claim 5, further comprising a second seed layer;
the second seed layer is arranged between the first metal layer and the second metal layer.
7. A method of manufacturing the piezoelectric microfluidic device according to any one of claims 1 to 6, comprising:
depositing a metal material on the upper surface of the substrate with the sacrificial layer to manufacture a first electrode;
manufacturing a piezoelectric material on the upper surface of the first electrode to obtain a piezoelectric layer;
etching the sacrificial layer to obtain a first cavity;
sequentially carrying out photoresist treatment and metal material electroplating on the second electrode to manufacture an electroplated metal layer so as to form a second cavity and a nozzle;
etching the substrate at the bottom of the first cavity to manufacture a runner.
8. The method of manufacturing according to claim 7, further comprising, after obtaining the piezoelectric layer:
depositing a metal material on a part of the area of the piezoelectric layer to manufacture a second electrode;
etching is carried out on the other partial area of the piezoelectric layer to obtain a connecting hole, and a metal connecting piece is used for penetrating the connecting hole to be in contact with the first electrode.
9. The method of manufacturing of claim 8, further comprising, after obtaining the first cavity:
passivating the upper surfaces of the second electrode, the piezoelectric layer and the metal connecting piece to manufacture a passivation layer;
electroplating the upper surface of the passivation layer to manufacture a first seed layer;
performing photoetching and electroplating processes on the first seed layer to form a first electroplated metal layer;
and manufacturing a second seed layer on the first electroplated metal layer, and carrying out a photoetching process and an electroplating process to form a second electroplated metal layer.
10. An integrated chip comprising a piezoelectric microfluidic device according to any one of claims 1 to 6 and CMOS control circuitry provided on a substrate of the piezoelectric microfluidic device.
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