CN107482114B - A kind of diffusion interlinked method of PZT/Si - Google Patents
A kind of diffusion interlinked method of PZT/Si Download PDFInfo
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- CN107482114B CN107482114B CN201710653766.3A CN201710653766A CN107482114B CN 107482114 B CN107482114 B CN 107482114B CN 201710653766 A CN201710653766 A CN 201710653766A CN 107482114 B CN107482114 B CN 107482114B
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- H—ELECTRICITY
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- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
- H10N30/072—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by laminating or bonding of piezoelectric or electrostrictive bodies
Abstract
The invention belongs to advanced manufacturing technology fields, provide a kind of diffusion interlinked method of PZT/Si.Firstly, preparing electrode layer on PZT bulk surface, and PZT film is deposited in electrode layer surface, forms PZT element；Then, under the conditions of certain temperature, by applying pressure to PZT element and silicon substrate, make lead element and silicon in PZT film that diffusion reaction occur, the diffusion interlinked layer with certain depth and high-bond is formed, to realize the firm combination of PZT element/silicon；Finally, obtaining the PZT piezoelectric layer of required thickness using subsequent mechanical grinding and polishing process.It is the bond strength height of bonding pattern PZT/Si, simple process, easy to implement, at low cost, it is conducive to commercialization and promotes and applies.
Description
Technical field
The invention belongs to advanced manufacturing technology fields, provide a kind of diffusion interlinked method of PZT/Si.
Background technique
In recent years, as information collection, processing, the integrated MEMS (Micro-Electro- of execution
Mechanical Systems, MEMS) with its micromation, low energy consumption, high sensitivity, it is highly integrated the advantages that by academia and
The highest attention of industrial circle.
Piezoelectric material has can be by electric energy and the mechanical sensing that can be carried out the characteristic mutually converted, made using piezoelectric material
The piezoelectric MEMS devices such as device, actuator, energy harvester (pMEMS) have become an important branch of MEMS research field.
Wherein, it occupies an leading position by the pMEMS device of substrate of silicon.Lead zirconate titanate (PZT) piezoceramic material has relatively because of it
High piezoelectric coefficient d33, and it is widely used in silicon based piezoelectricity device.
To prepare Silicon PZT piezoelectric device, it is necessary first to integrate PZT piezoelectric layer with silicon substrate, in pMEMS device
Piezoelectric layer thickness is usually 10~500 μm or so, to adapt to different application demands, generally also there is patterning to require it.
Currently, the method for preparing PZT on a silicon substrate specifically includes that (1) deposition prepares the PZT film of target thickness on a silicon substrate, so
Pattern is prepared by micro fabrications such as photoetching, etchings afterwards.This method heat of silicon and PZT in PZT sintering crystallization process is lost
With larger stress is generated, it is easy to cause PZT to crack and then influences PZT film piezoelectric property.It (2) will by machining process
PZT bulk is thinned to target thickness, on a silicon substrate by glue bond, then passes through the preparation of the micro fabrications such as photoetching, etching
Pattern.It has been the machining limit that PZT bulk, which is thinned to 100 μm, and yield rate is only 10%, and subsequent transfer was bonded
Journey is complicated, operating difficulties.
Summary of the invention
The invention solves technical problem be to overcome the shortcomings of above-mentioned technology, invent a kind of diffusion interlinked side of PZT/Si
Method.Firstly, preparing electrode layer and PZT film on PZT bulk surface, PZT element is formed；Then, under the conditions of certain temperature, pass through
Pressure is applied to PZT element and silicon substrate, makes lead element and silicon in PZT film that diffusion reaction occur and forms diffusion interlinked layer, from
And realize the firm combination of PZT element/silicon；Finally, obtaining the PZT of required thickness using subsequent mechanical grinding and polishing process
Piezoelectric layer.It is the bond strength height of bonding pattern PZT/Si, simple process, easy to implement, at low cost, it promotes and answers conducive to commercialization
With.
Technical solution of the present invention:
A kind of diffusion interlinked method of PZT/Si, firstly, preparing electrode layer 2 on 1 surface of PZT bulk, and on 2 surface of electrode layer
PZT film 3 is deposited, PZT element is formed；Then, under the conditions of certain temperature, by applying pressure to PZT element and silicon substrate 4,
Make lead element and silicon in PZT film 3 that diffusion reaction occur, forms the diffusion interlinked layer with certain depth and high-bond, from
And realize the firm combination of PZT element/silicon；Finally, obtaining the PZT of required thickness using subsequent mechanical grinding and polishing process
Piezoelectric layer.
Specific step is as follows:
1) surface preparation of PZT bulk
Firstly, carrying out mechanical lapping polishing treatment to PZT bulk 1, surface smoothness is allowed to lower than 800nm, roughness is
100~500nm is required with meeting electrode layer sputtering；Then, adhered to using acetone, deionized water removal 1 surface of PZT bulk
Organic impurities；Finally, carrying out oil removal treatment, removal 1 surface saponification of PZT bulk oil and mineral to PZT bulk 1 using degreasing fluid
Oil；
2) preparation of electrode layer and PZT film
Bottom working electrode of the 1 surface sputtering electrode layer 2 of PZT bulk as PZT element after the pre-treatment；In electrode layer
The PZT film 3 that 2 surfaces deposit 10~70 μ m-thicks is used as bonded layer；PZT bulk 1, electrode layer 2 and PZT film 3 constitute PZT element；
3) surface preparation of PZT element and silicon substrate
For PZT element, firstly, carrying out mechanical lapping polishing treatment to PZT film 3, it is allowed to surface smoothness and is lower than
600nm, roughness are lower than 500nm, are required with meeting bonding；Then, adhered to using acetone, deionized water removal 3 surface of PZT film
Organic impurities；Finally, carrying out oil removal treatment to PZT element using degreasing fluid, the saponified oil and mineral on 3 surface of PZT film are removed
Oil；
It for silicon substrate 4, is cleaned by RCA standard cleaning method, to remove the impurity of surface attachment；
4) PZT element is bonded with the High temperature diffusion of silicon substrate
5~30N pressure is applied to PZT element and silicon substrate 4, in the case where keeping pressure condition, by PZT element and silicon substrate 4
It is integrally placed under 700~1000 DEG C of hot environments, and keeps the temperature 10~60min, complete the High temperature diffusion of PZT element and silicon substrate 4
Bonding；
5) reduction processing of PZT element
After completion PZT element is bonded with the High temperature diffusion of silicon substrate 4, using mechanical lapping and polishing process, to PZT element
PZT bulk 1 carry out reduction processing, obtain the PZT piezoelectric layer of required thickness.Meanwhile PZT piezoelectric layer surface flatness is lower than
800nm, roughness are 100~500nm.
The electrode layer 2 includes that Ti electrode layer 2-1 and Pt electrode layer 2-2, Ti electrode layer 2-1 sputters at PZT bulk 1
Surface, Pt electrode layer 2-2 sputter at the surface of Ti electrode layer 2-1.
The Ti electrode layer 2-1 thickness is 20~50nm, and Pt electrode layer 2-2 thickness is 100~500nm.
Beneficial effects of the present invention: the present invention provides a kind of diffusion interlinked method of PZT/Si, firstly, making on PZT bulk
Standby electrode layer and PZT film, form PZT element；Then, it under the conditions of certain temperature, is pressed by applying to PZT element and silicon substrate
Power forms diffusion interlinked layer, realizes the firm combination of PZT element/silicon；Finally, being obtained using subsequent mechanical grinding and polishing process
Obtain the PZT piezoelectric layer of required thickness.It is the bond strength height of bonding pattern PZT/Si, simple process, easy to implement, at low cost,
It is promoted and applied conducive to commercialization.
Detailed description of the invention
Fig. 1 is the diffusion interlinked method schematic diagram of PZT/Si.
Fig. 2 is the diffusion interlinked method and process route map of PZT/Si.
In figure: 1PZT bulk；2-1Ti electrode layer；2-2Pt electrode layer；3PZT film；4 silicon substrates；
The processing of 5PZT bulk grinding and polishing；6PZT bulk surface sputtering electrode layer；
The preparation of 7PZT bulk electrode layer surface PZT film；8PZT element grinding polishing treatment；
9PZT element is bonded with silicon substrate High temperature diffusion；10PZT element reduction processing.
Specific embodiment
Below in conjunction with technical solution and the attached drawing specific embodiment that the present invention will be described in detail.
Firstly, being polished directly to PZT bulk, decontamination and oil removal treatment；Then, Ti is sputtered on PZT bulk surface
Electrode and Pt electrode, and certain thickness PZT film is deposited in Pt electrode surface, PZT bulk, electrode layer and PZT film constitute PZT
Element.The diffusion interlinked process of PZT/Si are as follows: under the conditions of certain temperature, by applying pressure to PZT element and silicon substrate, make
Diffusion interlinked, the realization firm combination of PZT element/silicon occurs with silicon for PZT film；Finally, utilizing subsequent mechanical grinding and buffer
Skill obtains the PZT piezoelectric layer of required thickness.
The specific implementation step of embodiment is as follows:
1) surface preparation of PZT bulk
1 model PZT-5H of PZT bulk in the present embodiment, having a size of 10mm × 7mm × 1mm (length × width x thickness).Firstly,
Mechanical lapping polishing treatment is carried out to it, surface smoothness is allowed to and roughness respectively reaches 500nm and 300nm, to meet electricity
Pole sputtering requires；Then, using 10min is successively cleaned by ultrasonic under acetone, ethyl alcohol, deionized water, trichloro ethylene room temperature, with removal
The organic impurities of surface attachment；Finally, carrying out 5~10min at a temperature of 30~40 DEG C using degreasing fluid and being ultrasonically treated, to go
Except surface saponification oil and mineral oil；
2) preparation of electrode layer and PZT film
After the surface preparation for completing PZT bulk 1, bottom of the electrode layer 2 as PZT element need to be prepared on 1 surface of PZT bulk
Portion's working electrode passes through magnetically controlled sputter method on 1 surface of PZT bulk for the bond strength for increasing electrode and PZT bulk 1 first
Sputter the Ti electrode 2-1 of 30nm thickness, then the Pt electrode 2-2 in the surface electrode 2-1 Ti sputtering 200nm thickness.Complete 1 table of PZT bulk
After the preparation of face electrode layer 2, deposition (Electrohydrodynamic atomization deposition) is printed using EFI
Technology is used as bonded layer in the PZT film 3 that 2 surface of electrode layer deposits 50 μ m-thicks.PZT bulk 1, electrode layer 2 and PZT film 3 constitute
PZT element；
3) surface preparation of PZT element and silicon substrate
Before the diffusion interlinked technique for implementing PZT/Si, surface preparation need to be carried out to PZT element and silicon substrate 4.For
PZT element is allowed to surface smoothness and respectively reaches with roughness firstly, mechanical lapping polishing treatment need to be carried out to PZT film 3
500nm and 300nm is required with meeting bonding；Then, clear using ultrasound under acetone, ethyl alcohol, deionized water, trichloro ethylene room temperature
Wash 10min, the organic impurities of removal surface attachment；Finally, it is super to carry out 5~10min using degreasing fluid at a temperature of 30~40 DEG C
Sonication, to remove surface saponification oil and mineral oil；
It for silicon substrate 4, is cleaned using preceding by RCA standard cleaning method, to remove the impurity of surface attachment.This reality
Applying the silicon wafer selected in example is single-sided polishing monocrystalline silicon piece, having a size of 15mm × 12mm × 0.3mm (length × width x thickness)；
4) PZT element is bonded with the High temperature diffusion of silicon substrate
After completing above-mentioned processing step, pressure F is applied to PZT element and silicon substrate 4 using the stainless steel counterweight of 2.5kg
(about 25N), and counterweight, PZT element and silicon substrate 4 are integrally placed in high temperature furnace.Furnace temperature is by room temperature (20 DEG C), with 25
DEG C/heating rate of min is gradually heated to 800 DEG C, and keeps the temperature 20min, then cool to room temperature with the furnace.Taking-up is successfully bonded
PZT element and silicon substrate 4；
5) reduction processing of PZT element
After completion PZT element is bonded with the High temperature diffusion of silicon substrate 4, using mechanical lapping and polishing process, to PZT bulk
1 carries out reduction processing, until 1 thickness of PZT bulk reaches about 200 μm, surface smoothness and roughness respectively reach 500nm and
300nm completes the preparation of PZT piezoelectric layer.
The present invention proposes a kind of diffusion interlinked method of PZT/Si.Firstly, preparing electrode layer 2, and benefit on 1 surface of PZT bulk
Electricity consumption spray printing deposition technique deposits preparation PZT film 3 on 2 surface of electrode layer, forms PZT element；Then, in certain temperature condition
Under, by applying pressure to PZT element and silicon substrate 4, occurs that PZT film 3 with silicon diffusion interlinked, realize that PZT element/silicon is steady
Consolidation is closed；Finally, obtaining the PZT piezoelectric layer of required thickness using subsequent mechanical grinding and polishing process.Bonding pattern PZT/
It is the bond strength height of Si, simple process, easy to implement, at low cost, it is conducive to commercialization and promotes and applies.
Claims (3)
1. a kind of diffusion interlinked method of PZT/Si, which is characterized in that steps are as follows:
1) surface preparation of PZT bulk
Firstly, carrying out mechanical lapping polishing treatment to PZT bulk (1), surface smoothness is allowed to lower than 800nm, roughness 100
~500nm is required with meeting electrode layer sputtering；Then, had using what acetone, deionized water removal PZT bulk (1) surface were adhered to
Machine impurity；Finally, carrying out oil removal treatment, removal PZT bulk (1) surface saponification oil and mineral to PZT bulk (1) using degreasing fluid
Oil；
2) preparation of electrode layer and PZT film
Bottom working electrode of PZT bulk (1) the surface sputtering electrode layer (2) as PZT element after the pre-treatment；In electrode layer
(2) PZT film (3) that surface deposits 10~70 μ m-thicks is used as bonded layer；PZT bulk (1), electrode layer (2) and PZT film (3) are constituted
PZT element；
3) surface preparation of PZT element and silicon substrate
For PZT element, firstly, carrying out mechanical lapping polishing treatment to PZT film (3), it is allowed to surface smoothness and is lower than 600nm,
Roughness is lower than 500nm, is required with meeting bonding；Then, had using what acetone, deionized water removal PZT film (3) surface were adhered to
Machine impurity；Finally, carrying out oil removal treatment to PZT element using degreasing fluid, the saponified oil and mineral oil on PZT film (3) surface are removed；
It for silicon substrate (4), is cleaned by RCA standard cleaning method, to remove the impurity of surface attachment；
4) PZT element is bonded with the High temperature diffusion of silicon substrate
5~30N pressure is applied to PZT element and silicon substrate (4), in the case where keeping pressure condition, by PZT element and silicon substrate (4)
It is integrally placed under 700~1000 DEG C of hot environments, and keeps the temperature 10~60min, the high temperature for completing PZT element and silicon substrate (4) expands
Dissipate bonding；
5) reduction processing of PZT element
After completion PZT element is bonded with the High temperature diffusion of silicon substrate (4), using mechanical lapping and polishing process, to PZT element
PZT bulk (1) carries out reduction processing, obtains the PZT piezoelectric layer of required thickness；Meanwhile PZT piezoelectric layer surface flatness is lower than
800nm, roughness are 100~500nm.
2. the diffusion interlinked method of PZT/Si according to claim 1, which is characterized in that the electrode layer (2) includes Ti
Electrode layer (2-1) and Pt electrode layer (2-2), Ti electrode layer (2-1) sputter at the surface of PZT bulk (1), Pt electrode layer (2-2)
Sputter at the surface of Ti electrode layer (2-1).
3. the diffusion interlinked method of PZT/Si according to claim 2, which is characterized in that described Ti electrode layer (2-1) layer
Thickness is 20~50nm, and Pt electrode layer (2-2) thickness is 100~500nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303952A (en) * | 2000-01-11 | 2001-07-18 | 中国科学院物理研究所 | Method for growing single-orientated lead zircotitanate film on silicon chip |
| CN101051668A (en) * | 2006-04-03 | 2007-10-10 | 佳能株式会社 | Piezoelectric element and manufacturing method thereof, electronic device, ink jet device |
| CN101122681A (en) * | 2006-08-09 | 2008-02-13 | 船井电机株式会社 | Manufacturing method for variable shape mirror |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6815219B2 (en) * | 1999-12-27 | 2004-11-09 | Hynix Semiconductor Inc. | Fabrication method and structure for ferroelectric nonvolatile memory field effect transistor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303952A (en) * | 2000-01-11 | 2001-07-18 | 中国科学院物理研究所 | Method for growing single-orientated lead zircotitanate film on silicon chip |
| CN101051668A (en) * | 2006-04-03 | 2007-10-10 | 佳能株式会社 | Piezoelectric element and manufacturing method thereof, electronic device, ink jet device |
| CN101122681A (en) * | 2006-08-09 | 2008-02-13 | 船井电机株式会社 | Manufacturing method for variable shape mirror |
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