CN107482114A - A kind of diffusion interlinked methods of PZT/Si - Google Patents
A kind of diffusion interlinked methods of PZT/Si Download PDFInfo
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- CN107482114A CN107482114A CN201710653766.3A CN201710653766A CN107482114A CN 107482114 A CN107482114 A CN 107482114A CN 201710653766 A CN201710653766 A CN 201710653766A CN 107482114 A CN107482114 A CN 107482114A
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Abstract
The invention belongs to advanced manufacturing technology field, there is provided a kind of diffusion interlinked methods of PZT/Si.First, electrode layer is prepared on PZT bulks 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 the lead element in PZT film that diffusion reaction occur with silicon, the diffusion interlinked layer with certain depth and high-bond is formed, so as to realize the firm combination of PZT element/silicon；Finally, subsequent mechanical grinding and glossing, the PZT piezoelectric layers of thickness needed for acquisition are utilized.Bonding pattern PZT/Si bond strength is high, technique is simple, easy to implement, cost is low, beneficial to commercialization popularization and application.
Description
Technical field
The invention belongs to advanced manufacturing technology field, there is provided a kind of diffusion interlinked methods of PZT/Si.
Background technology
In recent years, as information gathering, processing, the MEMS (Micro-Electro- for performing integration
Mechanical Systems, MEMS) with its miniaturization, low energy consumption, high sensitivity, it is highly integrated the advantages that by academia and
The highest attention of industrial circle.
Piezoelectric has the characteristic that can be mutually converted electric energy and mechanical energy, the sensing made using piezoelectric
The piezoelectric MEMS devices such as device, actuator, energy harvester (pMEMS) have become an important branch of MEMS research fields.
Wherein, the pMEMS devices using silicon as substrate are occupied an leading position.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 integrated PZT piezoelectric layers with silicon substrate, in pMEMS devices
Piezoelectric layer thickness is usually 10~500 μm or so, general also with patterning requirement to it to adapt to different application demands.
At present, preparing PZT method on a silicon substrate mainly includes：(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 silicon and PZT heat in PZT sinters crystallization process is lost
With larger stress is produced, easily cause PZT to crack and then influence PZT film piezoelectric property.(2) will by machining process
PZT bulks are thinned to target thickness, are then prepared by micro fabrications such as photoetching, etchings by glue bond on a silicon substrate
Pattern.It has been the machining limit that PZT bulks are thinned into 100 μm, and yield rate is only 10%, and subsequent transfer was bonded
Journey is complicated, operating difficulties.
The content of the invention
The invention solves technical barrier be to overcome the shortcomings of above-mentioned technology, invent a kind of diffusion interlinked sides of PZT/Si
Method.First, electrode layer and PZT film are prepared on PZT bulks surface, forms PZT element；Then, under the conditions of certain temperature, pass through
Pressure is applied to PZT element and silicon substrate, makes the lead element in PZT film that diffusion reaction occur with silicon and forms diffusion interlinked layer, from
And realize the firm combination of PZT element/silicon；Finally, using subsequent mechanical grinding and glossing, the PZT of thickness needed for acquisition
Piezoelectric layer.Bonding pattern PZT/Si bond strength is high, technique is simple, easy to implement, cost is low, and being promoted beneficial to commercialization should
With.
Technical scheme：
A kind of diffusion interlinked methods of PZT/Si, first, electrode layer 2 is prepared on the surface of PZT bulks 1, and on the surface of electrode layer 2
PZT film 3 is deposited, forms PZT element；Then, under the conditions of certain temperature, by applying pressure to PZT element and silicon substrate 4,
Make the lead element in PZT film 3 that diffusion reaction occur with silicon, form the diffusion interlinked layer with certain depth and high-bond, from
And realize the firm combination of PZT element/silicon；Finally, using subsequent mechanical grinding and glossing, the PZT of thickness needed for acquisition
Piezoelectric layer.
Comprise the following steps that：
1) surface preparation of PZT bulks
First, mechanical lapping polishing is carried out to PZT bulks 1, is allowed to surface smoothness and is less than 800nm, roughness is
100~500nm, to meet that electrode layer sputtering requires；Then, the surface attachment of PZT bulks 1 is removed using acetone, deionized water
Organic impurities；Finally, oil removal treatment is carried out to PZT bulks 1 using degreasing fluid, removes the surface saponification oil of PZT bulks 1 and mineral
Oil；
2) preparation of electrode layer and PZT film
Bottom working electrode of the surface sputtering electrode layer 2 of PZT bulks 1 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 bulks 1, electrode layer 2 and PZT film 3 form PZT element；
3) surface preparation of PZT element and silicon substrate
For PZT element, first, mechanical lapping polishing is carried out to PZT film 3, surface smoothness is allowed to and is less than
600nm, roughness are less than 500nm, to meet that bonding requires；Then, the surface attachment of PZT film 3 is removed using acetone, deionized water
Organic impurities；Finally, oil removal treatment is carried out to PZT element using degreasing fluid, removes the saponified oil and mineral on the surface of PZT film 3
Oil；
For silicon substrate 4, cleaned by RCA standard cleaning methods, 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 is incubated 10~60min, completes 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 glossing, to PZT element
PZT bulks 1 carry out reduction processing, the PZT piezoelectric layers of thickness needed for acquisition.Meanwhile PZT piezoelectric layer surface flatness is less than
800nm, roughness are 100~500nm.
Described electrode layer 2 sputters at PZT bulks 1 including Ti electrode layer 2-1 and Pt electrode layer 2-2, Ti electrode layers 2-1
Surface, Pt electrode layers 2-2 sputter at Ti electrode layers 2-1 surface.
Described 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 methods of PZT/Si, first, is made on PZT bulks
Standby electrode layer and PZT film, form PZT element；Then, under the conditions of certain temperature, pressed by applying to PZT element and silicon substrate
Power forms diffusion interlinked layer, realizes the firm combination of PZT element/silicon；Finally, using subsequent mechanical grinding and glossing, obtain
The PZT piezoelectric layers of thickness needed for obtaining.Bonding pattern PZT/Si bond strength is high, technique is simple, easy to implement, cost is low,
Beneficial to commercialization popularization and application.
Brief description of the drawings
Fig. 1 is the diffusion interlinked method schematic diagrams of PZT/Si.
Fig. 2 is the diffusion interlinked method process route charts of PZT/Si.
In figure：1PZT bulks；2-1Ti electrode layers；2-2Pt electrode layers；3PZT films；4 silicon substrates；
The processing of 5PZT bulks grinding and polishing；6PZT bulks surface sputtering electrode layer；
It is prepared by 7PZT bulk electrode layer surfaces PZT film；8PZT element grinding polishings；
9PZT elements are bonded with silicon substrate High temperature diffusion；10PZT element reduction processings.
Embodiment
Describe the embodiment of the present invention in detail below in conjunction with technical scheme and accompanying drawing.
First, polishing, decontamination and oil removal treatment are ground to PZT bulks；Then, Ti is sputtered on PZT bulks surface
Electrode and Pt electrodes, and certain thickness PZT film is deposited in Pt electrode surfaces, PZT bulks, electrode layer and PZT film constitute PZT
Element.The diffusion interlinked processes of PZT/Si are：Under the conditions of certain temperature, by applying pressure to PZT element and silicon substrate, make
PZT film and silicon generation are diffusion interlinked, realize the firm combination of PZT element/silicon；Finally, subsequent mechanical grinding and buffer are utilized
Skill, the PZT piezoelectric layers of thickness needed for acquisition.
The specific implementation step of embodiment is as follows：
1) surface preparation of PZT bulks
The model PZT-5H of PZT bulks 1 in the present embodiment, size are 10mm × 7mm × 1mm (length × width x thickness).First,
Mechanical lapping polishing is carried out to it, surface smoothness is allowed to and respectively reaches 500nm and 300nm with roughness, to meet electricity
Pole sputtering requires；Then, using 10min is cleaned by ultrasonic successively under acetone, ethanol, deionized water, trichloro ethylene normal temperature, to remove
The organic impurities of surface attachment；Finally, at a temperature of 30~40 DEG C, carry out 5~10min using degreasing fluid and be 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 bulks 1, bottom of the electrode layer 2 as PZT element need to be prepared on the surface of PZT bulks 1
Portion's working electrode, to increase the bond strength of electrode and PZT bulks 1, first by magnetically controlled sputter method on the surface of PZT bulks 1
The thick Ti electrode 2-1 of 30nm are sputtered, then in Pt electrodes 2-2 thick Ti electrode 2-1 surfaces sputtering 200nm.Complete the table of PZT bulks 1
After the preparation of face electrode layer 2, deposition (Electrohydrodynamic atomization deposition) is printed using EFI
The PZT film 3 that technology deposits 50 μ m-thicks on the surface of electrode layer 2 is used as bonded layer.PZT bulks 1, electrode layer 2 and PZT film 3 constitute
PZT element；
3) surface preparation of PZT element and silicon substrate
Before PZT/Si diffusion interlinked technique is implemented, surface preparation need to be carried out to PZT element and silicon substrate 4.For
PZT element, first, mechanical lapping polishing need to be carried out to PZT film 3, be allowed to surface smoothness and respectively reached with roughness
500nm and 300nm, to meet that bonding requires；Then, it is clear using ultrasound under acetone, ethanol, deionized water, trichloro ethylene normal temperature
10min is washed, removes the organic impurities of surface attachment；Finally, at a temperature of 30~40 DEG C, carry out 5~10min using degreasing fluid and surpass
Sonication, to remove surface saponification oil and mineral oil；
For silicon substrate 4, cleaned using preceding by RCA standard cleaning methods, to remove the impurity of surface attachment.This reality
It is single-sided polishing monocrystalline silicon piece to apply the silicon chip selected in example, and size is 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 2.5kg stainless steel counterweight
(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/min heating rate is gradually heating to 800 DEG C, and is incubated 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 glossing, to PZT bulks
1 carries out reduction processing, until the thickness of PZT bulks 1 reaches about 200 μm, surface smoothness and roughness respectively reach 500nm and
300nm, complete the preparation of PZT piezoelectric layers.
The present invention proposes a kind of diffusion interlinked methods of PZT/Si.First, electrode layer 2, and profit are prepared on the surface of PZT bulks 1
Electricity consumption spray printing deposition technique deposits on the surface of electrode layer 2 and prepares PZT film 3, forms PZT element；Then, in certain temperature condition
Under, by applying pressure to PZT element and silicon substrate 4, PZT film 3 is occurred with silicon diffusion interlinked, realize the steady of PZT element/silicon
Consolidation is closed；Finally, subsequent mechanical grinding and glossing, the PZT piezoelectric layers of thickness needed for acquisition are utilized.Bonding pattern PZT/
Si bond strength is high, technique is simple, easy to implement, cost is low, beneficial to commercialization popularization and application.
Claims (3)
- A kind of 1. diffusion interlinked methods of PZT/Si, it is characterised in that step is as follows：1) surface preparation of PZT bulksFirst, mechanical lapping polishing is carried out to PZT bulks (1), is allowed to surface smoothness and is less than 800nm, roughness 100 ~500nm, to meet that electrode layer sputtering requires；Then, having for PZT bulk (1) surface attachments is removed using acetone, deionized water Machine impurity；Finally, oil removal treatment is carried out to PZT bulks (1) using degreasing fluid, removes PZT bulks (1) surface saponification oil and mineral Oil；2) preparation of electrode layer and PZT filmBottom working electrode of PZT bulks (1) the surface sputtering electrode layer (2) as PZT element after the pre-treatment；In electrode layer (2) PZT film (3) of 10~70 μ m-thicks of surface deposition is used as bonded layer；PZT bulks (1), electrode layer (2) and PZT film (3) are formed PZT element；3) surface preparation of PZT element and silicon substrateFor PZT element, first, mechanical lapping polishing is carried out to PZT film (3), surface smoothness is allowed to and is less than 600nm, Roughness is less than 500nm, to meet that bonding requires；Then, having for PZT film (3) surface attachment is removed using acetone, deionized water Machine impurity；Finally, oil removal treatment is carried out to PZT element using degreasing fluid, removes the saponified oil and mineral oil on PZT film (3) surface；For silicon substrate (4), cleaned by RCA standard cleaning methods, to remove the impurity of surface attachment；4) PZT element is bonded with the High temperature diffusion of silicon substrate5~30N 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 is incubated 10~60min, the high temperature for completing PZT element and silicon substrate (4) expands Dissipate bonding；5) reduction processing of PZT elementAfter completion PZT element is bonded with the High temperature diffusion of silicon substrate (4), using mechanical lapping and glossing, to PZT element PZT bulks (1) carry out reduction processing, the PZT piezoelectric layers of thickness needed for acquisition；Meanwhile PZT piezoelectric layer surface flatness is less than 800nm, roughness are 100~500nm.
- 2. the diffusion interlinked methods of PZT/Si according to claim 1, it is characterised in that described electrode layer (2) includes Ti Electrode layer (2-1) and Pt electrode layers (2-2), Ti electrode layers (2-1) sputter at the surface of PZT bulks (1), Pt electrode layers (2-2) Sputter at Ti electrode layers (2-1) surface.
- 3. the diffusion interlinked methods of PZT/Si according to claim 1 or 2, it is characterised in that described Ti electrode layers (2-1) Thickness is 20~50nm, and Pt electrode layers (2-2) thickness is 100~500nm.
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Citations (4)
| 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 |
| US20010051436A1 (en) * | 1999-12-27 | 2001-12-13 | Kim Hong Koo | Fabrication method and structure for ferroelectric nonvolatile memory field effect transistor |
| 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 |
-
2017
- 2017-08-03 CN CN201710653766.3A patent/CN107482114B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010051436A1 (en) * | 1999-12-27 | 2001-12-13 | Kim Hong Koo | Fabrication method and structure for ferroelectric nonvolatile memory field effect transistor |
| 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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