CN109761605A - One kind having the PZT thin film and preparation method thereof of (100) preferable grain orientation - Google Patents
One kind having the PZT thin film and preparation method thereof of (100) preferable grain orientation Download PDFInfo
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Abstract
One kind having the PZT thin film and preparation method thereof of (100) preferable grain orientation, belongs to piezoelectric material film preparation field.Preparation step: 1) raw material butyl titanate being added in acetylacetone,2,4-pentanedione, and raw acetic acid lead and zirconium nitrate is added after stirring clarification, adds ethylene glycol monomethyl ether, finally adds formamide, and preparing chemical formula is Pbx(ZryTi1‑y)O3Lead zirconate titanate seed layer precursor solution；2) lead zirconate titanate seed layer precursor solution is deposited on Pt/Ti/SiO2It on/Si substrate, and is heat-treated, lead zirconate titanate seed layer is prepared in repeated deposition and heat treatment step；3) amorphous state pzt thin film is obtained by r. f. magnetron sputtering in lead zirconate titanate seed layer, then after heat treatment obtains the PZT thin film of (100) preferred orientation.The PZT thin film of (100) preferable grain orientation and excellent electrical property can be made using the method for the present invention.
Description
Technical field
The invention belongs to piezoelectric material film preparation fields, are related to a kind of zirconium metatitanic acid with (100) preferable grain orientation
Thin film lead and preparation method thereof.
Background technique
The chemical formula of lead zirconate titanate (abbreviation PZT) is Pb (ZryTi1-y)O3, it is ABO3Type Perovskite Phase compound has good
Good dielectric, ferroelectricity and piezoelectric property.Lead zirconat-titanato material has been widely used for RAM device and microelectron-mechanical
In system, such as microactrator, microsensor etc., execution unit is largely using the material as driving part.In view of micro-
Mechatronic Systems has many characteristics, such as microsize, therefore it is required that the thickness of PZT material range in the micron-scale.The preparation side of piezoelectric membrane
Method mainly has: pulsed laser deposition, hydro-thermal method, electrospray, metal organic chemical vapor deposition method, sol-gel method and sputtering
Method.
In order to which the PZT thin film of (100) preferred orientation and excellent electrical property is prepared, doping vario-property is generallyd use
Or the methods of sputtering kind crystal layer.Doping vario-property is metallic element of the addition in addition to Pb, Zr, Ti, doped chemical into PZT material
Replace perovskite structure the position A or B, improve the electrical property of PZT material by generation lead vacancy or compensation Lacking oxygen.It compares
Sol-gel method, when preparing doped PZT film using sputtering method, there are doped chemical component is not easy to control when making target, and
Target production amount leads to problems such as greatly the period longer.Sputtering kind crystal layer is usually to sputter one layer and pzt thin film in advance on substrate
For the more matched material of lattice as kind of a crystal layer, kind seed layer materials for example can be SrRuO3、LaNiO3, PbO etc..
In recent years, there is the lead zirconate titanate seed layer of (100) orientation using sol-gel method production, pulse is recycled to swash
Light deposition is come the excellent PZT thin film of dielectric and piezoelectric properties is prepared is also one of research hotspot.For example, Wang Zhanjie
Deng using PLD and sol-gel group technology in Pt/Ti/SiO2Growth in situ pzt thin film in/Si substrate, they have found PZT
The preferred orientation of film can be controlled by basal layer prepared by sol-gel method (referring to Z.J.Wang, H.Kokawa,
R.Maeda,In situ growth of lead zirconate titanate thin films by hybrid
process:sol–gel method and pulsed-laser deposition,Acta Materialia,53,2005,pp
593-600).However the pzt thin film component and the component of sol-gel substrate PZT of PLD method deposition are consistent in their experiments
, in addition the content of substrate Pb element also has influence strongly to the nucleation and growth of subsequent pzt thin film, therefore studies kind
Influence of the sublayer Pb constituent content to rear sputtering sedimentation pzt thin film performance is extremely important.
Summary of the invention
The present invention is intended to provide a kind of PZT thin film and preparation method thereof with (100) preferable grain orientation, it should
The PZT thin film of (100) preferred orientation and excellent electrical property can be made in method.
Technical solution of the present invention:
One kind having the preparation method of the PZT thin film of (100) preferable grain orientation, includes the following steps:
1) raw material butyl titanate is added in acetylacetone,2,4-pentanedione, raw acetic acid lead and zirconium nitrate is added after stirring clarification, then
Ethylene glycol monomethyl ether is added as solvent, finally adds stabilizer formamide, preparing chemical formula is Pbx(ZryTi1-y)O3Zirconium titanium
Lead plumbate seed layer precursor solution, wherein x is 1.1-1.3, y 0.4-0.5；
2) lead zirconate titanate seed layer precursor solution is deposited on Pt/Ti/SiO2It on/Si substrate, and is heat-treated, weight
Multiple deposition and heat treatment step, are prepared the lead zirconate titanate seed layer with a thickness of 150-220nm；
3) amorphous state pzt thin film is obtained by r. f. magnetron sputtering in lead zirconate titanate seed layer, amorphous state PZT is thin
Film after heat treatment obtains the PZT thin film of (100) preferred orientation again, PZT thin film with a thickness of 600-1000nm.
Method of the invention uses above-mentioned specific raw material, solvent and stabilizer, is prepared using sol-gel method different
The lead zirconate titanate seed layer of Pb content, then use rf magnetron sputtering in the lead zirconate titanate seed layer and Pt/Ti/ of different Pb contents
SiO2The PZT thin film different with the seed layer component is prepared in/Si substrate, can be obviously improved PZT thin film
Dielectric and ferroelectric properties.
Further, in step 1), when preparing the lead zirconate titanate seed layer precursor solution, can control lead acetate,
Molar ratio between zirconium nitrate, butyl titanate, acetylacetone,2,4-pentanedione and formamide is (1.1-1.3): y:(1-y): (0.7-1.2):
(1.8-2.4).Wherein, (1.1-1.3) indicates that lead component is excessive when preparing the lead zirconate titanate seed layer precursor solution
10%-30%, excessive purpose are that the loss of lead in lead zirconate titanate seed layer heat treatment process is prepared for compensation；In particular,
The lead excessive amount can also compensate the lead loss in the heat treatment of sputtering sedimentation PZT thin film, to be conducive to improve zirconium metatitanic acid
The microstructure and electrical property of thin film lead.
Further, the pH value of the lead zirconate titanate seed layer precursor solution is 3.8-5.5, wherein Pbx(ZryTi1-y)
O3Concentration be 0.25-0.50mol/L.
Further, in step 2), the lead zirconate titanate seed layer precursor solution is sunk using conventional method in that art
On substrate, deposition method for example may include: by the lead zirconate titanate seed layer precursor solution at 600-800 revs/min to product
Spin coating 8-14 seconds under clock, then rejection film 20-36 seconds on substrate under 2700-3500 revs/min.Aforesaid way can make zirconium metatitanic acid
Lead seed layer precursor solution uniform fold is over the substrate.The heat treatment includes: first 5-8 dry at 120-180 DEG C
Minute；Then it is thermally decomposed 4-8 minutes at 350-450 DEG C；It is made annealing treatment 10-15 minutes at 600-700 DEG C again.The progress
Heat treatment lead zirconate titanate seed layer can be made to form fine and close perovskite structure.
Further, in step 3), using rf magnetron sputtering in the resulting lead zirconate titanate seed layer of step 2) and Pt/
Ti/SiO2Pzt thin film is prepared in/Si substrate, closes heater after sample stage is heated to 80-120 DEG C before deposition, is dropped to temperature
Start sputtering sedimentation when to 50-80 DEG C: being passed through Ar and O2Mixed gas controls Ar and O2Flow-ratio control is in (90/1)-(90/
10)；Deposition pressure 1-2Pa, sputtering power 100W are adjusted, chip bench drives substrate to rotate with the constant rotational speed of 2-6rpm, control
It sedimentation time 2-3 hours, takes out and is heat-treated immediately after thin film sputtering deposition.Heat treatment process packet after the sputtering
It includes: first film rapidly pre-warming being handled 3-8 minutes at 350-450 DEG C, then is made annealing treatment 20-60 minutes at 550-650 DEG C.
Substrate of the invention can be typical substrate, such as Pt/Ti/SiO2/ Si substrate；In particular, the substrate is warp
The Pt/Ti/SiO of 120-180 DEG C of drying 8-20 minutes2/ Si substrate.Before the deposition to Pt/Ti/SiO2/ Si substrate is dried
Moisture solution is removed, is conducive to improve the bond strength between substrate and film.The substrate can be by a si substrate with warm
The conventional methods such as oxidation form SiO2Layer, then with conventional methods such as d.c. sputterings in SiO2Ti layers and Pt layers are formed on layer, are made
Above-mentioned Pt/Ti/SiO2/ Si substrate.
The present invention does not limit the target thickness of lead zirconate titanate seed layer and PZT thin film strictly, can be as needed
It reasonably selects, the target thickness of lead zirconate titanate seed layer can be 150-220 ran；The target thickness of PZT thin film
It can be 600-1000 ran.It is possible to further repeating said steps 2), until obtaining that there is the target thickness
Lead zirconate titanate seed layer.
The present invention also provides a kind of PZT thin films with (100) preferable grain orientation, according to any of the above-described described
Preparation method be made.
Further, the PZT thin film with (100) preferable grain orientation of the invention is perovskite structure；
(100) crystal orientation degree of orientation > 55%, further > 69%；Further >=85%.
Beneficial effects of the present invention:
1, preparation method of the invention avoids all using multiplicating deposition bring pollution when sol gel process
Problem；In particular, (100) preferred orientation of film can be significantly improved by using the lead zirconate titanate seed layer of different Pb contents
Degree, and can effectively inhibit Jiao Lvshi phase, as shown in Figure 7.
2, PZT thin film dielectric properties prepared by the present invention are excellent, and relative dielectric constant up to 918.26, damage by dielectric
Consumption is only 0.026, as shown in Figure 4 and Figure 6.
Detailed description of the invention
Fig. 1 is the XRD curve of PZT thin film prepared by embodiment 1；
Fig. 2 is the dielectric and magnetic curve of PZT thin film prepared by embodiment 1；
Fig. 3 is the XRD curve of PZT thin film prepared by embodiment 2；
Fig. 4 is the dielectric and magnetic curve of PZT thin film prepared by embodiment 2；
Fig. 5 is the XRD curve of PZT thin film prepared by reference examples 1；
Fig. 6 is the dielectric and magnetic curve of PZT thin film prepared by reference examples 1；
Fig. 7 is PZT thin film XRD curve combination figure；
Wherein: being (a) result figure of embodiment 2；It (c) is the result figure of reference examples 1；Pv indicates that Perovskite Phase, Py indicate
Jiao Lvshi phase.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention and attached
Figure, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention
A part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment provides the preparation method of the PZT thin film with (100) preferable grain orientation, specific steps are as follows:
S101, lead zirconate titanate seed layer precursor solution is prepared；
Ingredient is carried out according to seed layer lead element excessive 15%, 2.9mL butyl titanate is first dissolved in 1.6mL levulinic
In ketone, 40 DEG C are then warming up to, keeps the temperature 1 hour；Then, 3.12 grams of zirconium nitrates, 7.55 grams of lead acetates and 30mL second are sequentially added
Glycol methyl ether, sufficiently dissolves and stirs evenly, then is warming up to 80 DEG C, keeps the temperature 1 hour；1.8mL formamide is added, is stirred evenly, so
After be cooled to 40 DEG C, keep the temperature 1 hour；It is eventually adding the acetic acid solution that 11mL mass content is 36%, 1 hour is kept the temperature, obtains dense
Degree is 0.35mol/L or so, meets the lead zirconate titanate seed layer precursor solution of the stoichiometry.
The deposition and heat treatment of S102, seed layer；
Above-mentioned lead zirconate titanate seed layer precursor solution is first glue 10 seconds equal through 700 revs/min, then through 2700 revs/min
Spin coating rejection film 25 seconds, the lead zirconate titanate seed layer precursor solution is deposited on Pt/Ti/SiO2On/Si substrate.
By the wet film being deposited on substrate, heat is dried 6 minutes at 160 DEG C, then thermally decomposes 6 minutes at 400 DEG C, finally
It is made annealing treatment 12 minutes at 650 DEG C, obtains the lead zirconate titanate single layer seed layers that single layer thickness is 75 rans.
S102 repeat the above steps three times, the lead zirconate titanate seed layer with a thickness of 180 rans is prepared.
S103, sputtering sedimentation PZT thin film；
It is prepared in the lead zirconate titanate seed layer for the lead element excessive 15% that above-mentioned steps obtain using rf magnetron sputtering
Pzt thin film (target component Pb1.1(Zr0.60Ti0.40)O3), deposition is preceding to be evacuated to 3.0 × 10 for deposition chambers vacuum degree-5Pa, then lead to
Sample stage is heated to 120 DEG C by toning current, closes heater after 2 minutes, start to be passed through when temperature drops to 70 DEG C Ar with
O2Mixed gas, control Ar/O2Flow-rate ratio is 90/10；Then deposition chambers stable gas pressure is made to exist by adjusting throttle valve
1.5Pa.Then opening radio-frequency power supply and sputtering power is arranged is 100W, and chip bench drives substrate to revolve with the constant rotational speed of 5rpm
Turn, control sedimentation time is 2 hours or so, obtains the PZT thin film that thickness is about 800nm.
The heat treatment of S104, PZT thin film；
It takes out, first handles film rapidly pre-warming 6 minutes at 400 DEG C, then at 600 DEG C immediately after thin film sputtering deposition
Lower annealing 40 minutes.
The XRD curve and room temperature dielectric spectrum curve of above-mentioned PZT thin film are shown in Fig. 1 and Fig. 2 respectively；As shown in Figure 1,
Above-mentioned PZT thin film shows as pure perovskite structure, wherein (100) degree of orientation of crystal orientation can be calculated by formula (1):
In formula (1), α is the degree of orientation of (100) crystal orientation, I(100)、I(110)And I(111)Respectively (100), (110) and (111)
The peak intensity of crystal orientation；It is computed, the degree of orientation of above-mentioned film (100) crystal orientation is 69%.
In addition, the dielectric constant of PZT thin film is calculated by formula (2):
In formula (2), εyFor relative dielectric constant, C is the capacitor that PZT thin film measures, and d is film thickness, ε0It is true
Empty dielectric constant, A are the electrode area of film.It is computed, above-mentioned PZT thin film is when frequency is 0.1kHz, opposite dielectric
Constant is 819.68, dielectric loss 0.035.
Embodiment 2
The present embodiment provides the preparation method of the PZT thin film with (100) preferable grain orientation, specific steps are as follows:
S201, lead zirconate titanate seed layer precursor solution is prepared；
Ingredient is carried out according to seed layer lead element excessive 30%, 6.3mL butyl titanate is first dissolved in 3.9mL levulinic
In ketone, 55 DEG C are then warming up to, keeps the temperature 70 minutes；Then, sequentially add 8.69 grams of zirconium nitrates, 14.61 grams of lead acetates and
35mL ethylene glycol monomethyl ether, sufficiently dissolves and stirs evenly, then is warming up to 105 DEG C, keeps the temperature 70 minutes；3.4mL formamide is added,
It stirs evenly, is then cooled to 55 DEG C, keep the temperature 70 minutes；It is eventually adding the acetic acid solution that 18mL mass content is 36%, keeps the temperature 70 points
Clock, obtaining concentration is 0.38mol/L or so, meets the lead zirconate titanate seed layer precursor solution of the stoichiometry.
The deposition and heat treatment of S202, seed layer；
Above-mentioned lead zirconate titanate seed layer precursor solution is first glue 9 seconds equal then even through 3000 revs/min through 750 revs/min
Glue rejection film 20 seconds, the lead zirconate titanate seed layer precursor solution is deposited on Pt/Ti/SiO2On/Si substrate.
By the wet film being deposited on substrate, heat is dried 6 minutes at 160 DEG C, then thermally decomposes 6 minutes at 450 DEG C, finally
It is made annealing treatment 12 minutes at 650 DEG C, obtains the lead zirconate titanate single layer seed layers that single layer thickness is 75 rans.
S102 repeat the above steps three times, the lead zirconate titanate seed layer with a thickness of 200 rans is prepared.
S203, sputtering sedimentation PZT thin film；
It is prepared in the lead zirconate titanate seed layer for the lead element excessive 30% that above-mentioned steps obtain using rf magnetron sputtering
Pzt thin film (target component Pb1.1(Zr0.60Ti0.40)O3), deposition is preceding to be evacuated to 3.0 × 10 for deposition chambers vacuum degree-5Pa, then lead to
Sample stage is heated to 100 DEG C by toning current, closes heater after 2 minutes, start to be passed through when temperature drops to 80 DEG C Ar with
O2Mixed gas, control Ar/O2Flow-rate ratio is 90/5；Then make deposition chambers stable gas pressure in 2Pa by adjusting throttle valve.
Then opening radio-frequency power supply and sputtering power is arranged is 100W, and chip bench drives substrate to rotate with the constant rotational speed of 5rpm, control
Sedimentation time is 2 hours or so, obtains the PZT thin film that thickness is about 800nm.
The heat treatment of S204, PZT thin film；
It takes out, first handles film rapidly pre-warming 8 minutes at 350 DEG C, then at 650 DEG C immediately after thin film sputtering deposition
Lower annealing 30 minutes.
The XRD curve and dielectric and magnetic curve of above-mentioned PZT thin film are shown in Fig. 3 and Fig. 4 respectively.As can be seen from figs. 3 and 4:
Above-mentioned PZT thin film mainly along (100) crystal orientation oriented growth, shows as pure perovskite structure, counts according to above-mentioned formula (1)
The degree of orientation of film (100) crystal orientation of calculation is 85%.
In addition, calculating opposite dielectric of the above-mentioned PZT thin film when frequency is 0.1kHz according to above-mentioned formula (2)
Constant is 918.26, dielectric loss 0.026.
Reference examples 1
It is different from Examples 1 and 2, lead zirconate titanate seed layer is free of in this reference examples.The specific steps of the present embodiment are as follows:
1, sputtering sedimentation PZT thin film；
Using rf magnetron sputtering in Pt/Ti/SiO2Pzt thin film (target component Pb is prepared in/Si substrate1.1
(Zr0.60Ti0.40)O3), deposition is preceding to be evacuated to 3.0 × 10 for deposition chambers vacuum degree-5Pa, then added sample stage by adjusting electric current
Heat starts to be passed through Ar and O when temperature drops to 80 DEG C to heater is closed after 100 DEG C, 2 minutes2Mixed gas, control Ar/O2
Flow-rate ratio is 90/5；Then make deposition chambers stable gas pressure in 2Pa by adjusting throttle valve.Then it opens radio-frequency power supply and is arranged
Sputtering power is 100W, and chip bench drives substrate to rotate with the constant rotational speed of 5rpm, and control sedimentation time is 2 hours or so, is obtained
The PZT thin film for being about 800nm to thickness.
2, the heat treatment of PZT thin film；
It takes out, first handles film rapidly pre-warming 8 minutes at 350 DEG C, then at 650 DEG C immediately after thin film sputtering deposition
Lower annealing 30 minutes.
The XRD curve and dielectric and magnetic curve of above-mentioned PZT thin film are shown in Fig. 5 and Fig. 6 respectively.From Fig. 5 and Fig. 6:
Above-mentioned PZT thin film mainly along (100) crystal orientation oriented growth, is mainly shown as perovskite structure, but there are part Jiao Lvshi
Phase.The degree of orientation of film (100) crystal orientation calculated according to above-mentioned formula (1) is 79%.
In addition, PZT thin film XRD curve combination figure prepared by embodiment 2 and reference examples 1 is shown in that Fig. 7, Fig. 7 (c) show
There is Jiao Lvshi phase at about 28.5 and 36 degree of the angle of diffraction in PZT thin film prepared by reference examples 1, and makes in embodiment 2
Similar Jiao Lvshi phase is not detected in standby PZT thin film, sees Fig. 7 (a).
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. the preparation method that one kind has the PZT thin film of (100) preferable grain orientation, which is characterized in that including walking as follows
It is rapid:
1) raw material butyl titanate is added in acetylacetone,2,4-pentanedione, raw acetic acid lead and zirconium nitrate is added after stirring clarification, adds
Ethylene glycol monomethyl ether finally adds stabilizer formamide as solvent, and preparing chemical formula is Pbx(ZryTi1-y)O3Lead zirconate titanate
Seed layer precursor solution, wherein x is 1.1-1.3, y 0.4-0.5；
2) lead zirconate titanate seed layer precursor solution is deposited on Pt/Ti/SiO2It on/Si substrate, and is heat-treated, it is heavy to repeat
Long-pending and heat treatment step, is prepared the lead zirconate titanate seed layer with a thickness of 150-220nm；
3) amorphous state pzt thin film is obtained by r. f. magnetron sputtering in lead zirconate titanate seed layer, amorphous state pzt thin film is again
After heat treatment obtain the PZT thin film of (100) preferred orientation, PZT thin film with a thickness of 600-1000nm.
2. a kind of preparation method of PZT thin film with (100) preferable grain orientation according to claim 1,
It is characterized in that, in the step 1), when preparing lead zirconate titanate seed layer precursor solution, controls lead acetate, zirconium nitrate, metatitanic acid four
Molar ratio between butyl ester, acetylacetone,2,4-pentanedione and formamide is (1.1-1.3): y:(1-y): (0.7-1.2): (1.8-2.4).
3. a kind of preparation side of PZT thin film with (100) preferable grain orientation according to claim 1 or 2
Method, which is characterized in that the pH value of the lead zirconate titanate seed layer precursor solution is 3.8-5.5, Pbx(ZryTi1-y)O3Concentration
For 0.25-0.50mol/L.
4. a kind of preparation side of PZT thin film with (100) preferable grain orientation according to claim 1 or 2
Method, which is characterized in that in the step 2), deposition method are as follows: by the lead zirconate titanate seed layer precursor solution in 600-800
Revs/min lower spin coating 8-14 seconds, then in Pt/Ti/SiO under 2700-3500 revs/min2Rejection film 20-36 seconds on/Si substrate；Heat
Processing method particularly includes: Pt/Ti/SiO2Wet film on/Si substrate is first 5-8 minutes dry at 120-180 DEG C；Then exist
It is thermally decomposed 4-8 minutes at 350-450 DEG C；It is made annealing treatment 10-15 minutes at 600-700 DEG C again.
5. a kind of preparation method of PZT thin film with (100) preferable grain orientation according to claim 3,
It is characterized in that, in the step 2), deposition method are as follows: by the lead zirconate titanate seed layer precursor solution at 600-800 revs/min
Spin coating 8-14 seconds under clock, then in Pt/Ti/SiO under 2700-3500 revs/min2Rejection film 20-36 seconds on/Si substrate；Heat treatment
Method particularly includes: Pt/Ti/SiO2Wet film on/Si substrate is first 5-8 minutes dry at 120-180 DEG C；Then in 350-
It is thermally decomposed 4-8 minutes at 450 DEG C；It is made annealing treatment 10-15 minutes at 600-700 DEG C again.
6. according to right want 1,2 or 5 described in one kind have (100) preferable grain orientation PZT thin film preparation side
Method, which is characterized in that in the step 3), close heater after sample stage is heated to 80-120 DEG C before deposition, dropped to temperature
Start sputtering sedimentation, deposition pressure 1-2Pa, sputtering power 100W when to 50-80 DEG C, deposition atmosphere is Ar and O2, Ar and O2Flow
Than controlling in 90/1-90/10；Chip bench drives substrate to rotate with the constant rotational speed of 2-6rpm, and sedimentation time 2-3 hours, deposition
It takes out and is heat-treated immediately afterwards.
7. a kind of preparation method of PZT thin film with (100) preferable grain orientation according to claim 3, special
Sign is, in the step 3), closes heater after sample stage is heated to 80-120 DEG C before deposition, drops to 50-80 to temperature
DEG C when start sputtering sedimentation, deposition pressure 1-2Pa, sputtering power 100W, deposition atmosphere are Ar and O2, Ar and O2Flow-ratio control
In 90/1-90/10；Chip bench drives substrate to rotate with the constant rotational speed of 2-6rpm, and sedimentation time 2-3 hours, after deposition immediately
Taking-up is heat-treated.
8. according to right want 4 described in one kind have (100) preferable grain orientation PZT thin film preparation method, it is special
Sign is, in the step 3), closes heater after sample stage is heated to 80-120 DEG C before deposition, drops to 50-80 to temperature
DEG C when start sputtering sedimentation, deposition pressure 1-2Pa, sputtering power 100W, deposition atmosphere are Ar and O2, Ar and O2Flow-ratio control
In 90/1-90/10；Chip bench drives substrate to rotate with the constant rotational speed of 2-6rpm, and sedimentation time 2-3 hours, after deposition immediately
Taking-up is heat-treated.
9. according to claim 1, preparation method described in 2,5,7 or 8, which is characterized in that in the step 3), heat treatment method
Are as follows: first film rapidly pre-warming is handled 3-8 minutes at 350-450 DEG C；Then 20-60 points are made annealing treatment at 550-650 DEG C
Clock.
10. the PZT thin film that one kind has (100) preferable grain orientation, which is characterized in that any according to claim 1-9
The preparation method is made, which is perovskite structure；(100) crystal orientation degree of orientation > 55%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110112285A (en) * | 2019-05-22 | 2019-08-09 | 大连瑞林数字印刷技术有限公司 | A kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode |
| CN111081864A (en) * | 2020-01-02 | 2020-04-28 | 大连理工大学 | Preparation method of (100) preferred orientation PMN-PZT/PZT heterostructure thin film |
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| CN111081864A (en) * | 2020-01-02 | 2020-04-28 | 大连理工大学 | Preparation method of (100) preferred orientation PMN-PZT/PZT heterostructure thin film |
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