CN101532175A - Method for the annealing preparation of tantalum scandium acid plumbum-based ferroelectric film by two step method - Google Patents
Method for the annealing preparation of tantalum scandium acid plumbum-based ferroelectric film by two step method Download PDFInfo
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- CN101532175A CN101532175A CN 200910058467 CN200910058467A CN101532175A CN 101532175 A CN101532175 A CN 101532175A CN 200910058467 CN200910058467 CN 200910058467 CN 200910058467 A CN200910058467 A CN 200910058467A CN 101532175 A CN101532175 A CN 101532175A
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- ferroelectric film
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- scandium acid
- tantalum scandium
- acid plumbum
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Abstract
A method for the annealing preparation of a tantalum scandium acid plumbum-based ferroelectric film by a two step method is disclosed, comprising the technological steps of preparing a transition layer, preparing the tantalum scandium acid plumbum-based ferroelectric film and annealing the tantalum scandium acid plumbum-based ferroelectric film; annealing the tantalum scandium acid plumbum-based ferroelectric film comprises the steps of: putting the tantalum scandium acid plumbum-based ferroelectric film in an annealing furnace, heating up to 800-850 DEG C at a heating rate of 40 DEG C/s in an oxygen flow and then stopping heating up at once so that the tantalum scandium acid plumbum-based ferroelectric film is naturally cooled to 500-600 DEG C along with the furnace, preserving the heat for 3-5 minutes, and afterwards naturally cooling the ferroelectric film to room temperature along with the furnace. The tantalum scandium acid plumbum-based ferroelectric film prepared by the method has a perovskite phase purity capable of reaching 100%, good crystallization performance and low RMS roughness on the surface as well as also has the characteristic of high polarization intensity and high preferred orientation.
Description
Technical field
The present invention relates to a kind of method for preparing tantalum scandium acid plumbum-based ferroelectric film.
Background technology
Ferroelectric membranc has character such as ferroelectricity, piezoelectricity, pyroelectric effect, acoustooptic effect, photorefractive effect, non-linear optical effect, thereby can utilize a kind of character in these character to make the function device, also can make the function device by the character that cross-couplings fully utilizes two or more, can also combine with the functional effect of other material and make the integrated functionality device, boundless application prospect is arranged.
Tantalum scandium acid plumbum Pb (Sc
0.5Ta
0.5) O
3Ferroelectric membranc is the ferroelectric thin-flim materials with very high pyroelectric coefficient, but its Tc is very high.At present, the tantalum scandium acid plumbum-based ferroelectric film that has been widely studied adopts the method that is incubated down at high temperature (generally at 700～800 ℃) to carry out anneal to obtain the film of height crystallization mostly.Because the Si based semiconductor device can be destroyed under such high temperature, therefore, is difficult to realize the integrated of tantalum scandium acid plumbum-based ferroelectric film and Si based semiconductor device.Moreover because plumbous fusing point lower (327 ℃) and volatile, insulation annealing easily causes plumbous a large amount of volatilization losses under the high temperature, dephasign occurs thereby often cause the composition of tantalum scandium acid plumbum base film to depart from, and influences the performance of tantalum scandium acid plumbum base film.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film is provided, with the composition skew problem of solution tantalum scandium acid plumbum-based ferroelectric film, and help realizing the integrated of tantalum scandium acid plumbum-based ferroelectric film and Si based semiconductor device.
The major technique skill scheme that realizes the object of the invention is: when tantalum scandium acid plumbum-based ferroelectric film is annealed, adopt the certain high temperature (being the required temperature of conventional annealing technology) that is rapidly heated earlier not to be incubated, immediately temperature is reduced by 200 ℃～300 ℃ two-step approach rta techniques that are incubated then.Can avoid at high temperature long-time insulation to cause plumbous a large amount of losses and Si based semiconductor device destroyed like this.
The method of two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film of the present invention, processing step comprise the anneal of preparation transition layer, preparation tantalum scandium acid plumbum-based ferroelectric film, tantalum scandium acid plumbum-based ferroelectric film; The anneal of tantalum scandium acid plumbum-based ferroelectric film is that tantalum scandium acid plumbum-based ferroelectric film is put into annealing furnace, at once stop heating after in Oxygen Flow, being warming up to 800 ℃～850 ℃ with 40 ℃/second temperature rise rate, make it cool to 500 ℃～600 ℃ insulations 3 minutes～5 minutes with the furnace, cool to room temperature (temperature-time diagram of annealing process is seen Fig. 1) then with the furnace.
In the aforesaid method, the preparation transition layer is with Pt/Ti/SiO
2/ Si is a substrate, and the material of transition layer is La
0.5Sr
0.5CoO
3Or LaNiO
3Or SrRuO
3, their lattice parameter is between tantalum scandium acid plumbum and substrate and have a perovskite structure.The method for preparing transition layer has methods such as sol-gel method, sputtering method, pulsed laser deposition, molecular beam epitaxy, the present invention selects sputtering method for use, after sputter finishes, the substrate that has deposited transition layer is packed in the annealing furnace, be warming up to 650 ℃ of insulation 1min with 40 ℃/s temperature rise rate, cool to room temperature then with the furnace.
In the aforesaid method, the preparation tantalum scandium acid plumbum-based ferroelectric film is a sputter tantalum scandium acid plumbum-based ferroelectric film on the substrate that has deposited transition layer, and sputtering condition is as follows:
Base vacuum degree≤3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2With the throughput ratio of Ar be 1:4, sputtering pressure is 2Pa, sputtering power 60W, the temperature of substrate is controlled at 350 ℃～400 ℃ in the sputter procedure.
When adopting sputtering method to prepare transition layer and tantalum scandium acid plumbum-based ferroelectric film, sputtering time is by transition layer, the desired thickness decision of tantalum scandium acid plumbum-based ferroelectric film.
The present invention has following beneficial effect:
1, adopts the tantalum scandium acid plumbum-based ferroelectric film uhligite phase purity height of the method for the invention preparation, can reach 100%.
2, adopt the method for the invention, help realizing that tantalum scandium acid plumbum-based ferroelectric film and Si based semiconductor device are integrated.
3, not only crystal property is good for the tantalum scandium acid plumbum-based ferroelectric film of the method for the invention preparation, and surperficial r.m.s. roughness is lower, but also has the characteristics of remnant polarization height and height preferred orientation.
Description of drawings
Fig. 1 is the annealing process temperature-time diagram of tantalum scandium acid plumbum-based ferroelectric film in the method for the invention;
Fig. 2 is atomic force microscope (AFM) collection of illustrative plates of the tantalum scandium acid plumbum-based ferroelectric film of embodiment 1 preparation;
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of the tantalum scandium acid plumbum-based ferroelectric film of embodiment 1 preparation, and among the figure, LSCO is La
0.5Sr
0.5CoO
3Write a Chinese character in simplified form;
Fig. 4 is the ferroelectric hysteresis loop collection of illustrative plates of the tantalum scandium acid plumbum-based ferroelectric film of embodiment 1 preparation;
Fig. 5 is atomic force microscope (AFM) collection of illustrative plates of the tantalum scandium acid plumbum-based ferroelectric film of embodiment 2 preparations;
Fig. 6 is X-ray diffraction (XRD) collection of illustrative plates of the tantalum scandium acid plumbum-based ferroelectric film of embodiment 2 preparations, and among the figure, LSCO is La
0.5Sr
0.5CoO
3Write a Chinese character in simplified form.
Embodiment
Also in conjunction with the accompanying drawings the method for the invention and prepared tantalum scandium acid plumbum-based ferroelectric film are further described below by embodiment.
Among the following embodiment, used magnetic control sputtering device is the JGP560C10 type high vacuum multifunctional magnetic control sputtering device that Shenyang Scientific Instrument Factory, Chinese Academy of Sciences produces.
Embodiment 1
Present embodiment prepares 0.95Pb (Sc
0.5Ta
0.5) O
3-0.05PbTiO
3Ferroelectric membranc (being abbreviated as PSTT5), processing step is as follows:
(1) processing of substrate
Substrate is selected Pt/Ti/SiO for use
2/ Si, with substrate ultrasonic cleaning 5 minutes in toluene, ultrasonic cleaning 5 minutes in acetone again, ultrasonic cleaning 5 minutes in dehydrated alcohol at last.
(2) preparation transition layer
The preparation transition layer adopts sputtering method, will be fixed on the substrate position of sputter equipment through the substrate after step (1) is cleaned.Target is La
0.5Sr
0.5CoO
3, according to La
0.5Sr
0.5CoO
3Stoichiometric ratio raw materials weighing PbO, La
2O
3, Co
2O
3And SrCO
3, adopt the traditional ceramics synthesis technique that raw material is made target.Target is fixed on the target position of sputter equipment, the spacing of target and substrate is 5cm.Sputtering condition is as follows: the base vacuum degree is 3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2Flow be 10sccm, the flow of Ar is 40sccm, sputtering pressure is 2Pa, substrate temperature is controlled at 350 ℃, the substrate rotational velocity is 10 rev/mins, sputtering power is 60W, sputtering time is 2 hours, the about 180nm of the transition region thickness of formation.
After sputter finishes, take out the substrate that has deposited transition layer and pack in the quick anneal oven, be warming up to 650 ℃ of insulations 1 minute, cool to room temperature then with the furnace with 40 ℃ of/second temperature rise rates.
(3) preparation tantalum scandium acid plumbum-based ferroelectric film
The preparation tantalum scandium acid plumbum-based ferroelectric film adopts sputtering method, with the deposition after the anneal of step (2) preparation the substrate of transition layer be fixed on the substrate position of sputter equipment.Target is 0.95Pb (Sc
0.5Ta
0.5) O
3-0.05PbTiO
3, with plumbous oxide (PbO), titanium oxide (TiO
2), Scium trioxide (Sc
2O
3), tantalum oxide (Ta
2O
5) be raw material, according to 0.95Pb (Sc
0.5Ta
0.5) O
3-0.05PbTiO
3Stoichiometric ratio raw materials weighing PbO, the TiO of-0.1PbO (adding excessive 0.1PbO is the loss that is used for compensating Pb in the sintering)
2, Sc
2O
3, Ta
2O
5, adopt the traditional ceramics synthesis technique that raw material is made target.Target is fixed on the target position of sputter equipment the spacing 5cm of target and substrate.Sputtering condition is as follows: the base vacuum degree is 3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2Flow be 10sccm, the flow of Ar is 40sccm, sputtering pressure is 2Pa, substrate temperature is controlled at 350 ℃, the substrate rotational velocity that has deposited transition layer is 10 rev/mins, sputtering power is 60W, sputtering time is 2 hours, the about 500nm of the film thickness of formation.
(4) anneal of tantalum scandium acid plumbum-based ferroelectric film
The tantalum scandium acid plumbum-based ferroelectric film of step (3) preparation is put into quick anneal oven, at Oxygen Flow (flow: stop heating at once after being warming up to 800 ℃ with 40 ℃/second temperature rise rate 2L/min), make it cool to 550 ℃ (using 10 second time approximately) insulation 4 minutes with the furnace, insulation cools to room temperature with the furnace after finishing.
Present embodiment obtain is seen Fig. 2 through atomic force microscope (AFM) scanning (sweep limit is 1 μ m * 1 μ m) collection of illustrative plates of two-step approach annealed tantalum scandium acid plumbum-based ferroelectric film, and X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 3, and the ferroelectric hysteresis loop collection of illustrative plates is seen Fig. 4.As can be seen from Figure 2, the r.m.s. roughness of tantalum scandium acid plumbum-based ferroelectric film (RMS) is 4.065nm; As can be seen from Figure 3, tantalum scandium acid plumbum-based ferroelectric film has formed the film of the complete perovskite structure of height (220) orientation; The remnant polarization P of tantalum scandium acid plumbum-based ferroelectric film as can be seen from Figure 4
rBigger, 2P
rBe 25.4 μ C/cm
2, and coercive field E
cLess, 2E
cBe 175.4kV/cm.
Embodiment 2
Present embodiment prepares 0.95Pb (Sc
0.5Ta
0.5) O
3-0.05PbTiO
3Ferroelectric membranc (being abbreviated as PSTT5), processing step is as follows:
(1) processing of substrate
Substrate is selected Pt/Ti/SiO for use
2/ Si, its clean is identical with embodiment 1.
(2) preparation transition layer
The preparation transition layer adopts sputtering method, will be fixed on the substrate position of sputter equipment through the substrate after step (1) is cleaned.Target is La
0.5Sr
0.5CoO
3, according to La
0.5Sr
0.5CoO
3Stoichiometric ratio raw materials weighing PbO, La
2O
3, Co
2O
3And SrCO
3, adopt the traditional ceramics synthesis technique that raw material is made target.Target is fixed on the target position of sputter equipment, the spacing of target and substrate is 5cm.Sputtering condition is as follows: the base vacuum degree is 3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2Flow be 10sccm, the flow of Ar is 40sccm, sputtering pressure is 2Pa, substrate temperature is controlled at 400 ℃, the substrate rotational velocity is 10 rev/mins, sputtering power is 60W, sputtering time is 2 hours, the about 180nm of the transition region thickness of formation.
After sputter finishes, take out the substrate that has deposited transition layer and pack in the quick anneal oven, be warming up to 650 ℃ of insulations 1 minute, cool to room temperature then with the furnace with 40 ℃ of/second temperature rise rates.
(3) preparation tantalum scandium acid plumbum-based ferroelectric film
The preparation tantalum scandium acid plumbum-based ferroelectric film adopts sputtering method, with the deposition after the anneal of step (2) preparation the substrate of transition layer be fixed on the substrate position of sputter equipment.Target is 0.95Pb (Sc
0.5Ta
0.5) O
3-0.05PbTiO
3, with plumbous oxide (PbO), titanium oxide (TiO
2), Scium trioxide (Sc
2O
3), tantalum oxide (Ta
2O
5) be raw material, according to 0.95Pb (Sc
0.5Ta
0.5) O
3-0.05PbTiO
3Stoichiometric ratio raw materials weighing PbO, the TiO of-0.1PbO (adding excessive 0.1PbO is the loss that is used for compensating Pb in the sintering)
2, Sc
2O
3, Ta
2O
5, adopt the traditional ceramics synthesis technique that raw material is made target.Target is fixed on the target position of sputter equipment the spacing 5cm of target and substrate.Sputtering condition is as follows: the base vacuum degree is 3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2Flow be 10sccm, the flow of Ar is 40sccm, sputtering pressure is 2Pa, substrate temperature is controlled at 400 ℃, the substrate rotational velocity that has deposited transition layer is 10 rev/mins, sputtering power is 60W, sputtering time is 2 hours, the about 500nm of the film thickness of formation.
(4) anneal of tantalum scandium acid plumbum-based ferroelectric film
The tantalum scandium acid plumbum-based ferroelectric film of step (3) preparation is put into quick anneal oven, at Oxygen Flow (flow: stop heating at once after being warming up to 850 ℃ with 40 ℃/second temperature rise rate 2L/min), make it cool to 600 ℃ (using 10 second time approximately) insulation 3 minutes with the furnace, insulation cools to room temperature with the furnace after finishing.
Present embodiment obtain is seen Fig. 5 through atomic force microscope (AFM) scanning (sweep limit is 1 μ m * 1 μ m) collection of illustrative plates of two-step approach annealed tantalum scandium acid plumbum-based ferroelectric film, and X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 6.As can be seen from Figure 5, the r.m.s. roughness of tantalum scandium acid plumbum-based ferroelectric film (RMS) is 4.764nm; From 6 as can be seen, tantalum scandium acid plumbum-based ferroelectric film has formed the film of the complete perovskite structure of (220) orientations.
Claims (5)
1, a kind of method of two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film, processing step comprises the anneal of preparation transition layer, preparation tantalum scandium acid plumbum-based ferroelectric film, tantalum scandium acid plumbum-based ferroelectric film, the anneal that it is characterized in that tantalum scandium acid plumbum-based ferroelectric film is that tantalum scandium acid plumbum-based ferroelectric film is put into annealing furnace, at once stop heating after in Oxygen Flow, being warming up to 800 ℃～850 ℃ with 40 ℃/second temperature rise rate, make it cool to 500 ℃～600 ℃ insulations 3 minutes～5 minutes with the furnace, cool to room temperature then with the furnace.
2, the method for two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film according to claim 1, the material that it is characterized in that transition layer is La
0.5Sr
0.5CoO
3Or LaNiO
3Or SrRuO
3
3, the method for two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film according to claim 1 and 2, it is characterized in that preparing transition layer and adopt sputtering method, after sputter finishes, the substrate that has deposited transition layer is packed in the annealing furnace, be warming up to 650 ℃ of insulation 1min with 40 ℃/s temperature rise rate, cool to room temperature then with the furnace.
4, the method for two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film according to claim 1 and 2, it is characterized in that preparing tantalum scandium acid plumbum-based ferroelectric film is sputter tantalum scandium acid plumbum-based ferroelectric film on the substrate that has deposited transition layer, sputtering condition is as follows:
Base vacuum degree≤3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2With the throughput ratio of Ar be 1:4, sputtering pressure is 2Pa, sputtering power 60W, the temperature of substrate is controlled at 350 ℃～400 ℃ in the sputter procedure.
5, the method for two-step approach annealing preparation of tantalum scandium acid plumbum-based ferroelectric film according to claim 3, it is characterized in that preparing tantalum scandium acid plumbum-based ferroelectric film is sputter tantalum scandium acid plumbum-based ferroelectric film on the substrate that has deposited transition layer, sputtering condition is as follows:
Base vacuum degree≤3 * 10
-4Pa, used atmosphere is that oxygen is argon-mixed, O
2With the throughput ratio of Ar be 1:4, sputtering pressure is 2Pa, sputtering power 60W, the temperature of substrate is controlled at 350 ℃～400 ℃ in the sputter procedure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558475A (en) * | 2013-11-08 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Method for detecting energy storage characteristic of ferroelectric ceramics |
| CN104084699A (en) * | 2014-06-26 | 2014-10-08 | 天津大学 | Method for manufacturing uniform organic and inorganic perovskite crystal film on flexible substrate |
-
2009
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558475A (en) * | 2013-11-08 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Method for detecting energy storage characteristic of ferroelectric ceramics |
| CN103558475B (en) * | 2013-11-08 | 2016-05-18 | 中国科学院上海硅酸盐研究所 | A kind of method for detection of ferroelectric ceramics energy storage characteristic |
| CN104084699A (en) * | 2014-06-26 | 2014-10-08 | 天津大学 | Method for manufacturing uniform organic and inorganic perovskite crystal film on flexible substrate |
| CN104084699B (en) * | 2014-06-26 | 2016-01-06 | 天津大学 | The method of even organic-inorganic perovskite crystal film prepared by a kind of flexible substrate |
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