CN114262870A - Lead-free thin film with high energy storage density and wide working temperature, capacitor and preparation method thereof - Google Patents
Lead-free thin film with high energy storage density and wide working temperature, capacitor and preparation method thereof Download PDFInfo
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- CN114262870A CN114262870A CN202111603394.6A CN202111603394A CN114262870A CN 114262870 A CN114262870 A CN 114262870A CN 202111603394 A CN202111603394 A CN 202111603394A CN 114262870 A CN114262870 A CN 114262870A
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- 238000004146 energy storage Methods 0.000 title claims abstract description 46
- 239000003990 capacitor Substances 0.000 title claims abstract description 30
- 239000010409 thin film Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010408 film Substances 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 43
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 29
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 11
- 229910002367 SrTiO Inorganic materials 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 description 21
- 238000000151 deposition Methods 0.000 description 15
- 230000008021 deposition Effects 0.000 description 15
- 239000000843 powder Substances 0.000 description 15
- 238000004544 sputter deposition Methods 0.000 description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 238000007747 plating Methods 0.000 description 10
- 239000013077 target material Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 230000010287 polarization Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 3
- 230000005684 electric field Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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Abstract
The invention discloses a lead-free film with high energy storage density and wide working temperature, a capacitor and a preparation method thereof, wherein the lead-free film with high energy storage density and wide working temperature comprises Nb, SrTiO3A substrate and a film disposed on the Nb SrTiO3A surface of a substrate; the film is BaHfxTi1‑xO3The value range of x is more than or equal to 0.05 and less than or equal to 0.32. The preparation is realized by utilizing BaHf in a magnetron sputtering modexTi1‑xO3A ceramic target of film, in which Nb is SrTiO3Preparation of BaHf on substrate surfacexTi1‑xO3And annealing the thin film to obtain the lead-free thin film with high energy storage density and wide working temperature. The lead-free film with high energy storage density and wide working temperature has the characteristics of high energy storage density and wide temperature range.
Description
Technical Field
The invention relates to the field of energy storage thin film materials, in particular to a lead-free thin film with high energy storage density and wide working temperature, a capacitor and a preparation method thereof.
Background
Dielectric capacitors are important energy storage elements, and have wide applications in various power electronic devices due to their high power density, fast charge and discharge speed, and long service life. However, their use in harsh environments is greatly limited by the relatively low energy storage density and low operating temperature. On the one hand, the current commercial dielectric capacitor can only work below 105 ℃, and the energy storage density is about 2J/cm3However, the temperature of the actual environment tends to be higher than this temperature. For example, in a hybrid vehicle, the capacitor is exposed to an ambient temperature of about 140 ℃, and therefore a cooling system has to be added, which undoubtedly adds additional weight, volume, and energy consumption. Worse still, in other cases, it is not practical to equip cooling systems. Such as oil rigs, oil and gas developments, with ambient temperatures in excess of 200 c, there is no space for installation of cooling systems, and even extremely high costs are required. This requires that the capacitor must operate at high temperatures. On the other hand, if the capacitor can keep higher energy storage density in a wide temperature area, the volume and the weight of equipment can be effectively reduced, thereby greatly reducing the cost. Therefore, the research and development of the capacitor with high energy storage density and wide working temperature have important significance.
In general, at higher operating temperatures, the capacitor is prone to breakdown even with lower applied voltages than at room temperature, which limits the operating temperature of the capacitor, due to the steep rise in leakage current density of the thermally activated dielectric material. At high temperatures, the remanent polarization of the dielectric increases rapidly with increasing temperature, resulting in a capacitor with lower energy storage density at high temperatures.
Therefore, the energy storage density of the capacitor is increased and the working temperature range is widened. 2 conditions need to be satisfied. On the one hand, the dielectric capacitor can apply a higher electric field at high temperature, and on the other hand, the residual polarization of the dielectric can keep a lower value at high temperature and high electric field.
Disclosure of Invention
In order to overcome the problems of low energy storage density and low working temperature of the lead-free film, the invention aims to provide the lead-free film with high energy storage density and wide working temperature, the capacitor and the preparation method thereof so as to improve the energy storage density and the working temperature range.
In order to achieve the purpose, the invention adopts the following technical scheme:
a lead-free film with high energy storage density and wide working temp is prepared from Nb SrTiO3A substrate and a film disposed on the Nb SrTiO3A surface of a substrate; the film is BaHfxTi1-xO3The value range of x is more than or equal to 0.05 and less than or equal to 0.32.
Preferably, Nb is SrTiO3The substrate adopts (001) oriented single crystal Nb SrTiO3A substrate.
Preferably, BaHfxTi1-xO3The thickness of the film is 395-405 nm.
Preferably, the breakdown field strength of the lead-free thin film with high energy storage density and wide working temperature is 4.4-7.8 MV/cm, and the energy storage density is 41-90J/cm3The wide temperature range is-100 to 400 ℃.
The invention also provides a preparation method of the lead-free film with high energy storage density and wide working temperature, which comprises the following steps:
at Nb, SrTiO3Preparation of BaHf on substrate surfacexTi1-xO3And (3) obtaining the lead-free thin film with high energy storage density and wide working temperature, wherein the value range of x is more than or equal to 0.05 and less than or equal to 0.32.
Preferably: by means of magnetron sputtering, BaHf is utilizedxTi1-xO3A ceramic target of film, in which Nb is SrTiO3Preparation of BaHf on substrate surfacexTi1-xO3And annealing the thin film to obtain the lead-free thin film with high energy storage density and wide working temperature.
Preferably, in Nb SrTiO3Preparation of BaHf on substrate surfacexTi1-xO3The temperature of the film is 700-850 ℃; the annealing temperature is 700-850 ℃.
Preferably, Nb is SrTiO3The substrate adopts (001) oriented single crystal Nb SrTiO3A substrate.
Preferably, BaHfxTi1-xO3The thickness of the film is 395-405 nm.
The invention also provides a capacitor, which comprises an electrode layer and the lead-free thin film with high energy storage density and wide working temperature, wherein the electrode layer is arranged on the BaHfxTi1-xO3The surface of the film.
The invention has the following beneficial effects:
BaHf of the inventionxTi1-xO3In the film, the value range of x is more than or equal to 0.05 and less than or equal to 0.32, the breakdown field strength of the film is improved by adding the hafnium element, and the residual polarization is reduced and the energy storage density is improved while the larger polarization is kept. Meanwhile, the addition of the hafnium element is beneficial to increasing the relaxation property of the film and improving the temperature stability, so that the working temperature of the film can be improved.
Further, Nb is SrTiO3The substrate adopts (001) oriented single crystal Nb SrTiO3A substrate is prepared by doping SrTiO with Nb3The reason for the substrate is that: nb SrTiO3The substrate is conductive and can be used as an electrode, and Nb is SrTiO3The substrate and the film are of perovskite structure, thereby facilitating BaHfxTi1-xO3And (5) film epitaxy.
Further, BaHfxTi1-xO3The thickness of the film is 395-405 nm, and the thicker film is beneficial to eliminating the influence of stress on the energy storage performance.
In the preparation process of the invention, SrTiO is added as Nb3BaHf prepared on substrate surfacexTi1-xO3The temperature of the film is 700-850 ℃; the annealing temperature is 700-850 ℃. At the temperature, the film has better crystallization quality, can reduce the formation of defects in the growth process, increase the breakdown field strength of the film, and improve the energy storage density and the working temperature.
Drawings
FIG. 1 is a Weibull plot of breakdown field strengths of films prepared in examples 1-5 of the present invention;
Detailed Description
In order to make the technical and technical advantages of the present invention more apparent, the present invention is further described with reference to the following examples, which are provided for illustration only and are not intended to limit the present invention.
Example 1
The capacitor of this example was prepared as follows:
Step 4, vacuumizing and ventilating: pumping the deposition chamber to a pressure less than 10-5mbar, and then introducing mixed gas again to ensure that the gas pressure is 0.135 mbar;
step 5, growing a film: opening the sputtering source to sputter BaHf0.05Ti0.95O3The sputtering time of the ceramic target is adjusted to 22 hours, and SrTiO is added into Nb3BaHf with thickness of 400nm (measured at 395-405 nm) is realized on the substrate0.05Ti0.95O3Growing a thin film;
step 6, annealing: the sputtering was stopped and the gas mixture was fed to bring the pressure in the deposition chamber to 200mbar, keeping 15 min.
Step 7, plating an electrode: and plating a Pt electrode with the thickness of 50nm on the surface of the film by using a mask plate to obtain the capacitor.
Example 2
The capacitor of this example was prepared as follows:
Step 4, vacuumizing and ventilating: pumping the deposition chamber to a pressure less than 10-5mbar, and then introducing mixed gas again to ensure that the gas pressure is 0.135 mbar;
step 5, growing a film: opening the sputtering source to sputter BaHf0.05Ti0.95O3The sputtering time of the ceramic target is adjusted to 23 hours, and SrTiO is added into Nb3BaHf with thickness of 400nm (measured at 395-405 nm) is realized on the substrate0.05Ti0.95O3Growing a thin film;
step 6, annealing: the sputtering was stopped and the gas mixture was fed to bring the pressure in the deposition chamber to 200mbar, keeping 15 min.
Step 7, plating an electrode: and plating a Pt electrode with the thickness of 50nm on the surface of the film by using a mask plate to obtain the capacitor.
Example 3
The capacitor of this example was prepared as follows:
Step 4, vacuumizing and ventilating: pumping the deposition chamber to a pressure less than 10-5mbar, and then introducing mixed gas again to ensure that the gas pressure is 0.135 mbar;
step 5, growing a film: opening the sputtering source to sputter BaHf0.05Ti0.95O3The sputtering time of the ceramic target is adjusted to 24 hours, and SrTiO is added into Nb3BaHf with thickness of 400nm (measured at 395-405 nm) is realized on the substrate0.05Ti0.95O3Growing a thin film;
step 6, annealing: the sputtering was stopped and the gas mixture was fed to bring the pressure in the deposition chamber to 200mbar, keeping 15 min.
Step 7, plating an electrode: and plating a Pt electrode with the thickness of 50nm on the surface of the film by using a mask plate to obtain the capacitor.
Example 4
The capacitor of this example was prepared as follows:
Step 4, vacuumizing and ventilating: pumping the deposition chamber to a pressure less than 10-5mbar, and then introducing mixed gas again to ensure that the gas pressure is 0.135 mbar;
step 5, growing a film: opening the sputtering source to sputter BaHf0.17Ti0.83O3The sputtering time of the ceramic target is adjusted to be 27 hours, and SrTiO is added into Nb3BaHf with thickness of 400nm (measured at 395-405 nm) is realized on the substrate0.17Ti0.83O3Growing a thin film;
step 6, annealing: the sputtering was stopped and the gas mixture was fed to bring the pressure in the deposition chamber to 200mbar, keeping 15 min.
Step 7, plating an electrode: and plating a Pt electrode with the thickness of 50nm on the surface of the film by using a mask plate to obtain the capacitor.
Example 5
The capacitor of this example was prepared as follows:
Step 4, vacuumizing and ventilating: pumping the deposition chamber to a pressure less than 10-5mbar, and then introducing mixed gas again to ensure that the gas pressure is 0.135 mbar;
step 5, growing a film: opening the sputtering source to sputter BaHf0.32Ti0.64O3The sputtering time of the ceramic target is adjusted to be 30 hours, and SrTiO is added into Nb3BaHf with thickness of 400nm (measured at 395-405 nm) is realized on the substrate0.32Ti0.64O3Growing a thin film;
step 6, annealing: the sputtering was stopped and the gas mixture was fed to bring the pressure in the deposition chamber to 200mbar, keeping 15 min.
Step 7, plating an electrode: and plating a Pt electrode with the thickness of 50nm on the surface of the film by using a mask plate to obtain the capacitor.
The performance of the capacitors made in each example is shown in table 1:
TABLE 1
As can be seen from table 1, the incorporation of hafnium elements in examples 1, 4 and 5 improves the energy storage density and operating temperature of the thin film at the growth temperature of 700 ℃. In addition, the growth temperature of the thin film also affects the energy storage characteristics of the thin film. BaHf in the same composition0.17Ti0.83O3The energy storage and wide temperature characteristics of the film grown at 700 ℃ are optimal in the film, examples 1-3.
Claims (10)
1. The lead-free film with high energy storage density and wide working temperature is characterized by comprising Nb, SrTiO3A substrate and a film disposed on the Nb SrTiO3A surface of a substrate; the film is BaHfxTi1-xO3The value range of x is more than or equal to 0.05 and less than or equal to 0.32.
2. The high energy storage density wide operating temperature lead-free thin film of claim 1, wherein Nb is SrTiO3The substrate adopts (001) oriented single crystal Nb SrTiO3A substrate.
3. The high energy storage density wide operating temperature lead-free film of claim 1, wherein BaHfxTi1-xO3The thickness of the film is 395-405 nm.
4. The high energy storage density wide operating temperature lead-free thin film of claim 1, wherein the high energy storage density wide operating temperature lead-free thin filmThe breakdown field intensity is 4.4-7.8 MV/cm, and the energy storage density is 41-90J/cm3The wide temperature range is-100 to 400 ℃.
5. The preparation method of the lead-free film with high energy storage density and wide working temperature is characterized by comprising the following steps:
at Nb, SrTiO3Preparation of BaHf on substrate surfacexTi1-xO3And (3) obtaining the lead-free thin film with high energy storage density and wide working temperature, wherein the value range of x is more than or equal to 0.05 and less than or equal to 0.32.
6. The method for preparing the lead-free thin film with high energy storage density and wide working temperature according to claim 5, wherein the method comprises the following steps:
by means of magnetron sputtering, BaHf is utilizedxTi1-xO3A ceramic target of film, in which Nb is SrTiO3Preparation of BaHf on substrate surfacexTi1-xO3And annealing the thin film to obtain the lead-free thin film with high energy storage density and wide working temperature.
7. The method for preparing the lead-free thin film with high energy storage density and wide working temperature as claimed in claim 6, wherein SrTiO is added into Nb3Preparation of BaHf on substrate surfacexTi1-xO3The temperature of the film is 700-850 ℃; the annealing temperature is 700-850 ℃.
8. The method for preparing the lead-free thin film with high energy storage density and wide working temperature as claimed in claim 5, wherein the Nb is SrTiO3The substrate adopts (001) oriented single crystal Nb SrTiO3A substrate.
9. The method of claim 5, wherein the BaHf solution is used to prepare the lead-free thin film with high energy storage density and wide working temperaturexTi1-xO3The thickness of the film is 395-405 nm.
10. A capacitor, characterized in that it comprises a capacitor body,the high energy storage density and wide working temperature lead-free film as claimed in any one of claims 1 to 4, comprising an electrode layer disposed on BaHfxTi1-xO3The surface of the film.
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|---|---|---|---|---|
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| CN109545548A (en) * | 2018-12-29 | 2019-03-29 | 西安交通大学 | A kind of warm film energy-storage capacitor of rare-earth element modified width and preparation method thereof |
| WO2020040127A1 (en) * | 2018-08-23 | 2020-02-27 | 東レ株式会社 | Polypropylene film, metal-membrane layered film using same, and film capacitor |
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2021
- 2021-12-24 CN CN202111603394.6A patent/CN114262870A/en active Pending
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