CN103993286B - A kind of preparation method of the voltage-controlled varactor of BST/BMN laminated film - Google Patents
A kind of preparation method of the voltage-controlled varactor of BST/BMN laminated film Download PDFInfo
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- CN103993286B CN103993286B CN201410241888.8A CN201410241888A CN103993286B CN 103993286 B CN103993286 B CN 103993286B CN 201410241888 A CN201410241888 A CN 201410241888A CN 103993286 B CN103993286 B CN 103993286B
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Abstract
The preparation method that the invention discloses a kind of voltage-controlled varactor of BST/BMN laminated film, prepares Bi initially with solid sintering technology1.5Mg1.0Nb1.5O7I.e. BMN target and Ba0.6Sr0.4TiO3I.e. BST target, adopts Pt-Si substrate, utilizes magnetron sputtered deposition technology, uses Ar and O2As sputter gas, deposition obtains the BMN thin layer that thickness is 150-300nm and the bst thin film layer that thickness is 150-300nm, carry out after annealing process then at 700 DEG C, utilize mask plate at bst thin film metal electrode prepared above, prepare the voltage-controlled varactor of BST/BMN laminated film. Dielectric loss of the present invention low (<0.005), tuning rate moderate (>=30%100KHz), and device stability is good, the development and application for electronics provides excellent electronic devices and components basis.
Description
Technical field
The present invention is about electronic information material and components and parts, particularly to the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film.
Background technology
Along with the development of the technology such as radar, satellite, communication, the application of phased array antenna is increasingly extensive. Microwave phase shifter is as the core component of phased array antenna, and its performance directly decides the important technology indexs such as the working frequency range of transmitting/receiving unit, response speed, insertion loss, power, volume. Traditional ferrite phase shifter and semiconductor PIN diode phase shifter are due to the defect of self, it is impossible to meet growing technology requirement. Adopt barium strontium titanate (Ba1-xSrxTiO3BST) phase shifter of ferroelectric thin film has the features such as cost is low, speed is fast, precision is high, volume is little, also there is high dielectric constant and significant dielectric, nonlinear, it is believed that be the ideal material making microwave phase shifter, become an international study hotspot in recent years.
But owing to bst thin film material has higher dielectric loss, which has limited the application of bst thin film. Nearest Bi1.5MgNb1.5O7(BMN) also beginning to step into the visual field of researcher, it has relatively low dielectric loss, but its dielectric tuning rate is relatively low. In order to reduce the loss factor of the voltage-controlled varactor of bst thin film, we attempt bst thin film material and BMM thin-film material have been carried out compound, it has been found that can within the scope of acceptable in dielectric tuning rate, and its recombination loss is substantially reduced.
Summary of the invention
The purpose of the present invention, in order to reduce the dielectric loss of prior art, improves dielectric tuning rate, it is provided that the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film.
The preparation method of the voltage-controlled varactor of BST/BMN laminated film of the present invention is as follows:
The preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film, has following steps:
(1) solid sintering technology is adopted to prepare Bi1.5Mg1.0Nb1.5O7I.e. BMN target and Ba0.6Sr0.4TiO3I.e. BST target:
By Bi1.5Mg1.0Nb1.5O7Stoichiometric proportion, weighs raw material Bi2O3, MgO and Nb2O5, compressing after being sufficiently mixed, fire BMN target in 1150 DEG C; )
By Ba0.6Sr0.4TiO3Stoichiometric proportion. Weigh raw material BaTiO3And SrTiO3, compressing after being sufficiently mixed, fire BST target in 1350 DEG C;
(2) the Pt-Si substrate that cleaning is dry is put on magnetron sputtering sample stage;
(3) base vacuum of magnetic control sputtering system is evacuated to P < 7.0 × 10-6Torr, then heating substrate is to 400～700 DEG C;
(4) in step (3) system, Ar and O is used2As sputter gas, sputtering power is 50～200W, is deposited obtaining the BMN thin layer that thickness is 150-400nm;
(5) after step (4) completes, Ar and O is used2As sputter gas, sputtering power is 50～200W, is deposited obtaining the bst thin film layer that thickness is 150-400nm; When underlayer temperature is down to below 100 DEG C, take out sample, in oxygen atmosphere stove, carry out after annealing process in 700 DEG C;
(6) after step (5) completes, metal electrode is prepared at BST/BMN laminated film above with mask plate.
The material purity of described step (1) is all more than 99%.
Ar and the O of described step (4)2Purity all more than 99.99%, oxygen in magnetic control sputtering system and the intrinsic standoff ratio of argon are between 1/15 and 1/4.
Described step (4) or step (5) control film thickness by regulating technological parameter or sedimentation time.
Oxygen pressure≤the 0.1Mpa passed in the oxygen atmosphere stove of described step (5), oxygen purity >=99%; Annealing time is 5～60min.
The electrode of described step (6) is circular electrode, and diameter is 0.2～0.3mm, and thickness of electrode is 100～600nm, and electrode material is Pt or Au, and electrode preparation method is magnetron sputtering method or vapour deposition method.
Tuning rate>=30% of prepared BST/BMN laminated film varactor, test frequency is 100KHz; Dielectric loss<0.005.
The dielectric loss of the BST/BMN laminated film varactor prepared by the present invention low (<0.005), tuning rate moderate (>=30%100KHz), and device stability is good, the development and application for electronics provides excellent electronic devices and components basis.
Accompanying drawing explanation
Fig. 1 is dielectric properties (electric field-tunable) collection of illustrative plates of the voltage-controlled varactor sample of BST/BMN laminated film;
Fig. 2 is the fissipation factor fissipation factor comparison diagram with monolayer bst thin film of the voltage-controlled varactor sample of BST/BMN laminated film.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, it should be appreciated that these embodiments are merely to illustrate the present invention rather than limit the scope of the invention.
Embodiment 1
(1) solid sintering technology is adopted to prepare BMN target and BST target:
Bi is pressed with electronic balance1.5MgNb1.5O7The stoichiometric proportion of corresponding element weighs Bi2O3, MgO and Nb2O5(purity is 99%), after sufficiently mixing, the pressure at 20Mpa makes type, then is placed in cabinet-type electric furnace and is progressively warming up to 1150 DEG C, and is incubated 5 hours;
Ba is pressed with electronic balance0.6Sr0.4TiO3The stoichiometric proportion of corresponding element weighs BaCO3、SrCO3And TiO2, (purity is 99%) after sufficiently mixing, the pressure at 30Mpa makes type, is finally placed in cabinet-type electric furnace and is progressively warming up to 1450 DEG C, and is incubated 10 hours.
(2) Pt-Si substrate is cleaned, with N2Dry up and put on magnetron sputtering sample stage.
(3) base vacuum of magnetic control sputtering system is evacuated to 8.0 × 10-6Torr, then heating substrate is to 400 DEG C.
(4) with high-purity (99.99%) Ar and O2Flow-rate ratio as sputter gas, argon and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, is deposited obtaining the Bi that thickness is 300nm1.5MgNb1.5O7Thin film, controls film thickness by regulating technological parameter or sedimentation time.
(5) with high-purity (99.99%) Ar and O2Flow-rate ratio as sputter gas, argon and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, is deposited obtaining the Ba that thickness is 300nm0.6Sr0.4TiO3Thin film, controls film thickness by regulating technological parameter or sedimentation time;When underlayer temperature is down to below 100 DEG C, taking out sample, carry out after annealing process in 750 DEG C in oxygen atmosphere stove, annealing time is 10min, and the purity passing into oxygen is 99%, and annealing gas pressure is 0.1Mpa.
(6) BST/BMN laminated film after annealing prepares metal electrode above with mask plate, and utilizes the method for magnetron sputtering to plate the Au electrode that diameter is 0.2mm, prepares the voltage-controlled varactor of BST/BMN laminated film.
Fig. 1 is dielectric properties (electric field-tunable) collection of illustrative plates of the voltage-controlled varactor sample of BST/BMN laminated film, it is seen that under the electric field of 1.3MV/cm, tuning rate is 37%.
Fig. 2 is the fissipation factor comparison diagram of fissipation factor and the monolayer bst thin film of the voltage-controlled varactor sample of BST/BMN laminated film, it is seen that the fissipation factor of BST/BMN laminated film is well below the fissipation factor of monolayer bst thin film.
Embodiment 2
(1) solid sintering technology is adopted to prepare BMN target and BST target:
Bi is pressed with electronic balance1.5MgNb1.5O7The stoichiometric proportion of corresponding element weighs Bi2O3, MgO and Nb2O5(purity is 99%), after sufficiently mixing, the pressure at 20Mpa makes type, then is placed in cabinet-type electric furnace and is progressively warming up to 1150 DEG C, and is incubated 5 hours;
Ba is pressed with electronic balance0.6Sr0.4TiO3The stoichiometric proportion of corresponding element weighs BaCO3、SrCO3And TiO2, (purity is 99%) after sufficiently mixing, the pressure at 30Mpa makes type, is finally placed in cabinet-type electric furnace and is progressively warming up to 1450 DEG C, and is incubated 10 hours.
(2) Pt-Si substrate is cleaned, with N2Dry up and put on magnetron sputtering sample stage.
(3) base vacuum of magnetic control sputtering system is evacuated to 8.0 × 10-6Torr, then heating substrate is to 400 DEG C.
(4) with high-purity (99.99%) Ar and O2Flow-rate ratio as sputter gas, argon and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, is deposited obtaining the Bi that thickness is 200nm1.5MgNb1.5O7Thin film, controls film thickness by regulating technological parameter or sedimentation time.
(5) with high-purity (99.99%) Ar and O2Flow-rate ratio as sputter gas, argon and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, is deposited obtaining the Ba that thickness is 400nm0.6Sr0.4TiO3Thin film, controls film thickness by regulating technological parameter or sedimentation time; When underlayer temperature is down to below 100 DEG C, taking out sample, carry out after annealing process in 750 DEG C in oxygen atmosphere stove, annealing time is 10min, and the purity passing into oxygen is 99%, and annealing gas pressure is 0.1Mpa.
(6) BST/BMN laminated film after annealing prepares metal electrode above with mask plate, and utilizes the method for magnetron sputtering to plate the Au electrode that diameter is 0.2mm, prepares the voltage-controlled varactor of BST/BMN laminated film.
Dielectric properties tuning rate under the electric field of 1.3MV/cm of the voltage-controlled varactor sample of BST/BMN laminated film obtained under such condition is 45%, and dielectric loss is about 0.02.
Claims (6)
1. a preparation method for the voltage-controlled varactor of BST/BMN laminated film, has following steps:
(1) solid sintering technology is adopted to prepare Bi1.5Mg1.0Nb1.5O7I.e. BMN target and Ba0.6Sr0.4TiO3I.e. BST target:
By Bi1.5Mg1.0Nb1.5O7Stoichiometric proportion, weighs raw material Bi2O3, MgO and Nb2O5, compressing after being sufficiently mixed, fire BMN target in 1150 DEG C;
By Ba0.6Sr0.4TiO3Stoichiometric proportion, weighs raw material BaTiO3And SrTiO3, compressing after being sufficiently mixed, fire BST target in 1350 DEG C;
(2) the Pt-Si substrate that cleaning is dry is put on magnetron sputtering sample stage;
(3) base vacuum of magnetic control sputtering system is evacuated to P < 7.0 × 10-6Torr, then heating substrate is to 400～700 DEG C;
(4) in step (3) system, Ar and O is used2As sputter gas, sputtering power is 50～200W, is deposited obtaining the BMN thin layer that thickness is 150-400nm;
(5) after step (4) completes, Ar and O is used2As sputter gas, sputtering power is 50～200W, is deposited obtaining the bst thin film layer that thickness is 150-400nm; When underlayer temperature is down to below 100 DEG C, take out sample, in oxygen atmosphere stove, carry out after annealing process in 700 DEG C; Oxygen pressure≤the 0.1Mpa passed in oxygen atmosphere stove, oxygen purity >=99%, annealing time is 5～60min;
(6) after step (5) completes, metal electrode is prepared at BST/BMN laminated film above with mask plate.
2. the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film according to claim 1, it is characterised in that the material purity of described step (1) is all more than 99%.
3. the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film according to claim 1, it is characterised in that Ar and the O of described step (4)2Purity all more than 99.99%, oxygen in magnetic control sputtering system and the intrinsic standoff ratio of argon are between 1/15 and 1/4.
4. the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film according to claim 1, it is characterised in that described step (4) or step (5) control film thickness by regulating technological parameter or sedimentation time.
5. the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film according to claim 1, it is characterized in that, the electrode of described step (6) is circular electrode, diameter is 0.2～0.3mm, thickness of electrode is 100～600nm, electrode material is Pt or Au, and electrode preparation method is magnetron sputtering method or vapour deposition method.
6. the preparation method of a kind of voltage-controlled varactor of BST/BMN laminated film according to claim 1, it is characterised in that tuning rate>=30% of prepared BST/BMN laminated film varactor, test frequency is 100KHz; Dielectric loss<0.005.
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| CN108411251A (en) * | 2018-03-28 | 2018-08-17 | 天津大学 | A kind of preparation method of BZN/BTS heterojunction structures dielectric tuning film |
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| CN108447789B (en) * | 2018-03-28 | 2020-06-02 | 天津大学 | Preparation method of flexible film varactor |
| CN109180178B (en) * | 2018-10-10 | 2021-11-02 | 中国科学院上海硅酸盐研究所 | Barium strontium titanate-based lead-free relaxation ferroelectric ceramic with high energy storage density and preparation method thereof |
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| CN108411251A (en) * | 2018-03-28 | 2018-08-17 | 天津大学 | A kind of preparation method of BZN/BTS heterojunction structures dielectric tuning film |
| CN108411251B (en) * | 2018-03-28 | 2020-03-03 | 天津大学 | Preparation method of BZN/BTS heterostructure dielectric tuning film |
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