CN103993286A - Method for preparing Ba1-xSrxTiO3/Bi1.5MgNb1.5O7 (BST/BMN) composite film voltage-controlled varactor tube - Google Patents

Method for preparing Ba1-xSrxTiO3/Bi1.5MgNb1.5O7 (BST/BMN) composite film voltage-controlled varactor tube Download PDF

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CN103993286A
CN103993286A CN201410241888.8A CN201410241888A CN103993286A CN 103993286 A CN103993286 A CN 103993286A CN 201410241888 A CN201410241888 A CN 201410241888A CN 103993286 A CN103993286 A CN 103993286A
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bst
bmn
voltage
laminated film
controlled varactor
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CN103993286B (en
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李玲霞
于仕辉
许丹
董和磊
金雨馨
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a method for preparing a Ba1-xSrxTiO3/Bi1.5MgNb1.5O7 (BST/BMN) composite film voltage-controlled varactor tube. The method comprises the following steps: firstly, preparing Bi1.5Mg1.0Nb1.5O7, namely a BMN target material and Ba0.6Sr0.4TiO3, namely a BST target material by adopting a solid-phase sintering method; adopting a Pt-Si substrate, utilizing a magnetron sputtering deposition technology, utilizing Ar and O2 as sputtering gases, and depositing to obtain a BMN film layer of which the thickness is 150-300nm and a BST film layer of which the thickness is 150-300nm; then carrying out post annealing treatment at 700 DEG C, and preparing a metal electrode by using a mask on the BST film, so as to prepare the BST/BMN composite film voltage-controlled varactor tube. The BST/BMN composite film voltage-controlled varactor tube is low in dielectric loss (lower than 0.005), moderate in tuning rate (greater than or equal to 30% @100KHz), and good in apparatus stability, and a good electronic component basis is provided for development and application of electronic communication equipment.

Description

The preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film
Technical field
The invention relates to electronic information material and components and parts, the particularly preparation method of the voltage-controlled varactor of a kind 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 is directly determining the important technology indexs such as the working frequency range, response speed, insertion loss, power, volume of transmitting/receiving assembly.Traditional ferrite phase shifter and semi-conductor PIN diode phase shifter, due to the defect of self, cannot meet growing technical requirements.Adopt strontium-barium titanate (Ba 1-xsr xtiO 3bST) phase shifter of ferroelectric membranc has the features such as cost is low, speed is fast, precision is high, volume is little, also there is high specific inductivity and significant dielectric, nonlinear, be considered to make the ideal material of microwave phase shifter, become an international study hotspot in recent years.
But because bst thin film material has higher dielectric loss, this has limited the application of bst thin film.Bi recently 1.5mgNb 1.5o 7(BMN) also start to step into investigator's the visual field, it has lower 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 to carry out compound, and discovery is within the scope of dielectric tuning rate can acceptable, and its recombination loss reduces greatly.
Summary of the invention
Object of the present invention, in order to reduce the dielectric loss of prior art, improves dielectric tuning rate, and the preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film is provided.
The preparation method of the voltage-controlled varactor of BST/BMN laminated film of the present invention is as follows:
A preparation method for the voltage-controlled varactor of BST/BMN laminated film, has following steps:
(1) adopt solid sintering technology to prepare Bi 1.5mg 1.0nb 1.5o 7be BMN target and Ba 0.6sr 0.4tiO 3be BST target:
Press Bi 1.5mg 1.0nb 1.5o 7stoichiometric ratio, takes raw material Bi 2o 3, MgO and Nb 2o 5, compression moulding after fully mixing, fires BMN target in 1150 DEG C; )
Press Ba 0.6sr 0.4tiO 3stoichiometric ratio.Take raw material BaTiO 3and SrTiO 3, compression moulding after fully mixing, fires BST target in 1350 DEG C;
(2) clean dry Pt-Si substrate is put in magnetron sputtering sample table;
(3) base vacuum of magnetic control sputtering system is evacuated to P<7.0 × 10 -6torr, then heated substrate to 400～700 DEG C;
(4), in step (3) system, use Ar and O 2as sputter gas, sputtering power is 50～200W, deposits and obtains the BMN thin film layer that thickness is 150-400nm;
(5), after step (4) completes, use Ar and O 2as sputter gas, sputtering power is 50～200W, deposits and obtains the bst thin film layer that thickness is 150-400nm; In the time that underlayer temperature is down to below 100 DEG C, take out sample, in oxygen atmosphere stove, carry out after annealing processing in 700 DEG C;
(6) after step (5) completes, on BST/BMN laminated film, utilize mask to prepare metal electrode.
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%, the oxygen in magnetic control sputtering system and the intrinsic standoff ratio of argon gas are between 1/15 and 1/4.
Described step (4) or step (5) are by adjusting process parameter or depositing time control film thickness.
Oxygen pressure≤the 0.1Mpa passing 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 materials 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 low (<0.005) of the prepared BST/BMN laminated film varactor of the present invention, tuning rate moderate (>=30%100KHz), and device stability is good, for the development and application of electronics provides good electronic devices and components basis.
Brief description of the drawings
Fig. 1 is dielectric properties (electric field the is adjustable) collection of illustrative plates of the voltage-controlled varactor sample of BST/BMN laminated film;
Fig. 2 is the dissipation factor of the voltage-controlled varactor sample of BST/BMN laminated film and the dissipation factor comparison diagram of individual layer bst thin film.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
(1) adopt solid sintering technology to prepare BMN target and BST target:
Press Bi with electronic balance 1.5mgNb 1.5o 7the stoichiometric ratio of corresponding element takes Bi 2o 3, MgO and Nb 2o 5(purity is 99%), after sufficiently mixing, compression moulding under the pressure of 20Mpa, then be placed in cabinet-type electric furnace and be progressively warming up to 1150 DEG C, and be incubated 5 hours;
Press Ba with electronic balance 0.6sr 0.4tiO 3the stoichiometric ratio of corresponding element takes BaCO 3, SrCO 3and TiO 2, (purity is 99%) after sufficiently mixing, compression moulding under the pressure of 30Mpa, is finally placed in cabinet-type electric furnace and is progressively warming up to 1450 DEG C, and be incubated 10 hours.
(2) Pt-Si substrate is cleaned, with N 2dry up and put in magnetron sputtering sample table.
(3) base vacuum of magnetic control sputtering system is evacuated to 8.0 × 10 -6torr, then heated substrate to 400 DEG C.
(4) with high-purity (99.99%) Ar and O 2as sputter gas, the throughput ratio of argon gas and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the Bi that thickness is 300nm 1.5mgNb 1.5o 7film, by adjusting process parameter or depositing time control film thickness.
(5) with high-purity (99.99%) Ar and O 2as sputter gas, the throughput ratio of argon gas and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the Ba that thickness is 300nm 0.6sr 0.4tiO 3film, by adjusting process parameter or depositing time control film thickness; In the time that underlayer temperature is down to below 100 DEG C, take out sample, in oxygen atmosphere stove, carry out after annealing processing in 750 DEG C, annealing time is 10min, and the purity that passes into oxygen is 99%, and annealing gas pressure is 0.1Mpa.
(6) above the BST/BMN laminated film after annealing, utilize mask to prepare metal electrode, and utilize the method for magnetron sputtering to plate the Au electrode that diameter is 0.2mm, make the voltage-controlled varactor of BST/BMN laminated film.
Fig. 1 is dielectric properties (electric field the is adjustable) collection of illustrative plates of the voltage-controlled varactor sample of BST/BMN laminated film, and under the electric field of 1.3MV/cm, tuning rate is 37% as seen.
Fig. 2 is the dissipation factor of the voltage-controlled varactor sample of BST/BMN laminated film and the dissipation factor comparison diagram of individual layer bst thin film, and the dissipation factor of visible BST/BMN laminated film is well below the dissipation factor of individual layer bst thin film.
Embodiment 2
(1) adopt solid sintering technology to prepare BMN target and BST target:
Press Bi with electronic balance 1.5mgNb 1.5o 7the stoichiometric ratio of corresponding element takes Bi 2o 3, MgO and Nb 2o 5(purity is 99%), after sufficiently mixing, compression moulding under the pressure of 20Mpa, then be placed in cabinet-type electric furnace and be progressively warming up to 1150 DEG C, and be incubated 5 hours;
Press Ba with electronic balance 0.6sr 0.4tiO 3the stoichiometric ratio of corresponding element takes BaCO 3, SrCO 3and TiO 2, (purity is 99%) after sufficiently mixing, compression moulding under the pressure of 30Mpa, is finally placed in cabinet-type electric furnace and is progressively warming up to 1450 DEG C, and be incubated 10 hours.
(2) Pt-Si substrate is cleaned, with N 2dry up and put in magnetron sputtering sample table.
(3) base vacuum of magnetic control sputtering system is evacuated to 8.0 × 10 -6torr, then heated substrate to 400 DEG C.
(4) with high-purity (99.99%) Ar and O 2as sputter gas, the throughput ratio of argon gas and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the Bi that thickness is 200nm 1.5mgNb 1.5o 7film, by adjusting process parameter or depositing time control film thickness.
(5) with high-purity (99.99%) Ar and O 2as sputter gas, the throughput ratio of argon gas and oxygen is 17:3, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the Ba that thickness is 400nm 0.6sr 0.4tiO 3film, by adjusting process parameter or depositing time control film thickness; In the time that underlayer temperature is down to below 100 DEG C, take out sample, in oxygen atmosphere stove, carry out after annealing processing in 750 DEG C, annealing time is 10min, and the purity that passes into oxygen is 99%, and annealing gas pressure is 0.1Mpa.
(6) above the BST/BMN laminated film after annealing, utilize mask to prepare metal electrode, and utilize the method for magnetron sputtering to plate the Au electrode that diameter is 0.2mm, make the voltage-controlled varactor of BST/BMN laminated film.
Under this kind of condition, dielectric properties tuning rate under the electric field of 1.3MV/cm of the voltage-controlled varactor sample of prepared BST/BMN laminated film is 45%, and dielectric loss is 0.02 left and right.

Claims (7)

1. a preparation method for the voltage-controlled varactor of BST/BMN laminated film, has following steps:
(1) adopt solid sintering technology to prepare Bi 1.5mg 1.0nb 1.5o 7be BMN target and Ba 0.6sr 0.4tiO 3be BST target:
Press Bi 1.5mg 1.0nb 1.5o 7stoichiometric ratio, takes raw material Bi 2o 3, MgO and Nb 2o 5, compression moulding after fully mixing, fires BMN target in 1150 DEG C;
Press Ba 0.6sr 0.4tiO 3stoichiometric ratio.Take raw material BaTiO 3and SrTiO 3, compression moulding after fully mixing, fires BST target in 1350 DEG C;
(2) clean dry Pt-Si substrate is put in magnetron sputtering sample table;
(3) base vacuum of magnetic control sputtering system is evacuated to P<7.0 × 10 -6torr, then heated substrate to 400～700 DEG C;
(4), in step (3) system, use Ar and O 2as sputter gas, sputtering power is 50～200W, deposits and obtains the BMN thin film layer that thickness is 150-400nm;
(5), after step (4) completes, use Ar and O 2as sputter gas, sputtering power is 50～200W, deposits and obtains the bst thin film layer that thickness is 150-400nm; In the time that underlayer temperature is down to below 100 DEG C, take out sample, in oxygen atmosphere stove, carry out after annealing processing in 700 DEG C;
(6) after step (5) completes, on BST/BMN laminated film, utilize mask to prepare metal electrode.
2. the preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film according to claim 1, is characterized in that, the material purity of described step (1) is all more than 99%.
3. the preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film according to claim 1, is characterized in that, Ar and the O of described step (4) 2purity all more than 99.99%, the oxygen in magnetic control sputtering system and the intrinsic standoff ratio of argon gas are between 1/15 and 1/4.
4. the preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film according to claim 1, is characterized in that, described step (4) or step (5) are by adjusting process parameter or depositing time control film thickness.
5. the preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film according to claim 1, is characterized in that, the oxygen pressure≤0.1Mpa passing in the oxygen atmosphere stove of described step (5), oxygen purity >=99%; Annealing time is 5～60min.
6. the preparation method of the voltage-controlled varactor of a kind 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 materials is Pt or Au, and electrode preparation method is magnetron sputtering method or vapour deposition method.
7. the preparation method of the voltage-controlled varactor of a kind of BST/BMN laminated film according to claim 1, is characterized in that, tuning rate >=30% of prepared BST/BMN laminated film varactor, and test frequency is 100KHz; Dielectric loss <0.005.
CN201410241888.8A 2014-05-30 2014-05-30 A kind of preparation method of the voltage-controlled varactor of BST/BMN laminated film Expired - Fee Related CN103993286B (en)

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Cited By (4)

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CN104591729A (en) * 2014-12-26 2015-05-06 天津大学 Preparation method of PBZ target for preparing PBZ thin film by virtue of magnetron sputtering method
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
CN108447789A (en) * 2018-03-28 2018-08-24 天津大学 A kind of preparation method of fexible film varactor
CN109180178A (en) * 2018-10-10 2019-01-11 中国科学院上海硅酸盐研究所 A kind of barium-strontium titanate-based unleaded relaxation ferroelectric ceramic of high energy storage density and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104591729A (en) * 2014-12-26 2015-05-06 天津大学 Preparation method of PBZ target for preparing PBZ thin film by virtue of magnetron sputtering method
CN104591729B (en) * 2014-12-26 2017-02-22 天津大学 Preparation method of PBZ target for preparing PBZ thin film by virtue of magnetron sputtering method
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
CN108447789A (en) * 2018-03-28 2018-08-24 天津大学 A kind of preparation method of fexible film varactor
CN108411251B (en) * 2018-03-28 2020-03-03 天津大学 Preparation method of BZN/BTS heterostructure dielectric tuning film
CN108447789B (en) * 2018-03-28 2020-06-02 天津大学 Preparation method of flexible film varactor
CN109180178A (en) * 2018-10-10 2019-01-11 中国科学院上海硅酸盐研究所 A kind of barium-strontium titanate-based unleaded relaxation ferroelectric ceramic of high energy storage density and preparation method thereof

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