CN104029432B - The preparation method of BST/BMN/BST multi-layer compound film - Google Patents
The preparation method of BST/BMN/BST multi-layer compound film Download PDFInfo
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- CN104029432B CN104029432B CN201410300414.6A CN201410300414A CN104029432B CN 104029432 B CN104029432 B CN 104029432B CN 201410300414 A CN201410300414 A CN 201410300414A CN 104029432 B CN104029432 B CN 104029432B
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Abstract
Of the present inventionly disclose a kind of BST/BMN/BST multi-layer compound film, by increasing the low-loss BMN dielectric layers of one deck thus reduce thin-film dielectric loss in the middle of two bst thin films.First prepare the precursor sol of barium strontium titanate and bismuth niobate magnesium, more above-mentioned precursor colloidal sol is dropped on substrate prepare corresponding film respectively, then carry out after annealing in 550 ~ 750 DEG C, obtain BST/BMN/BST multi-layer compound film.The present invention, using brium carbonate, strontium carbonate and titanium dioxide as raw material, substitutes part alkoxide and butyl titanate, reduces the production cost of film.Magnesium carbonate replaces nitric hydrate magnesium, makes stoicheiometry more accurate; The present invention adopts the new technology improving Sol-Gel, laminated film excellent performance, and process is simple, has broad application prospects.
Description
Technical field
The invention belongs to electronic information material and components and parts field, particularly a kind of BST/BMN/BST multi-layer compound film for microwave-tuned components and parts and preparation method thereof.
Background technology
In recent years, radio communication develop rapidly, network system presents diversity (as cell phone network, personal area network (PAN), WLAN (WLAN) coexist), needs the compatible various communication standard of restructural smart machine.Dielectric tunable radio frequency electric capacity because its tunability is high, volume is little and cost is low, as restructural device intelligence radio frequency applications elementary cell and cause extensive concern; Dielectric adjustable condenser material aspect is concentrated on to its research.
Perovskite structure BST sill studies a class dielectric tunable medium material the most widely at present.The feature of BST based film material is that dielectric tuning rate is high, but there is the large unfavorable factor of its dielectric loss.There is pyrochlore structure Bi
1.5mgNb
1.5o
7(BMN) material has dielectric adjustable equally, and its dielectric loss is lower than BST.The loss of BMN thin-film dielectric is little, and dielectric constant is moderate, good temperature stability, is one very promising novel microwave dielectric material with adjustable.But compared with BST sill, its tuning rate is relatively little.
The advantage of the comprehensive two kinds of thin-film materials of the present invention, adopts multi-layer compound film structure, by increasing the low-loss BMN dielectric layer of one deck thus reduce thin-film dielectric loss in the middle of bst thin film, improves the combination property of film.
The preparation method of dielectric film mainly contains rf magnetron sputtering (RF-Magnetronsputtering), pulsed laser deposition (PLD), metal organic chemical vapor deposition (MOCVD) and sol-gel process (Sol-Gel); Compared with additive method, Preparation of Thin Films by Sol-Gel Method has the advantages such as uniformity is good, stoichiometric proportion easily controls, equipment is simple, has been widely used in the preparation of dielectric film; Simultaneously conventional sol-gel processes prepares bst thin film many employings barium, the alkoxide of strontium or acetate and butyl titanate makes raw material, and cost is higher, raw material unstable chemcial property and not easily obtaining.Using brium carbonate, strontium carbonate and titanium dioxide as raw material, adopt improvement Sol-Gel to prepare BST ferroelectric thin film and have no report; When preparing BMN film, the nitrate of usual use bismuth, magnesium and niobium alkoxide are as raw material, and cost is higher, and the volatile water and cause the composition of final material to depart from of decrystallizing of nitric hydrate magnesium, the present invention utilizes magnesium carbonate to replace nitric hydrate magnesium, adopts Sol-Gel technology to prepare BMN film;
Summary of the invention
Object of the present invention, be the shortcoming and defect overcoming prior art, a kind of BST/BMN/BST multi-layer compound film for microwave-tuned components and parts and preparation method thereof is provided, by increasing the low-loss BMN dielectric layer of one deck thus reduce thin-film dielectric loss in the middle of bst thin film, improve the object of the combination property of film.
The present invention is achieved by following technical solution.
A preparation method for BST/BMN/BST multi-layer compound film, has following steps:
(1) barium strontium titanate precursor sol is prepared
1. titanium-citric acid-ethylene glycol solution is prepared
A () is according to Ba
0.5sr
0.5tiO
3stoichiometric proportion take titanium dioxide powder, titanium dioxide is put into hydrofluoric acid, and heating water bath all dissolves to it;
B () adds ammoniacal liquor in the solution of step (a), neutralization reaction generates metatitanic acid precipitation;
C () suction filtration, washing step (b) gained metatitanic acid precipitate, then add in nitric acid by metatitanic acid, and magnetic agitation is dissolved completely to precipitation, obtains Titanium Nitrate solution; Wherein the mol ratio of metatitanic acid and nitric acid is 1:2;
D () adds citric acid in step (c) gained Titanium Nitrate solution, magnetic agitation makes citric acid dissolve completely; In solution, add ethylene glycol solution again, heating magnetic agitation 2h makes solution mix, and wherein Titanium Nitrate, mol ratio between citric acid and ethylene glycol are 1:4:4;
E (), by step (d) gained solution left standstill 24h, makes reaction carry out completely, obtaining the aqueous solution of nitric acid of titanium-citric acid-ethylene glycol; Solution, through 60 DEG C of magnetic agitation heating 4h, obtains stable titanium-citric acid-glycol water;
2. barium-strontium-citric acid-ethylene glycol solution is prepared
A () prepares citric acid-ethylene glycol solution according to molar ratio 1:4;
B () takes barium titanate, strontium titanates according to the stoichiometric proportion of barium strontium titanate, added in above-mentioned citric acid-ethylene glycol solution, magnetic agitation is heated to powder and all dissolves, and obtains stable barium-strontium-citric acid-ethylene glycol solution;
3. barium-strontium-citric acid-ethylene glycol solution step 2. configured adds step and 1. configures in titanium-citric acid-glycol water, and stir to obtain barium strontium titanate precursor sol;
(2) bismuth niobate magnesium precursor sol is prepared
1. niobium-aqueous citric acid solution is prepared
A () takes niobium pentaoxide, added by niobium pentaoxide powder in hydrofluoric acid, and heating water bath all dissolves to it, wherein Nb
2o
5be 1:10 with the mol ratio of HF;
B () adds ammoniacal liquor in step (a) solution, neutralization generates niobic acid precipitation;
C () filtering and washing step (b) gained niobic acid precipitates, remove F-and NH
4 +;
D step (c) gained niobic acid precipitation adds in aqueous citric acid solution by (), magnetic agitation makes citric acid dissolve completely; Obtain niobium-aqueous citric acid solution, wherein the mol ratio of niobium pentaoxide and citric acid is 1:4 ~ 1:6;
E step (d) gained niobium-aqueous citric acid solution is heated to moisture evaporation through 60 DEG C of magnetic agitation by () complete, obtains stable niobium-citric acid solution;
2. Bi is pressed
1.5mgNb
1.5o
7stoichiometric proportion take five water bismuth nitrates, magnesium carbonate, add step 1. in niobium-aqueous citric acid solution, add thermal agitation and obtain bismuth niobate magnesium precursor sol;
(3) in step (1), (2) obtained barium strontium titanate precursor sol and bismuth niobate magnesium precursor sol, add methyl alcohol and make diluent, add thermal agitation and obtain required barium strontium titanate precursor sol and bismuth niobate magnesium precursor sol;
(4) the barium strontium titanate precursor colloidal sol that step (3) configures is dropped on substrate, with the even glue of desk-top sol evenning machine, colloidal sol is coated on substrate equably, then heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that barium strontium titanate and bst thin film reach thickness;
(5) bismuth niobate magnesium precursor colloidal sol step (3) configured drops on the barium strontium titanate of step (4) gained, and the even glue of desk-top sol evenning machine, makes colloidal sol be coated in equably on substrate, heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that bismuth niobate magnesium and BMN film reach thickness;
(6) the barium strontium titanate precursor colloidal sol that step (3) configures is dripped on the bismuth niobate magnesium film of step (5) gained, with the even glue of desk-top sol evenning machine, colloidal sol is coated on substrate equably, then heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that barium strontium titanate and bst thin film reach thickness;
(7) film after step (6) heat treatment is carried out after annealing in 550 ~ 750 DEG C, obtain BST/BMN/BST multi-layer compound film.
Described step (2) the 1. niobium pentaoxide of (d) and the mol ratio of citric acid is 1:4.
The after annealing temperature of described step (7) is 700 DEG C.
BST/BMN/BST multi-layer compound film of the present invention, by increasing the low-loss BMN dielectric layer of one deck thus reduce thin-film dielectric loss in the middle of two bst thin films, makes the combination property of film be improved.The present invention, using brium carbonate, strontium carbonate and titanium dioxide as raw material, substitutes part alkoxide and butyl titanate, reduces the production cost of film.Magnesium carbonate replaces nitric hydrate magnesium, makes stoicheiometry more accurate; In addition, the present invention adopts improved Sol Gel method to prepare the new technology of dielectric film, the multi-layer compound film excellent performance of acquisition, and process is simple, is that one has broad application prospects.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction resolution chart of embodiment 4.
Detailed description of the invention
The present invention is raw materials used is the pure raw material of commercially available analysis, is described further the present invention below by specific embodiment.
The preparation method of BST/BMN/BST multi-layer compound film of the present invention, step is as follows:
(1) barium strontium titanate precursor sol is prepared
1. titanium-citric acid-ethylene glycol solution is prepared
A () is according to Ba
0.5sr
0.5tiO
3stoichiometric proportion take titanium dioxide powder, titanium dioxide is put into hydrofluoric acid, and heating water bath all dissolves to it;
B () adds ammoniacal liquor in the solution of step (a), neutralization reaction generates metatitanic acid precipitation;
C () suction filtration, washing step (b) gained metatitanic acid precipitate, then add in nitric acid by metatitanic acid, and magnetic agitation is dissolved completely to precipitation, obtains Titanium Nitrate solution; Wherein the mol ratio of metatitanic acid and nitric acid is 1:2;
D () adds 25g citric acid in step (c) gained Titanium Nitrate solution, magnetic agitation makes citric acid dissolve completely; In solution, add 8ml ethylene glycol solution again, heating magnetic agitation 2h makes solution mix,
E (), by step (d) gained solution left standstill 24h, makes reaction carry out completely, obtaining the aqueous solution of nitric acid of titanium-citric acid-ethylene glycol; Solution, through 60 DEG C of magnetic agitation heating 4h, obtains stable titanium-citric acid-glycol water;
2. barium-strontium-citric acid-ethylene glycol solution is prepared
A () prepares citric acid-ethylene glycol solution according to molar ratio 1:4;
B () takes 2.961g barium titanate BaCO according to the stoichiometric proportion of barium strontium titanate
3with 2.214g strontium titanates, added in above-mentioned citric acid-ethylene glycol solution, magnetic agitation is heated to powder and all dissolves, and obtains stable barium-strontium-citric acid-ethylene glycol solution;
3. barium-strontium-citric acid-ethylene glycol solution step 2. configured adds step and 1. configures in titanium-citric acid-glycol water, and stir to obtain barium strontium titanate precursor sol;
(2) bismuth niobate magnesium precursor sol is prepared
1. niobium-aqueous citric acid solution is prepared
A () takes 2.658g niobium pentaoxide powder, added in 5ml hydrofluoric acid, heating water bath all dissolves to it;
B () adds ammoniacal liquor in step (a) solution, neutralization generates niobic acid precipitation;
C () filtering and washing step (b) gained niobic acid precipitates, remove F-and NH
4 +;
D step (c) gained niobic acid precipitation adds in 64g aqueous citric acid solution by (), magnetic agitation makes citric acid dissolve completely; Obtain niobium-aqueous citric acid solution, wherein the mol ratio of niobium pentaoxide and citric acid is 1:3;
E step (d) gained niobium-aqueous citric acid solution is heated to moisture evaporation through 60 DEG C of magnetic agitation by () complete, obtains stable niobium-citric acid solution;
3. take 4.851g five water bismuth nitrate, 0.562g magnesium carbonate by the stoichiometric proportion of bismuth niobate magnesium, add step 1. in niobium-aqueous citric acid solution, add thermal agitation and obtain bismuth niobate magnesium precursor sol;
(3) in step (1), (2) obtained barium strontium titanate precursor sol and bismuth niobate magnesium precursor sol, add methyl alcohol and make diluent, add thermal agitation and obtain required barium strontium titanate precursor sol and bismuth niobate magnesium precursor sol;
(4) the barium strontium titanate precursor colloidal sol that step (3) configures is dropped on substrate, with the even glue of desk-top sol evenning machine, colloidal sol is coated on substrate equably, then heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that barium strontium titanate and bst thin film reach thickness;
(5) bismuth niobate magnesium precursor colloidal sol step (3) configured drops on the barium strontium titanate of step (4) gained, and the even glue of desk-top sol evenning machine, makes colloidal sol be coated in equably on substrate, heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that bismuth niobate magnesium and BMN film reach thickness;
(6) the barium strontium titanate precursor colloidal sol that step (3) configures is dropped on the bismuth niobate magnesium film of step (5) gained, with the even glue of desk-top sol evenning machine, colloidal sol is coated on substrate equably, then heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that barium strontium titanate and bst thin film reach thickness;
(7) film after step (6) heat treatment is carried out after annealing in 550 ~ 750 DEG C, obtain BST/BMN/BST multi-layer compound film.
Distinguishing characteristics and the correlated performance testing result of each embodiment of the present invention and above-mentioned preparation process refer to table 1.
Table 1
Fig. 1 is the X-ray diffraction resolution chart of embodiment 4, adopts the test of Rigaku company DMAX/RC type X-ray diffractometer, shows that this BST/BMN/BST multi-layer compound film is cube BST and BMN phase coexisting structure.
Claims (3)
1. a preparation method for BST/BMN/BST multi-layer compound film, has following steps:
(1) barium strontium titanate precursor sol is prepared
1. titanium-citric acid-ethylene glycol solution is prepared
A () is according to Ba
0.5sr
0.5tiO
3stoichiometric proportion take titanium dioxide powder, titanium dioxide is put into hydrofluoric acid, and heating water bath all dissolves to it;
B () adds ammoniacal liquor in the solution of step (a), neutralization reaction generates metatitanic acid precipitation;
C () suction filtration, washing step (b) gained metatitanic acid precipitate, then add in nitric acid by metatitanic acid, and magnetic agitation is dissolved completely to precipitation, obtains Titanium Nitrate solution; Wherein the mol ratio of metatitanic acid and nitric acid is 1:2;
D () adds citric acid in step (c) gained Titanium Nitrate solution, magnetic agitation makes citric acid dissolve completely; In solution, add ethylene glycol solution again, heating magnetic agitation 2h makes solution mix, and wherein Titanium Nitrate, mol ratio between citric acid and ethylene glycol are 1:4:4;
E (), by the solution left standstill 24h of previous step gained, makes reaction carry out completely, obtaining the aqueous solution of nitric acid of titanium-citric acid-ethylene glycol; Solution, through 60 DEG C of magnetic agitation heating 4h, obtains stable titanium-citric acid-glycol water;
2. barium-strontium-citric acid-ethylene glycol solution is prepared
A () prepares citric acid-ethylene glycol solution according to molar ratio 1:4;
B () takes barium titanate, strontium titanates according to the stoichiometric proportion of barium strontium titanate, added in above-mentioned citric acid-ethylene glycol solution, magnetic agitation is heated to powder and all dissolves, and obtains stable barium-strontium-citric acid-ethylene glycol solution;
3. barium-strontium-citric acid-ethylene glycol solution step 2. configured adds in titanium-citric acid-ethylene glycol solution that 1. step configure, and stir to obtain barium strontium titanate precursor sol;
(2) bismuth niobate magnesium precursor sol is prepared
1. niobium-aqueous citric acid solution is prepared
A () takes niobium pentaoxide, added by niobium pentaoxide powder in hydrofluoric acid, and heating water bath all dissolves to it, wherein Nb
2o
5be 1:10 with the mol ratio of HF;
B () adds ammoniacal liquor in the solution of previous step gained, neutralization generates niobic acid precipitation;
C () filtering and washing step (b) gained niobic acid precipitates, remove F
-with NH
4 +;
D step (c) gained niobic acid precipitation adds in aqueous citric acid solution by (), magnetic agitation makes citric acid dissolve completely; Obtain niobium-aqueous citric acid solution, wherein the mol ratio of niobium pentaoxide and citric acid is 1:4 ~ 1:6;
E step (d) gained niobium-aqueous citric acid solution is heated to moisture evaporation through 60 DEG C of magnetic agitation by () complete, obtains stable niobium-citric acid solution;
2. Bi is pressed
1.5mgNb
1.5o
7stoichiometric proportion take five water bismuth nitrates, magnesium carbonate, add step 1. in niobium-aqueous citric acid solution, add thermal agitation and obtain bismuth niobate magnesium precursor sol;
(3) in step (1), (2) obtained barium strontium titanate precursor sol and bismuth niobate magnesium precursor sol, add methyl alcohol and make diluent, add thermal agitation and obtain required barium strontium titanate precursor sol and bismuth niobate magnesium precursor sol;
(4) the barium strontium titanate precursor colloidal sol that step (3) configures is dropped on substrate, with the even glue of desk-top sol evenning machine, colloidal sol is coated on substrate equably, then heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that barium strontium titanate and bst thin film reach thickness;
(5) bismuth niobate magnesium precursor colloidal sol step (3) configured drops on the barium strontium titanate of step (4) gained, and the even glue of desk-top sol evenning machine, makes colloidal sol be coated in equably on substrate, heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that bismuth niobate magnesium and BMN film reach thickness;
(6) the barium strontium titanate precursor colloidal sol that step (3) configures is dripped on the bismuth niobate magnesium film of step (5) gained, with the even glue of desk-top sol evenning machine, colloidal sol is coated on substrate equably, then heat treatment at 500 DEG C, organics removal; Repeat spin coating-heat treatment process, until it is 100nm that barium strontium titanate and bst thin film reach thickness;
(7) film after step (6) heat treatment is carried out after annealing in 550 ~ 750 DEG C, obtain BST/BMN/BST multi-layer compound film.
2. the preparation method of BST/BMN/BST multi-layer compound film according to claim 1, is characterized in that, described step (2) the 1. niobium pentaoxide of (d) and the mol ratio of citric acid is 1:4.
3. the preparation method of BST/BMN/BST multi-layer compound film according to claim 1, is characterized in that, the after annealing temperature of described step (7) is 700 DEG C.
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| CN104087904B (en) * | 2014-07-08 | 2016-06-29 | 天津大学 | A kind of preparation method of high tuning rate BMNT thin-film material |
| CN108467267A (en) * | 2018-03-23 | 2018-08-31 | 天津大学 | A kind of three layers of composite dielectric materials of temperature-stable |
| CN108411256B (en) * | 2018-03-28 | 2020-03-03 | 天津大学 | Preparation method of BTS/BST/BZT multilayer structure dielectric tuning film |
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| CN102229265B (en) * | 2011-04-29 | 2013-09-25 | 中国科学院合肥物质科学研究院 | Barium strontium titanate multilayered film, and preparation method thereof |
| CN102249307B (en) * | 2011-05-06 | 2012-12-12 | 天津大学 | Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film |
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