CN102249307A - Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film - Google Patents

Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film Download PDF

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CN102249307A
CN102249307A CN2011101166513A CN201110116651A CN102249307A CN 102249307 A CN102249307 A CN 102249307A CN 2011101166513 A CN2011101166513 A CN 2011101166513A CN 201110116651 A CN201110116651 A CN 201110116651A CN 102249307 A CN102249307 A CN 102249307A
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bismuth
magnesium
niobium
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CN102249307B (en
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李玲霞
宁平凡
吴海涛
冀璐洁
王洪茹
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Tianjin University
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Abstract

The invention discloses a preparation method of a BMN dielectric film, comprising the steps of: (1) preparing a citric acid water solution of niobium; (2) adding glycol into the water solution, and conducting heating and stirring; (3) preparing a glycol solution of magnesium and bismuth; (4) adding the prepared glycol solution of magnesium and bismuth into the solution obtained in step (2), thus obtaining a bismuth-magnesium-niobium sol; (5) adding ethanol into the bismuth-magnesium-niobium sol, and carrying out heating and stirring so as to obtain a bismuth-magnesium-niobium precursor solution; (6) coating a substrate with the precursor solution uniformly and drying the substrate; (7) subjecting a dried film to a heat treatment at a temperature of 500-800DEG C for 10min; (8) repeating step (6) and (7) so as to prepare a multilayered film; (9) conducting a heat treatment to the multilayer film at a temperature of 550-800DEG C for 0.5-2h, thus obtaining a BMN dielectric film with a cubic pyrochlore structure. With accurately controlled chemical components and high density, the BMN dielectric film provided in the invention has no crack and pin hole as well as other defects. Characterized by simple process and low cost, the film of the invention as a microwave dielectric adjustable material boasts good application prospects.

Description

The preparation method of niobic acid bismuth magnesium dielectric film
Technical field
The invention relates to electronic information material and components and parts field, the particularly a kind of Bi that is used for microwave-tuned components and parts 1.5MgNb 1.5O 7The preparation method of dielectric thin-film material.
Background technology
Along with the fast development of microwave telecommunication system, people are to microwave device, and especially microwave-tuned device is had higher requirement.Have fast response speed, little size, broadband and highly sensitive, the microwave device of low operating voltage is present and the requisite integral part of next generation communication system.These require to give present electronic material and components and parts to bring great challenge.
The micro-wave dielectric material with adjustable has wide application prospect on the adjustable components and parts of microwave, as the phase shifter on the phased array antenna, resonator, wave filter etc.With regard to material system, the strontium-barium titanate BST (Ba of perovskite structure xSr 1-xTiO 3) sill is the class dielectric adjustable microwave medium material the most widely of research at present.The characteristics of BST based film material are dielectric tuning rate height, but dielectric loss is big, common tg δ＞0.01, and the minimal losses of report is 0.005.
The Bi of cube pyrochlore structure 1.5ZnNb 1.5O 7(BZN) and Bi 1.5MgNb 1.5O 7(BMN) material also has dielectric adjustable, and its dielectric loss is lower than BST.BMN compares with BZN has bigger dielectric adjustable and BMN thin-film dielectric loss little (about 0.002), specific inductivity moderate (about 86), and the temperature stability of performance is good.And owing to do not contain volatile Zn, the relative BZN material of film preparation is than being easier to, and is better repeated.The burnt green stone material of BMN bismuthino is a kind of very promising novel microwave dielectric material with adjustable.
Along with the miniaturization of development of electronic devices and integrated, thin-film material has embodied great superiority, so thin-film material related process and Study on Theory have obtained suitable attention.Research work to the BMN thin film preparation process just begins, and human magnetron sputtering techniques such as Jiang Shuwen have prepared the BMN dielectric film, but magnetron sputtering technique exists the target density is had relatively high expectations and shortcoming such as chemical composition is wayward.Wet chemical method has that technology is simple, the film chemical component of preparation evenly, be easy to advantage such as ion doping modification.
Summary of the invention
Purpose of the present invention is overcome that magnetron sputtering technique exists the target density is had relatively high expectations and shortcoming such as chemical composition is wayward, and a kind of preparation method who utilizes the niobic acid bismuth magnesium dielectric film of polymkeric substance precursor method preparation cube pyrochlore structure is provided.
The present invention is achieved by following technical solution, and step is as follows.
(1) aqueous citric acid solution of preparation niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing Nb 2O 5, with Nb 2O 5Put into hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) add ammoniacal liquor in above-mentioned solution, regulating pH value is 8～9 generation niobic acid precipitations;
(c) the above-mentioned precipitation of filtering and washing adds niobic acid in the lemon aqueous acid then, obtains the aqueous citric acid solution of niobium, and wherein the mol ratio of niobium ion and citric acid is 1: 2～1: 6;
(2) in the aqueous citric acid solution of the niobium that step (1) makes, add ethylene glycol, heated and stirred, the mole of citric acid and ethylene glycol is 1: 1～1: 4.
(3) ethylene glycol solution of preparation magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrates, is dissolved in the ethylene glycol to stir.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate, is dissolved in the ethylene glycol to stir.
(4) with step (3) (a), the ethylene glycol solution of (3) bismuth of (b) disposing and the ethylene glycol solution of magnesium add in the liquid of step (2) configuration, stir bismuth magnesium niobium colloidal sol;
(5) add 5～40ml ethanol in the bismuth magnesium niobium colloidal sol that step (4) makes and make thinner, heated and stirred obtains bismuth magnesium niobium precursor liquid;
(6) precursor liquid with step (5) preparation drops on the substrate, with the even glue of desk-top sol evenning machine, precursor liquid is coated on the substrate equably, and is dry on hot plate then;
(7) the dried film of step (6) is heat-treated 10min at 500～800 ℃;
(8) repeating step (6), (7) preparation multilayer film;
(9) multilayer film that step (8) is prepared obtains the niobic acid bismuth magnesium dielectric film of cube pyrochlore structure at 550～800 ℃ of thermal treatment 0.5～2h.
The amount of the hydrofluoric acid of described step (1) is every 0.03mol Nb 2O 5Use hydrofluoric acid 5～8ml
The concentration of the bismuth magnesium niobium precursor liquid of described step (5) is 0.05～1mol/L.
The substrate of described step (6) is indium tin oxide-coated glass substrate or the Si substrate that has metal electrode.
The hot plate temperature of described step (6) is 100～200 ℃.
The thickness of the niobic acid bismuth magnesium dielectric film of described step (9) is 100 nanometers～10 micron.
The invention has the beneficial effects as follows, a kind of niobic acid bismuth magnesium (BMN) film of single thing phase cube pyrochlore structure of easy preparation is provided, advantage with accurate control film chemical component, higher-density, there are not defectives such as crackle and pin hole, and preparation technology is simple, replaced the expensive raw material niobium alkoxides that uses in the conventional wet chemistry method with Niobium Pentxoxide, with low cost, have a good application prospect.
Embodiment
The present invention is further described below by example, raw materials usedly in the example is commercially available analytical pure raw material.Specific embodiment is as follows:
Embodiment 1
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing the Nb of 0.003mol 2O 5, with Nb 2O 5Put into 5ml hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) adding ammoniacal liquor in the above-mentioned solution, to regulate pH value be 8 to generate the niobic acids precipitation;
(c) the above-mentioned precipitation of filtering and washing joins niobic acid in the lemon aqueous acid then, and heating in water bath makes niobic acid be dissolved in the lemon aqueous acid fully, obtains the aqueous citric acid solution of niobium, and the content of citric acid is 0.012mol.
2. add ethylene glycol in the aqueous citric acid solution of the niobium that step 1 makes, heated and stirred, the add-on of ethylene glycol are 0.012mol.
3. prepare the ethylene glycol solution of magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrate 0.006mol, is dissolved in the 0.005mol ethylene glycol.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate 0.004mol, is dissolved in the 0.005mol ethylene glycol.
4. the ethylene glycol solution of the ethylene glycol solution of the bismuth that step 3 (a), 3 (b) are disposed and magnesium adds in the liquid of step 2 configuration, and 70 ℃ of heated and stirred 2h get bismuth magnesium niobium colloidal sol.
5. add 40ml ethanol and make thinner in the bismuth magnesium niobium colloidal sol that step 4 makes, heated and stirred obtains bismuth magnesium niobium precursor liquid;
6. the precursor liquid with step 5 preparation drops on the indium tin oxide-coated glass substrate, with the even glue of desk-top sol evenning machine precursor liquid is coated on the substrate equably, and is dry on 100 ℃ hot plate then;
7. dried film is heat-treated 10min at 500 ℃;
8. repeating step 6～7 three time, preparation multilayer BMN film;
With the preparation multilayer film at 550 ℃ of thermal treatment 2h, obtain a cube pyrochlore structure BMN dielectric film.
Adopt the Japanese DMAX/RC of company type X-ray diffractometer test of science, film is a cube pyrochlore structure; Adopt the test of the U.S. DEKTAK6M of VEECO company face topography measurement instrument, the thickness of film is 220 nanometers; Adopt field emission scanning electron microscope (JEOL JSM-7600F, Japan) test, the fine and close flawless of film.
Embodiment 2
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing the Nb of 0.003mol 2O 5, with Nb 2O 5Put into 6ml hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) adding ammoniacal liquor in the above-mentioned solution, to regulate pH value be 9 to generate the niobic acids precipitation;
(c) the above-mentioned precipitation of filtering and washing joins niobic acid in the lemon aqueous acid then, and heating in water bath makes niobic acid be dissolved in the lemon aqueous acid fully, obtains the aqueous citric acid solution of niobium, and the content of citric acid is 0.02mol.
2. add ethylene glycol in the aqueous citric acid solution of the niobium that step 1 makes, heated and stirred, the add-on of ethylene glycol are 0.08mol.
3. prepare the ethylene glycol solution of magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrate 0.006mol, is dissolved in the 0.005mol ethylene glycol.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate 0.004mol, is dissolved in the 0.005mol ethylene glycol.
4. the ethylene glycol solution of the ethylene glycol solution of the bismuth that step 3 (a), 3 (b) are disposed and magnesium adds in the liquid of step 2 configuration, and 90 ℃ of heated and stirred 2h get bismuth magnesium niobium colloidal sol.
5. add 20ml ethanol and make thinner in the bismuth magnesium niobium colloidal sol that step 4 makes, heated and stirred obtains bismuth magnesium niobium precursor liquid.
6. the precursor liquid with step 5 preparation drops on the indium tin oxide-coated glass substrate, with the even glue of desk-top sol evenning machine precursor liquid is coated on the substrate equably, and is dry on 120 ℃ hot plate then.
7. dried film is heat-treated 10min at 550 ℃.
8. repeating step 6～7 five time, preparation multilayer BMN film.
With the preparation multilayer film at 600 ℃ of thermal treatment 2h, obtain a cube pyrochlore structure BMN dielectric film.
Adopt the Japanese DMAX/RC of company type X-ray diffractometer test of science, film is a cube pyrochlore structure; Adopt the test of the U.S. DEKTAK6M of VEECO company face topography measurement instrument, the thickness of film is 500 nanometers; Adopt field emission scanning electron microscope (JEOL JSM-7600F, Japan) test, the fine and close flawless of film.
Embodiment 3
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing the Nb of 0.003mol 2O 5, with Nb 2O 5Put into 8ml hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) adding ammoniacal liquor in the above-mentioned solution, to regulate pH value be 9 to generate the niobic acids precipitation;
(c) the above-mentioned precipitation of filtering and washing joins niobic acid in the lemon aqueous acid then, and heating in water bath makes niobic acid be dissolved in the lemon aqueous acid fully, obtains the aqueous citric acid solution of niobium, and the content of citric acid is 0.028mol.
2. add ethylene glycol in the aqueous citric acid solution of the niobium that step 1 makes, heated and stirred, the add-on of ethylene glycol are 0.056mol.
3. prepare the ethylene glycol solution of magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrate 0.006mol, is dissolved in the 0.005mol ethylene glycol.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate 0.004mol, is dissolved in the 0.005mol ethylene glycol.
4. the ethylene glycol solution of the ethylene glycol solution of the bismuth that step 3 (a), 3 (b) are disposed and magnesium adds in the liquid of step 2 configuration, and 60 ℃ of heated and stirred 2h get bismuth magnesium niobium colloidal sol.
5. add 25ml ethanol and make thinner in the bismuth magnesium niobium colloidal sol that step 4 makes, heated and stirred obtains bismuth magnesium niobium precursor liquid.
6. the precursor liquid with step 5 preparation drops on the indium tin oxide-coated glass substrate, with the even glue of desk-top sol evenning machine precursor liquid is coated on the substrate equably, and is dry on 150 ℃ hot plate then.
7. dried film is heat-treated 10min at 600 ℃.
8. repeating step 6～7 eight time, preparation multilayer BMN film.
With the preparation multilayer film at 700 ℃ of thermal treatment 2h, obtain a cube pyrochlore structure BMN dielectric film.
Adopt the Japanese DMAX/RC of company type X-ray diffractometer test of science, film is a cube pyrochlore structure; Adopt the test of the U.S. DEKTAK6M of VEECO company face topography measurement instrument, the thickness of film is 7 microns; Adopt field emission scanning electron microscope (JEOL JSM-7600F, Japan) test, the fine and close flawless of film.
Embodiment 4
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing the Nb of 0.003mol 2O 5, with Nb 2O 5Put into 5ml hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) adding ammoniacal liquor in the above-mentioned solution, to regulate pH value be 9 to generate the niobic acids precipitation;
(c) the above-mentioned precipitation of filtering and washing joins niobic acid in the lemon aqueous acid then, and heating in water bath makes niobic acid be dissolved in the lemon aqueous acid fully, obtains the aqueous citric acid solution of niobium, and the content of citric acid is 0.036mol.
2. add ethylene glycol in the aqueous citric acid solution of the niobium that step 1 makes, heated and stirred, the add-on of ethylene glycol are 0.08mol.
3. prepare the ethylene glycol solution of magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrate 0.006mol, is dissolved in the 0.005mol ethylene glycol.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate 0.004mol, is dissolved in the 0.005mol ethylene glycol.
4. the ethylene glycol solution of the ethylene glycol solution of the bismuth that step 3 (a), 3 (b) are disposed and magnesium adds in the liquid of step 2 configuration, and 60 ℃ of heated and stirred 2h get bismuth magnesium niobium colloidal sol.
5. add 5ml ethanol and make thinner in the bismuth magnesium niobium colloidal sol that step 4 makes, heated and stirred obtains bismuth magnesium niobium precursor liquid.
6. the precursor liquid with step 5 preparation drops on the Si substrate, with the even glue of desk-top sol evenning machine precursor liquid is coated on the substrate equably, and is dry on 120 ℃ hot plate then.
7. dried film is heat-treated 10min at 800 ℃.
8. repeating step 6～7 eight time, preparation multilayer BMN film.
With the preparation multilayer film at 800 ℃ of thermal treatment 2h, obtain a cube pyrochlore structure BMN dielectric film.
Adopt the Japanese DMAX/RC of company type X-ray diffractometer test of science, film is a cube pyrochlore structure; Adopt the test of the U.S. DEKTAK6M of VEECO company face topography measurement instrument, the thickness of film is 10 microns; Adopt field emission scanning electron microscope (JEOL JSM-7600F, Japan) test, the fine and close flawless of film.
Embodiment 5
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing the Nb of 0.003mol 2O 5, with Nb 2O 5Put into 6ml hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) adding ammoniacal liquor in the above-mentioned solution, to regulate pH value be 8 to generate the niobic acids precipitation;
(c) the above-mentioned precipitation of filtering and washing joins niobic acid in the lemon aqueous acid then, and heating in water bath makes niobic acid be dissolved in the lemon aqueous acid fully, obtains the aqueous citric acid solution of niobium, and the content of citric acid is 0.03mol.
2. add ethylene glycol in the aqueous citric acid solution of the niobium that step 1 makes, heated and stirred, the add-on of ethylene glycol are 0.09mol.
3. prepare the ethylene glycol solution of magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrate 0.006mol, is dissolved in the 0.005mol ethylene glycol.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate 0.004mol, is dissolved in the 0.005mol ethylene glycol.
4. the ethylene glycol solution of the ethylene glycol solution of the bismuth that step 3 (a), 3 (b) are disposed and magnesium adds in the liquid of step 2 configuration, and 80 ℃ of heated and stirred 2h get bismuth magnesium niobium colloidal sol.
5. add 35ml ethanol and make thinner in the bismuth magnesium niobium colloidal sol that step 4 makes, heated and stirred obtains bismuth magnesium niobium precursor liquid.
6. the precursor liquid with step 5 preparation drops on the Si substrate, with the even glue of desk-top sol evenning machine precursor liquid is coated on the substrate equably, and is dry on 200 ℃ hot plate then.
7. dried film is heat-treated 10min at 700 ℃.
8. repeating step 6～7 once.
With the preparation multilayer film at 750 ℃ of thermal treatment 2h, obtain a cube pyrochlore structure BMN dielectric film.
Adopt the Japanese DMAX/RC of company type X-ray diffractometer test of science, film is a cube pyrochlore structure; Adopt the test of the U.S. DEKTAK6M of VEECO company face topography measurement instrument, the thickness of film is 100 nanometers; Adopt field emission scanning electron microscope (JEOL JSM-7600F, Japan) test, the fine and close flawless of film.
Embodiment 6
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing the Nb of 0.003mol 2O 5, with Nb 2O 5Put into 5ml hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) adding ammoniacal liquor in the above-mentioned solution, to regulate pH value be 8 to generate the niobic acids precipitation;
(c) the above-mentioned precipitation of filtering and washing joins niobic acid in the lemon aqueous acid then, and heating in water bath makes niobic acid be dissolved in the lemon aqueous acid fully, obtains the aqueous citric acid solution of niobium, and the content of citric acid is 0.036mol.
2. add ethylene glycol in the aqueous citric acid solution of the niobium that step 1 makes, heated and stirred, the add-on of ethylene glycol are 0.08mol.
3. prepare the ethylene glycol solution of magnesium and bismuth
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing five water Bismuth trinitrate 0.006mol, is dissolved in the 0.005mol ethylene glycol.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio takes by weighing magnesium nitrate hexahydrate 0.004mol, is dissolved in the 0.005mol ethylene glycol.
4. the ethylene glycol solution of the ethylene glycol solution of the bismuth that step 3 (a), 3 (b) are disposed and magnesium adds in the liquid of step 2 configuration, and 60 ℃ of heated and stirred 2h get bismuth magnesium niobium colloidal sol.
5. add 30ml ethanol and make thinner in the bismuth magnesium niobium colloidal sol that step 4 makes, heated and stirred obtains bismuth magnesium niobium precursor liquid.
6. the precursor liquid with step 5 preparation drops on the Si substrate, with the even glue of desk-top sol evenning machine precursor liquid is coated on the substrate equably, and is dry on 160 ℃ hot plate then.
7. dried film is heat-treated 10min at 650 ℃.
8. repeating step 6～7 five time, preparation multilayer BMN film.
With the preparation multilayer film at 750 ℃ of thermal treatment 2h, obtain a cube pyrochlore structure BMN dielectric film.
Adopt the Japanese DMAX/RC of company type X-ray diffractometer test of science, film is a cube pyrochlore structure; Adopt the test of the U.S. DEKTAK6M of VEECO company face topography measurement instrument, the thickness of film is 1 micron; Adopt field emission scanning electron microscope (JEOL JSM-7600F, Japan) test, the fine and close flawless of film.

Claims (6)

1. the preparation method of a niobic acid bismuth magnesium dielectric film has following steps:
(1) aqueous citric acid solution of preparation niobium
(a) according to Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing Nb 2O 5, with Nb 2O 5Put into hydrofluoric acid, heating in water bath is to Nb 2O 5All dissolvings;
(b) add ammoniacal liquor in above-mentioned solution, regulating pH value is 8～9 generation niobic acid precipitations;
(c) the above-mentioned precipitation of filtering and washing adds niobic acid in the lemon aqueous acid then, obtains the aqueous citric acid solution of niobium, and wherein the mol ratio of niobium ion and citric acid is 1: 2～1: 6;
(2) in the aqueous citric acid solution of the niobium that step (1) makes, add ethylene glycol, heated and stirred, the mole of citric acid and ethylene glycol is 1: 1～1: 4.
(3) ethylene glycol solution of preparation bismuth and magnesium
(a) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing five water Bismuth trinitrates, be dissolved in the ethylene glycol and stir.
(b) press Bi 1.5MgNb 1.5O 7Stoichiometric ratio take by weighing magnesium nitrate hexahydrate, be dissolved in the ethylene glycol and stir.
(4) with step (3) (a), the ethylene glycol solution of (3) bismuth of (b) disposing and the ethylene glycol solution of magnesium add in the liquid of step (2) configuration, stir bismuth magnesium niobium colloidal sol;
(5) add 5～40ml ethanol in the bismuth magnesium niobium colloidal sol that step (4) makes and make thinner, heated and stirred obtains bismuth magnesium niobium precursor liquid;
(6) precursor liquid with step (5) preparation drops on the substrate, with the even glue of desk-top sol evenning machine, precursor liquid is coated on the substrate equably, and is dry on hot plate then;
(7) the dried film of step (6) is heat-treated 10min at 500～800 ℃;
(8) repeating step (5), (7) preparation multilayer film;
(9) multilayer film that step (8) is prepared obtains the niobic acid bismuth magnesium dielectric film of cube pyrochlore structure at 550～800 ℃ of thermal treatment 0.5～2h.
2. according to the preparation method of the niobic acid bismuth magnesium dielectric film of claim 1, it is characterized in that the amount of the hydrofluoric acid of described step (1) is every 0.03mol Nb 2O 5Use hydrofluoric acid 5～8ml.
3. according to the preparation method of the niobic acid bismuth magnesium dielectric film of claim 1, it is characterized in that the concentration of the bismuth magnesium niobium precursor liquid of described step (5) is 0.05～1mol/L.
4. according to the preparation method of the niobic acid bismuth magnesium dielectric film of claim 1, it is characterized in that the substrate of described step (6) is indium tin oxide-coated glass substrate or the Si substrate that has metal electrode.
5. according to the preparation method of the niobic acid bismuth magnesium dielectric film of claim 1, it is characterized in that the hot plate temperature of described step (6) is 100～200 ℃.
6. according to the preparation method of the niobic acid bismuth magnesium dielectric film of claim 1, it is characterized in that the thickness of the niobic acid bismuth magnesium dielectric film of described step (9) is 100 nanometers～10 micron.
CN 201110116651 2011-05-06 2011-05-06 Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film Expired - Fee Related CN102249307B (en)

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CN111876756A (en) * 2020-07-15 2020-11-03 齐鲁工业大学 BMN multilayer dielectric film and preparation method thereof
CN113402275A (en) * 2021-08-12 2021-09-17 齐鲁工业大学 Multilayer BMN dielectric thin film material and preparation method thereof
CN117328046A (en) * 2023-09-22 2024-01-02 齐鲁工业大学(山东省科学院) BZN/BMN dielectric tuning composite film with heterostructure and preparation method thereof
CN117486608A (en) * 2023-11-16 2024-02-02 齐鲁工业大学(山东省科学院) BMZN film material with adjustable dielectric and low dielectric loss, and preparation method and application thereof

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CN113402275A (en) * 2021-08-12 2021-09-17 齐鲁工业大学 Multilayer BMN dielectric thin film material and preparation method thereof
CN113402275B (en) * 2021-08-12 2022-09-02 齐鲁工业大学 Multilayer BMN dielectric thin film material and preparation method thereof
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CN117328046B (en) * 2023-09-22 2024-04-26 齐鲁工业大学(山东省科学院) BZN/BMN dielectric tuning composite film with heterostructure and preparation method thereof
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