CN109279614B - Bi2SiO5Bismuth silicate film material and preparation method and application thereof - Google Patents

Bi2SiO5Bismuth silicate film material and preparation method and application thereof Download PDF

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CN109279614B
CN109279614B CN201811348246.2A CN201811348246A CN109279614B CN 109279614 B CN109279614 B CN 109279614B CN 201811348246 A CN201811348246 A CN 201811348246A CN 109279614 B CN109279614 B CN 109279614B
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bismuth silicate
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CN109279614A (en
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包定华
柯一夫
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Sun Yat Sen University
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract

The invention discloses a Bi2SiO5The preparation method comprises the steps of selecting acetylacetone to match tetraethyl orthosilicate and cooperating with organic salt solution containing Bi to prepare a bismuth silicate precursor film, sintering the bismuth silicate precursor film at a specific temperature, and successfully preparing Bi2SiO5Bismuth silicate film material. The method is a chemical solution deposition method, does not need vacuum conditions, has low sintering temperature, simple preparation process and low cost, and the prepared Bi2SiO5The bismuth silicate film material is uniform and compact, has no impurity phase generation, has stable dielectric constant, smaller dielectric loss, higher Curie temperature, good dielectric property, no lead, environmental friendliness and no toxicity; can be used for preparing dielectric film capacitors and has important application prospect in the fields of microelectronic devices such as photoelectric devices and the like and integrated circuits.

Description

Bi2SiO5Bismuth silicate film material and preparation method and application thereof
Technical Field
The invention relates to the technical field of functional thin film materials, in particular to Bi2SiO5Bismuth silicate film material and its preparation method and application.
Background
Pb-containing perovskite oxides such as PbTiO3、Pb(Zr,Ti)O3Etc. although having a high dielectric constant, the use of Pb has been banned in many places because Pb is toxic and volatile, which presents serious environmental problems. Such as BaTiO3The lead-free materials have low Curie temperature (120 ℃), so that the application range is limited, and the research of novel dielectric materials is significant, particularly lead-free thin film materials with high Curie temperature.
Therefore, it is necessary to develop a lead-free dielectric thin film material having a high curie temperature and a method for preparing the same.
Disclosure of Invention
In order to overcome the defect of lower Curie temperature in the prior art, the invention provides Bi2SiO5The preparation method of the bismuth silicate film material adopts a chemical solution deposition method, does not need vacuum conditions, has low sintering temperature and simple preparation process, and the prepared Bi2SiO5The bismuth silicate film material has high Curie temperature, good dielectric property, no lead and no para-ringIs environment-friendly.
Another object of the present invention is to provide Bi2SiO5Bismuth silicate film material.
It is still another object of the present invention to provide the above-mentioned Bi2SiO5The bismuth silicate film material is applied to a dielectric film material.
It is still another object of the present invention to provide the above-mentioned Bi2SiO5The bismuth silicate film material is applied to the preparation of dielectric film capacitors.
It is still another object of the present invention to provide the above-mentioned Bi2SiO5The bismuth silicate film material is applied to the preparation of photoelectric devices.
In order to solve the technical problems, the invention adopts the technical scheme that:
bi2SiO5The preparation method of the bismuth silicate film material comprises the following steps:
s1, preparing an acidic organic salt solution containing Bi;
s2, uniformly mixing tetraethyl orthosilicate and acetylacetone to obtain a mixed solution; the molar ratio of the acetylacetone to the tetraethyl orthosilicate is (2.0-3.0) to 1.0;
s3, uniformly mixing the mixed solution in the step S2 with the organic salt solution in the step S1 at room temperature, and reacting to obtain a bismuth silicate precursor solution;
s4, preparing a bismuth silicate precursor film on the substrate by using the bismuth silicate precursor solution prepared in the step S3;
s5, performing heat treatment on the bismuth silicate precursor film obtained in the step S4 to prepare Bi2SiO5Bismuth silicate film material; the temperature of the heat treatment is 475-575 ℃.
The method comprises the steps of selecting acetylacetone and tetraethyl orthosilicate with the molar ratio of (2.0-3.0) to 1.0, cooperating with organic salt solution containing Bi, reacting tetraethyl orthosilicate with water in air under the catalysis of acid to hydrolyze and polymerize to obtain bismuth silicate precursor solution, carrying out heat treatment on a bismuth silicate precursor film prepared from the bismuth silicate precursor solution at a specific temperature of 475-575 ℃, and carrying out heat treatment on the bismuth silicate precursor filmLine annealing is carried out to successfully prepare Bi2SiO5Bismuth silicate film material. Bi2SiO5Bismuth silicate is a silicon-oxygen tetrahedral chain (SiO)4 4+) And Bi2O2 2-And (3) alternately arranging the formed laminated structure materials.
The preparation method is a chemical solution deposition method, does not need vacuum conditions, has low sintering temperature, simple preparation process and low cost, and the prepared Bi2SiO5The bismuth silicate film material is uniform and compact, has no impurity phase generation, has stable dielectric constant, smaller dielectric loss, higher Curie temperature, good dielectric property, no lead, environmental friendliness and no toxicity; can be used for preparing dielectric film capacitors and has a middle-inferior application prospect in the fields of microelectronic devices such as photoelectric devices and integrated circuits. Moreover, the chemical solution deposition method is easy to control the components of the film, has good uniformity, low preparation cost and low processing temperature, and is easy to form a large-area film.
The acetylacetone and tetraethyl orthosilicate are subjected to substitution reaction to effectively control the hydrolysis rate of the tetraethyl orthosilicate, the molar ratio of the acetylacetone and the tetraethyl orthosilicate is controlled to be (2.0-3.0) to 1.0, so that linear long chains are more prone to be generated during the hydrolysis polymerization of the tetraethyl orthosilicate and combined with Bi, and finally the Bi is generated by heat treatment at the temperature of 475-575 DEG C2SiO5Bismuth silicate film material.
Its curie temperature is approximately 663K.
Preferably, the molar ratio of acetylacetone to tetraethylorthosilicate is 2.0: 1.0. The tetraethoxysilane is easy to hydrolyze, the hydrolysis of the tetraethoxysilane can be effectively inhibited when the molar ratio of the acetylacetone to the tetraethoxysilane is 2.0: 1.0, and the viscosity can be controlled not to be too large.
Preferably, the temperature of the heat treatment in step S4. is 500 ℃.
Preferably, the step s1. specifically includes dissolving bismuth salt with glacial acetic acid and ethylene glycol monomethyl ether to prepare the organic salt solution.
Preferably, the volume ratio of the glacial acetic acid to the ethylene glycol monomethyl ether is (2.0-3.0) to 1.0. Ethylene glycol monomethyl ether is mainly used as a solvent to dissolve bismuth nitrate, and glacial acetic acid is mainly used to dilute the solution and adjust the viscosity of the solution. The reason for controlling the volume ratio of the two components to be (2.0-3.0) to 1.0 is as follows: too much glacial acetic acid may dilute the solution and may result in a discontinuous film being produced, while too little glacial acetic acid may concentrate the solution and may result in an uneven film being produced. The volume ratio of glacial acetic acid to ethylene glycol monomethyl ether is preferably 2.0: 1.0. Therefore, more preferably, the volume ratio of the glacial acetic acid to the ethylene glycol monomethyl ether is 2.0: 1.0.
Preferably, in step S1. glacial acetic acid and ethylene glycol monomethyl ether are stirred by heating to dissolve the bismuth salt. Preferably, the temperature of the heating and stirring is 80 ℃.
Preferably, the amount concentration of the Bi substance in the organic salt solution is 0.40-0.50 mol/L. More preferably, the amount concentration of the substance of Bi in the organic salt solution is 0.44 mol/L.
Preferably, the bismuth salt is bismuth nitrate. Preferably, the bismuth nitrate is bismuth nitrate pentahydrate.
Preferably, the molar ratio of the Bi to the tetraethyl orthosilicate is (2.0-2.2) to 1.0. More preferably, the molar ratio of Bi to tetraethyl orthosilicate is 2.2: 1.0.
Preferably, the reaction time in the step S3 is 3-5 h. More preferably, the reaction time in step s3. is 4 h.
Preferably, the specific step of preparing the bismuth silicate precursor film in the step s4. is to prepare a wet bismuth silicate precursor film on the substrate, dry the wet bismuth silicate precursor film after drying to obtain a dry bismuth silicate precursor film, and repeating the steps for a plurality of times to prepare the bismuth silicate precursor film with a plurality of layers of dry bismuth silicate precursor films.
In general, Bi2SiO5The thickness of the bismuth silicate film material is 300 nm. The thickness of the primary coating film is generally about 50 nm.
Preferably, in step s4, a bismuth silicate precursor wet film is prepared on the substrate by spin coating.
Preferably, in the spin coating method, the spin coating speed is 3000rpm, and the spin coating time is 30 s.
Preferably, the drying temperature in the step S4 is 320-380 ℃. More preferably, the temperature for drying in step s4. is 350 ℃.
Preferably, in the step S4, the temperature rise rate of the heat treatment is 3-5 ℃/min. More preferably, in step S4, the temperature rise rate of the heat treatment is 3 ℃/min. Preferably, the heat preservation time of the heat treatment in the step S4 is more than 1 h.
The invention also protects Bi prepared by the preparation method2SiO5Bismuth silicate film material. The bismuth silicate film material has the advantages of higher Curie temperature, good dielectric property, no lead and environmental friendliness.
Bi as defined above2SiO5The application of the bismuth silicate film material in the dielectric film material is also within the protection scope of the invention.
Meanwhile, the invention also protects the Bi2SiO5The application of bismuth silicate film material in preparing microelectronic device.
The invention also protects the Bi2SiO5The bismuth silicate film material is applied to the preparation of dielectric film capacitors.
The invention also protects the Bi2SiO5The bismuth silicate film material is applied to the preparation of photoelectric devices.
Compared with the prior art, the invention has the beneficial effects that:
the invention successfully prepares Bi by selecting acetylacetone to match tetraethyl orthosilicate and cooperating with organic salt solution containing Bi to prepare the bismuth silicate precursor film which is sintered at a specific temperature2SiO5Bismuth silicate film material. The preparation method is a chemical solution deposition method, does not need vacuum conditions, has low sintering temperature, simple preparation process and low cost, and the prepared Bi2SiO5The bismuth silicate film material is uniform and compact, has no impurity phase generation, has stable dielectric constant, smaller dielectric loss, higher Curie temperature, good dielectric property, no lead, environmental friendliness and no toxicity; can be used for preparing dielectric film capacitor, microelectronic devices such as photoelectric devices and integrated circuitThe domain has a middle-Asian application prospect.
Drawings
FIG. 1 shows Bi of example 12SiO5XRD pattern of bismuth silicate thin film material.
FIG. 2 shows Bi of example 12SiO5Dielectric temperature spectrum of the bismuth silicate film material under different frequencies.
FIG. 3 shows Bi of example 12SiO5Dielectric spectrum of bismuth silicate thin film material at different temperatures.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The starting materials in the examples are all commercially available;
reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
Preparation of Bi2SiO5Bismuth silicate film material:
s1, weighing 6.4676 g bismuth nitrate pentahydrate (Bi (NO)3)3•5H2O) is dissolved in the mixed solution of 20 mL of glacial acetic acid and 10 mL of ethylene glycol methyl ether, stirred and heated to 80 ℃ for dissolution to obtain the Bi organic salt solution, and the Bi organic salt solution is naturally cooled to room temperature.
S2, mixing 1.2134 g of acetylacetone with 1.2374 g of ethyl orthosilicate; the molar ratio of acetylacetone to tetraethoxysilane was 2: 1.
And S3, adding the mixed solution of acetylacetone and ethyl orthosilicate into the organic salt solution of Bi cooled to room temperature, and continuing stirring for more than 4 hours to obtain a stable and clear bismuth silicate precursor solution.
S4, adding the prepared bismuth silicate precursor solution into the cleaned Pt/TiO2/SiO2Carrying out spin coating on the Si substrate, wherein the spin coating speed is 3000rpm, the spin coating time is 30s, each spin coating layer is baked on a baking table at 350 ℃, and the next spin coating layer is cooled. Repeating the steps for 8 times to obtain the bismuth silicate precursor film with the required thickness.
S5, placing the obtained bismuth silicate precursor film in a tube furnace for annealing heat treatment, keeping the heating rate at 3 ℃/min, sintering at 500 ℃, keeping the temperature for 1 hour, and then naturally cooling along with the furnace to obtain Bi2SiO5Bismuth silicate film material.
Example 2
This example is Bi of the present invention2SiO5The second embodiment of the preparation method of bismuth silicate thin film material is different from embodiment 1 in that the molar ratio of acetylacetone to tetraethoxysilane is 3: 1;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Example 3
Unlike example 1, the molar ratio of acetylacetone to tetraethoxysilane in this example was 2.5: 1;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Example 4
Unlike example 1, the molar ratio of Bi to tetraethoxysilane in this example is 2: 1;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Comparative example 1
Different from the embodiment 1, acetylacetone is not added in the embodiment, namely the molar ratio of the acetylacetone to the tetraethoxysilane is 0: 1;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Comparative example 2
Unlike example 1, the molar ratio of acetylacetone to tetraethoxysilane in this example is 1: 1;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Comparative example 3
Unlike example 1, the molar ratio of acetylacetone to tetraethoxysilane in this example was 4: 1;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Comparative example 4
Unlike example 1, the sintering temperature in this example was 475 ℃;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Comparative example 5
Unlike example 1, the sintering temperature in this example was 575 ℃;
the amounts of other raw materials and the operation procedure were the same as in example 1.
Testing and characterization
XRD testing
The instrument was manufactured by Rigaku corporation of Japan, model No. D-MAX 2200 VPC, and tested under room temperature conditions, Cu Ka radiation, tube voltage 40 kV, tube current 26 mA, and scanning rate 8o/min。
2. Dielectric property test
(1) Dielectric temperature spectrum
The electrical test equipment is manufactured by Agilent 4284A. The temperature control system is manufactured by Novocontrol, model Cryosystem. The temperature is 200K to 500K.
(2) Dielectric spectrum
The electrical test equipment is manufactured by Agilent 4284A. The temperature control system is manufactured by Novocontrol, model Cryosystem. The temperature is 200K to 500K.
Test results
Bi obtained in example 12SiO5The XRD patterns of the bismuth silicate thin film materials are shown in FIG. 1, and Bi of examples 2 to 42SiO5The XRD pattern of the bismuth silicate thin film material was substantially identical to that of example 1.XRD tests show that diffraction peaks near 40 degrees are derived from substrate Pt, and other diffraction peaks belong to Bi2SiO5Indicating that no hetero-phase was formed in the film. Therefore, the prepared film material is bismuth silicate Bi2SiO5Pure phase.
The dielectric characteristics of example 1 were measured as shown in FIGS. 2 and 3, and Bi in FIG. 22SiO5Dielectric temperature spectra of the films tested at different frequencies of 100 kHz. The dielectric constant and dielectric loss of the film are shown in the temperature range of-40 deg.C to 125 deg.CThe change is small, and the temperature stability is good. FIG. 3 shows Bi2SiO5The dielectric spectrum of the film was measured at room temperature, which was 300K. The dielectric constant and dielectric loss of the film in the figure are less changed along with the frequency, and the film has good frequency stability.
Comparative examples 1 to 3: comparative example 1 no acetylacetone was added, ethyl orthosilicate was easily hydrolyzed, and a solution prepared without adding acetylacetone was precipitated, and a uniform and stable solution was not obtained. Comparative example 2 where acetylacetone was added in a molar ratio of 1:1, hydrolysis of ethyl orthosilicate could not be completely inhibited due to insufficient amount of acetylacetone, and precipitation still occurred. Comparative example 3 acetylacetone was added in a molar ratio of 4:1, and the addition of excess acetylacetone caused a significant increase in the viscosity of the solution, resulting in discontinuity of the resulting film.
The sintering temperature of comparative example 4 was 475 deg.c, and the resulting film was insufficiently crystallized due to the excessively low sintering temperature. The sintering temperature of comparative example 5 was 575 deg.c, and the phase transition of the film occurred due to the excessively high sintering temperature.
In addition, further comparing examples 1-4, the sample of example 1 performed best in terms of better temperature stability, better frequency stability, and less loss than the other examples.
In example 4, the ratio of Bi to Si is 2:1, and Bi is volatile, so that the sample in example 4 has defects due to the decrease of Bi, and the sample in example 4 has slightly inferior performance to that in example 1, and shows that the film is not uniform enough and the insulating performance is reduced.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (6)

1. Bi2SiO5The preparation method of the bismuth silicate film material is characterized by comprising the following steps:
s1, dissolving bismuth salt in glacial acetic acid and ethylene glycol monomethyl ether to obtain a Bi-containing organic salt solution;
s2, uniformly mixing tetraethyl orthosilicate and acetylacetone to obtain a mixed solution; the molar ratio of the acetylacetone to the tetraethyl orthosilicate is (2.0-3.0) to 1.0;
s3, uniformly mixing the mixed solution of S2 with the organic salt solution of S1 at room temperature, and reacting to obtain a bismuth silicate precursor solution;
s4, preparing a bismuth silicate precursor film on the substrate by using the bismuth silicate precursor solution prepared in the step S3;
s5, performing heat treatment on the bismuth silicate precursor film obtained in the step S4 to prepare Bi2SiO5Bismuth silicate film material; the temperature of the heat treatment is 475-575 ℃.
2. The method of claim 1, wherein the molar ratio of acetylacetone to tetraethyl orthosilicate is 2.0: 1.0.
3. The preparation method according to claim 1, wherein the volume ratio of the glacial acetic acid to the ethylene glycol monomethyl ether is (2.0-3.0) to 1.0.
4. The preparation method according to claim 1, wherein the molar ratio of Bi to tetraethyl orthosilicate is (2.0-2.2) to 1.0.
5. The method according to claim 1, wherein the reaction time in step S3 is 3-5 h.
6. The method according to claim 1, wherein the step S4 of preparing the bismuth silicate precursor film comprises the following steps: preparing a wet film of a bismuth silicate precursor on a substrate, drying to obtain a dry film of the bismuth silicate precursor, and repeating for a plurality of times to obtain the bismuth silicate precursor film with a plurality of layers of the dry film of the bismuth silicate precursor.
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CN101229510A (en) * 2008-01-31 2008-07-30 福州大学 Synthesis and applications of silicate containing Bi
CN102275944A (en) * 2011-07-06 2011-12-14 陕西科技大学 Preparation method of new scintillating bismuth silicate powder
CN102351204A (en) * 2011-07-06 2012-02-15 陕西科技大学 Method for preparing scintillation bismuth silicate powder by molten salt method
CN104637675A (en) * 2013-11-07 2015-05-20 Tdk株式会社 Dielectric composition, dielectric film, and electronic component
CN105967746A (en) * 2016-05-05 2016-09-28 陕西科技大学 Preparation method of porous Bi2SiO5 block
CN107162044A (en) * 2017-06-23 2017-09-15 广州特种承压设备检测研究院 A kind of compound nuclear shell structure nano powder preparation method

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PT104751A (en) * 2009-09-18 2011-03-18 Univ Aveiro METHOD FOR THE PREPARATION OF LOW TEMPERATURES OF FERROELECTRIC FINE FILMS, THE FERROELECTRIC FINE FILMS SO OBTAINED AND THEIR APPLICATIONS

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101229510A (en) * 2008-01-31 2008-07-30 福州大学 Synthesis and applications of silicate containing Bi
CN102275944A (en) * 2011-07-06 2011-12-14 陕西科技大学 Preparation method of new scintillating bismuth silicate powder
CN102351204A (en) * 2011-07-06 2012-02-15 陕西科技大学 Method for preparing scintillation bismuth silicate powder by molten salt method
CN104637675A (en) * 2013-11-07 2015-05-20 Tdk株式会社 Dielectric composition, dielectric film, and electronic component
CN105967746A (en) * 2016-05-05 2016-09-28 陕西科技大学 Preparation method of porous Bi2SiO5 block
CN107162044A (en) * 2017-06-23 2017-09-15 广州特种承压设备检测研究院 A kind of compound nuclear shell structure nano powder preparation method

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