CN101016643A - Method and device for preparing dielectric film of BaTiO3 doping metallic ion - Google Patents
Method and device for preparing dielectric film of BaTiO3 doping metallic ion Download PDFInfo
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- CN101016643A CN101016643A CN 200610155879 CN200610155879A CN101016643A CN 101016643 A CN101016643 A CN 101016643A CN 200610155879 CN200610155879 CN 200610155879 CN 200610155879 A CN200610155879 A CN 200610155879A CN 101016643 A CN101016643 A CN 101016643A
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Abstract
The invention discloses a preparing method of dielectric film BaTiO3 doping metallic ion and device in electronic engineering technical domain, which comprises the following steps: choosing alkaline agent Ba(OH)2 electrolytic solution; adding into WO42-, Mo7O242- and SnO32- acid ion salt with content at 5-15g/L at the same time; proceeding micro plasma oxidation treatment; forming (Ba, Ca)TiO3, (Ba, W)TiO3, (Ba, Sn)TiO3 film layer on the surface of anode; consisting this device with impulsing power source, negative pole, anode, electrolytic solution, positive electrode, negative electrode and oxidation treatment ditch. This invention possesses simple device, which can be utilized widely.
Description
Technical field
The invention belongs to the electronic engineering technical field, relate to a kind of dielectric film BaTiO
3The preparation method of doped metal ion and device.
Background technology
Current electronic devices and components just develop towards lightness, slimming and subminiaturization direction, improve the room temperature dielectric constant of dielectric substance, reduce the focus that dissipation loss and temperature factor become scientific and technological circle's research.BaTiO
3Be a kind of strong dielectric material, be described as " pillar of electronic industry ".But because molecular structure, make t
cHigher 120 ℃, maximum dielectric constant value～10 are arranged just in the time of 120 ℃ promptly
4And the specific inductivity under the room temperature only has 1/5～2000 of Curie temperature, thereby has influenced its use properties greatly.Industrial terms of settlement is in the manufacturing processed of electronic devices and components at present, adopts the solid phase adulterating method, in BaTiO
3Mix the oxide compound of an amount of strontium, calcium, zirconium, tin and some rare earth elements in the powder, to improve its performance.But because the solid phase uneven doped is improved unsatisfactory to the parameters of components and parts.Present method mostly is technologies such as sol-gel method, microwave method and carries out ion doping.Though external useful sol-gel method is to BaTiO
3Carry out the research of doping vario-property, but can't be put to produce in China because the prices of raw and semifnished materials are expensive.
Summary of the invention
The objective of the invention is in order to solve BaTiO
3The shortcoming that complex process and cost are high, the BaTiO that preparation and improvement are produced
3Performance provides dielectric film BaTiO
3The preparation method of doped metal ion and device, Processes and apparatus is simple, is suitable for (Ba, X) TiO of the realization metal ion mixing of scale operation
3The rete preparation method.X＝Ca、Sr、Mo、Mo、Sn。
The technical solution adopted in the present invention is: dielectric film BaTiO
3The preparation method of doped metal ion, step is:
One, preparation electrolyte solution:
Electrolyte solution compound method 1: preparation electrolyte solution 4 in micro-plasma oxidation treatment trough 9, electrolyte solution 4 adopts alkaline medium, is Ba (OH)
2, regulate the pH value between 7.5～9.0;
Electrolyte solution compound method 2: preparation electrolyte solution 4 in micro-plasma oxidation treatment trough 9, electrolyte solution 4 adopts alkaline medium, is Ba (OH)
2, regulate the pH value between 7.5～9.0, adding content simultaneously is that 5～15g/L contains WO
4 2-, Mo
7O
24 2-, SnO
3 2-The salt of acid ion.
Two, micro-plasma oxidation is handled:
When using the electrolyte solution 4 that electrolyte solution compound method 1 is mixed with, anode 5 surfaces form BaTiO
3Oxidation film layer;
When using the electrolyte solution 4 that electrolyte solution compound method 2 is mixed with, the Ca in the electrolytic solution 4 (OH)
2, WO
4 2-, Mo
7O
24 2-, SnO
3 2-Plasma is under the electric field action between negative electrode 8 and the anode 5, and anode 5 is moved, and under electrochemical effect, metal ion enters in the film, and anode 5 surfaces form (Ba, Ca) TiO
3, (Ba, W) TiO
3, (Ba, Sn) TiO
3Rete.
The WO that contains of the present invention
4 2-, Mo
7O
24 2-, SnO
3 2-The salt of acid ion is Na
2WO
4, Na
2Mo
7O
24, Na
2SnO
3In one or more.
Implement dielectric film BaTiO
3The preparation method's of doped metal ion device, form by the pulse power 1, negative pole 2, positive pole 3, electrolytic solution 4, anode electrode 5, cathode electrode 8, oxide treatment groove 9, the positive pole 3 of the pulse power 1 links to each other with anode electrode 5, negative pole 2 links to each other with cathode electrode 8, anode electrode 5 and cathode electrode 8 insert and are equipped with in the micro-plasma oxidation treatment trough 9 of electrolytic solution 4, be provided with cooling duct 6 in the micro-plasma oxidation treatment trough 9, the lower end in the micro-plasma oxidation treatment trough 9 is provided with agitator 7.Micro-plasma oxidation is a kind of new technology at non-ferrous metal surface in situ growing oxide film, and is directly at the thicker film of a surface of metal titanium growth skim, good with the bonding force of matrix, and can prepare large area film.Simultaneously, change the preparation condition of film, add mineral compound, can realize that the technology ionic mixes.Ba (OH) with certain mass
2Be dissolved in the distilled water, evenly stir, treat Ba (OH)
2After the dissolving, the energising back forms micro-arc discharge in the metallic surface, form BaTiO fully
3Film.Add different metal ionic inorganic salt simultaneously, form (Ba, X) TiO
3Film can be realized the doping of metal ion, thereby changes BaTiO
3The dielectric properties of film.
The invention has the beneficial effects as follows that technology and simple in structure directly in the metallic surface film forming, realizes the doping of metal ion, according to the content that adds salt, regulates the content of doped metal ion in rete, improves the performance of rete.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the structural representation of apparatus of the present invention.
Fig. 2 is the BaTiO that the present invention prepares
3The SEM shape appearance figure of film.
Among Fig. 1: 1, the pulse power, 2, negative pole, 3, positive pole, 4, electrolytic solution, 5, anode electrode, 6, cooling duct, 7, agitator, 8, cathode electrode, 9, the micro-plasma oxidation treatment trough.
Embodiment
As Fig. 1, device comprises the pulse power 1 and 9 liang of major parts of differential of the arc reactive tank, the special-purpose pulse dc power of metallic surface micro-plasma oxidation, and voltage 500～600 V all can regulate, and anode electrode 5 is the Ti sheet, and cathode electrode 8 is a stainless steel plate.
Embodiment 1
With concentration is 0.1mol/L Ba (OH)
2Solution as electrolyte solution 4, stirred 5 minutes for 120 rev/mins with stirring velocity, apply dc pulse voltage between anode 5 and negative electrode 8, then anode Ti surface forms plasma discharge, be 10～20min discharge time, and it is the thick BaTiO of 10～15 μ m that anode 5 surfaces form thickness
3Rete.
Embodiment 2
With concentration is 0.1mol/L Ba (OH)
2Solution in add 10g/L Ca (OH)
2, preparation electrolyte solution 4 stirred 5 minutes for 120 rev/mins with stirring velocity, apply dc pulse voltage between anode 5 and negative electrode 8, then anode Ti surface forms plasma discharge, and be 10～20min discharge time, forming thickness on anode 5 surfaces is thick (Ba, Ca) TiO of 15～20 μ m
3Rete.
With concentration is 0.1mol/L Ba (OH)
2Solution in add 10g/L Na
2SnO
3, preparation electrolyte solution 4 stirred 5 minutes for 120 rev/mins with stirring velocity, apply dc pulse voltage between anode 5 and negative electrode 8, then anode Ti surface forms plasma discharge, and be 10～20min discharge time, forming thickness on anode 5 surfaces is thick (Ba, Sn) TiO of 15～20 μ m
3Rete.
Claims (4)
1, dielectric film BaTiO
3The preparation method of doped metal ion is characterized in that, the step of this method is:
(1), preparation electrolyte solution:
The electrolyte solution compound method: preparation electrolyte solution (4) in micro-plasma oxidation treatment trough (9), electrolyte solution (4) adopts alkaline medium, is Ba (OH)
2, regulate the pH value between 7.5～9.0;
(2), micro-plasma oxidation is handled:
Agitator (7) stirs electrolyte solution (4) with stirring velocity 120-150 rev/min, reacted 5-10 minute, apply voltage 500～600V DC pulse on the anode (5), anode (5) surface forms microplasma discharge, be 10～20min discharge time, anode (5) surface forms oxidation film layer, anode (5) material selection Ti.
2, dielectric film BaTiO according to claim 1
3The preparation method of doped metal ion is characterized in that, described electrolyte solution compound method is, preparation electrolyte solution (4) in micro-plasma oxidation treatment trough (9), and electrolyte solution (4) adopts alkaline medium, is Ba (OH)
2, regulate the pH value between 7.5～9.0, adding content simultaneously is that 5～15g/L contains WO
4 2-, Mo
7O
24 2-, SnO
3 2-The salt of acid ion.
3, dielectric film BaTiO according to claim 1
3The preparation method of doped metal ion is characterized in that, the described WO that contains
4 2-, Mo
7O
24 2-, SnO
3 2-The salt of acid ion is Na
2WO
4, Na
2Mo
7O
24, Na
2SnO
3In one or more.
4, implement the described dielectric film BaTiO of claim 1
3The preparation method's of doped metal ion device, it is characterized in that, by the pulse power (1), negative pole (2), anodal (3), electrolytic solution (4), anode electrode (5), cathode electrode (8), oxide treatment groove (9) is formed, the positive pole (3) of the pulse power (1) links to each other with anode electrode (5), negative pole (2) links to each other with cathode electrode (8), anode electrode (5) and cathode electrode (8) insert and are equipped with in the micro-plasma oxidation treatment trough (9) of electrolytic solution (4), be provided with cooling duct (6) in the micro-plasma oxidation treatment trough (9), the lower end in the micro-plasma oxidation treatment trough (9) is provided with agitator (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610155879 CN101016643A (en) | 2006-12-29 | 2006-12-29 | Method and device for preparing dielectric film of BaTiO3 doping metallic ion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610155879 CN101016643A (en) | 2006-12-29 | 2006-12-29 | Method and device for preparing dielectric film of BaTiO3 doping metallic ion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101016643A true CN101016643A (en) | 2007-08-15 |
Family
ID=38725867
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610155879 Pending CN101016643A (en) | 2006-12-29 | 2006-12-29 | Method and device for preparing dielectric film of BaTiO3 doping metallic ion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102574072A (en) * | 2009-07-20 | 2012-07-11 | 金属膜克姆有限公司 | Method for producing a membrane and such membrane |
| CN113912392A (en) * | 2021-11-10 | 2022-01-11 | 西安交通大学 | High-dielectric high-breakdown energy storage ceramic and preparation method thereof |
-
2006
- 2006-12-29 CN CN 200610155879 patent/CN101016643A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102574072A (en) * | 2009-07-20 | 2012-07-11 | 金属膜克姆有限公司 | Method for producing a membrane and such membrane |
| CN107419313A (en) * | 2009-07-20 | 2017-12-01 | 金属膜克姆有限公司 | For the method for producing film and such film |
| CN113912392A (en) * | 2021-11-10 | 2022-01-11 | 西安交通大学 | High-dielectric high-breakdown energy storage ceramic and preparation method thereof |
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Open date: 20070815 |