CN102304744A - Barium strontium titanate dielectric film prepared through micro-arc oxidation and method thereof - Google Patents
Barium strontium titanate dielectric film prepared through micro-arc oxidation and method thereof Download PDFInfo
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- CN102304744A CN102304744A CN201110268892A CN201110268892A CN102304744A CN 102304744 A CN102304744 A CN 102304744A CN 201110268892 A CN201110268892 A CN 201110268892A CN 201110268892 A CN201110268892 A CN 201110268892A CN 102304744 A CN102304744 A CN 102304744A
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Abstract
The invention discloses a barium strontium titanate dielectric film prepared through micro-arc oxidation and a method thereof. The method comprises the following steps: preparing electrolyte from barium acetate or strontium acetate or mixture thereof, wherein the molar concentration of the barium acetate solution is 0-2.0 mol/L and the molar concentration of the strontium acetate is 0-1.2 mol/L; treating with a direct-current pulse power supply for 6-60 min, wherein the current density is 10-50 A/dm<2>, the pulse frequency is 50-250 Hz, and the duty cycle is 60%-95%; connecting a titanium substrate with an anode, and keeping the temperature of the electrolyte at 50-60 DEG C during the reaction; and taking down the treated titanium after the reaction, washing with distilled water and drying. The method has simple working procedures and high film-forming speed; and the film and the titanium (Ti) substrate are in metallurgical bonding, and the film has excellent dielectric properties.
Description
Technical field
The present invention relates to the electronic engineering technical field, specifically is that a kind of differential arc oxidation prepares strontium-barium titanate dielectric film and method thereof.
Background technology
The world today is to the development of electronic devices and components miniaturization, high performance requirement and film preparing technology, and dielectric film material arises at the historic moment.Ba
xSr
1-xTiO
3(x=0 ~ 1) dielectric film has higher dielectric constant and lower dielectric loss, is that very the ideal high voltage ceramic capacitor prepares material, is described as " pillar of electronic industry ".The technology that is used to prepare titanate at present and is dielectric film is more; Mainly comprise pulsed laser deposition, magnetron sputtering deposition method, sol-gel method, metal-organic chemical vapor deposition equipment method etc.; Though these methods respectively have advantage and characteristic, exist limitation separately.Though the film kind that pulsed laser deposition can prepare is many and composition is easy to control, the film forming area is little; Film and matrix bond that magnetron sputtering method can prepare are good, but film growth rates is slow and be difficult to the big area film forming; Sol-gel method has and is easy to mix up modification, advantage such as cost is low, and the film forming area is big, but operation is more loaded down with trivial details and thermal treatment subsequently causes the film surface tiny crack easily; The advantage that the metal-organic chemical vapor deposition equipment method has can be prepared large area film fast, can accurately control film chemical component and thickness, but its limitation is raw-material poor stability.These are all restricting further developing and using of dielectric film.The technology of preparing of China's dielectric film and international advanced technologies gap are obvious, and the technology of therefore developing suitable preparation titanate and be dielectric film is very important.Differential arc oxidization technique is a kind of directly in the new technology of non-ferrous metal surface in situ growth ceramic membrane, has fast, efficient, cheaply characteristics; Be suitable for preparing the dielectric film of large size and complex configuration, treating processes temperature low (even room temperature), and need not atmosphere control.Adopting differential arc oxidization technique at titanium matrix surface growth in situ dielectric film, is the innovation on a kind of preparation technology, has the favorable industrial prospect of production.
At present to adopting differential arc oxidization technique less in the research that surface of metal titanium prepares dielectric film, application number is to have described in surface of metal titanium in 200610155879.2 the patent to prepare BaTiO
3The method of doped metal ion dielectric film, yet and unexposed its performance perameter, the film kind of preparation is also more single.
Summary of the invention
The objective of the invention is to deficiency, provide a kind of differential arc oxidation to prepare strontium-barium titanate to prior art
Ba
xSr
1-xTiO
3(x=0 ~ 1) dielectric film and method thereof, the inventive method operation is simple, film forming speed is fast, and the film of generation has excellent dielectric properties.
The object of the invention can be realized through following technical scheme:
A kind of preparation method at surface of metal titanium growth in situ dielectric film comprises the steps:
(1) configuration electrolytic solution: electrolytic solution adopts barium acetate or strontium acetate or both mixed solutions, and wherein the volumetric molar concentration of barium acetate solution is 0 ~ 2.0mol/L, and the volumetric molar concentration of strontium acetate solution is 0 ~ 1.2mol/L; Said electrolytic solution stirs on the electromagnetism heating stirrer, and solute dissolves fully and gets final product;
(2) the mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 10 ~ 50A/dm
2, pulse-repetition is 50 ~ 250Hz, dutycycle is 60% ~ 95%; Treatment time is 6 ~ 60min;
(3) differential arc oxidation: the titanium metal matrix is connected to anode, is immersed in and carries out differential arc oxidation in the above-mentioned electrolytic solution, the control electrolyte temperature remains between 50～60 ℃ in the reaction process; After the reaction, take off titanium metal, behind distilled water flushing, in distilled water, soaked 1～2 hour again, oven dry can make required strontium-barium titanate dielectric film.
Titanium metal matrix in the said step (3) also need carry out following steps before differential arc oxidation: with surface of metal titanium with sand papering after; Place by volume to 1:3 blended hydrofluoric acid and nitric acid mixed solution and carry out pre-treatment; In acetone and distilled water, clean respectively then, dry up subsequent use.
The weight percent of titanium elements is greater than 95% in the said titanium metal matrix.
The electrolyte temperature control process is in said step (3) the differential arc oxidation process: measure electrolyte temperature in real time with thermometer; After solution temperature surpassed 50 ℃, the trigger pressure pump injected thermostatic bath with cold water; Simultaneously hot water is discharged, thereby guarantee that electrolyte temperature is controlled between 50～60 ℃.
When electrolytic solution stirred on the electromagnetism heating stirrer in the said step (1), heating and temperature control was 60 ℃, and churning time is 10 ~ 60min, and solute dissolves fully and gets final product.
When electrolytic solution only was barium acetate solution in the said step (1), then the dielectric film of Sheng Chenging was a barium titanate; When electrolytic solution only was strontium acetate solution in the said step (1), then the dielectric film of Sheng Chenging was a strontium titanate; Electrolytic solution is barium acetate when 1:1 mixes in molar ratio with strontium acetate in the said step (1), and then the dielectric film of Sheng Chenging is a strontium-barium titanate, and barium, strontium atom compares is 0.5:0.5; Electrolytic solution is barium acetate when 3:1 mixes in molar ratio with strontium acetate in the said step (1), and then the dielectric film of Sheng Chenging is a strontium-barium titanate, and barium, strontium atom compares is 0.77:0.23; Electrolytic solution is barium acetate when 3:2 mixes in molar ratio with strontium acetate in the said step (1), and then the dielectric film of Sheng Chenging is a strontium-barium titanate, and barium, strontium atom compares is 0.6:0.4.
Compared with prior art, the present invention has following advantage and beneficial effect:
(1) the technology operation that the present invention adopted is simple, facility investment is little, can accurately realize the change and the setting of processing condition such as electrical parameter.
(2) electrolytic solution that the present invention adopted through regulating its solution ratio, can simply, conveniently be prepared the dielectric film of heterogeneity; Adopt alkaline electrolyte simultaneously, environmental pollution is less.
(3) prepared film film forming speed of the present invention is fast, and reaction 6～60min can generate the thick thin film layer of 15～60um, film and matrix metallurgical binding, and dielectric properties are excellent.
Description of drawings
Fig. 1 is a micro-arc oxidation device synoptic diagram of the present invention; Wherein 1 represent mao power source, 2 represent agitator, and 3 represent electrolyzer, and 4 represent thermostatic bath, and 5 represent the differential arc oxidation anode; 6 represent the differential arc oxidation negative electrode;
Fig. 2 is the film XRD diffracting spectrum among the embodiment 1;
Fig. 3 is the film XRD diffracting spectrum among the embodiment 2;
Fig. 4 is the film XRD diffracting spectrum among the embodiment 3;
Fig. 5 is the film XRD diffracting spectrum among the embodiment 4;
Fig. 6 is the film XRD diffracting spectrum among the embodiment 5.
Embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiment of the present invention is not limited thereto, the processing parameter for not indicating especially can carry out with reference to routine techniques.
As shown in Figure 1; Apparatus of the present invention comprise mao power source 1, agitator 2, thermostatic bath 3, electrolyzer 4, differential arc oxidation anode 5,6 six parts of differential arc oxidation negative electrode; Electrolyzer places thermostatic bath; Differential arc oxidation cathode and anode self-control anchor clamps are immersed in the electrolytic solution, and electrolytic solution stirs through the electromagnetism heating stirrer.Among the present invention, metal titanium substrate connects the mao power source anode, and negative electrode can adopt common stainless steel plate.
The used mao power source of the present invention adopts direct current pulse power source, and pulse waveform is a square wave, and pattern is a constant current mode.
Embodiment 1
(1) configuration electrolytic solution: with Sr (CH
3COO)
2Solution is electrolytic solution, and the electrolytic solution volume is 400mL, and strength of solution is 0.4mol/L, on the electromagnetism heating stirrer, stirs, Heating temperature is set to 60 ℃, and churning time is 20min.
(2) direct current mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 20A/dm
2(matrix Ti is of a size of 20mm*20mm*2.5
Mm, Ti element Wt% is 96.47%), pulse-repetition is 100Hz, dutycycle is 85%; Treatment time is 25min.
(3) differential arc oxidation is handled: the Ti matrix is after sand papering, and that uses hydrofluoric acid and nitric acid carries out pre-treatment as 1:3 blended mixed solution by volume, in acetone and distilled water, cleans respectively then, after drying up the Ti matrix is connected to anode, and places electrolytic solution; Start direct current pulse power source, the differential arc oxidation process electrical parameter of (2) setting is set by step carried out, and needs the control electrolyte temperature remain on 55 ℃ in the reaction process; Pending finishing takes off the Ti metal that is processed, and behind distilled water flushing, is placed in the distilled water and soaks 1 hour, promptly obtains dielectric film after the heat oven dry.
The XRD diffracting spectrum of dry back dielectric film as shown in Figure 2, software analysis show this collection of illustrative plates and thing mutually card PDF00-040-1500 (be SrTiO
3) conform to, show that this film is mainly by SrTiO
3Constitute.Record film thickness and be about 41. 46um, specific inductivity and the dielectric loss of film under the 100Hz frequency is respectively 414.6 and 0.051.
(1) configuration electrolytic solution: with Ba (CH
3COO)
2Solution is electrolytic solution, and the electrolytic solution volume is 400mL, and the solution volumetric molar concentration is 0.6mol/L, on the electromagnetism heating stirrer, stirs, Heating temperature is set to 60 ℃, and churning time is 15min.
(2) direct current mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 15A/dm
2(matrix Ti is of a size of 20mm*20mm*2.5
Mm, Ti element Wt% is 96.35%), pulse-repetition is 200Hz, dutycycle is 85%; Treatment time is 25min.
(3) differential arc oxidation: the Ti matrix uses hydrofluoric acid and nitric acid to carry out pre-treatment as 1:3 blended mixed solution by volume after sand papering, in acetone and distilled water, cleans respectively then, after drying up the Ti matrix is connected to anode, and places electrolytic solution; Start direct current pulse power source, the differential arc oxidation electrical parameter of (2) setting set by step carries out, and needs the control electrolyte temperature remain on 50 ℃ in the reaction process; Pending finishing takes off the Ti metal that is processed, and uses distilled water flushing, in distilled water, soaks after 2 hours again, and the heat oven dry promptly obtains dielectric film.
The XRD diffracting spectrum of dry back dielectric film as shown in Figure 3, software analysis show this collection of illustrative plates and thing mutually card PDF 01-074-1963 (be BaTiO
3) conform to, show that this film is mainly by BaTiO
3Constitute.The thickness that records film is about 36.40um, and specific inductivity and the dielectric loss of film under the 100Hz frequency is respectively 151.4 and 0.087.
(1) preparing electrolyte: with the volumetric molar concentration is the Ba (CH of 0.3mol/L
3COO)
2With volumetric molar concentration be the Sr (CH of 0.3mol/L
3COO)
2Solution, 1:1 blended mixed solution is an electrolytic solution in molar ratio, and liquor capacity is 400mL, on the electromagnetism heating stirrer, stirs, Heating temperature is set to 60 ℃, and churning time is 20min.
(2) direct current mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 20A/dm
2(matrix Ti is of a size of 20mm*20mm*2.5
Mm, Ti element Wt% is 95.47%), pulse-repetition is 100Hz, dutycycle is 85%; Treatment time is 25min.
(3) differential arc oxidation: the Ti matrix after sand papering, with hydrofluoric acid and nitric acid by volume 1:3 blended mixed solution carry out pre-treatment, in acetone and distilled water, clean respectively then, after drying up the Ti matrix is connected to anode, and places electrolytic solution; Start direct current pulse power source, differential arc oxidation process (2) set electrical parameter is set by step carried out, and needs the control electrolyte temperature to remain on 57 ℃ in the reaction process; Pending finishing takes off and is processed the Ti metal, behind distilled water flushing, in distilled water, soaks 1 hour again, promptly obtains dielectric film after the heat oven dry.
The XRD diffracting spectrum of dry back dielectric film as shown in Figure 4, software analysis show this collection of illustrative plates and thing mutually card PDF00-039-1395 (be Ba
0.5Sr
0.5TiO
3) conform to, show that this film is mainly by Ba
0.5Sr
0.5TiO
3Constitute.Record film thickness and be about 28.47um, specific inductivity and the dielectric loss of film under the 100Hz frequency is respectively 442.3 and 0.051.
(1) preparing electrolyte: volumetric molar concentration is the Ba (CH of 0.6mol/L
3COO)
2Solution and volumetric molar concentration are the Sr (CH of 0.2mol/L
3COO)
2Solution 3:1 in molar ratio mixes, and liquor capacity is 400mL, on the electromagnetism heating stirrer, stirs, Heating temperature is set to 60 ℃, and churning time is 20min.
(2) direct current mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 20A/dm
2(matrix Ti is of a size of 20mm*20mm*2.5
Mm, Ti element Wt% is 95.47%), pulse-repetition is 100Hz, dutycycle is 85%; Treatment time is 25min.
(3) differential arc oxidation: the Ti matrix after sand papering, with hydrofluoric acid and nitric acid by volume 1:3 blended mixed solution carry out pre-treatment, in acetone and distilled water, clean respectively then, after drying up the Ti matrix is connected anode, and places electrolytic solution; Start direct current pulse power source, the differential arc oxidation electrical parameter of (2) setting set by step carries out, and needs the control electrolyte temperature remain on 60 ℃ in the reaction process; Pending finishing takes off and is processed the Ti metal, behind distilled water flushing, in distilled water, soaks 1 hour again, promptly obtains dielectric film after the heat oven dry.
The XRD diffracting spectrum of dry back dielectric film as shown in Figure 5, software analysis show this collection of illustrative plates and thing mutually card PDF00-044-0093 (be Ba
0.77Sr
0.23TiO
3) conform to, show this film mainly by
Ba
0.77Sr
0.23TiO
3Constitute.Record film thickness and be about 27.46um, specific inductivity and the dielectric loss of film under the 100Hz frequency is respectively 396.5 and 0.075.
(1) preparing electrolyte: volumetric molar concentration is the Ba (CH of 0.6mol/L
3COO)
2Solution and volumetric molar concentration are the Sr (CH of 0.4mol/L
3COO)
2Solution 3:2 in molar ratio mixes, and liquor capacity is 400mL, on the electromagnetism heating stirrer, stirs, Heating temperature is set to 60 ℃, and churning time is 20min.
(2) direct current mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 20A/dm
2(matrix Ti is of a size of 20mm*20mm*2.5
Mm, Ti element Wt% is 95.47%), pulse-repetition is 100Hz, dutycycle is 85%; Treatment time is 25min.
(3) differential arc oxidation: the Ti matrix after sand papering, with hydrofluoric acid and nitric acid by volume 1:3 blended mixed solution carry out pre-treatment, in acetone and distilled water, clean respectively then, after drying up the Ti matrix is connected to anode, and places electrolytic solution; Start direct current pulse power source, the differential arc oxidation electrical parameter of (2) setting set by step carries out, and needs the control electrolyte temperature remain on 60 ℃ in the reaction process; Pending finishing takes off and is processed the Ti metal, behind distilled water flushing, in distilled water, soaks 1 hour again, promptly obtains dielectric film after the heat oven dry.
The XRD diffracting spectrum of dry back dielectric film as shown in Figure 6, software analysis show this collection of illustrative plates and thing mutually card PDF00-034-0411 (be Ba
0.6Sr
0.4TiO
3) conform to, show that this film is mainly by Ba
0.6Sr
0.4TiO
3Constitute.Record film thickness and be about 32.46um, specific inductivity and the dielectric loss of film under the 100Hz frequency is respectively 383.5 and 0.082.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. a differential arc oxidation prepares the method for strontium-barium titanate dielectric film, it is characterized in that, comprises the steps:
(1) configuration electrolytic solution: electrolytic solution adopts barium acetate or strontium acetate or both mixed solutions, and wherein the volumetric molar concentration of barium acetate solution is 0 ~ 2.0mol/L, and the volumetric molar concentration of strontium acetate solution is 0 ~ 1.2mol/L; Said electrolytic solution stirs on the electromagnetism heating stirrer, and solute dissolves fully and gets final product;
(2) the mao power source electrical parameter is set: adopt direct current pulse power source, pulse waveform is a square wave, and pattern is a constant current mode; Current density is 10 ~ 50A/dm
2, pulse-repetition is 50 ~ 250Hz, dutycycle is 60% ~ 95%; Treatment time is 6 ~ 60min;
(3) differential arc oxidation: the titanium metal matrix is connected to anode, is immersed in and carries out differential arc oxidation in the above-mentioned electrolytic solution, the control electrolyte temperature remains between 50～60 ℃ in the reaction process; After the reaction, take off titanium metal, behind distilled water flushing, in distilled water, soaked 1～2 hour again, oven dry can make required strontium-barium titanate dielectric film.
2. method according to claim 1; It is characterized in that; Titanium metal matrix in the said step (3) also need be handled before differential arc oxidation as follows: with surface of metal titanium with sand papering after; Use hydrofluoric acid and nitric acid to carry out pre-treatment as 1:3 blended mixed solution by volume; In acetone and distilled water, clean respectively then, dry up subsequent use.
3. method according to claim 1 and 2 is characterized in that, the weight percent of titanium elements is greater than 95% in the said titanium metal matrix.
4. method according to claim 3; It is characterized in that; The electrolyte temperature control process is in said step (3) the differential arc oxidation process: measure electrolyte temperature in real time with thermometer; After solution temperature surpasses 50 ℃; The trigger pressure pump; Cold water is injected thermostatic bath, simultaneously hot water is discharged, thereby guarantee that electrolyte temperature is controlled between 50～60 ℃.
5. method according to claim 4 is characterized in that, when electrolytic solution stirred on the electromagnetism heating stirrer in the said step (1), heating and temperature control was 60 ℃, and churning time is 10 ~ 60min.
6. a differential arc oxidation prepares the strontium-barium titanate dielectric film, it is characterized in that, is prepared from the described any method of claim 1 to 5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103290454A (en) * | 2012-02-28 | 2013-09-11 | 广东技术师范学院 | Method for improving surface morphologies of BaTiO3 and SrTiO3 dielectric films prepared by micro-arc oxidation technology |
| CN103409781A (en) * | 2013-08-05 | 2013-11-27 | 青岛农业大学 | Preparation method for bismuth titanate film layer on basis of micro-arc oxidation technology |
| CN103741188A (en) * | 2014-01-24 | 2014-04-23 | 长安大学 | Method for preparing steady-persistence luminous ceramic membrane through aluminum or aluminum alloy surface micro-arc oxidation |
| CN105937047A (en) * | 2016-06-29 | 2016-09-14 | 华南理工大学 | Method for growing barium strontium titanate ferroelectric film on surface of titanium substrate in situ, and microarc oxidation electrolyte |
| CN106521597A (en) * | 2016-11-09 | 2017-03-22 | 青岛科技大学 | Method for preparing strontium titanate film through electrochemical method |
-
2011
- 2011-09-13 CN CN201110268892A patent/CN102304744A/en active Pending
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103290454A (en) * | 2012-02-28 | 2013-09-11 | 广东技术师范学院 | Method for improving surface morphologies of BaTiO3 and SrTiO3 dielectric films prepared by micro-arc oxidation technology |
| CN103409781A (en) * | 2013-08-05 | 2013-11-27 | 青岛农业大学 | Preparation method for bismuth titanate film layer on basis of micro-arc oxidation technology |
| CN103409781B (en) * | 2013-08-05 | 2016-09-07 | 青岛农业大学 | A kind of method preparing bismuth titanates film layer based on differential arc oxidization technique |
| CN103741188A (en) * | 2014-01-24 | 2014-04-23 | 长安大学 | Method for preparing steady-persistence luminous ceramic membrane through aluminum or aluminum alloy surface micro-arc oxidation |
| CN103741188B (en) * | 2014-01-24 | 2016-05-25 | 长安大学 | Aluminum or aluminum alloy surface by micro-arc oxidation is prepared the method for long-persistence luminous ceramic membrane |
| CN105937047A (en) * | 2016-06-29 | 2016-09-14 | 华南理工大学 | Method for growing barium strontium titanate ferroelectric film on surface of titanium substrate in situ, and microarc oxidation electrolyte |
| CN106521597A (en) * | 2016-11-09 | 2017-03-22 | 青岛科技大学 | Method for preparing strontium titanate film through electrochemical method |
| CN106521597B (en) * | 2016-11-09 | 2018-06-05 | 青岛科技大学 | A kind of method that electrochemical process prepares strontium titanate film |
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Application publication date: 20120104 |