CN101302100A - Material and method for preparing strontium titanate and barium titanate electronic function ceramic using laser - Google Patents
Material and method for preparing strontium titanate and barium titanate electronic function ceramic using laser Download PDFInfo
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- CN101302100A CN101302100A CNA2008103024229A CN200810302422A CN101302100A CN 101302100 A CN101302100 A CN 101302100A CN A2008103024229 A CNA2008103024229 A CN A2008103024229A CN 200810302422 A CN200810302422 A CN 200810302422A CN 101302100 A CN101302100 A CN 101302100A
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Abstract
The invention discloses a material for making electrically-functional strontium barium niobate ceramic by laser and a method thereof. The material consists of barium carbonate, strontium carbonate and titanium dioxide which are compounded according to a molar ratio of (1-x) to x to 1, wherein the x represents a molar mass fraction, and the x is more than 0 or less than 1; the used material is subject to mixture, ball milling, plasticization, granulation, green compaction and evacuation and sintering by CO2 laser, so as to be made into the electrically-functional strontium barium niobate ceramic. The material is low in cost, the laser sintering method consumes less energy, the sintering time is short, and the electrically-functional strontium barium niobate ceramic made by the laser sintering has the advantages of little crystal grain, small porosity, high tightness, high reliability, safety, electricity conservation, etc. In addition, strontium barium niobate is a sosoloid totally combining the barium carbonate and the strontium carbonate, the continuous solid solubility of the strontium barium niobate makes dielectric and optical performances of the ceramic adjusted continuously under the condition that the quantity relative ration between Ba and Sr is in a range of between 0 and 1; meanwhile, the electrically-functional ceramic with a big dielectric coefficient and less dielectric loss can be obtained through adjusting the ration between the Ba and the Sr.
Description
Technical field:
The present invention relates to a kind of material and method of preparing strontium titanate and barium titanate electronic function ceramic using laser, belong to the preparing technical field of electric function ceramic.
Background technology:
Strontium-barium titanate is BaTiO
3And SrTiO
3Sosoloid completely, its continuous solid solubility can make the dielectric of material and optical property regulate continuously in than scope in the amount of Ba/Sr, and this has very important significance in the Application Areas of electronic component.At present, the preparation method of electric function ceramic mainly contains solid sintering technology and liquid phase synthesizing method, but these two kinds of preparation methods exist shortcoming separately: the solid sintering technology product is difficult to reach molecular level and mixes, the material activity is low, energy expenditure is big, introduces impurity easily, and its purity, homogeneity are relatively poor, sintering time is long, reaction is difficult to control, and the ceramic components yield rate that obtains is low, and withstand voltage properties is poor, ceramic crystalline grain is bigger, and defectives such as pore are arranged; The lqiuid phase sintering method technical process is long, easily causes environmental pollution, and powder is easily reunited, expensive raw material price, and need higher temperature and higher pressure, facility investment is big etc., has also limited the application of this method.In recent years, begin to have the people laser technology to be applied in the preparation of electric function ceramic, but domestic main employing laser of narrowband prepares electric function ceramic at present, its shortcoming is that the sintering width is narrow, have only 1～3mm, pressed compact is in laser sintered process, because thermograde is bigger, very easily cracking causes pressed compact to be difficult to sintering and embarks on journey.
Summary of the invention:
The objective of the invention is to: provide a kind of material and method of preparing strontium titanate and barium titanate electronic function ceramic using laser, to overcome the existing defective of traditional preparation method.
The present invention constitutes like this: a kind of material of preparing strontium titanate and barium titanate electronic function ceramic using laser is to be (1-x): x by mol ratio: 1 barium carbonate BaCO
3, Strontium carbonate powder SrCO
3With titanium dioxide TiO
2Form, wherein x represents the molar mass mark, 0＜x＜1.
The purity of described barium carbonate, Strontium carbonate powder and titanium dioxide is more than 99%.
Adopt the method for preparing strontium titanate and barium titanate electronic function ceramic using laser to be with above-mentioned materials: to take by weighing barium carbonate, Strontium carbonate powder and titanium dioxide in molar ratio, mix, oven dry, with ball mill dry grinding 3 hours, added the appropriate amount of deionized water wet-milling then 5 hours, and took out oven dry, adding additives plasticizing, granulation, pressed compact under 25MPa pressure, pressurize 5min; Green compact under 80 ℃ of temperature dry 1 hour, under 350 ℃ of temperature dry 4 hours again, furnace cooling; Take out sample, use broadband CO
2The laser direct sintering promptly makes strontium titanate and barium titanate electronic function ceramic.
CO
2In the laser sintered process, broad band laser density is 0.25kW/cm
2～0.35kW/cm
2, adopt two-sided sintering.
Preferred laser sintering process parameter is: the broad band laser output rating is 450W, and sweep velocity is 150mm/min, and facula area is 14 * 2mm
2, defocusing amount is 315mm.These processing parameters are contrivers at fixing facula area (14 * 2mm
2) and the prerequisite of defocusing amount (315mm) under, change broad band laser output rating and sweep velocity, by orthogonal experiment optimization, the optimal processing parameter that screens.The ceramic product performance that sintering goes out under these processing condition is best.
Wherein used binding agent is that concentration is 5% polyvinyl alcohol solution; The polymerization degree of described polyvinyl alcohol is 1750.
The principles of chemistry of the present invention are: BaCO
3, SrCO
3And TiO
2Be mixed in proportion, after ball milling, plasticizing, granulation, compressing tablet, drying remove moisture and binding agent, at broadband CO
2The effect of laser issues biochemical reaction: (1-x) BaCO
3+ xSrCO
3+ TiO
2→ (Ba
(1-x), Sr
x) TiO
3+ CO
2↑ because BaCO
3, SrCO
3And TiO
2With (1-x): x: 1 mixed in molar ratio can react the CO that the reaction back generates fully
2Gas evolution promptly gets the higher strontium titanate and barium titanate electronic function ceramic of purity.
Innovation point of the present invention is mainly reflected in the following aspects:
1. adopt BaCO simultaneously
3, SrCO
3And TiO
2Be starting material, make the more superior strontium titanate and barium titanate electronic function ceramic of performance.Because strontium-barium titanate is BaTiO
3And SrTiO
3Sosoloid completely, its continuous solid solubility can make the dielectric and the optical property of pottery regulate continuously than the scope that is 0～1 at the Ba/Sr amount of substance; Simultaneously, BaTiO
3And SrTiO
3The Curie temperature difference, can change the Curie temperature of strontium-barium titanate by the ratio of adjusting Ba/Sr, obtain the electric function ceramic that specific inductivity is big, dielectric loss is little.
2. the preparation technology of base material: the preparation of base material is bigger to the influence of laser sintered effect, be mainly reflected in: (1) pressed compact pressure and dwell time: under suitable pressure, can make mixed powder tightr in conjunction with getting, when pressure was not enough, base substrate inside will exist some micro-bubbles to cause the easy layering of base substrate.When the defective base substrate of laser radiation, base substrate just absorbs big energy at short notice, and bubble sharply is heated and causes base substrate inside to blast, and can form some irregular projections at sample surfaces after base substrate solidifies.(2) binder removal and drying process: carry out binder removal when temperature during at 350 ℃ the intravital polyvinyl alcohol of base (PVA) is discharged fully, can be not exclusively if be lower than this temperature binder removal, cause base substrate that bubble is arranged, easily blast in base substrate inside when the incomplete base substrate of laser radiation binder removal, thereby cause phenomenons such as billet surface injustice, body cracking.
3. adopt the broad band laser sintering: under the broad band laser pattern, not only increased the sintering zone width, and, caused molten bath middle section thermograde to descend because the local fast swing of laser beam spot changes the vertex of surface temperature of molten pool fast, crack sensitivity reduces, and apparent mass improves.Simultaneously, can utilize the surface tension field of the thermograde formation of melt tank edge again, play the stirring melt and make the equally distributed effect of element.Therefore adopt broad band laser sintering strontium titanate and barium titanate electronic function ceramic, can obtain the pressed compact that dense structure, sintering width reach 15mm, surfacing.
Compared with prior art, material therefor low price of the present invention, laser sintered method power consumption is few, sintering time is extremely short, the laser sintered strontium titanate and barium titanate electronic function ceramic that makes has advantages such as crystal grain is tiny, void content is little, density is high, reliability is high, safety, economize on electricity, mainly as aspects such as sensitive components, piezoelectric ceramics, high voltage capacitor potteries.In addition, (Ba
1-x, Sr
x) TiO
3Be BaTiO
3And SrTiO
3Sosoloid completely, its continuous solid solubility can make the dielectric and the optical property of pottery regulate continuously than the scope that is 0～1 at the Ba/Sr amount of substance; Simultaneously, BaTiO
3And SrTiO
3The Curie temperature difference, can change the Curie temperature of strontium-barium titanate by the ratio of adjusting Ba/Sr, obtain the electric function ceramic that specific inductivity is big, dielectric loss is little.
Embodiment:
Embodiments of the invention 1: material therefor: BaCO
3, SrCO
3, and TiO
2(purity is more than 99%).
Take by weighing BaCO
3, SrCO
3And TiO
2, press BaCO
3: SrCO
3: TiO
2=0.5: 0.5: 1 mixed in molar ratio, and dry.After the oven dry mixed powder was dry grinded 3 hours with ball mill, added the proper amount of deionized water wet-milling then 5 hours.Take out oven dry, add the polymerization degree and be 1750 5% polyvinyl alcohol solution as binding agent plastify, granulation, pressed compact under 25MPa pressure, pressurize 5min.Green compact under 80 ℃ of temperature dry 1 hour, under 350 ℃ of temperature dry 4 hours again, furnace cooling.Take out sample, use broadband CO
2Laser carries out two-sided sintering, and in the sintering process, the broad band laser output rating is 450W, and sweep velocity is 150mm/min, and facula area is 14 * 2mm
2, defocusing amount is 315mm; Promptly make strontium titanate and barium titanate electronic function ceramic.
Embodiments of the invention 2: material therefor: BaCO
3, SrCO
3, and TiO
2(purity is more than 99%).
Take by weighing BaCO
3, SrCO
3And TiO
2, press BaCO
3: SrCO
3: TiO
2=0.9: 0.1: 1 mixed in molar ratio, and dry.After the oven dry mixed powder was dry grinded 3 hours with ball mill, added the proper amount of deionized water wet-milling then 5 hours.Take out oven dry, add 5% polyvinyl alcohol solution as binding agent plastify, granulation, pressed compact under 25MPa pressure, pressurize 5min.Green compact under 80 ℃ of temperature dry 1 hour, under 350 ℃ of temperature dry 4 hours again, furnace cooling.Take out sample, use broadband CO
2The laser direct sintering, in the sintering process, the broad band laser output rating is 450W, and sweep velocity is 150mm/min, and facula area is 14 * 2mm
2, defocusing amount is 315mm; Promptly make strontium titanate and barium titanate electronic function ceramic.
Embodiments of the invention 3: take by weighing BaCO
3, SrCO
3And TiO
2, press BaCO
3: SrCO
3: TiO
2=0.05: 0.95: 1 mixed in molar ratio, all the other are operated with embodiment 2, make strontium titanate and barium titanate electronic function ceramic.
Claims (7)
1. the material of a preparing strontium titanate and barium titanate electronic function ceramic using laser is characterized in that: it is (1-x): x by mol ratio: 1 barium carbonate, Strontium carbonate powder and titanium dioxide are formed, and wherein x represents the molar mass mark, 0＜x＜1.
2. according to the material of the described preparing strontium titanate and barium titanate electronic function ceramic using laser of claim 1, it is characterized in that: the purity of described barium carbonate, Strontium carbonate powder and titanium dioxide is more than 99%.
3. adopt the method for preparing strontium titanate and barium titanate electronic function ceramic using laser with claim 1 or 2 described materials, it is characterized in that: take by weighing barium carbonate, Strontium carbonate powder and titanium dioxide in molar ratio, mix, oven dry with ball mill dry grinding 3 hours, added the appropriate amount of deionized water wet-milling 5 hours then, take out oven dry, adding additives plasticizing, granulation, pressed compact under 25MPa pressure, pressurize 5min; Green compact under 80 ℃ of temperature dry 1 hour, under 350 ℃ of temperature dry 4 hours again, furnace cooling; Take out sample,, promptly make strontium titanate and barium titanate electronic function ceramic with broadband CO2 laser direct sintering.
4. according to the method for the described preparing strontium titanate and barium titanate electronic function ceramic using laser of claim 3, it is characterized in that: in the laser sintered process of CO2, broad band laser density is 0.25kW/cm2～0.35kW/cm2, adopts two-sided sintering.
5. according to the method for claim 3 or 4 described preparing strontium titanate and barium titanate electronic function ceramic using lasers, it is characterized in that: in the laser sintered process of CO2, the broad band laser output rating is 450W, and sweep velocity is 150mm/min, facula area is 14 * 2mm2, and defocusing amount is 315mm.
6. according to the method for the described preparing strontium titanate and barium titanate electronic function ceramic using laser of claim 3, it is characterized in that: used binding agent is that concentration is 5% polyvinyl alcohol solution.
7. according to the method for the described preparing strontium titanate and barium titanate electronic function ceramic using laser of claim 6, it is characterized in that: the polymerization degree of described polyvinyl alcohol is 1750.
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|---|---|---|---|
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|---|---|---|---|
| CN2008103024229A CN101302100B (en) | 2008-06-30 | 2008-06-30 | Material and method for preparing strontium titanate and barium titanate electronic function ceramic using laser |
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| CN101302100B CN101302100B (en) | 2011-06-22 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104529430A (en) * | 2014-12-04 | 2015-04-22 | 山东大学 | Titanium dioxide-based composite ceramic dielectric material, and preparation method and application thereof |
| CN104609867A (en) * | 2015-02-15 | 2015-05-13 | 上海材料研究所 | Densifying method for selective laser sintered ceramic parts |
| CN106268612A (en) * | 2016-08-09 | 2017-01-04 | 南京航空航天大学 | A kind of porous barium strontium titanate raw powder's production technology |
| CN107602114A (en) * | 2017-10-26 | 2018-01-19 | 贵州大学 | A kind of barium calcium zirconate titanate BCZT piezoelectric ceramics and its texturing preparation method |
| CN111574794A (en) * | 2020-05-15 | 2020-08-25 | 浙江科赛新材料科技有限公司 | High-dielectric-constant polytetrafluoroethylene film and preparation method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041589B (en) * | 2007-03-29 | 2010-08-11 | 贵州大学 | Material and method for preparing strontium titanate electric function ceramic by laser |
| CN101041588A (en) * | 2007-03-29 | 2007-09-26 | 贵州大学 | Material and method for preparing electric function ceramic by laser |
-
2008
- 2008-06-30 CN CN2008103024229A patent/CN101302100B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104529430A (en) * | 2014-12-04 | 2015-04-22 | 山东大学 | Titanium dioxide-based composite ceramic dielectric material, and preparation method and application thereof |
| CN104529430B (en) * | 2014-12-04 | 2015-09-30 | 山东大学 | Titanium dioxide base composite ceramic dielectric materials and preparation method thereof and application |
| CN104609867A (en) * | 2015-02-15 | 2015-05-13 | 上海材料研究所 | Densifying method for selective laser sintered ceramic parts |
| CN104609867B (en) * | 2015-02-15 | 2016-10-26 | 上海材料研究所 | A kind of method for densifying of selective laser sintering ceramic member |
| CN106268612A (en) * | 2016-08-09 | 2017-01-04 | 南京航空航天大学 | A kind of porous barium strontium titanate raw powder's production technology |
| CN107602114A (en) * | 2017-10-26 | 2018-01-19 | 贵州大学 | A kind of barium calcium zirconate titanate BCZT piezoelectric ceramics and its texturing preparation method |
| CN107602114B (en) * | 2017-10-26 | 2022-05-20 | 贵州大学 | Barium calcium zirconate titanate BCZT piezoelectric ceramic and texturing preparation method thereof |
| CN111574794A (en) * | 2020-05-15 | 2020-08-25 | 浙江科赛新材料科技有限公司 | High-dielectric-constant polytetrafluoroethylene film and preparation method and application thereof |
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