CN103833350A - Materials and method used for preparing calcium aluminum titanate electronic functional ceramic using laser - Google Patents
Materials and method used for preparing calcium aluminum titanate electronic functional ceramic using laser Download PDFInfo
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- CN103833350A CN103833350A CN201210475108.7A CN201210475108A CN103833350A CN 103833350 A CN103833350 A CN 103833350A CN 201210475108 A CN201210475108 A CN 201210475108A CN 103833350 A CN103833350 A CN 103833350A
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Abstract
The invention discloses materials and a method used for preparing calcium aluminum titanate electronic functional ceramic using laser. The preparation method comprises following steps: calcium carbonate, aluminum carbonate, and titanium dioxide are taken according to a molar ratio of (1-x):x:1, are mixed and dried, are subjected to dry grinding using a ball miller for 2h, and are subjected to wet grinding for 3h after adding of an appropriate amount of deionized water; an obtained mixture is collected and are dried; a binder is added for plasticization and granulation, an obtained material is subjected to pressed compact under a pressure of 35MPa, and the pressure is maintained for 8min; obtained green body is dried for 2h at a temperature of 70 DEG C, is dried for 5h at a temperature of 250 DEG C, and is subjected to furnace cooling; an obtained sample is collected, and is subjected to sintering using broadband carbon dioxide laser directly so as to obtain the calcium aluminum titanate electronic functional ceramic; wherein x is used for representing molar mass fraction, and 0<x<1. The materials of the method are cheap; energy consumption of laser sintering is less; sintering time is extremely short (about 1.5s); the calcium aluminum titanate electronic functional ceramic prepared via laser sintering is small in crystal grain size, possesses no pore, is high in density, and possesses a certain degree of strength, and stable and reliable performance.
Description
Technical field
The present invention relates to laser and prepare material and the method for calcium titanate aluminium electric function ceramic, belong to the preparing technical field of electric function ceramic.
Background technology
Calcium titanate aluminium is calcium titanate and aluminium titanates sosoloid completely, and its continuous solid solubility can make the dielectric of material and optical property regulate continuously in than scope in the amount of calcium/aluminium, and this has very important significance in the Application Areas of electronic component.At present, the preparation method of electric function ceramic is mainly by solid sintering technology and lqiuid phase sintering method, but these two kinds of preparation methods exist shortcoming separately: solid sintering technology product is difficult to reach molecular level and mixes, the ceramic components yield rate obtaining is low, withstand voltage properties is poor, ceramic crystalline grain is larger, has the defects such as pore; 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 large etc.But domestic main employing laser of narrowband is prepared electric function ceramic at present, and its shortcoming is that sintering width is narrow, only has 1～3mm, pressed compact is in laser sintered process, and because thermograde is larger, very easily cracking, causes pressed compact to be difficult to sintering and embark on journey.
Summary of the invention
The object of the invention is to, the material and the method that provide a kind of laser to prepare calcium titanate aluminium electric function ceramic, it can effectively solve the problem that prior art exists.
Technical scheme of the present invention is to form like this: laser is prepared the method for calcium titanate aluminium electric function ceramic, take calcium carbonate, aluminium carbonate and titanium dioxide according to the mol ratio of (1-x): x:1, mix, dry, with ball mill dry grinding 2 hours, then add appropriate amount of deionized water wet-milling 3 hours, take out and dry, adding additives plasticizing, granulation, pressed compact under 35MPa pressure, pressurize 8min; Green compact are dried 2 hours at 70 ℃ of temperature, then at 250 ℃ of temperature, are dried 5 hours, furnace cooling; Take out sample, with broadband carbon dioxide laser direct sintering, make calcium titanate aluminium electric function ceramic; Wherein, x represents molar mass mark, 0 ﹤ x ﹤ 1.
The purity of described calcium carbonate, aluminium carbonate and titanium dioxide is more than 99%.
Above-mentioned laser is prepared the method for calcium titanate aluminium electric function ceramic, and in carbon dioxide laser sintering process, broad band laser density is 0.15kW/c ㎡～0.25 kW/c ㎡, adopts two-sided sintering.
Above-mentioned laser is prepared the method for calcium titanate aluminium electric function ceramic, in carbon dioxide laser sintering process, broad band laser output rating is 350W, sweep velocity is 100mm/min, facula area is 14*2m ㎡, and defocusing amount is 315mm, and these processing condition are that contriver is under the prerequisite of fixed light spot size (14*2m ㎡) and defocusing amount (315mm), change broad band laser output rating and sweep velocity, the optimal processing parameter of electing by orthogonal experiment optimization, general.The ceramic product performance that sintering goes out under these processing condition is best.
Above-mentioned laser is prepared in the method for calcium titanate aluminium electric function ceramic, and caking agent used is that concentration is 5% polyvinyl alcohol solution.
The polymerization degree of aforesaid polyvinyl alcohol is 1850.
Prepare according to aforesaid laser the calcium titanate aluminium electric function ceramic material that the method for calcium titanate aluminium electric function ceramic makes.
The prepared electric function ceramic of the present invention has the advantages such as reliability is high, safety, economize on electricity, be mainly used in the aspects such as temperature-sensing element, threshold currents element and constant temperature heating element, be specifically related to the fields such as communication, household electrical appliances, aviation, automobile, power equipment.
Compared with prior art, material therefor low price of the present invention, laser sintered method power consumption is few, sintering time extremely short (about 1.5 seconds), the laser sintered calcium titanate aluminium ceramic product crystal grain making is very tiny, pore-free, and density is very high, make product have certain intensity, its performance (as electric conductivity, specific inductivity etc.) is reliable and stable.The present invention is for using electric function ceramic that a new selection is provided.
Embodiment
Embodiment 1: take purity according to the mol ratio of 0.8:0.2:1 and be 99.5 calcium carbonate, aluminium carbonate and titanium dioxide, mix, dry, with ball mill dry grinding 2 hours, then add appropriate amount of deionized water wet-milling 3 hours, take out and dry, adding additives plasticizing, granulation, pressed compact under 35MPa pressure, pressurize 8min; Green compact are dried 2 hours at 70 ℃ of temperature, then at 250 ℃ of temperature, are dried 5 hours, furnace cooling; Take out sample, with broadband carbon dioxide laser direct sintering, make calcium titanate aluminium electric function ceramic.In carbon dioxide laser sintering process, broad band laser density is 0.20 kW/c ㎡, adopts two-sided sintering.Broad band laser output rating is 350W, and sweep velocity is 100mm/min, and facula area is 14*2m ㎡, and defocusing amount is 315mm.Caking agent used is that concentration is 5% polyvinyl alcohol solution.The polymerization degree of described polyvinyl alcohol is 1850.
Embodiment 2: take purity according to the mol ratio of 0.5:0.5:1 and be 99.8% calcium carbonate, aluminium carbonate and titanium dioxide, mix, dry, with ball mill dry grinding 2 hours, then add appropriate amount of deionized water wet-milling 3 hours, take out and dry, adding additives plasticizing, granulation, pressed compact under 35MPa pressure, pressurize 8min; Green compact are dried 2 hours at 70 ℃ of temperature, then at 250 ℃ of temperature, are dried 5 hours, furnace cooling; Take out sample, with broadband carbon dioxide laser direct sintering, make calcium titanate aluminium electric function ceramic.In carbon dioxide laser sintering process, broad band laser density is 0.15kW/c ㎡～0.25 kW/c ㎡, adopts two-sided sintering.Broad band laser output rating is 350W, and sweep velocity is 100mm/min, and facula area is 14*2m ㎡, and defocusing amount is 315mm.Caking agent used is that concentration is 5% polyvinyl alcohol solution.The polymerization degree of described polyvinyl alcohol is 1850.
Embodiment 3: take purity according to the mol ratio of 0.3:0.7:1 and be 99.9% calcium carbonate, aluminium carbonate and titanium dioxide, mix, dry, with ball mill dry grinding 2 hours, then add appropriate amount of deionized water wet-milling 3 hours, take out and dry, adding additives plasticizing, granulation, pressed compact under 35MPa pressure, pressurize 8min; Green compact are dried 2 hours at 70 ℃ of temperature, then at 250 ℃ of temperature, are dried 5 hours, furnace cooling; Take out sample, with broadband carbon dioxide laser direct sintering, make calcium titanate aluminium electric function ceramic.In carbon dioxide laser sintering process, broad band laser density is 0.15kW/c ㎡～0.25 kW/c ㎡, adopts two-sided sintering.Broad band laser output rating is 350W, and sweep velocity is 100mm/min, and facula area is 14*2m ㎡, and defocusing amount is 315mm.Caking agent used is that concentration is 5% polyvinyl alcohol solution.The polymerization degree of described polyvinyl alcohol is 1850.
Embodiment 4: prepare the calcium titanate aluminium electric function ceramic material that the method for calcium titanate aluminium electric function ceramic makes according to the laser described in embodiment 1～3.
Claims (7)
1. laser is prepared the method for calcium titanate aluminium electric function ceramic, it is characterized in that, take calcium carbonate, aluminium carbonate and titanium dioxide according to the mol ratio of (1-x): x:1, mix, dry, with ball mill dry grinding 2 hours, then add appropriate amount of deionized water wet-milling 3 hours, take out and dry, adding additives plasticizing, granulation, pressed compact under 35MPa pressure, pressurize 8min; Green compact are dried 2 hours at 70 ℃ of temperature, then at 250 ℃ of temperature, are dried 5 hours, furnace cooling; Take out sample, with broadband carbon dioxide laser direct sintering, make calcium titanate aluminium electric function ceramic; Wherein, x represents molar mass mark, 0 ﹤ x ﹤ 1.
2. laser according to claim 1 is prepared the method for calcium titanate aluminium electric function ceramic, it is characterized in that, the purity of described calcium carbonate, aluminium carbonate and titanium dioxide is more than 99%.
3. laser according to claim 1 is prepared the method for calcium titanate aluminium electric function ceramic, it is characterized in that, in carbon dioxide laser sintering process, broad band laser density is 0.15kW/c ㎡～0.25 kW/c ㎡, adopts two-sided sintering.
4. the method for preparing calcium titanate aluminium electric function ceramic according to the laser described in claim 1 or 3, is characterized in that, in carbon dioxide laser sintering process, broad band laser output rating is 350W, sweep velocity is 100mm/min, and facula area is 14*2m ㎡, and defocusing amount is 315mm.
5. laser according to claim 1 is prepared the method for calcium titanate aluminium electric function ceramic, it is characterized in that, caking agent used is that concentration is 5% polyvinyl alcohol solution.
6. laser according to claim 5 is prepared the method for calcium titanate aluminium electric function ceramic, it is characterized in that, the polymerization degree of described polyvinyl alcohol is 1850.
7. prepare according to the laser described in claim 1～6 any one the calcium titanate aluminium electric function ceramic material that the method for calcium titanate aluminium electric function ceramic makes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109704396A (en) * | 2019-01-28 | 2019-05-03 | 广东朗研科技有限公司 | A kind of preparation method of CaCu 3 Ti 4 O |
| CN109704754A (en) * | 2019-03-15 | 2019-05-03 | 上海朗研光电科技有限公司 | The preparation method of CaCu 3 Ti 4 O base ceramic material and its huge dielectric constant ceramic capacitor |
| CN109721353A (en) * | 2019-03-15 | 2019-05-07 | 上海朗研光电科技有限公司 | A kind of preparation method of huge dielectric constant CCTO based film material |
| CN109734437A (en) * | 2019-03-15 | 2019-05-10 | 上海朗研光电科技有限公司 | A kind of preparation method of giant dielectric, low-loss CCTO base ceramic material |
| CN115974533A (en) * | 2022-12-02 | 2023-04-18 | 新化县顺达电子陶瓷有限公司 | High strength 5G signal basic station ceramic cover plate |
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2012
- 2012-11-20 CN CN201210475108.7A patent/CN103833350A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704396A (en) * | 2019-01-28 | 2019-05-03 | 广东朗研科技有限公司 | A kind of preparation method of CaCu 3 Ti 4 O |
| CN109704396B (en) * | 2019-01-28 | 2021-06-01 | 广东朗研科技有限公司 | Preparation method of calcium copper titanate |
| CN109704754A (en) * | 2019-03-15 | 2019-05-03 | 上海朗研光电科技有限公司 | The preparation method of CaCu 3 Ti 4 O base ceramic material and its huge dielectric constant ceramic capacitor |
| CN109721353A (en) * | 2019-03-15 | 2019-05-07 | 上海朗研光电科技有限公司 | A kind of preparation method of huge dielectric constant CCTO based film material |
| CN109734437A (en) * | 2019-03-15 | 2019-05-10 | 上海朗研光电科技有限公司 | A kind of preparation method of giant dielectric, low-loss CCTO base ceramic material |
| CN115974533A (en) * | 2022-12-02 | 2023-04-18 | 新化县顺达电子陶瓷有限公司 | High strength 5G signal basic station ceramic cover plate |
| CN115974533B (en) * | 2022-12-02 | 2023-12-08 | 新化县顺达电子陶瓷有限公司 | High-strength 5G signal base station ceramic cover plate |
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Application publication date: 20140604 |