CN102173781A - Preparation method of CaCu3Ti4O12 ceramic - Google Patents
Preparation method of CaCu3Ti4O12 ceramic Download PDFInfo
- Publication number
- CN102173781A CN102173781A CN2011100450419A CN201110045041A CN102173781A CN 102173781 A CN102173781 A CN 102173781A CN 2011100450419 A CN2011100450419 A CN 2011100450419A CN 201110045041 A CN201110045041 A CN 201110045041A CN 102173781 A CN102173781 A CN 102173781A
- Authority
- CN
- China
- Prior art keywords
- ceramic
- ccto
- sintering
- ball
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a preparation method of CaCu3Ti4O12 (CCTO) ceramic, and the method can be used for solving the technical problem of high dielectric loss caused by the existing preparation method of the CaCu3Ti4O12 ceramic. The technical scheme of the invention is as follows: a casting technology is adopted to prepare a CCTO ceramic wafer, then a two-step sintering technology is adopted to obtain a ceramic material with dense structure and uniform particle size; and according to the changes of the dielectric constant epsilon r and dielectric loss tan delta of the CCTO ceramic along with the testing frequency and the temperature, CCTO crystalline integrity, grain boundary, defect and other aspects can directly influence the high dielectric constant. In addition, at the room temperature and 1KHz, when the sintering temperature is 1025-1100 DEG C and heat preservation is performed for 10 hours, the epsilon r of the CCTO ceramic prepared through two-step sintering is 104, which is more or less the same with the value reported in literatures; and the dielectric loss is reduced from 0.3-0.6 reported in the background art to 0.03, which shows that the concentration of oxygen vacancies can be reduced by adopting the two-step sintering method. Therefore, the high-temperature low-frequency dissipation of the ceramic can be significantly reduced; and the lattice distortions can be reduced along with the increase of the heat preservation time.
Description
Technical field
The present invention relates to a kind of preparation method of pottery, particularly a kind of CaCu
3Ti
4O
12The preparation method of pottery.
Background technology
Ceramic dielectric capacitor is a kind of widely used electronic component, in order to realize miniaturization, wishes that its dielectric material has high-k.CaCu
3Ti
4O
12(CCTO) be a kind of high dielectric constant material of discovered in recent years, it is not recurring structure phase transformation in the scope of 100～600K, has good temperature stability.Therefore, it has been caused people's extensive concern as the possibility that high dielectric constant material is applied on high density information storage, thin-film device and the high dielectric container.
For the research of CCTO, there is the difference on the order of magnitude in the ε r that present different researchers is reported, and from 478 to 300000 do not wait.Document 1 " Giant dielectric constant response in a copper-titanate[J] .Solid State Commun; 2000; 115:217-220. " to obtain ε r under the room temperature with traditional solid reaction process be 10000～20000 CCTO material, and other scholars make the ε r that obtains material that uses the same method be respectively 478,2400 and 18700.The highest ε r of CCTO pottery that is reported at present reaches 300000, and this mixes the back at ball milling and obtains in 1100 ℃ of sintering 24h.Can find out that thus experiment specific inductivity that different researchers is reported also exists the difference on the order of magnitude, and the temperature range that bigger variation takes place specific inductivity has nothing in common with each other also.This has just reflected that different experimentations, experimental technique and preparation technology are still waiting further investigation to the dielectric material Effect on Performance.As everyone knows, sintering is one of most important process procedure of preparation stupalith.The crystal grain secondary that is prone to of structure and densification, particularly sintering later stage that the selection of sintering temperature, soaking time and heat-up rate all directly affect pottery is grown up and is often caused ceramic performance to worsen.This situation is particularly serious in the sintering of nano material.So someone just proposes to adopt two-step sintering method to prepare nano ceramics, by the variation of controlled temperature dexterously, when suppressing crystal boundary migration, keep the crystal boundary diffusion to be in active state, finish the agglomerating purpose to be implemented under the prerequisite that crystal grain do not grow up.
Document 2 " Sintering behavior and dielectric properties of polycrystalline CaCu
3Ti
4O
12.J Mater Sci:Mater Electron (2009) 20:680-684 " disclose a kind of employing conventional solid-state method and prepared powder; and sintering is carried out in compression moulding then; at first be to be raised to 1080 ℃ of top temperatures with higher speed; be cooled fast to 950 ℃ and be incubated 0-20h then; the CCTO pottery that it obtains at room temperature ε r only has only 3000; relatively low, and dielectric loss tan δ is up to 0.3～0.6.
Summary of the invention
In order to overcome the CaCu of existing method preparation
3Ti
4O
12The deficiency that the ceramic dielectric loss is high the invention provides a kind of CaCu
3Ti
4O
12The preparation method of pottery adopts casting technique to prepare ceramic CCTO thin slice, then it is carried out two-step sintering, can reduce prepared CaCu
3Ti
4O
12The dielectric loss of pottery.
The technical solution adopted for the present invention to solve the technical problems: a kind of CaCu
3Ti
4O
12The preparation method of pottery is characterized in comprising the steps:
(a) with high-purity CaCO
3(＞99%), CuO (＞99%), TiO
2(＞99%) powder is a raw material, presses 1: 3: 4 batching of CCTO stoichiometric ratio, ball milling 10～12h in the distilled water medium;
(b) powder after oven dry is sieved is in 900 ℃～1000 ℃ pre-burning 2～3h;
(c) powder after the pre-burning adds 29.4～29.9% ethanol, 0.5～1.0% propyl carbinol and 0.8～1% triolein, puts into nylon ball grinder then, with ZrO
2Ball is a grinding medium, and putting into rotating speed is 350～400rad/min planetary ball mill wet-milling, 20～24h;
(d) in the wet feed that grinds 20～24h, add 2.33～2.35% polyoxyethylene glycol, 2.35～2.37% dinoctyl phthalates, 3.2～3.6% polyvinyl butyral acetals and 0.4～0.6% hexanaphthene, and then ball milling 20～24h, rotating speed 350～400rad/min;
(e) slurry is poured in the small beaker, taken out all ZrO
2Ball is poured slurry into then and is positioned in the casting machine that has clean smooth glass plate, makes it at the uniform velocity mobile on glass ribbon, forms thin casting belt;
(f) opened the blowing apparatus drying 10～12 hours, demoulding is handled the green compact just can obtain flow casting molding then, and the green compact of moulding are cut into the orthogonal thin slice;
(g) carry out binder removal then and handle, the control of binder removal temperature rise rate is as follows: room temperature to 80～100 ℃, 2～3 ℃/min, insulation 1～2h in the time of 80～100 ℃; 80～100 ℃ to 500～600 ℃, 1～2 ℃/min, insulation 2～3h removes organism fully in the time of 500～600 ℃;
(h) green compact after the binder removal processing are carried out sintering at 1025 ℃～1100 ℃, the control of sintering temperature rise rate: room temperature is to 1025 ℃～1100 ℃ of required sintering temperatures, 3～4 ℃/min; 1025 ℃～1100 ℃ to 900～1000 ℃, 3～4 ℃/min, furnace cooling then.
The invention has the beneficial effects as follows: utilize casting technique successfully to prepare the CCTO ceramic sheet, it is adopted two-step sintering technology, obtained the evenly (stupalith of 50nm～60nm) of compact structure, particle diameter, simultaneously from the DIELECTRIC CONSTANT r of CCTO pottery and dielectric loss tan δ with test frequency and variation of temperature rule, find that CCTO crystalline perfection, crystal boundary and defective etc. have direct influence to the size of its high-k.And at normal temperature, under the 1KHz, when sintering temperature 1025 ℃～1100 ℃ insulations during 10h, the ε r of two-step sintering gained CCTO pottery of the present invention is 10
4The value of this and bibliographical information is more or less the same, and dielectric loss tan δ reduces to 0.03 by 0.3～0.6 of background technology, this has illustrated that the employing two-step sintering method reduces oxygen vacancy concentration, thereby significantly having weakened ceramic high temperature low frequency dissipates, along with the increase of soaking time, lattice distortion also reduces gradually.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the embodiment of the invention 2 gained high dielectric constant material CaCu
3Ti
4O
12Pattern.
Fig. 2 is the embodiment of the invention 3 gained high dielectric constant material CaCu
3Ti
4O
12Pattern.
Embodiment
EXAMPLE l: with high-purity 3.0414g CaCO
3(＞99%), 7.2514g CuO (＞99%), 9.7074gTiO
2(＞99%) powder is a raw material, matches well the material of 20g, ball milling 12h in the distilled water medium by the CCTO stoichiometry; Powder after oven dry sieved is in 960 ℃ of pre-burning 2h. Powder after the pre-burning adds 15.4ml ethanol, 0.25ml propyl carbinol and 0.36ml triolein, puts into nylon ball grinder then, with ZrO
2Ball is a grinding medium, and putting into rotating speed is 400rad/min planetary ball mill wet-milling 23h; In the wet feed that grinds 23h, add 0.9592g polyoxyethylene glycol, 1.0ml dinoctyl phthalate, 1.3174g polyvinyl butyral acetal and 0.24ml hexanaphthene, and then ball milling 20h, rotating speed 350rad/min; Slurry is poured in the small beaker, taken out all ZrO
2Ball is poured slurry into then and is positioned in the casting machine that has clean smooth glass plate, makes it at the uniform velocity mobile on glass ribbon, forms thin casting belt.Wherein the thickness of curtain coating is by curtain coating blade control, and the speed that moves also has direct influence to the thickness of strip; Opened blowing apparatus dry 12 hours, demoulding is handled the green compact that just can obtain flow casting molding then, and the green compact of moulding are cut into the orthogonal thin slice; Carry out binder removal then and handle, the control of binder removal temperature rise rate is as follows: room temperature to 100 ℃, 2 ℃/min, insulation 1h in the time of 100 ℃; 100 ℃ to 550 ℃, 1 ℃/min, insulation 2h can remove fully to guarantee organism in the time of 550 ℃, creates conditions and makes base substrate obtain certain mechanical strength for burning till; Green compact after the binder removal processing are carried out sintering at 1025 ℃, and the control of sintering temperature rise rate: room temperature is to 1050 ℃ of required sintering temperatures, 3 ℃/min; 1025 ℃ to 960 ℃, 4 ℃/min, furnace cooling then.
Embodiment 2: with high-purity 3.344g CaCO
3(＞99%), 7.9765g CuO (＞99%), 10.6788gTiO
2(＞99%) powder is a raw material, matches well 22g material, ball milling 12h in the distilled water medium by the CCTO stoichiometry; Powder after oven dry sieved is in 960 ℃ of pre-burning 2h.Powder after the pre-burning adds 15.48ml ethanol, 0.3ml propyl carbinol and 0.4ml triolein, puts into nylon ball grinder then, with ZrO
2Ball is a grinding medium, and putting into rotating speed is 400rad/min planetary ball mill wet-milling 20h; In the wet feed that grinds 20h, add 0.960g polyoxyethylene glycol, 0.997ml dinoctyl phthalate, 1.321g polyvinyl butyral acetal and 0.28ml hexanaphthene, and then ball milling 20h, rotating speed 400rad/min; Slurry is poured in the small beaker, taken out all ZrO
2Ball is poured slurry into then and is positioned in the casting machine that has clean smooth glass plate, makes it at the uniform velocity mobile on glass ribbon, forms thin casting belt.Wherein the thickness of curtain coating is by curtain coating blade control, and the speed that moves also has direct influence to the thickness of strip; Opened blowing apparatus dry 12 hours, demoulding is handled the green compact that just can obtain flow casting molding then, and the green compact of moulding are cut into the orthogonal thin slice; Carry out binder removal then and handle, the control of binder removal temperature rise rate is as follows: room temperature to 100 ℃, 2 ℃/min, insulation 1h in the time of 100 ℃; 100 ℃ to 550 ℃, 1 ℃/min, insulation 2h can remove fully to guarantee organism in the time of 550 ℃, creates conditions and makes base substrate obtain certain mechanical strength for burning till; Green compact after the binder removal processing are carried out sintering at 1050 ℃, and the control of sintering temperature rise rate: room temperature is to 1050 ℃ of required sintering temperatures, 3 ℃/min; 1050 ℃ to 960 ℃, 4 ℃/min, furnace cooling then.As can be seen from Figure 1 relatively fine and close, particle alignment is even and rib type border clearly occurs, forms Polygons particle preferably, and crystalline form is better, but crystal grain is little relatively and have little crystal grain to be mingled with.
Embodiment 3: with high-purity 3.7561g CaCO
3(＞99%), 8.9555g CuO (＞99%), 11.9886gTiO
2(＞99%) powder is a raw material, matches well 24.7g material, ball milling 10h in the distilled water medium by the CCTO stoichiometry; Powder after oven dry sieved is in 960 ℃ of pre-burning 2h. Powder after the pre-burning adds 15.5ml ethanol, 0.4ml propyl carbinol and 0.4ml triolein, puts into nylon ball grinder then, with ZrO
2Ball is a grinding medium, and putting into rotating speed is 400rad/min planetary ball mill wet-milling 24h; In the wet feed that grinds 24h, add 0.9663g polyoxyethylene glycol, 0.99ml dinoctyl phthalate, 1.34g polyvinyl butyral acetal and 0.3ml hexanaphthene, and then ball milling 20h, rotating speed 400rad/min; Slurry is poured in the small beaker, taken out all ZrO
2Ball is poured slurry into then and is positioned in the casting machine that has clean smooth glass plate, makes it at the uniform velocity mobile on glass ribbon, forms thin casting belt.Wherein the thickness of curtain coating is by curtain coating blade control, and the speed that moves also has direct influence to the thickness of strip; Opened blowing apparatus dry 12 hours, demoulding is handled the green compact that just can obtain flow casting molding then, and the green compact of moulding are cut into the orthogonal thin slice; Carry out binder removal then and handle, the control of binder removal temperature rise rate is as follows: room temperature to 100 ℃, 2 ℃/min, insulation 1h in the time of 100 ℃; 100 ℃ to 550 ℃, 1 ℃/min, insulation 2h can remove fully to guarantee organism in the time of 550 ℃, creates conditions and makes base substrate obtain certain mechanical strength for burning till; Green compact after the binder removal processing are carried out sintering at 1075 ℃, and the control of sintering temperature rise rate: room temperature is to 1750 ℃ of required sintering temperatures, 3 ℃/min; 1750 ℃ to 960 ℃, 4 ℃/min, furnace cooling then.As can be seen from Figure 2 particle obviously increases, and contact closely between particle.
Embodiment 4: with high-purity 3.8018g CaCO
3(＞99%), 9.0643g CuO (＞99%), 12.1343gTiO
2(＞99%) powder is a raw material, matches well 25g material, ball milling 12h in the distilled water medium by the CCTO stoichiometry; Powder after oven dry sieved is in 960 ℃ of pre-burning 2h.Powder after the pre-burning adds 15.6ml ethanol, 0.5ml propyl carbinol and 0.45ml triolein, puts into nylon ball grinder then, with ZrO
2Ball is a grinding medium, and putting into rotating speed is 350rad/min planetary ball mill wet-milling 20h; In the wet feed that grinds 20h, add 0.9674g polyoxyethylene glycol, 0.99ml dinoctyl phthalate, 1.4820g polyvinyl butyral acetal and 0.36ml hexanaphthene, and then ball milling 22h, rotating speed 350rad/min; Slurry is poured in the small beaker, taken out all ZrO
2Ball is poured slurry into then and is positioned in the casting machine that has clean smooth glass plate, makes it at the uniform velocity mobile on glass ribbon, forms thin casting belt.Wherein the thickness of curtain coating is by curtain coating blade control, and the speed that moves also has direct influence to the thickness of strip; Opened blowing apparatus dry 10 hours, demoulding is handled the green compact that just can obtain flow casting molding then, and the green compact of moulding are cut into the orthogonal thin slice; Carry out binder removal then and handle, the control of binder removal temperature rise rate is as follows: room temperature to 100 ℃, 2 ℃/min, insulation 1h in the time of 100 ℃; 100 ℃ to 550 ℃, 1 ℃/min, insulation 2h can remove fully to guarantee organism in the time of 550 ℃, creates conditions and makes base substrate obtain certain mechanical strength for burning till; Green compact after the binder removal processing are carried out sintering at 1100 ℃, and the control of sintering temperature rise rate: room temperature is to 1100 ℃ of required sintering temperatures, 3 ℃/min; 1100 ℃ to 960 ℃, 4 ℃/min, furnace cooling then.
Claims (1)
1. CaCu
3Ti
4O
12The preparation method of pottery is characterized in that comprising the steps:
(a) with high-purity CaCO
3(＞99%), CuO (＞99%), TiO
2(＞99%) powder is a raw material, presses 1: 3: 4 batching of CCTO stoichiometric ratio, ball milling 10～12h in the distilled water medium;
(b) powder after oven dry is sieved is in 900 ℃～1000 ℃ pre-burning 2～3h;
(c) powder after the pre-burning adds 29.4～29.9% ethanol, 0.5～1.0% propyl carbinol and 0.8～1% triolein, puts into nylon ball grinder then, with ZrO
2Ball is a grinding medium, and putting into rotating speed is 350～400rad/min planetary ball mill wet-milling, 20～24h;
(d) in the wet feed that grinds 20～24h, add 2.33～2.35% polyoxyethylene glycol, 2.35～2.37% dinoctyl phthalates, 3.2～3.6% polyvinyl butyral acetals and 0.4～0.6% hexanaphthene, and then ball milling 20～24h, rotating speed 350～400rad/min;
(e) slurry is poured in the small beaker, taken out all ZrO
2Ball is poured slurry into then and is positioned in the casting machine that has clean smooth glass plate, makes it at the uniform velocity mobile on glass ribbon, forms thin casting belt;
(f) opened the blowing apparatus drying 10～12 hours, demoulding is handled the green compact just can obtain flow casting molding then, and the green compact of moulding are cut into the orthogonal thin slice;
(g) carry out binder removal then and handle, the control of binder removal temperature rise rate is as follows: room temperature to 80～100 ℃, 2～3 ℃/min, insulation 1～2h in the time of 80～100 ℃; 80～100 ℃ to 500～600 ℃, 1～2 ℃/min, insulation 2～3h removes organism fully in the time of 500～600 ℃;
(h) green compact after the binder removal processing are carried out sintering at 1025 ℃～1100 ℃, the control of sintering temperature rise rate: room temperature is to 1025 ℃～1100 ℃ of required sintering temperatures, 3～4 ℃/min; 1025 ℃～1100 ℃ to 900～1000 ℃, 3～4 ℃/min, furnace cooling then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100450419A CN102173781A (en) | 2011-02-24 | 2011-02-24 | Preparation method of CaCu3Ti4O12 ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100450419A CN102173781A (en) | 2011-02-24 | 2011-02-24 | Preparation method of CaCu3Ti4O12 ceramic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102173781A true CN102173781A (en) | 2011-09-07 |
Family
ID=44517079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100450419A Pending CN102173781A (en) | 2011-02-24 | 2011-02-24 | Preparation method of CaCu3Ti4O12 ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102173781A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172363A (en) * | 2012-09-10 | 2013-06-26 | 常州大学 | Preparation method of high-dielectric-constant perovskite CaCu3Ti4O12 (CCTO) pressure-sensitive material |
| CN103695872A (en) * | 2013-12-23 | 2014-04-02 | 电子科技大学 | Preparation method of low dielectric-loss CaCu3Ti4O12 film |
| CN103805969A (en) * | 2013-12-27 | 2014-05-21 | 电子科技大学 | Preparation method of zirconium-doped CaCu3Ti4O12 film |
| CN103922394A (en) * | 2014-04-12 | 2014-07-16 | 中国科学院新疆理化技术研究所 | Preparation method of copper calcium titanate (CaCu3Ti4O12) with super-long nanowire structure and nanoribbon structure |
| CN103933990A (en) * | 2014-04-12 | 2014-07-23 | 中国科学院新疆理化技术研究所 | Preparation method of CaCu3Ti4O12 in icoshexahedron structure |
| CN104261817A (en) * | 2014-09-18 | 2015-01-07 | 中国人民大学 | CaCu3Ti4O12 system multilayer ceramic capacitor and preparation method thereof |
| CN105568383A (en) * | 2016-01-06 | 2016-05-11 | 中国科学院上海光学精密机械研究所 | Synthesis method of raw material for CaCuTi4O12 crystal growth and preparation method of CaCuTi4O12 crystal |
| CN106430983A (en) * | 2016-09-30 | 2017-02-22 | 济南大学 | Glass ceramic with CaCu3Ti4O12 phase and preparation method thereof |
| 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 |
| CN112457026A (en) * | 2020-12-14 | 2021-03-09 | 江西科技学院 | Copper calcium titanate ceramic reduction-oxidation atmosphere co-sintering method |
| CN112521166A (en) * | 2020-12-14 | 2021-03-19 | 江西科技学院 | Low dielectric loss CaCu3Ti4O12Negative pressure sintering method of ceramic |
| CN112552039A (en) * | 2020-12-14 | 2021-03-26 | 江西科技学院 | CaCu3Ti4O12Powder preparation and ceramic sintering method |
| CN113264766A (en) * | 2021-06-07 | 2021-08-17 | 西安交通大学 | Lead-free piezoelectric film material and preparation method thereof |
| CN115781894A (en) * | 2021-12-31 | 2023-03-14 | 江苏惟哲新材料有限公司 | Preparation method of low-temperature co-fired ceramic |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070245A (en) * | 2007-06-18 | 2007-11-14 | 厦门大学 | Low dielectric comsumption CaCu3Ti4O12 ceramic preparing method |
| CN101747058A (en) * | 2009-10-21 | 2010-06-23 | 南昌大学 | Method for synthesizing CaCu3Ti4O12 ceramic powder at low temperature |
| CN101747051A (en) * | 2009-10-21 | 2010-06-23 | 南昌大学 | Low-temperature sintering method of CaCu3Ti4O12 ceramic material |
| CN101792308A (en) * | 2010-02-11 | 2010-08-04 | 哈尔滨工业大学 | Shell-core structure ceramic material CaCu3Ti4O12 and preparation method thereof |
-
2011
- 2011-02-24 CN CN2011100450419A patent/CN102173781A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070245A (en) * | 2007-06-18 | 2007-11-14 | 厦门大学 | Low dielectric comsumption CaCu3Ti4O12 ceramic preparing method |
| CN101747058A (en) * | 2009-10-21 | 2010-06-23 | 南昌大学 | Method for synthesizing CaCu3Ti4O12 ceramic powder at low temperature |
| CN101747051A (en) * | 2009-10-21 | 2010-06-23 | 南昌大学 | Low-temperature sintering method of CaCu3Ti4O12 ceramic material |
| CN101792308A (en) * | 2010-02-11 | 2010-08-04 | 哈尔滨工业大学 | Shell-core structure ceramic material CaCu3Ti4O12 and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《硅酸盐通报》 20101031 周建民等 "制备电子陶瓷基片用的流延成型工艺" 第1114页倒数第1段至第1116页倒数第1段 1 第29卷, 第5期 * |
| 周建民等: ""制备电子陶瓷基片用的流延成型工艺"", 《硅酸盐通报》, vol. 29, no. 5, 31 October 2010 (2010-10-31) * |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172363B (en) * | 2012-09-10 | 2014-08-13 | 常州大学 | Preparation method of high-dielectric-constant perovskite CaCu3Ti4O12 (CCTO) pressure-sensitive material |
| CN103172363A (en) * | 2012-09-10 | 2013-06-26 | 常州大学 | Preparation method of high-dielectric-constant perovskite CaCu3Ti4O12 (CCTO) pressure-sensitive material |
| CN103695872B (en) * | 2013-12-23 | 2016-06-29 | 电子科技大学 | A kind of low-dielectric loss CaCu3Ti4O12The preparation method of thin film |
| CN103695872A (en) * | 2013-12-23 | 2014-04-02 | 电子科技大学 | Preparation method of low dielectric-loss CaCu3Ti4O12 film |
| CN103805969A (en) * | 2013-12-27 | 2014-05-21 | 电子科技大学 | Preparation method of zirconium-doped CaCu3Ti4O12 film |
| CN103805969B (en) * | 2013-12-27 | 2016-01-20 | 电子科技大学 | A kind of CaCu mixing zirconium 3ti 4o 12the preparation method of film |
| CN103922394A (en) * | 2014-04-12 | 2014-07-16 | 中国科学院新疆理化技术研究所 | Preparation method of copper calcium titanate (CaCu3Ti4O12) with super-long nanowire structure and nanoribbon structure |
| CN103933990A (en) * | 2014-04-12 | 2014-07-23 | 中国科学院新疆理化技术研究所 | Preparation method of CaCu3Ti4O12 in icoshexahedron structure |
| CN103933990B (en) * | 2014-04-12 | 2016-01-20 | 中国科学院新疆理化技术研究所 | A kind of preparation method of 26 body structure CaCu 3 Ti 4 Os |
| CN103922394B (en) * | 2014-04-12 | 2016-03-02 | 中国科学院新疆理化技术研究所 | The preparation method of a kind of overlong nanowire structure and nano belt structure CaCu 3 Ti 4 O |
| CN104261817A (en) * | 2014-09-18 | 2015-01-07 | 中国人民大学 | CaCu3Ti4O12 system multilayer ceramic capacitor and preparation method thereof |
| CN105568383A (en) * | 2016-01-06 | 2016-05-11 | 中国科学院上海光学精密机械研究所 | Synthesis method of raw material for CaCuTi4O12 crystal growth and preparation method of CaCuTi4O12 crystal |
| CN106430983A (en) * | 2016-09-30 | 2017-02-22 | 济南大学 | Glass ceramic with CaCu3Ti4O12 phase and preparation method thereof |
| CN106430983B (en) * | 2016-09-30 | 2018-11-20 | 济南大学 | One kind containing CaCu3Ti4O12Devitrified glass of phase and preparation method thereof |
| 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 |
| CN112457026A (en) * | 2020-12-14 | 2021-03-09 | 江西科技学院 | Copper calcium titanate ceramic reduction-oxidation atmosphere co-sintering method |
| CN112521166A (en) * | 2020-12-14 | 2021-03-19 | 江西科技学院 | Low dielectric loss CaCu3Ti4O12Negative pressure sintering method of ceramic |
| CN112552039A (en) * | 2020-12-14 | 2021-03-26 | 江西科技学院 | CaCu3Ti4O12Powder preparation and ceramic sintering method |
| CN112552039B (en) * | 2020-12-14 | 2022-12-06 | 江西科技学院 | CaCu 3 Ti 4 O 12 Powder preparation and ceramic sintering method |
| CN113264766A (en) * | 2021-06-07 | 2021-08-17 | 西安交通大学 | Lead-free piezoelectric film material and preparation method thereof |
| CN115781894A (en) * | 2021-12-31 | 2023-03-14 | 江苏惟哲新材料有限公司 | Preparation method of low-temperature co-fired ceramic |
| CN115781894B (en) * | 2021-12-31 | 2024-06-07 | 江苏惟哲新材料有限公司 | Preparation method of low-temperature co-fired ceramic |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102173781A (en) | Preparation method of CaCu3Ti4O12 ceramic | |
| CN104016674B (en) | A kind of barium titanate-based lead-free piezoelectric ceramic and preparation method thereof | |
| CN103613382B (en) | Sodium bismuth titanate-barium titanate-potassium bismuth titanate lead-free piezoelectric texture ceramic and preparation method thereof | |
| CN107573050B (en) | Preparation method of ultra-large manganese-zinc ferrite magnetic core | |
| CN101805185A (en) | Method for preparing leadmagnesio-niobate lead titanate relaxation ferroelectric ceramics | |
| CN114644523A (en) | Perovskite structure high-entropy dielectric ceramic and preparation method thereof | |
| CN111233465A (en) | Sodium bismuth titanate-barium titanate lead-free piezoelectric textured ceramic and preparation method thereof | |
| CN107840655B (en) | Preparation method of bismuth potassium titanate-based lead-free relaxation ferroelectric ceramic with morphotropic phase boundary | |
| CN108947504A (en) | Submicrometer structure ultrathin alumina ceramic substrate and preparation method | |
| CN103787653A (en) | Preparation method of carbon-modified CaCu3Ti4O12 high dielectric material | |
| CN113880576B (en) | Low sintering temperature and anisotropic strontium barium niobate sodium tungsten bronze type piezoelectric ferroelectric ceramic material and preparation method thereof | |
| CN114436643A (en) | Giant dielectric constant and low dielectric loss ceramic and preparation method thereof | |
| CN104098330B (en) | Post growth annealing is adopted to prepare the method for high-performance barium strontium titanate pyroelectric ceramics | |
| CN111004030B (en) | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof | |
| CN104909747A (en) | Preparation method for CaCu3Ti4-xZrxO12 ceramic with high dielectric constant and low dielectric loss | |
| Yan et al. | Grain growth, densification and electrical properties of lead-free piezoelectric ceramics from nanocrystalline (Ba 0.85 Ca 0.15)(Ti 0.90 Zr 0.10) O 3 powder by sol–gel technique | |
| CN112645709A (en) | PZT-based piezoelectric ceramic and preparation method thereof | |
| Wang et al. | Investigation on the phase transition behavior and electrical properties of textured Lix (K0. 48Na0. 52) 1− xNbO3 piezoelectric ceramics | |
| CN115417670B (en) | High-dielectric-constant ceramic with high-entropy design at B site and preparation method thereof | |
| CN115849905A (en) | High-temperature piezoelectric ceramic material, preparation method and application | |
| CN114276128B (en) | Method for reducing leakage current of bismuth ferrite-barium titanate piezoelectric ceramic and improving high-temperature resistivity of bismuth ferrite-barium titanate piezoelectric ceramic | |
| CN102060527A (en) | Doped and modified barium strontium calcium titanate heat-release pyroelectric ceramic material and preparation method thereof | |
| CN105272217B (en) | A kind of barium-strontium titanate-based Toughened Alumina Ceramics of high energy storage density and preparation method thereof | |
| CN113773073A (en) | Strontium titanate-based ceramic material and preparation method and application thereof | |
| CN109704760B (en) | Single-phase multiferroic ceramic with Oliviz structure and non-stoichiometric ratio and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110907 |