CN100420653C - Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic - Google Patents
Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic Download PDFInfo
- Publication number
- CN100420653C CN100420653C CNB2006101652563A CN200610165256A CN100420653C CN 100420653 C CN100420653 C CN 100420653C CN B2006101652563 A CNB2006101652563 A CN B2006101652563A CN 200610165256 A CN200610165256 A CN 200610165256A CN 100420653 C CN100420653 C CN 100420653C
- Authority
- CN
- China
- Prior art keywords
- laser
- nitrogen
- piezoelectric ceramic
- preheating
- ceramics
- 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.)
- Expired - Fee Related
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 239000011734 sodium Substances 0.000 title claims description 19
- 238000000034 method Methods 0.000 title claims description 17
- 229910052700 potassium Inorganic materials 0.000 title description 3
- 229910052708 sodium Inorganic materials 0.000 title description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title 1
- 239000011591 potassium Substances 0.000 title 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 235000015895 biscuits Nutrition 0.000 claims abstract description 7
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 9
- 238000010438 heat treatment Methods 0.000 abstract 2
- 238000005507 spraying Methods 0.000 abstract 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 10
- 238000005245 sintering Methods 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- 239000010955 niobium Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 239000013068 control sample Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000009770 conventional sintering Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 1
- 239000011222 crystalline ceramic Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The laser preparation process of no-lead potassium sodium niobate piezoelectric ceramic belongs to the field of no-lead piezoelectric ceramic technology. The preparation process includes compounding material based on NaxK1-xNbO3, pre-baking, pressing into ceramic biscuit, pre-heating with laser as heat source at 150-300 deg.c for 30-60 sec, heating in the temperature raising speed of 10-20 deg.c/min, at 800-1100 deg.c while spraying oxygen or nitrogen, axially drawing after 30-120 sec at the speed of 0.02-0.06 mm/s for 1-10 mm, turning off laser to cool while further spraying oxygen or nitrogen. The piezoelectric ceramic has average density over 97 %, Tc up to 400 deg.c, and d33 of 30-70pC/N.
Description
Technical field
The invention belongs to the leadless piezoelectric ceramics preparation field.
Background technology
Piezoelectric ceramics is widely used in high-tech sectors such as information, laser, navigation and biology.Yet now extensive use mostly be the lead base piezoceramic material, produce, use and discarded after treating processes in cause serious harm all can for the mankind and ecotope, so development of new high-performance Pb-free piezoelectric ceramics be one urgent, have a task of great society and economic implications.Compare with the lead base material, the leadless piezoelectric ceramics density of conventional sintering method preparation is low, and performance is difficult to satisfy produces actual needs, and the main path that improves its performance is always to seek new high performance composition system.Therefore at present disclosed the and report of document is adopting ion doping or replacing the protection of metathetical multicomponent columbate leadless piezoelectric ceramics system Recipe; as Chinese patent publication number CN1511802A; Chinese patent publication number CN1644562A, Chinese patent publication number CN1810711A etc.Document " development of high-performance potassium-sodium niobate lead-free piezoelectric ceramics " (electronic component and material Vol.24No.11), the representative document of " preparation and performance of niobium tantalate leadless piezoelectric ceramics " (electronic component and material Vol.23No.11) and other relevant potassium sodium niobate research: Y.P.Guo, K.I.Kakimoto, et al.:Materials Letters, 59 (2005) 241, S.D.Bu, E.Shin, et al:Applied Physics Letters, the piezoelectric that also is near the new chemical composition system of searching accurate similar shape phase boundary that 73 (1998) 1442 grades are reported is to reach the purpose of improving the piezoelectric ceramics performance.
Mono-crystalline piezoelectric materials can present the piezoelectric property more much bigger than other direction in a certain direction, but the preparation cost height, preparation size is limited.Utilize the crystal grain orienting technology, might produce the new ceramic material that has the oriented growth feature with the similar crystal grain of monocrystalline, reach the purpose of improving piezoelectric property.Document Nature, 432 (2004) 84 reports, people such as Yasuyoshi Saito adopt the method for reaction template, by with epitaxially grown thin slice multilayer stack back sintering, prepare (the K with grain orientation feature that performance can reach the practical application standard
0.44Na
0.52Li
0.04) (Nb
0.84Ta
0.10Sb
0.06) O
3Polycrystalline ceramics.But this kind technical matters link is many, the flow process complexity, and the cost height, but also the necessary interpolation of considering suitable template crystal grain should not realize large-scale mass production.Document " piezoelectric ceramics crystal grain orienting technology " (electronic component and material Vol.23No.11) is also concentrated to have introduced and is comprised that the several frequently seen of this achievement in research reaches in the piezoelectric ceramics crystal grain orienting technology of grinding, but the report of not relevant with laser preparation grain orientation growth technology.Chinese patent ZL200410050131.7, ZL03148244.9, ZL03148245.7 etc. have reported laser sintered dielectric ceramic and crystalline ceramics technology, but the potassium-sodium niobate series piezoelectric ceramic has the advantages that to be different from above-mentioned pottery, thereby himself characteristics and unique severity are arranged on technology of preparing, be different from the technology of preparing of above-mentioned pottery.Be embodied in: 1, need special technique technology to realize the oriented growth of crystal grain in the pottery, reach the purpose of improving the piezoelectric ceramics performance.2, need in sintering process, suppress the volatilization of easy volatile elements such as Na, K, can guarantee that just obtaining high-compactness becomes porcelain.3, need strict monitoring temperature in the preparation, therefore need to be converted into by temp measuring system the monitoring of laser power the real-time strictness of sample temperature is monitored, control with generation and disappearance process Transient liquid phase in the sintering, improve the density of pottery, and help obtaining the pure phase structure of ceramic uhligite, to guarantee into the good physical behavior of porcelain.These all be the above-mentioned Chinese patent technical scheme of having announced can't realize.
Through document and patent retrieval, relevant at present high-compactness lead free piezoelectric ceramics of potassium sodium niobate and the laser preparation method thereof with grain orientation growth characteristics yet there are no report.
Summary of the invention
The object of the present invention is to provide a kind of employing laser as direct heat source, do not adding template crystal grain, under the situation without post-processed such as forge hot, hot pressing, preparation has the high-compactness lead free piezoelectric ceramics of potassium sodium niobate of grain orientation growth characteristics, obtains good physicals.
The objective of the invention is to be achieved through the following technical solutions:
1) with Nb
2O
5, K
2CO
3, Na
2CO
3Be raw material, according to chemical formula Na
xK
1-xNbO
3Prepare burden, after pre-burning, compressing tablet become biscuit of ceramics, be that thermal source carries out the irradiation preheating with laser, warm up time 30～60s, 150～300 ℃ of preheating temperatures;
2) preheating finishes the back intensification, and 10～20 ℃/min of heat-up rate sprays oxygen or nitrogen to this ceramic sample when being warming up to 800～1100 ℃;
3) behind 30～120s, above-mentioned ceramic sample is in axial direction lifted motion, speed is 0.02～0.06mm/s;
4) finish lift distance 1～10mm after, light is closed in cooling, continues logical oxygen or nitrogen 3～10min;
In above-mentioned steps 3) and the process of step 4) in always to this ceramic sample spray oxygen or nitrogen, the temperature control in the whole process is to be that thermal source carries out irradiation with laser.
According to above-mentioned processing method, can obtain having the high-compactness (ρ=4.41～4.46g/cm of grain orientation growth characteristics
3) piezoelectric ceramics, Curie temperature height (T
c＞400 ℃).After polarization, piezoelectric constant d
33Between 30～70pC/N.
Compared with prior art, the invention has the beneficial effects as follows:
1. in open sintering process, can carry out instantaneous adjusting and pass through the real-time strict temperature control of temp measuring system laser power by program, also can be aided with lifting and in sintering process, feeding work atmosphere of microcomputer control sample table or laser head, come to control more exactly the oriented growth process and the densification process of ceramic crystalline grain.
2. the Na for preparing
xK
1-xNbO
3Leadless piezoelectric ceramics density height (ρ=4.41～4.46g/cm
3), relative density can be greater than 97%.
3. elapsed-time standards short (＜10 minutes) under the sintering high temperature (800～1100 ℃) passes to work atmosphere in addition, is easy to suppress atom volatilizations at high temperature such as Na, K, guarantees the set of dispense ratio.
4. the Na for preparing
xK
1-xNbO
3Leadless piezoelectric ceramics has the perovskite structure of pure phase, helps the raising of piezoelectric property.
5. the present invention improves the piezoelectric property of perovskite typed leadless piezoelectric ceramics with the approach that obtains grain orientation growth and raising ceramic dense degree, so is not subject to the set of dispense ratio, and processing method is suitable for preparing the potassium-sodium niobate series ceramic material of each set of dispense ratio.
Description of drawings
Fig. 1 is the prepared Na of the present invention
0.5K
0.5NbO
3The leadless piezoelectric ceramics x-ray diffractogram of powder.As can be seen, prepared leadless piezoelectric ceramics has the perovskite structure of pure phase.
Fig. 2 (a) is the prepared Na of the present invention
0.5K
0.5NbO
3Leadless piezoelectric ceramics microstructure laser confocal scanning figure.With comparing with the component microstructure of ceramics of the preparation of conventional sintering method shown in Fig. 2 (b), the crystal grain of laser sintered sample has tangible oriented growth feature as can be seen, and void content is low, the density height.
Fig. 3 is the prepared Na of the present invention
0.35K
0.65NbO
3Leadless piezoelectric ceramics dielectric thermogram.Laser sintered as can be seen Na
0.5K
0.5NbO
3Leadless piezoelectric ceramics with 410 ℃ have tangible transformation temperature, meet the pure phase phase change characteristics of this kind material, have 410 ℃ high curie point simultaneously, demonstrate the good operation temperature profile.
Fig. 4 is the prepared Na of the present invention
0.85K
0.15NbO
3Leadless piezoelectric ceramics tuning curve figure, line smoothing does not have clutter.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Embodiment 1:
Adopt the low-power laser irradiation preheating by Nb
2O
5, K
2CO
3, Na
2CO
3The biscuit of ceramics that powder forms through batching, pre-burning, compressing tablet carries out sample temperature by temp measuring system and monitors in real time, warm up time 30s, 150 ℃ of preheating temperatures, speed raising laser power density with 20 ℃/min heats up then, during to 900 ℃, adopts the logical oxygen of nozzle ceramic plate in sintering, behind the 50s, microcomputer control sample table or laser head lift along the ceramic plate axial direction due and move, and pull rate is 0.02mm/s, finish to lift apart from behind the 1mm, light is closed in cooling, continues logical oxygen 5min.
Sample performance value: ρ=4.45g/cm
3, Tc=400 ℃, d
33=57pC/N, ε=311.52, tan δ (%)=4.94.
Embodiment 2:
Adopt the low-power laser irradiation preheating by Nb
2O
5, K
2CO
3, Na
2CO
3The biscuit of ceramics that powder forms through batching, pre-burning, compressing tablet, warm up time 60s, 270 ℃ of preheating temperatures improve laser power density with the speed of 15 ℃/min then and heat up, during to 1100 ℃, adopt the logical oxygen of nozzle ceramic plate in sintering, behind the 30s, microcomputer control sample table or laser head lift along the ceramic plate axial direction due and move, pull rate is 0.05mm/s, finish lifting apart from behind the 5mm, light is closed in cooling, continues logical oxygen 3min.
Sample performance value: ρ=4.46g/cm
3, Tc=410 ℃, d
33=63pC/N, ε=303.46, tan δ (%)=4.09.
Embodiment 3:
Adopt the low-power laser irradiation preheating by Nb
2O
5, K
2CO
3, Na
2CO
3The biscuit of ceramics that powder forms through batching, pre-burning, compressing tablet, warm up time 50s, 300 ℃ of preheating temperatures improve laser power density with the speed of 10 ℃/min then and heat up, during to 800 ℃, adopt the logical oxygen of nozzle ceramic plate in sintering, behind the 120s, microcomputer control sample table or laser head lift along the ceramic plate axial direction due and move, pull rate is 0.06mm/s, finish lifting apart from behind the 10mm, light is closed in cooling, continues logical oxygen 10min.
Sample performance value: ρ=4.46g/cm
3, Tc=412 ℃, d
33=70pC/N, ε=309.78, tan δ (%)=4.25.
Embodiment 4:
Adopt the low-power laser irradiation preheating by Nb
2O
5, K
2CO
3, Na
2CO
3The biscuit of ceramics that powder forms through batching, pre-burning, compressing tablet, warm up time 60s, 300 ℃ of preheating temperatures improve laser power density with the speed of 10 ℃/min then and heat up, during to 900 ℃, adopt the logical nitrogen of nozzle ceramic plate in sintering, behind the 80s, microcomputer control sample table or laser head lift along the ceramic plate axial direction due and move, pull rate is 0.05mm/s, finish lifting apart from behind the 10mm, light is closed in cooling, continues logical nitrogen 10min.
Sample performance value: ρ=4.41g/cm
3, Tc=385 ℃, d
33=34pC/N, ε=297.21, tan δ (%)=4.02.
Claims (1)
1. the laser preparation method of a lead free piezoelectric ceramics of potassium sodium niobate is characterized in that, may further comprise the steps:
1) with Nb
2O
5, K
2CO
3, Na
2CO
3Be raw material, according to chemical formula Na
xK
1-xNbO
3Prepare burden, after pre-burning, compressing tablet become biscuit of ceramics, be that thermal source carries out the irradiation preheating with laser, warm up time 30～60s, 150～300 ℃ of preheating temperatures;
2) preheating finishes the back intensification, and 10～20 ℃/min of heat-up rate sprays oxygen or nitrogen to this ceramic sample when being warming up to 800～1100 ℃;
3) behind 30～120s, above-mentioned ceramic sample is in axial direction lifted motion, speed is 0.02～0.06mm/s;
4) finish lift distance 1～10mm after, light is closed in cooling, continues logical oxygen or nitrogen 3～10min;
In above-mentioned steps 3) and the process of step 4) in always to this ceramic sample spray oxygen or nitrogen, the temperature control in the whole process is to be that thermal source carries out irradiation with laser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101652563A CN100420653C (en) | 2006-12-15 | 2006-12-15 | Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101652563A CN100420653C (en) | 2006-12-15 | 2006-12-15 | Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1974481A CN1974481A (en) | 2007-06-06 |
| CN100420653C true CN100420653C (en) | 2008-09-24 |
Family
ID=38124876
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101652563A Expired - Fee Related CN100420653C (en) | 2006-12-15 | 2006-12-15 | Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100420653C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337813B (en) * | 2008-08-15 | 2012-07-04 | 合肥学院 | Multicomponent few-lead piezoelectric ceramics of high tension performance and method for preparing same |
| CN106087058A (en) * | 2016-06-22 | 2016-11-09 | 桂林电子科技大学 | A kind of K0.5na0.5nbO3base ferroelectric piezoelectric single crystal and preparation method thereof |
| CN107892567B (en) * | 2017-11-03 | 2020-12-04 | 北京工业大学 | (Bi)1/2K1/2)TiO3Base binary leadless piezoelectric ceramic and preparation thereof |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460657A (en) * | 2003-07-04 | 2003-12-10 | 北京工业大学 | Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics |
| CN1480427A (en) * | 2003-07-04 | 2004-03-10 | 北京工业大学 | Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant |
| CN1587200A (en) * | 2004-06-28 | 2005-03-02 | 北京工业大学 | Laser preparing method for Ta2O5 base transparent ceramics |
-
2006
- 2006-12-15 CN CNB2006101652563A patent/CN100420653C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460657A (en) * | 2003-07-04 | 2003-12-10 | 北京工业大学 | Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics |
| CN1480427A (en) * | 2003-07-04 | 2004-03-10 | 北京工业大学 | Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant |
| CN1587200A (en) * | 2004-06-28 | 2005-03-02 | 北京工业大学 | Laser preparing method for Ta2O5 base transparent ceramics |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1974481A (en) | 2007-06-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102311266B (en) | Preparation method of (K05Na05) NbO3 (KNN) lead-free piezoelectric ceramic material | |
| CN101913868B (en) | Method for preparing potassium-sodium niobate textured ceramic and potassium-sodium niobate single crystal | |
| CN104876567B (en) | High tension electricity coefficient potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof | |
| CN102815939B (en) | Leadless piezoelectric textured ceramic material and preparation method thereof | |
| CN102503413B (en) | Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof | |
| CN101486570B (en) | Leadless piezoelectric structured thick film and preparation thereof | |
| Sasmal et al. | Effects of lanthanum oxide on the properties of barium-free alkaline-earth borosilicate sealant glass | |
| CN100420653C (en) | Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic | |
| CN102817080A (en) | Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof | |
| CN107098699A (en) | The leadless piezoelectric structured ceramics and preparation method of width sintering warm area and wide composition regulation | |
| CN103911662B (en) | The manufacture method of LGS piezoquartz and goods thereof | |
| CN105198417A (en) | Preparation method of zirconic acid sodium bismuthide lithium cerium doped potassium-sodium niobate based ceramic material | |
| CN104557058A (en) | Method for preparing high-transparency transparent electrooptic ceramics by performing composite vacuum-oxygen hot pressed sintering | |
| CN101429027A (en) | Potassium sodium niobate based leadless piezoelectric ceramic and low-temperature sintering production process | |
| CN104628379A (en) | Highly-oriented lead-free piezoelectric textured ceramic material and preparation method and application thereof | |
| CN101670691B (en) | Antiferroelectric film with adjustable working temperature zone and higher pyroelectric coefficient and preparation method thereof | |
| CN104557040B (en) | High-temperature thermistor material and preparation method thereof | |
| CN104744033A (en) | Sodium bismuth titanate-barium titanate lead-free transparent electro-optic ceramic and preparation method thereof | |
| CN102731107A (en) | Method for preparing Mn-doped bismuth sodium titanate-barium titanate film | |
| CN105254298A (en) | Lithium-doped potassium-sodium niobate single crystal with high piezoelectric property and preparation method thereof | |
| CN109626828A (en) | Containing NaNbO3The Na of phase2O-Nb2O5-SiO2High dielectric constant energy storage glass ceramics and preparation method | |
| CN101343729A (en) | Method for preparing lanthanum nickelate conductive metallic oxide nano-film | |
| CN113582692A (en) | Low-temperature sintered potassium-sodium niobate-based leadless piezoelectric ceramic material and preparation method thereof | |
| CN100500897C (en) | Process for preparing piezo-electricity composite material of ceramal | |
| CN104402426A (en) | Novel high temperature piezoelectric ceramic with ternary system of bismuth ferrite-lead titanate-lead zincate niobate (BF-PT-PZN) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: CHENGDU 3D CHANGE TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: BEIJING INDUSTRY UNIVERSITY Effective date: 20131024 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100022 CHAOYANG, BEIJING TO: 610000 CHENGDU, SICHUAN PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20131024 Address after: 610000, No. 199, West Avenue, hi tech Zone, Sichuan, Chengdu Patentee after: Chengdu 3D Change Technology Co., Ltd. Address before: 100022 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee before: Beijing University of Technology |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080924 Termination date: 20151215 |
|
| EXPY | Termination of patent right or utility model |