CN101265094A - Pyroelectric lithium tantalite LiTa3O8 thin film and preparation technique thereof - Google Patents
Pyroelectric lithium tantalite LiTa3O8 thin film and preparation technique thereof Download PDFInfo
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- CN101265094A CN101265094A CNA2008100449636A CN200810044963A CN101265094A CN 101265094 A CN101265094 A CN 101265094A CN A2008100449636 A CNA2008100449636 A CN A2008100449636A CN 200810044963 A CN200810044963 A CN 200810044963A CN 101265094 A CN101265094 A CN 101265094A
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Abstract
The invention relates to a pyroelectric lithium tantalate (LiTa3O8) film and a sol-gel production method thereof. The pyroelectric lithium tantalate (LiTa3O8) film is novel in composition, has lower leakage current than the common lithium tantalate (LiTa3) film, and can bear higher polarization voltage. Beside of non-cooled pyroelectric property, the lithium tantalate (LiTa3O8) film has good ferroelectric, piezoelectric, photoelectric and nonlinear optical properties. The lithium tantalate (LiTa3O8) film can be used to produce functional device based on one or more properties thereof. The sol-gel production method of the lithium tantalate (LiTa3O8) film comprises the following steps: using platinum-gold or silicon single crystal as substrate, high-purity metallic lithium and tantalum ethoxide as raw materials and ethylene glycol monomethyl ether as solvent; preparing a LiTa3O8 sol in the presence of argon protective gas, spin-coating on the substrate to obtain a LiTa3O8 wet film, and rapidly annealing the wet film to obtain LiTa3O8 film with a thickness of 0.2-5 Mum.
Description
Technical field
The present invention relates to a kind of pyroelectric lithium tantalite LiTa
3O
8Film and preparation technology thereof refer to that especially sol-gel process prepares lithium tantalate LiTa
3O
8The technology of film.
Background technology
The performance indications of uncooled pyroelectric infrared detectors such as current-responsive, voltage responsive and detectivity, are inversely proportional to the responsive first thickness of rpyroelectric infrared, responsive unit more thin (in μ m magnitude), and device performance is just more good.And rpyroelectric infrared is responsive first at present, nearly all make with crystalline material, owing to be subjected to restrictions such as device geometries, gauge, very difficult manufacturing obtains the pyroelectric crystal thin slice of 1~2 μ m or following thickness, thereby has limited the application of pyroelectric crystal material aspect the detection of high-performance rpyroelectric infrared.
In recent years, inorganic pyroelectricity material, such as lead base pottery series material, TGS series material and lithium tantalate series material progressively develop into the main flow material of non-refrigeration Pyroelectric Thin Film Infrared Detector.From product both domestic and external and technical research report, the research of ceramic pyroelectric film material such as lead base PZT, PT, PLCT and device thereof is maximum, is the main flow of domestic and international practical pyroelectric electric device.Yet lead base pottery electric heating film also has its fatal shortcoming, because Tc is too high, with silicon technology and incompatible, makes the device manufacturing cost very high, has limited its commercial market competitive power.There is in addition serious lead contamination problem in lead base ceramic membrane and the device manufacturing processes, makes its development be subjected to environmentalist's censure and the restriction of various countries' environmental protection policy.The inorganic pyroelectric film material that can effectively substitute the environmental protection of lead base ceramic membrane at present mainly contains TGS series material and lithium tantalate series material.From the independent a certain index of device pyroelectric property (such as detectivity), the TGS material is better than the lithium tantalate material; Make angle from device, the TGS material brittle, the device fabrication difficulty, the production cost height, and lithium tantalate materials processing is good, has several different methods to produce, production cost is lower; From application point of view, TGS material Curie temperature is about 49 ℃, Curie temperature (618 ℃) than lithium tantalate material is much lower, the spendable temperature range of pyroelectric detector that the TGS material is made is very narrow, and the lithium tantalate material can use between room temperature to 618 ℃, and operating temperature range is very wide.Heat extraction is released outside the electrical characteristic, and the lithium tantalate material still is a kind of multifunctional material, also has characteristics such as good ferroelectric, piezoelectricity, electric light and nonlinear optics, usually utilizes its one or more characteristics to make functional device.So this patent has proposed a kind of pyroelectric lithium tantalite LiTa
3O
8Film can utilize its good pyroelectricity characteristic to make uncooled pyroelectric infrared detectors.
In lithium tantalate thin film preparation technology, select a kind of film quality and well behaved manufacturing process not a duck soup of guaranteeing again cheaply.From domestic and international research in recent years, attempted respectively making lithium tantalate thin film and device with technologies such as chemical mechanical polishing, ion etching, metal organic chemical vapor deposition (MOCVD), deposition of metal organic (MOD), rf magnetron sputtering, pyrosol, sol-gels.Comparatively speaking, chemical mechanical polishing and ion etching mainly obtain lithium tantalate thin film with the physics reduction process, because the factor of manufacturing limit, the film thickness of manufacturing generally more than 5 μ m, is difficult to reach 1~2 μ m.MOCVD and pyrosol technology are to make lithium tantalate thin film by chemical deposition process, and is same because its producing apparatus price is higher, is difficult to the thin film fabrication cost is lowered.The another kind of technology of making lithium tantalate thin film is rf magnetron sputtering technology, and it is to come the physical deposition lithium tantalate thin film by bombardment lithium tantalate ceramic target.Rf magnetron sputtering technology can only be made amorphous lithium tantalate thin film, and in the manufacturing processed, the lithium tantalate ceramic target often is not by the Li that estimates
+, Ta
+ 5The stoichiometric ratio sputtering sedimentation is so the microstructure of film crystal and large area deposition film consistence have much room for improvement.
Sol-gel technology is a kind of low cost process of making lithium tantalate thin film.Its advantage is accurately to control Li
+, Ta
+ 5Stoichiometric ratio, can make the high conformity of large area film and film at lesser temps, equipment and manufacturing expense are lower.Its shortcoming is the difficult grasp of the blending process of lithium tantalate colloidal sol; The thickness of film is all relevant with the concentration of even glue whirl coating speed, time and colloidal sol preparation, needs to determine with experiment as the case may be.
In addition, the lithium tantalate LiTaO of the common component of collosol and gel manufactured
3The leakage current of film is bigger, is difficult to bear high polarizing voltage in polarization process, is very easy to cause the puncture of thin-film device, makes the element manufacturing failure.So we have proposed a kind of lithium tantalate LiTa of new component in the sol-gel technology research process
3O
8Film has solved common lithium tantalate LiTaO by experiment
3The film leakage current is excessive, be difficult to bear high polarizing voltage problem in the polarization.
Summary of the invention
The present invention relates to a kind of pyroelectric lithium tantalite LiTa
3O
8Film and preparation technology thereof refer to that especially sol-gel process prepares lithium tantalate LiTa
3O
8The technology of film.
The pyroelectric lithium tantalite LiTa that the purpose of this invention is to provide a kind of new component
3O
8Film is with the lithium tantalate LiTaO of common component
3Film is compared, and has littler leakage current, can bear higher polarizing voltage, can produce the better lithium tantalate thin film device of performance.The lithium tantalate LiTa of new component provided by the invention
3O
8Film, it is a kind of electric heating film of non-refrigeration, cryogenic refrigeration can be worked, be need not to Infrared Detectors based on its manufacturing at ambient temperature, can solve the essential super low temperature refrigeration guarantee device normal operation of photon type Infrared Detectors, and cause detector manufacturing cost height, the problem of system architecture complexity.Heat extraction is released outside the electrical characteristics, lithium tantalate LiTa
3O
8Film also has good ferroelectric, piezoelectricity, electric light and nonlinear optical properties, utilizes its one or more characteristics can make function element.In addition, lithium tantalate LiTa
3O
8Film or a kind of electric heating film of environmental type can replace lead base pottery electric heating film, avoid lead base pottery electric heating film in the film preparation process problem, the problem includes: the lead contamination problem.
Another object of the present invention has provided a kind of sol-gel process and has prepared lithium tantalate LiTa
3O
8The technology of film.With Pt/Ti/SiO
2/ Si (100) or Si monocrystalline are substrate, take highly purified lithium metal and ethanol tantalum as raw material, take analytically pure EGME as solvent, at first prepare LiTa
3O
8Colloidal sol obtains LiTa by the spin-coating technology in substrate then
3O
8Wet film is by obtaining LiTa to the wet film rapid thermal annealing
3O
8Film.Repeat the LiTa that above-mentioned technology obtains desired thickness
3O
8Film.The lithium tantalate LiTa of sol-gel technology preparation provided by the invention
3O
8Film, its thickness can be accomplished 0.2~5 μ m or following, can take full advantage of the advantage that this thin-film material thermal capacitance is little, be not subjected to device geometries and gauge restriction, can replace the lithium tantalate material, prepare high performance non-refrigeration lithium tantalate Infrared Detectors.
Purpose of the present invention is realized by the following technical programs:
A kind of pyroelectric lithium tantalite LiTa
3O
8Thin film technology technology refers to that especially sol-gel process prepares lithium tantalate LiTa
3O
8The technology of film.Comprise:
A kind of lithium tantalate LiTa
3O
8The colloidal sol preparing process: adopt purity be 99.97% or above lithium metal and purity be 99.996% or above ethanol tantalum be initiation material, take analytically pure EGME as solvent, a certain amount of lithium metal is dissolved in the EGME of low-grade fever (40~70 ℃) earlier, prepares the alkoxide LiOC of lithium
2H
4OCH
3Then solution is poured in the clean beaker and placed baking oven to remove moisture, oven temperature is made as 100~140 ℃, storing time 300~400min; Add in the solution of cool to room temperature again after baking is good the analytically pure acetate regulator solution of 2~20ml acidity in the pH value between 3~7; Then add the proper amount of glycol methyl ether in the solution, and place on the magnetic stirring apparatus of band well heater solution is mixed, the heated and stirred temperature is made as 30~80 ℃, and the heated and stirred time is 10~60min; In solution, added ethanol tantalum solution in 1: 3 in molar ratio then, and solution stirring is heated to makes solution fully react the moisture of removing simultaneously in the solution more than 30~110 ℃, the stirring heating time is 30~120min, remove byproduct of reaction (ethanol) and water, the filtering particulate matter, add the proper amount of glycol methyl ether at last, adjusting and obtaining concentration is 0.2mol.L
-1Faint yellow LiTa
3O
8Colloidal sol.
A kind of lithium tantalate LiTa
3O
8The sol-gel technology of thin film fabrication: the LiTa that will prepare as stated above
3O
8It is 0.1mol.L that colloidal sol spent glycol methyl ether is diluted to concentration
-1, on even glue photoresist spinner with the colloidal sol spin coated on electroded monocrystal silicon substrate, form wet film, even adhesive tape part: 100~800rpm, 2~20s; Whirl coating condition: 2000~8000rpm, 10~100s.The wet film that obtains is placed rapid heat-treatment furnace, under oxygen atmosphere, anneal, crystallization.Annealing process is in two steps: organic solvent on the first step elder generation cracking film, temperature are set at 400~470 ℃ and keep 2~10min; Second step was crystallization of thin films, and Tc is made as 650~950 ℃ and keeps 2~8min.Repeatedly repeat above sol-gel technology, till film reaches desired thickness.In the thin film fabrication process,, guarantee that film is smooth, even, flawless with X-ray diffractometer XRD and scanning electron microscope sem viewing film quality.
The invention has the advantages that provides a kind of lithium tantalate of new component LiTa
3O
8Film is with the lithium tantalate LiTaO of common component
3Film is compared, and has littler leakage current, can bear higher polarizing voltage, when the test electric field is 47.6kV/cm, and LiTa
3O
8The film electric leakage is not more than 2.54 * 10
-7A/cm
2The thick LiTa of 1 μ m
3O
8Film can bear not breakdown up to the electric-field intensity of 700kV/cm.
The lithium tantalate LiTa of the new component that provides is provided
3O
8Film is a kind of electric heating film of non-refrigeration, can work at ambient temperature, need not cryogenic refrigeration, and can solve the photon type Infrared Detectors must 70~90K cryogenic refrigeration work and the cost height, the infrared system complex structure problem that cause.
The lithium tantalate LiTa of the new component that provides is provided
3O
8Film is a kind of electric heating film of environmental protection, can replace lead base pottery electric heating film and make pyroelectric electric device, the environmental protection problem that the serious lead contamination that can avoid lead base ceramic membrane and device to exist brings in manufacture process.
The present invention be advantageous in that the preparation lithium tantalate LiTa that is proposed
3O
8The sol-gel technology of film is a kind of low-cost manufacturing process, makes full use of it and can accurately control Li
+, Ta
+ 5Stoichiometric ratio, can make the high conformity of large area film and film at lesser temps, equipment and manufacturing expense are lower.Make full use of film sol-gel technology and the good advantage of device MEMS processing compatibility, solve lead base pottery electric heating film because Tc is too high, incompatible with silicon technology, cause the high problem of device manufacturing cost.
Description of drawings
Fig. 1 is a kind of lithium tantalate LiTa
3O
8The colloidal sol preparation process.
Fig. 2 is a kind of lithium tantalate LiTa
3O
8The sol-gel technology flow process of thin film fabrication.
Fig. 3 is Pt/Ti/SiO
2The amorphous lithium tantalate LiTa that sol-gel process prepares in/Si (100) substrate
3O
8The X-ray diffraction curve of film.
Fig. 4 is Pt/Ti/SiO
2The amorphous lithium tantalate LiTa that/Si (100) substrate sol-gel process prepares
3O
8The scanning electron microscope sem picture of film, Fig. 4 (a) scanning electron microscope sem plane, Fig. 4 (b) scanning electron microscope sem sectional drawing.
Embodiment
Lithium tantalate LiTa with reference to figure 1
3O
8The colloidal sol preparation process.Described lithium tantalate LiTa
3O
8The colloidal sol preparing process is sol-gel technology, adopt purity be 99.97% or above lithium metal and purity be 99.996% or above ethanol tantalum be initiation material, take analytically pure EGME as solvent.Under the argon atmospher protection, accurately take by weighing a certain amount of high-purity lithium earlier; put into eggplant shape beaker; add a certain amount of glycol monoethyl ether (MOE), low-grade fever (40~70 ℃) is reacted until lithium metal all dissolves, and the spent glycol monomethyl ether is diluted to the alkoxide LiOC of lithium
2H
4OCH
3Concentration is 0.5mol.L
-1Then solution is poured in the clean beaker and placed baking oven to remove moisture, oven temperature is made as 100~124 ℃, storing time 300~400min; Add in the solution of cool to room temperature again after baking is good analytically pure acetate of 2~10ml or butyric acid regulator solution acidity in the pH value between 3~7; Then add the proper amount of glycol monomethyl ether in the solution, and place on the magnetic stirring apparatus of band well heater solution is mixed, the heated and stirred temperature is made as 50~60 ℃, and the heated and stirred time is 10~30min; In solution, added ethanol tantalum solution in 1: 3 in molar ratio then, with the about 30~120min of Rotary Evaporators reflux, be heated to more than 30~110 ℃, byproduct of reaction (ethanol) and moisture are removed in evaporation, the filtering particulate matter adds proper amount of glycol methyl ether diluting soln at last to 0.2mol.L
-1Faint yellow LiTa
3O
8Colloidal sol.
A kind of new component lithium tantalate LiTa with reference to figure 2
3O
8The sol-gel technology flow process of thin film fabrication: the LiTa that will prepare as stated above
3O
8It is 0.1mol.L that colloidal sol spent glycol methyl ether is diluted to concentration
-1, on desk-top even glue photoresist spinner with the colloidal sol spin coated in platinum Pt/Ti/SiO
2On/Si (100) substrate or the Si single crystal substrates, form wet film, even glue whirl coating condition is: even glue: 100~800rpm keeps 2~20s; Whirl coating: 2000~8000rpm keeps 10~100s.The wet film that obtains is placed rapid heat-treatment furnace, under oxygen atmosphere, anneal, crystallization.Annealing process is in two steps: organic solvent on the first step elder generation cracking film, temperature are set at 400~470 ℃ and keep 2~10min; Second step was crystallization of thin films, and Tc is made as 650~950 ℃, kept 2~8min.Repeatedly repeat above sol-gel technology, film thickness can reach between 0.2~5 μ m.In the thin film fabrication process,, guarantee that film is smooth, even, flawless by X-ray diffractometer XRD and scanning electron microscope SFM viewing film quality of forming film.
Embodiment
Adopting highly purified metallic lithium and ethanol tantalum is raw material, is solvent with analytically pure ethylene glycol monomethyl ether, prepares LiTa under the argon atmospher protection
3O
8It is 0.1mol.L that colloidal sol, spent glycol monomethyl ether are diluted to concentration
-1, on desk-top even glue photoresist spinner with the colloidal sol spin coated in Pt/Ti/SiO
2In/Si (100) substrate, form wet film, wet film is placed rapid heat-treatment furnace is annealed, crystallization treatment under oxygen atmosphere.Repeat above-mentioned technology, prepare the amorphous LiTa of desired thickness
3O
8Film, its X-ray diffraction curve as shown in Figure 3.Utilize the scanning electron microscope sem test to find that film is smooth, even, flawless, with Pt/Ti/SiO
2/ Si (100) substrate is in conjunction with good, and film thickness is about 1 μ m, as shown in Figure 4.
Claims (9)
1, a kind of pyroelectric lithium tantalite LiTa
3O
8Film and preparation technology thereof refer to that especially sol-gel process prepares lithium tantalate LiTa
3O
8The technology of film comprises:
A kind of pyroelectric lithium tantalite LiTa
3O
8Film.Described pyroelectric lithium tantalite LiTa
3O
8Film is a kind of lithium tantalate thin film of new component, than common lithium tantalate LiTaO
3Film has littler leakage current, can bear higher polarizing voltage.Described lithium tantalate LiTa
3O
8Film, it is a kind of electric heating film of non-refrigeration, cryogenic refrigeration can be worked, be need not to Infrared Detectors based on its manufacturing at ambient temperature, solved the essential super low temperature refrigeration guarantee device normal operation of photon type Infrared Detectors, and cause detector manufacturing cost height, the problem of system architecture complexity.Heat extraction is released outside the electrical characteristics, described lithium tantalate LiTa
3O
8Film also has good ferroelectric, piezoelectricity, electric light and nonlinear optical properties, utilizes its one or more characteristics can make function element.In addition, described lithium tantalate LiTa
3O
8Film or a kind of electric heating film of environmental type can replace lead base pottery electric heating film and make pyroelectric infrared detector, can avoid lead base pottery electric heating film in film and device preparation process problem, the problem includes: the lead contamination problem.
A kind of sol-gel process prepares lithium tantalate LiTa
3O
8The technology of film.Described pyroelectric lithium tantalite LiTa
3O
8Film sol-gel process preparation technology is with platinum substrate (Pt/Ti/SiO
2/ Si (100)) or silicon single crystal be substrate, take highly purified lithium metal and ethanol tantalum as raw material, take analytically pure EGME as solvent, under the argon atmospher protection, prepare LiTa
3O
8Colloidal sol is at the fixing Pt/Ti/SiO of desk-top even glue photoresist spinner
2/ Si (100) substrate or Si single crystal substrates, form wet film by spin coated in substrate, the wet film that obtains is placed rapid heat-treatment furnace, under oxygen atmosphere, anneal, crystallization heat processes, and repeats smooth, even, the flawless LiTa that above-mentioned technology obtains desired thickness at last
3O
8Film.The lithium tantalate LiTa of above-mentioned sol-gel technology preparation
3O
8Film, its thickness can be accomplished 0.2~5 μ m or following, can take full advantage of the advantage that this thin-film material thermal capacitance is little, be not subjected to device geometries and gauge restriction, have greatly improved the performance of non-refrigeration lithium tantalate Infrared Detectors.The pyroelectric lithium tantalite LiTa of described new component
3O
8Film sol-gel process preparation technology is a kind of low-cost manufacturing process, has accurately to control Li
+, Ta
+ 5Stoichiometric ratio, can make the high conformity of large area film and film at lesser temps, the advantage that equipment and manufacturing expense are lower.Make full use of film sol-gel technology and the good advantage of device MEMS processing compatibility, can solve lead base pottery electric heating film because Tc is too high, incompatible with silicon technology, cause the high problem of device manufacturing cost.
2, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: described lithium tantalate thin film is meant Li in the film
+, Ta
+ 5Stoichiometric ratio is 1: 3 LiTa
3O
8Film, rather than LiTaO
3Film.
3, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: described pyroelectric lithium tantalite LiTa
3O
8Film is a kind of lead-free non-refrigeration electric heating film, can be used for preparing uncooled pyroelectric infrared detectors.
4, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: described pyroelectric lithium tantalite LiTa
3O
8Film is than common LiTaO
3Film has littler leakage current, tolerates higher polarizing voltage.When the test electric field is 47.6kV/cm, LiTa
3O
8The film electric leakage is not more than 2.54 * 10
-7A/cm
2The thick LiTa of 1 μ m
3O
8Film can bear the electric-field intensity that is not more than 700kV/cm and be not breakdown.
5, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof refer to that especially sol-gel process prepares lithium tantalate LiTa
3O
8The technology of film is characterized in that: the lithium tantalate LiTa of described sol-gel technology preparation
3O
8Film thickness can arrive 0.2~5 μ m or following, can replace the lithium tantalate material, prepares high performance non-refrigeration lithium tantalate Infrared Detectors.
6, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: lithium tantalate LiTa
3O
8Thin film preparation process refers in particular to sol-gel technology, used LiTa
3O
8Colloidal sol is to be 99.996% or above ethanol tantalum Ta (OC2H5) 5 and lithium ethoxide LiOC with purity
2H
4OCH
3The raw material preparation.Lithium ethoxide LiOC wherein
2H
4OCH
3Be by purity be 99.996% or above lithium metal in the glycol monoethyl ether of low-grade fever (40~70 ℃), dissolve and obtain.Be dissolved in the glycol monoethyl ether by mixed ethanol tantalum and lithium ethoxide, be heated to 30~110 ℃ of swirling recirculation flow 30~120min and obtain LiTa
3O
8Colloidal sol.Preparation LiTa
3O
8Protective gas in the sol-process is argon gas.
7, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: LiTa
3O
8The film preparation substrate is platinum substrate (Pt/Ti/SiO
2/ Si (100)) or the silicon single crystal substrate.
8, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: described preparation lithium tantalate LiTa
3O
8The sol-gel technology of film forms LiTa
3O
8The even adhesive tape part of wet film is rotating speed 100~800rpm, keeps 2~20s; The whirl coating condition is that rotating speed is 2000~8000rpm, keeps 10~100s.
9, according to the described pyroelectric lithium tantalite LiTa of claim 1
3O
8Film and preparation technology thereof is characterized in that: described preparation lithium tantalate LiTa
3O
8The short annealing condition of wet film is to carry out double annealing: organic solvent on the first step elder generation cracking film, and Temperature Setting is 400~470 ℃, keeps 2~10min; Second step is crystallization of thin films, and crystallization temperature is made as 650~950 ℃, keeps 2~8min.
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CN101538160B (en) * | 2009-04-14 | 2011-11-09 | 桂林工学院 | Temperature-stable tantalate dielectric ceramic and preparation method thereof |
CN101531512B (en) * | 2009-04-11 | 2011-11-30 | 桂林工学院 | Temperature stable type tungsten bronze structure dielectric ceramic and preparation method thereof |
CN103011813A (en) * | 2013-01-06 | 2013-04-03 | 电子科技大学 | Method for preparing high-concentration lithium tantalite thin film by sol-gel method |
CN104779143A (en) * | 2015-02-13 | 2015-07-15 | 济南晶正电子科技有限公司 | Thin film arranged on substrate and preparation method of thin film |
CN110981467A (en) * | 2019-12-09 | 2020-04-10 | 华中科技大学 | Lead-free pyroelectric composite ceramic material and preparation method thereof |
CN114456808A (en) * | 2022-02-22 | 2022-05-10 | 同济大学 | Tantalate-based red long-afterglow luminescent material and preparation method thereof |
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2008
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101531512B (en) * | 2009-04-11 | 2011-11-30 | 桂林工学院 | Temperature stable type tungsten bronze structure dielectric ceramic and preparation method thereof |
CN101538160B (en) * | 2009-04-14 | 2011-11-09 | 桂林工学院 | Temperature-stable tantalate dielectric ceramic and preparation method thereof |
CN103011813A (en) * | 2013-01-06 | 2013-04-03 | 电子科技大学 | Method for preparing high-concentration lithium tantalite thin film by sol-gel method |
CN103011813B (en) * | 2013-01-06 | 2014-07-16 | 电子科技大学 | Method for preparing high-concentration lithium tantalite thin film by sol-gel method |
CN104779143A (en) * | 2015-02-13 | 2015-07-15 | 济南晶正电子科技有限公司 | Thin film arranged on substrate and preparation method of thin film |
CN110981467A (en) * | 2019-12-09 | 2020-04-10 | 华中科技大学 | Lead-free pyroelectric composite ceramic material and preparation method thereof |
CN110981467B (en) * | 2019-12-09 | 2020-12-29 | 华中科技大学 | Lead-free pyroelectric composite ceramic material and preparation method thereof |
CN114456808A (en) * | 2022-02-22 | 2022-05-10 | 同济大学 | Tantalate-based red long-afterglow luminescent material and preparation method thereof |
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