CN1157498C - Preparationof plumbous zirconate titanate (PZT) - Google Patents
Preparationof plumbous zirconate titanate (PZT) Download PDFInfo
- Publication number
- CN1157498C CN1157498C CNB00125278XA CN00125278A CN1157498C CN 1157498 C CN1157498 C CN 1157498C CN B00125278X A CNB00125278X A CN B00125278XA CN 00125278 A CN00125278 A CN 00125278A CN 1157498 C CN1157498 C CN 1157498C
- Authority
- CN
- China
- Prior art keywords
- pzt
- solution
- alkoxide
- zirconium
- mixing solutions
- 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
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 14
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 38
- 238000002360 preparation method Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 229910052745 lead Inorganic materials 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 229910052451 lead zirconate titanate Inorganic materials 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 7
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims description 47
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 150000004703 alkoxides Chemical class 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 11
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical group CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- JEHCHYAKAXDFKV-UHFFFAOYSA-J lead tetraacetate Chemical compound CC(=O)O[Pb](OC(C)=O)(OC(C)=O)OC(C)=O JEHCHYAKAXDFKV-UHFFFAOYSA-J 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- -1 acetate trihydrate lead Chemical compound 0.000 claims description 4
- 208000005156 Dehydration Diseases 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical group CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000009987 spinning Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 42
- 239000000463 material Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000000280 densification Methods 0.000 description 3
- 230000012010 growth Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a new method for preparing lead zirconate titanate thick films, which belongs to the field of preparing ceramic thick films. The method has the key points that a special precursor liquid is prepared, and the processor liquid is prepared by that aggregates of hydrolyzates of Pb, Zr and Ti are mixed with solutions of PbZr1-x-TixO3 (PZT); the hydrolyzates of Pb, Zr and Ti and the PZT solutions have the same stoichiometry that the ratio of Pb to Zr to Ti is 1 to X to (1-X), wherein X is equal to or larger than zero and equal to or less than one. The processor liquid is deposited on a substrate by spinning; then, crystallized PZT thick films are formed on the substrate after the processor liquid is pyrolyzed and annealed. The method has the characteristics of easy preparation of thick film layers, difficult cracking, uniform and favorable properties, etc.
Description
The present invention relates to a kind of method for preparing Pb-based lanthanumdoped zirconate titanates (PZT) thick film, belong to the preparation field of ceramic thick film.
The PZT material has very excellent functional effect, in recent years along with micromechanics---and the develop rapidly of having never heard of of microelectronic device, urgent need development thickness is the PZT thick film between the 1-10 μ m, to produce the enough big displacement and the quantity of electric charge.So processability excellence and uniform PZT thick film have become a focus of current investigation of materials simply.At present the technology at the preparation thick film of usefulness has two kinds, and one of method is a solution method.Promptly Pb, Zr, Ti inorganic salt or organic alkoxide are dissolved in organic solvent, and ECDC is shaped as the PZT precursor liquid, forms wet film with the Sol-gel method by whirl coating on substrate then, makes solvent evaporates, pyrolysis through heating again and forms dry film.But the thickness of individual layer dry film limited (as 200-300 ) so will improve the thickness of film through repeatedly whirl coating and heat-processed, when treating that thickness reaches desired thickness, forms crystalline PZT thick film through anneal again.In order to reach thickness greater than 1 micron (μ m) even when thicker, whirl coating number of times nearly tens times even up to a hundred times.Obviously, this technology is long flow path but also very loaded down with trivial details not only, the thermal shocking that different rete bore and impact history and have nothing in common with each other, so component and structure are difficult to evenly will influence the final properties of mould material.Simultaneously heat treated repeatedly makes the existence that is difficult to avoid stress in the rete, and this is to cause rete rimose immediate cause.Two of method is 0/3 composite algorithm, promptly agglomerating PZT powder is dispersed in the PZT solution, because the existence of powder, under the whirl coating condition identical with method 1, thickness of monolayer can increase, simultaneously the degree that film shrinks can be reduced again in heat-processed, the cracking of rete can be overcome effectively.But owing to including PZT powder and PZT liquid in the wet film that is deposited on the substrate, and PZT powder sintering, so mainly be that liquid phase part participates in all kinds of reactions in heat-processed, because solid, liquid two-phase speed of response and level of response have very big difference, therefore the structure of film and performance can not be evenly, pattern is coarse, and structure is not fine and close.
The objective of the invention is to propose a kind of new film-forming method, at first prepare Pb, Zr, the aggregate of the hydrolyzate of Ti joins it according to a certain percentage and forms new precursor liquid in the solution of PZT.The aggregate of hydrolyzate does not pass through any thermal treatment, and each stage such as nucleation, growth, crystallization is experienced in mutual diffusion mutually between aggregate and the PZT solution of hydrolyzate simultaneously in the process of heating.So the even structure of film, densification are not easy to crack; Performance is even and excellent, can be comparable with block materials.Key point is to accomplish that the composition of the component of aggregate of hydrolyzate and solution is identical.
This shows that precursor liquid preparation new in the preparation PZT thick-film methods that the present invention proposes had two steps: the one, the preparation of the aggregate of Pb, Zr, Ti hydrolyzate; The 2nd, the aggregate of hydrolyzate mixes the new precursor liquid of generation with the solution of the Pb with identical stoicheiometry, Zr, Ti.It is described in detail in detail respectively below.
The preparation of the aggregate of the first step: Pb, Zr, Ti hydrolyzate, its process is according to this:
1, acetate trihydrate lead is dissolved in the ethylene glycol monomethyl ether solvent, is heated to 105 ℃ of dehydrations, and stirs, and obtains limpid plumbic acetate solution;
2, the alkoxide (as propyl alcohol zirconium, butanols zirconium etc.) of zirconium and the alkoxide of titanium (as titanium propanolate, titanium isopropylate, metatitanic acid fourth fat etc.) are dissolved in ethylene glycol monomethyl ether solvent and stirring respectively;
3, the alkoxide solution of zirconium is poured in the alkoxide solution of titanium with required Zr/Ti stoicheiometry and stirred, generate the binary mixing solutions of zirconium and titanium;
4, pour above-mentioned binary mixing solutions into plumbic acetate solution with certain proportioning, three's proportioning is: Pb: Zr: Ti=1: X: (1-X) 0<X<1, form PZT solution, and the concentration of spent glycol methyl ether regulator solution is at 0.2-0.6 mol/milliliter;
5, use acetone as thinner, acetone is joined in the PZT solution and constantly stir; Add-on is looked the molconcentration difference of solution and different, and the corresponding add-on that concentration is high is also big, and the volume ratio of general acetone/PZT solution is 5: 1~10: 1;
6, joining above-mentioned solution as catalyzer with ammoniacal liquor, the pH value of control solution makes to form a large amount of white precipitates, from solution, take out precipitation and with acetone cleaning, airing, sieving obtains Pb, Zr, Ti hydrolyzate aggregate; The particle diameter of hydrolyzate aggregate is 100-200 nanometer (a 0.1-0.2 micron);
Second step was Pb, Zr, and Ti hydrolyzate aggregate mixes the new precursor liquid of generation with the PZT solution with identical stoicheiometry.
The hydrolyzate aggregate of the first step preparation is joined in the PZT solution for preparing by above-mentioned (1)-(4) process, the Pb of the two, Zr, the stoicheiometry of Ti is identical to be important condition.The ratio of the add-on of aggregate and PZT solution is that every milliliter of PZT solution adds the 0.1-0.5 gram.The amount advantage then of the present invention very little that aggregate adds is difficult for showing; And the amount that adds can make subsequent film forming difficulty too much.
After new precursor liquid is produced, precursor liquid is deposited on Pt/Ti/SiO with lacquering technique
2Film forming on the substrate of/Si, the thickness of film depends on aggregate add-on and whirl coating speed and number of times in the new precursor liquid, wet film is removed organic solvent through preceding baking (350 ℃) earlier behind each whirl coating, repeat 5-10 time and reach required thickness, anneal in oxygen atmosphere, annealing temperature is 600-700 ℃ again, makes film from the amorphous PZT thick film that is transformed into perovskite structure in 20 minutes, whirl coating speed is 2000-3000 rev/min, time 3-10 second.
Because hydrolyzate has identical proportioning with PZT solution, each stage such as nucleation, growth, crystallization is experienced in mutual diffusion mutually between hydrolyzate and the PZT solution simultaneously in the process that heats.So even structure, densification through the film of anneal.This is the bright distinguishing feature of this law.Owing to the existence of hydrolyzate, the thickness of single whirl coating is significantly improved simultaneously.On the principle, be unlimited and flawless, and performance evenly and excellent, can compare with block materials with the thickness of the film of this invention preparation.
Fig. 1 is the SEM shape appearance figure (b) of SEM side shape appearance figure (a) and the PZT thick film of 0/3 composite algorithm preparation of the PZT thick film of method provided by the invention preparation.Can be clear that the texture densification of the thick film of method provided by the invention preparation, evenly from Fig. 1.This is because hydrolyzate and the mutual diffusion mutually in the annealed process of PZT solution, nucleation, growth simultaneously.Formed a uniform structure.And the white sparklet (b) joins the PZT particle in the PZT solution just.Because these particles are far above sintering under the annealing temperature, thus in annealing process, demonstrate its inherent " rigidity ", can not be again with PZT solution mutually mutual diffusion and with solution in Pb, Zr, the Ti ion further reacts.Can measure thickness from SEM figure is 3.5 microns.
Fig. 2 is respectively the X diffractogram of the thick film (b) for preparing with the thick film (a) of the present invention preparation with 0/3 composite algorithm, all has the pure perovskite phase structure.
Its residual polarization of ferroelectric properties (a) pr=44.01 μ C/cm of the thick film of Fig. 3 the present invention preparation
2All better than the performance of having reported at present.Abscissa is voltage (V), and ordinate is Pr (μ C/cm
2).For the purpose of contrast, mark respective performances (b) simultaneously with the thick film of 0/3 composite algorithm preparation.Ferroelectric hysteresis loop is all used the RT-66A Instrument measuring among the figure.
Further specify creation of the present invention and be confined to embodiment absolutely not below by embodiment.
Further specify creation of the present invention and be confined to embodiment absolutely not below by embodiment.
Embodiment 1 film-forming method provided by the invention follows these steps to preparation:
1, acetate trihydrate lead is dissolved in ethylene glycol monomethyl ether, and heating is also stirred, and forms plumbic acetate solution;
2, propyl alcohol zirconium, titanium isopropylate are dissolved in the ethylene glycol monomethyl ether respectively, and are mixed with the binary solution of Zr and Ti with Zr/Ti=40/60 (mol ratio);
3, above-mentioned solution is joined in the plumbic acetate solution, with Pb: Zr: Ti=100: 40: 60 ratio (mol) forms PZT solution, and it is 0.4mol that the spent glycol methyl ether is adjusted to molconcentration;
4, propyl alcohol is joined in the PZT ternary mixing solutions acetone as thinner: PZT ternary mixing solutions=10: 1 (volume ratio), stir;
5, ammoniacal liquor is joined above-mentioned solution as catalyzer, making the solution pH value is 7~8, at this moment a large amount of white precipitate-Pb, and Zr, the Ti hydrolyzate forms; Pb, Zr, the Ti hydrolyzate takes out, and with propyl alcohol cleaning, airing, forms Pb, Zr, the aggregation of Ti hydrolyzate;
6, restrain Pb to add 0.128 in every milliliter of PZT ternary mixing solutions, Zr, the Ti hydrolyzate forms new precursor liquid;
7, with new precursor liquid through whirl coating (3000 rev/mins) at Pt/Ti/SiO
2Film forming on the/Si substrate, baking repeats 5 whirl coating-preceding bakings before 350 ℃, and annealing formed the PZT thick film in 20 minutes in 650 ℃ of oxygen atmospheres again;
Measuring thickness with SEM then is 3.5 μ m, observes pattern; Structure with the XRD method analyzing film; And, measure the ferroelectric properties of PZT thick film with RT-66A at the surface evaporation deposit Au of this film point electrode.Respectively as Fig. 1, Fig. 2, shown in Figure 3.
Embodiment 2 Pb, Zr, hydrolyzate aggregate and the Pb of Ti, Zr, Ti ternary mixed solution preparation process
1-6 is identical with example 1, restrains Pb to add 0.128 in every milliliter of PZT ternary mixing solutions then, Zr, and the ratio of Ti hydrolyzate adds the new precursor liquid of formation, and other implementation condition is with example 1.Result and embodiment 1 are similar: the compact structure of film, even has excellent ferroelectric properties, shown in Fig. 3 (b).The thickness of film is 2 microns, and this is because of Pb in solution, Zr, the reason that the ratio of Ti hydrolyzate is little.
Embodiment 3
With the butanols zirconium is the zirconium source, and butyl (tetra) titanate is the titanium source, Zr: Ti=60: the thickness that made in 20 minutes of annealing under 40,680 ℃ of oxygen atmospheres is 3.5 microns.All the other are with embodiment 1.
Claims (8)
1, a kind of method for preparing lead zirconate titanate thick film comprises preparation, whirl coating film forming, oven dry, the high temperature annealing down of precursor liquid, it is characterized in that:
(1) precursor liquid is by Pb, and Zr, the aggregate of the hydrolyzate of Ti join the identical Pb of stoicheiometry, Zr, and in the Ti ternary mixing solutions, add-on is the 0.1-0.5 grams per milliliter;
(2) precursor liquid is deposited on Pt/Ti/SiO
2On/Si the substrate, the thickness of film depends on add-on and the whirl coating speed and the number of times of aggregate in the precursor liquid;
(3) wet film baking before 350 ℃ earlier behind each whirl coating repeats 5-10 time, reaches required thickness, anneals 20 minutes under 600 ℃ of-700 ℃ of oxygen atmospheres again, and the composition that makes film is transformed into uhligite shape from amorphous.
2, by the preparation method of the described thick film of claim 1, it is characterized in that described Pb, Zr, the preparation process of the aggregate of the hydrolyzate of Ti is:
(1) acetate trihydrate lead is dissolved in the ethylene glycol monomethyl ether solvent, is heated to 105 ℃ of dehydrations, and stirs, and obtains limpid plumbic acetate solution;
(2) alkoxide of zirconium and the alkoxide of titanium are dissolved in ethylene glycol monomethyl ether solvent and stirring respectively;
(3) alkoxide solution of zirconium is poured in the alkoxide solution of titanium with required Zr/Ti stoicheiometry and stirred, generate the binary mixing solutions of zirconium and titanium;
(4) pour above-mentioned binary mixing solutions into plumbic acetate solution with certain proportion, three's mol proportioning is Pb: Zr: Ti=1: x: (1-x), 0<x<1 forms PZT ternary mixing solutions;
(5) make thinner with acetone, join in the PZT solution, and constantly stir, the volume ratio of acetone/PZT solution is 5: 1-10: 1;
(6) ammoniacal liquor is joined above-mentioned solution as catalyzer, regulate pH=7-8, generate Pb, Zr, the white hydrolyzate of Ti after acetone cleans, airing, sieves and obtains grain through being the aggregate of 100-200 nanometer.
3, by the preparation method of the described thick film of claim 1, it is characterized in that described Pb, Zr, the ternary mixing solutions of Ti, preparation process is:
(1) acetate trihydrate lead is dissolved in the ethylene glycol monomethyl ether solvent, is heated to 105 ℃ of dehydrations, and stirs, and obtains limpid plumbic acetate solution;
(2) alkoxide of zirconium and the alkoxide of titanium are dissolved in ethylene glycol monomethyl ether solvent and stirring respectively;
(3) alkoxide solution of zirconium is poured in the alkoxide solution of titanium with required Zr/Ti stoicheiometry and stirred, generate the binary mixing solutions of zirconium and titanium;
(4) pour above-mentioned binary mixing solutions into plumbic acetate solution with certain proportion, three's mol proportioning is Pb: Zr: Ti=1: x: (1-x), 0<x<1 forms PZT ternary mixing solutions.
4, by claim 2 or 3 described thick film preparation methods, the alkoxide that it is characterized in that described zirconium is propyl alcohol zirconium, butanols zirconium; The alkoxide of titanium is titanium propanolate, titanium isopropylate, butyl (tetra) titanate.
5, by claim 2 or 3 described thick film preparation methods, it is characterized in that described PZT ternary mixing solutions, the concentration of spent glycol methyl ether regulator solution is in 0.2-0.6 mol/milliliter scope.
6,, it is characterized in that whirl coating speed is 2000-3000 rev/min, time 3-10 second by the described thick film preparation method of claim 1.
7,, it is characterized in that Pb: Zr: Ti=1 in the ternary mixing solutions of PZT: 0.4: 0.6, identical with the stoicheiometry of hydrolyzate aggregate by the described thick film preparation method of claim 1.
8, by claim 1 or 6 described thick film preparation methods, the add-on that it is characterized in that aggregate is 0.26 grams per milliliter, and baking repeats 5 times whirl coating before 350 ℃, preceding baking, and annealing formed 3.5 microns thick films in 20 minutes under 650 ℃ of oxygen atmospheres again.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB00125278XA CN1157498C (en) | 2000-09-19 | 2000-09-19 | Preparationof plumbous zirconate titanate (PZT) |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB00125278XA CN1157498C (en) | 2000-09-19 | 2000-09-19 | Preparationof plumbous zirconate titanate (PZT) |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1288976A CN1288976A (en) | 2001-03-28 |
CN1157498C true CN1157498C (en) | 2004-07-14 |
Family
ID=4591070
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB00125278XA Expired - Fee Related CN1157498C (en) | 2000-09-19 | 2000-09-19 | Preparationof plumbous zirconate titanate (PZT) |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1157498C (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1298674C (en) * | 2005-04-06 | 2007-02-07 | 清华大学 | Method for preparing piezoelectric ceramic film |
CN102242356A (en) * | 2011-06-09 | 2011-11-16 | 哈尔滨工业大学 | Titanium-zirconium solid solution micro/nano film on amorphous metal surface and preparation method of titanium-zirconium solid solution micro/nano film |
CN103193482B (en) * | 2013-03-11 | 2015-09-09 | 华中科技大学 | A kind of lead zirconate titanate thick film and preparation method thereof |
CN110359058B (en) * | 2019-07-22 | 2021-08-03 | 肇庆市华师大光电产业研究院 | Preparation method of lead zirconate titanate modified hematite nanorod array photoanode |
-
2000
- 2000-09-19 CN CNB00125278XA patent/CN1157498C/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
CN1288976A (en) | 2001-03-28 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US5116643A (en) | Method for preparing PLZT, PZT and PLT sol-gels and fabricating ferroelectric thin films | |
JP5208758B2 (en) | Coating film manufacturing process based on oxide ceramics adapted to the shape of the substrate with relief characteristics | |
Dawley et al. | Sol-gel derived bismuth titanate thin films with c-axis orientation | |
CN1157498C (en) | Preparationof plumbous zirconate titanate (PZT) | |
WO2015147259A1 (en) | Mn-doped pzt-based piezoelectric film formation composition and mn-doped pzt-based piezoelectric film | |
WO2015146607A1 (en) | Composition for forming manganese- and niobium-doped pzt piezoelectric film | |
Chen et al. | Low temperature growth of (100)-oriented Ba (Zr0. 2Ti0. 8) O3-0.5 (Ba0. 7Ca0. 3) TiO3 thin films using a LaNiO3 seed layer | |
JP4237967B2 (en) | Method for producing zirconate-lead titanate thick film using sol-gel process | |
JP7222647B2 (en) | Coating liquid composition for forming piezoelectric film, manufacturing method thereof, oriented piezoelectric film, and liquid ejection head | |
JP3213295B2 (en) | Method for forming piezoelectric / electrostrictive film element at low temperature using electrophoretic film forming method and piezoelectric / electrostrictive film element | |
JP2015192009A (en) | Manganese- and niobium-doped pzt based piezoelectric material film | |
JP3953810B2 (en) | Method for manufacturing ferroelectric thin film using sol-gel process | |
CN107275475B (en) | A kind of TiO2@PZT nano-wire array/polymer composite dielectric material and preparation method thereof | |
CN109761605A (en) | One kind having the PZT thin film and preparation method thereof of (100) preferable grain orientation | |
CN1350071A (en) | Wet chemical prepn process of leadless functional barium titanate ceramic film | |
CN1210223C (en) | Preparation method of lead zirconate titanate thick film material | |
Wang et al. | Effect of excess Pb in PbTiO 3 precursors on ferroelectric and fatigue property of sol–gel derived PbTiO 3/PbZr 0.3 Ti 0.7 O 3/PbTiO 3 thin films | |
JPH10116965A (en) | Nonvolatile memory thin film and its manufacturing method | |
CN115974548B (en) | Leadless high-entropy ferroelectric film, preparation method and application thereof | |
CN114956812B (en) | Lead titanate-lead zirconate nano composite film and preparation method thereof | |
LU101884B1 (en) | Material deposition method | |
CN110451954B (en) | Sodium bismuth titanate-based low-lead piezoelectric film with high inverse piezoelectric coefficient and preparation method thereof | |
KR20000028974A (en) | Method for forming piezoelectric/electrostrictive film element at low temperature using electrophoretic deposition and the piezoelectric/electrostrictive film element formed by the method | |
JP4649573B2 (en) | BLT type ferroelectric thin film manufacturing method and coating liquid manufacturing method therefor | |
Khakhomov et al. | Synthesis and Study of High-Performance Ferroelectric Materials for Advanced Non-Volatile Memory Devices |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C06 | Publication | ||
PB01 | Publication | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C19 | Lapse of patent right due to non-payment of the annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |