CN102299251B - Preparation method for perovskite buffer layer - Google Patents
Preparation method for perovskite buffer layer Download PDFInfo
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- CN102299251B CN102299251B CN 201110231598 CN201110231598A CN102299251B CN 102299251 B CN102299251 B CN 102299251B CN 201110231598 CN201110231598 CN 201110231598 CN 201110231598 A CN201110231598 A CN 201110231598A CN 102299251 B CN102299251 B CN 102299251B
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- pentanedione
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Abstract
The invention discloses a preparation method for a perovskite buffer layer. The method comprises the following steps: 1, preparing a precursor solution; 2, carrying out dilution on a portion of precursor solution; 3, coating a substrate by the portion of precursor solution that is processed by the dilution and then placing the coated substrate in a tube furnace to carry out heating followed by cooling, so that a SrTiO3 nuclear layer thin film is obtained ; 4, coating the SrTiO3 nuclear layer thin film by the residual precursor solution that is not diluted and placing the coated SrTiO3 nuclearlayer thin film in the tube furnace to carry out heating followed by cooling, so that a perovskite SrTiO3 buffer layer is obtained. According to the invention, a spin coating method is employed to carry out spin coating on a substrate by a diluted precursor solution so as to prepare a SrTiO3 nuclear layer thin film; and then another precursor solution that is not diluted is spun for coating. Therefore, a preparation technology for a buffer layer is simplified and low-cost and large-scale preparation for a SrTiO3 buffer layer is also realized. The perovskite SrTiO3 buffer layer, which is prepared by the method provided in the invention, has a good c-shaft texture and a flat surface.
Description
Technical field
The invention belongs to the thin-film material technical field, be specifically related to a kind of preparation method of perovskite type buffer layer.
Background technology
Second generation conductor of high-temperature superconductor coat makes it become the preferred material that substitutes the practical high temperature superconducting materia of the first generation at the superior high-field performance of 77K.The sandwich construction that coating conductor is made up of base band/barrier layer/superconducting layer/protective layer.At present; Domestic coating conductor research and development are all lagging far behind world standard aspect basic research and the technology of preparing; Particularly bigger in buffer layer deposition technical elements gap; Therefore, from the practicability angle, pressing for low-cost deposition technique is the technical problem that approach solves resilient coating preparation in the coating conductor.
Resilient coating is being born transmission texture and chemical barrier two main tasks.People adopt the resilient coating of multi-layer film structure to realize above-mentioned two big major functions more at present; But the resilient coating number of plies is many more; Preparation technology is more complicated, and cost is just high more, and the difficulty of controlling its growth, microstructure and interfacial structure is also just big more; Therefore simplify buffer layer structure, or even to adopt single resilient coating be the target that people make great efforts always.Because SrTiO
3Have less oxygen diffusion coefficient, and Ni and YBCO between chemical compatibility fine, and and YBCO between lattice mismatch very little again, so people are consistent thinks that it is the preferred material of preparation coating conductor list resilient coating.
The technology of preparing of resilient coating adopts physical vacuum vapour deposition (PVD) and antivacuum chemical solution deposition (CSD) more at present; The former technical characterstic is to obtain high performance thin film easily, but complex equipments, preparation speed is slow; Cost is higher, and the long band of preparation practicability has difficulties; And that the latter's characteristics are technology is simple relatively, can accurately control the proportioning of metal constituent element, can be in the even film forming of surfaces of complex shape, and equipment cost is low, realizes preparation continuously easily, and wherein metal organic deposit (MOD) process application is more in the CSD technology.Utilize the MOD legal system to be equipped with SrTiO at present
3What titanium was selected for use usually in the predecessor of resilient coating is the alkoxide of titanium, but metal alkoxide facile hydrolysis characteristic in air can make the preparation of precursor liquid and storage difficulty strengthen, and is unfavorable for the deposition of normal condition bottom breaker, in addition, because SrTiO
3And there is very big lattice mismatch between the NiW base band, causes adopting conventional spin coating Technology for Heating Processing to be difficult to obtain the SrTiO of good c axle orientation
3Buffer layer thin film, thus select appropriate predecessor to prepare the precursor liquid that has good stability, thus the SrTiO of coating simultaneously reasonable in design, Technology for Heating Processing preparation c axle texture
3Resilient coating will promote the progress of Preparation Technology of coating conductor effectively.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art, provides a kind of preparation method simple, adopts conventional raw material, does not need special installation, the preparation method of the perovskite type buffer layer that production cost is low.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of perovskite type buffer layer is characterized in that this method may further comprise the steps:
(1) be that 1: 1 ratio is carried out weighing with acetylacetone,2,4-pentanedione oxygen titanium and the strontium acetate that contains 1/2 crystallization water according to mol ratio; The mixed solvent that in strontium acetate, adds volume ratio then and be 1～10: 1 propionic acid and acetylacetone,2,4-pentanedione dissolves and makes solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.1mol/L～1.0mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, add volume ratio and be 1～10: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.003mol/L～0.05mol/L;
(3) speed of the precursor liquid after the dilution in the step (2) with 2000 rev/mins～5000 rev/mins is spun in the substrate with the acetone ultrasonic cleaning; The spin coating time is 10s～60s; Then the substrate behind the spin coating precursor liquid is placed tube furnace, in low-oxygen environment, temperature in the stove is incubated 0.1h～1h after room temperature is heated to 850 ℃～1100 ℃ with the heating rate that is not less than 50 ℃/min; Be cooled to room temperature with the rate of temperature fall that is not less than 2 ℃/min again, obtain SrTiO
3The forming core layer film; Said low-oxygen environment is that quality purity is 99.999% high-purity Ar, or for the oxygen mass content be 10
-10Ppm～10
-3The Ar-H of ppm
2Mixed atmosphere, or for the oxygen mass content be 10
-10Ppm～10
-3The N of ppm
2-H
2Mixed atmosphere;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2000 rev/mins～5000 rev/mins speed
3On the forming core layer film, the spin coating time is 10s～60s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace; In low-oxygen environment; Heating rate to be not less than 50 ℃/min is incubated 0.5h～3h with temperature in the stove after room temperature is heated to 900 ℃～1100 ℃, be cooled to room temperature with the rate of temperature fall that is not less than 2 ℃/min again, obtains Ca-Ti ore type SrTiO
3Resilient coating; Said low-oxygen environment is that quality purity is 99.999% high-purity Ar, or for the oxygen mass content be 10
-10Ppm～10
-3The Ar-H of ppm
2Mixed atmosphere, or for the oxygen mass content be 10
-10Ppm～10
-3The N of ppm
2-H
2Mixed atmosphere.
Described in the above-mentioned steps (1) in the mixed solvent volume ratio of propionic acid and acetylacetone,2,4-pentanedione be 2～5: 1.
Described in the above-mentioned steps (2) in the mixed solvent volume ratio of propionic acid and acetylacetone,2,4-pentanedione be 2～5: 1.
The volume ratio of mixed solvent and 2-methyl cellosolve is 3: 1 described in the above-mentioned steps (2).
Substrate described in the above-mentioned steps (3) is NiW base band, NdGaO
3Monocrystal chip, LaAlO
3Monocrystal chip or YSZ single-crystal substrate, wherein YSZ is meant the zirconia that yttrium is stable.
The present invention compared with prior art has the following advantages:
1, preparation method of the present invention is simple, adopts conventional raw material, does not need special installation, and production cost is low.
2, the present invention adopts common metal salt preparation precursor liquid, has improved the stability of precursor liquid effectively, has simplified the preparation condition of precursor liquid.
3, the present invention adopts the basad precursor liquid of going up after spin coating is diluted of spin-coating method to prepare SrTiO earlier
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation.
4, adopt the Ca-Ti ore type SrTiO of method preparation of the present invention
3Resilient coating has good c axle texture and flat surface.
Through accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is the Ca-Ti ore type SrTiO of the embodiment of the invention 1 preparation
3The X diffracting spectrum of resilient coating.
Fig. 2 is the Ca-Ti ore type SrTiO of the embodiment of the invention 1 preparation
3AFM microscope (AFM) photo of resilient coating.
Fig. 3 is the Ca-Ti ore type SrTiO of the embodiment of the invention 2 preparations
3The X diffracting spectrum of resilient coating.
Fig. 4 is the Ca-Ti ore type SrTiO of the embodiment of the invention 2 preparations
3AFM microscope (AFM) photo of resilient coating.
Fig. 5 is the Ca-Ti ore type SrTiO of the embodiment of the invention 3 preparations
3The X diffracting spectrum of resilient coating.
Fig. 6 is the Ca-Ti ore type SrTiO of the embodiment of the invention 3 preparations
3AFM microscope (AFM) photo of resilient coating.
Fig. 7 is the Ca-Ti ore type SrTiO of the embodiment of the invention 11 preparations
3The X diffracting spectrum of resilient coating.
Fig. 8 is the Ca-Ti ore type SrTiO of the embodiment of the invention 11 preparations
3AFM microscope (AFM) photo of resilient coating.
Embodiment
Embodiment 1
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 2: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make yellow transparent solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.3mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 2: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.003mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) speed of the precursor liquid after the dilution in the step (2) with 4000 rev/mins is spun on the NiW base band with the acetone ultrasonic cleaning; The spin coating time is 30s; Then the NiW base band behind the spin coating precursor liquid is placed tube furnace, in quality purity is 99.999% high-purity Ar atmosphere, temperature in the stove is incubated 0.1h after room temperature is heated to 1000 ℃ with the heating rate of 300 ℃/min; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2500 rev/mins speed
3On the forming core layer film, the spin coating time is 30s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace; In quality purity is 99.999% high-purity Ar atmosphere; Heating rate with 300 ℃/min is incubated 0.5h with temperature in the stove after room temperature is heated to 950 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Fig. 1 is the Ca-Ti ore type SrTiO of present embodiment preparation
3The X diffracting spectrum of resilient coating, ordinate is diffracted intensity (Intensity) among the figure, arbitrary unit (a.u.); Abscissa is the angle of diffraction 2 θ, and unit has only NiW base band and SrTiO for degree (deg) among the figure
3(200) diffraction maximum occur, the SrTiO that has obtained to have good c axle texture is described
3Buffer layer thin film.Fig. 2 is the Ca-Ti ore type SrTiO of present embodiment preparation
3AFM microscope (AFM) photo of resilient coating, as can be seen from the figure SrTiO
3Buffer layer thin film is fully with NiW base band surface coverage; Continuous, the even and non-microcracked appearance in buffer layer thin film surface; In addition; Buffer layer thin film surface r.m.s. roughness is 4.31nm in the scope of 10 μ m * 10 μ m, explains that its surface is comparatively smooth, is fit to continue other sull of deposition above that.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 2: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make yellow transparent solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.3mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 2: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.006mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) speed of the precursor liquid after the dilution in the step (2) with 5000 rev/mins is spun on the NiW base band with the acetone ultrasonic cleaning, the spin coating time is 40s, then the NiW base band behind the spin coating precursor liquid is placed tube furnace, is 10 in the oxygen mass content
-6The Ar-H of ppm
2In the mixed atmosphere, with the heating rate of 300 ℃/min temperature in the stove is incubated 1h after room temperature is heated to 850 ℃, the rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2000 rev/mins speed
3On the forming core layer film, the spin coating time is 30s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-6The Ar-H of ppm
2In the mixed atmosphere; Heating rate with 300 ℃/min is incubated 0.5h with temperature in the stove after room temperature is heated to 970 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Fig. 3 is the Ca-Ti ore type SrTiO of present embodiment preparation
3The X diffracting spectrum of resilient coating, ordinate is diffracted intensity (Intensity) among the figure, arbitrary unit (a.u.); Abscissa is the angle of diffraction 2 θ, and unit has only NiW base band and SrTiO for degree (deg) among the figure
3(200) diffraction maximum occur, the SrTiO that has obtained to have good c axle texture is described
3Buffer layer thin film.Fig. 4 is the Ca-Ti ore type SrTiO of present embodiment preparation
3AFM microscope (AFM) photo of resilient coating, as can be seen from the figure SrTiO
3Buffer layer thin film is fully with NiW base band surface coverage; Continuous, the even and non-microcracked appearance in buffer layer thin film surface; In addition; Buffer layer thin film surface r.m.s. roughness is 4.47nm in the scope of 10 μ m * 10 μ m, explains that its surface is comparatively smooth, is fit to continue other sull of deposition above that.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 3
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 1: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 1.0mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 1: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.05mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) speed of the precursor liquid after the dilution in the step (2) with 2000 rev/mins is spun on the NiW base band with the acetone ultrasonic cleaning, the spin coating time is 60s, then the NiW base band behind the spin coating precursor liquid is placed tube furnace, is 10 in the oxygen mass content
-10The N of ppm
2-H
2In the mixed atmosphere, with the heating rate of 100 ℃/min temperature in the stove is incubated 0.3h after room temperature is heated to 950 ℃, the rate of temperature fall with 10/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 3000 rev/mins speed
3On the forming core layer film, the spin coating time is 40s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-10The N of ppm
2-H
2In the mixed atmosphere; Heating rate with 200 ℃/min is incubated 3h with temperature in the stove after room temperature is heated to 900 ℃; Rate of temperature fall with 5 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Fig. 5 is the Ca-Ti ore type SrTiO of present embodiment preparation
3The X diffracting spectrum of resilient coating, ordinate is diffracted intensity (Intensity) among the figure, arbitrary unit (a.u.); Abscissa is the angle of diffraction 2 θ, and unit has only NiW base band and SrTiO for degree (deg) among the figure
3(200) diffraction maximum occur, the SrTiO that has obtained to have good c axle texture is described
3Buffer layer thin film.Fig. 6 is the Ca-Ti ore type SrTiO of present embodiment preparation
3AFM microscope (AFM) photo of resilient coating, as can be seen from the figure SrTiO
3Buffer layer thin film is fully with NiW base band surface coverage; Continuous, the even and non-microcracked appearance in buffer layer thin film surface; In addition; Buffer layer thin film surface r.m.s. roughness is 4.19nm in the scope of 10 μ m * 10 μ m, explains that its surface is comparatively smooth, is fit to continue other sull of deposition above that.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 4
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 10: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make yellow transparent solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.5mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 10: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.008mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) precursor liquid after the dilution in the step (2) is spun on the NdGaO with the acetone ultrasonic cleaning with 3500 rev/mins speed
3On the monocrystal chip, the spin coating time is 10s, then with the NdGaO behind the spin coating precursor liquid
3Monocrystal chip places tube furnace, is 10 in the oxygen mass content
-3The Ar-H of ppm
2In the mixed atmosphere, with the heating rate of 50 ℃/min temperature in the stove is incubated 0.5h after room temperature is heated to 900 ℃, the rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 4000 rev/mins speed
3On the forming core layer film, the spin coating time is 20s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-3The Ar-H of ppm
2In the mixed atmosphere; Heating rate with 250 ℃/min is incubated 0.5h with temperature in the stove after room temperature is heated to 1000 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 5
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 5: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.1mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 5: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.003mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) precursor liquid after the dilution in the step (2) is spun on the LaAlO with the acetone ultrasonic cleaning with 2000 rev/mins speed
3On the monocrystal chip, the spin coating time is 10s, then with the LaAlO behind the spin coating precursor liquid
3Monocrystal chip places tube furnace, is 10 in the oxygen mass content
-3The N of ppm
2-H
2In the mixed atmosphere, with the heating rate of 50 ℃/min temperature in the stove is incubated 0.5h after room temperature is heated to 900 ℃, the rate of temperature fall with 10 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 3500 rev/mins speed
3On the forming core layer film, the spin coating time is 40s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-3The N of ppm
2-H
2In the mixed atmosphere; Heating rate with 50 ℃/min is incubated 1h with temperature in the stove after room temperature is heated to 950 ℃; Rate of temperature fall with 10 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 6
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 3: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.6mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 3: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.02mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) speed of the precursor liquid after the dilution in the step (2) with 3000 rev/mins is spun on YSZ (zirconia that yttrium the is stable) monocrystal chip with the acetone ultrasonic cleaning; The spin coating time is 20s; Then the YSZ single-crystal substrate behind the spin coating precursor liquid being placed tube furnace, is 10 in the oxygen mass content
-10The Ar-H of ppm
2In the mixed atmosphere, with the heating rate of 200 ℃/min temperature in the stove is incubated 0.2h after room temperature is heated to 980 ℃, the rate of temperature fall with 5 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 5000 rev/mins speed
3On the forming core layer film, the spin coating time is 10s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-10The Ar-H of ppm
2In the mixed atmosphere; Heating rate with 100 ℃/min is incubated 2h with temperature in the stove after room temperature is heated to 980 ℃; Rate of temperature fall with 5 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 7
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 2: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 1.0mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 2: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.01mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) precursor liquid after the dilution in the step (2) is spun on the LaAlO with the acetone ultrasonic cleaning with 4000 rev/mins speed
3On the monocrystal chip, the spin coating time is 30s, then with the LaAlO behind the spin coating precursor liquid
3Monocrystal chip places tube furnace, is 10 in the oxygen mass content
-8The N of ppm
2-H
2In the mixed atmosphere, with the heating rate of 300 ℃/min temperature in the stove is incubated 0.1h after room temperature is heated to 1100 ℃, the rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2500 rev/mins speed
3On the forming core layer film, the spin coating time is 20s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-8The N of ppm
2-H
2In the mixed atmosphere; Heating rate with 300 ℃/min is incubated 0.5h with temperature in the stove after room temperature is heated to 1000 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 8
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 8: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.2mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 8: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.005mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) precursor liquid after the dilution in the step (2) is spun on the NdGaO with the acetone ultrasonic cleaning with 3000 rev/mins speed
3On the monocrystal chip, the spin coating time is 60s, then with the NdGaO behind the spin coating precursor liquid
3Monocrystal chip places tube furnace, in quality purity is 99.999% high-purity Ar atmosphere, with the heating rate of 150 ℃/min temperature in the stove is incubated 0.2h after room temperature is heated to 970 ℃, and the rate of temperature fall with 5 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2000 rev/mins speed
3On the forming core layer film, the spin coating time is 40s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace; In quality purity is 99.999% high-purity Ar atmosphere; Heating rate with 150 ℃/min is incubated 0.6h with temperature in the stove after room temperature is heated to 980 ℃; Rate of temperature fall with 5 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 9
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 10: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.5mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 10: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.005mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) precursor liquid after the dilution in the step (2) is spun on the LaAlO with the acetone ultrasonic cleaning with 5000 rev/mins speed
3On the monocrystal chip, the spin coating time is 20s, then with the LaAlO behind the spin coating precursor liquid
3Monocrystal chip places tube furnace, in quality purity is 99.999% high-purity Ar atmosphere, with the heating rate of 200 ℃/min temperature in the stove is incubated 0.3h after room temperature is heated to 940 ℃, and the rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 3000 rev/mins speed
3On the forming core layer film, the spin coating time is 60s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace; In quality purity is 99.999% high-purity Ar atmosphere; Heating rate with 300 ℃/min is incubated 0.5h with temperature in the stove after room temperature is heated to 1100 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 10
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 2: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.1mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 2: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.003mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) precursor liquid after the dilution in the step (2) is spun on the NdGaO with the acetone ultrasonic cleaning with 4000 rev/mins speed
3On the monocrystal chip, the spin coating time is 40s, then with the NdGaO behind the spin coating precursor liquid
3Monocrystal chip places tube furnace, is 10 in the oxygen mass content
-10The N of ppm
2-H
2In the mixed atmosphere, with the heating rate of 100 ℃/min temperature in the stove is incubated 0.5h after room temperature is heated to 920 ℃, the rate of temperature fall with 6 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 5000 rev/mins speed
3On the forming core layer film, the spin coating time is 20s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-10The N of ppm
2-H
2In the mixed atmosphere; Heating rate with 100 ℃/min is incubated 1h with temperature in the stove after room temperature is heated to 950 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 11
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 1: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.1mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 1: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.003mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) speed of the precursor liquid after the dilution in the step (2) with 2000 rev/mins is spun on YSZ (zirconia that yttrium the is stable) monocrystal chip with the acetone ultrasonic cleaning; The spin coating time is 10s; Then the YSZ single-crystal substrate behind the spin coating precursor liquid being placed tube furnace, is 10 in the oxygen mass content
-3The N of ppm
2-H
2In the mixed atmosphere, with the heating rate of 50 ℃/min temperature in the stove is incubated 0.5h after room temperature is heated to 900 ℃, the rate of temperature fall with 10 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 3500 rev/mins speed
3On the forming core layer film, the spin coating time is 40s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace, is 10 in the oxygen mass content
-3The N of ppm
2-H
2In the mixed atmosphere; Heating rate with 50 ℃/min is incubated 1h with temperature in the stove after room temperature is heated to 950 ℃; Rate of temperature fall with 10 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Fig. 7 is the Ca-Ti ore type SrTiO of present embodiment preparation
3The X diffracting spectrum of resilient coating, ordinate is diffracted intensity (Intensity) among the figure, arbitrary unit (a.u.); Abscissa is the angle of diffraction 2 θ, and unit has only YSZ single-crystal substrate and SrTiO for degree (deg) among the figure
3(l00) diffraction maximum occur, the SrTiO that has obtained to have good c axle texture is described
3Buffer layer thin film.Fig. 8 is the Ca-Ti ore type SrTiO of present embodiment preparation
3AFM microscope (AFM) photo of resilient coating, as can be seen from the figure SrTiO
3Continuous, the even and non-microcracked appearance in buffer layer thin film surface; In addition; Buffer layer thin film surface r.m.s. roughness is 3.16nm in the scope of 10 μ m * 10 μ m, explains that the buffer layer thin film surface is comparatively smooth, is fit to continue other sull of deposition above that.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film, the precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO
3Resilient coating has been simplified the preparation technology of resilient coating, and can have been realized SrTiO
3The low cost of resilient coating, mass preparation, the Ca-Ti ore type SrTiO of preparation
3Resilient coating has good c axle texture and flat surface.
Embodiment 12
(1) with acetylacetone,2,4-pentanedione oxygen titanium TiO (CH
3COCHCOCH
3)
2With the strontium acetate Sr (CH that contains 1/2 crystallization water
3COO)
21/2H
2O is that 1: 1 ratio is carried out weighing according to mol ratio; In strontium acetate, adding volume ratio then is that 10: 1 the propionic acid and the mixed solvent dissolving of acetylacetone,2,4-pentanedione make solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 1.0mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, adding volume ratio is 10: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.05mol/L; The mixed solvent of said propionic acid and acetylacetone,2,4-pentanedione and the volume ratio of 2-methyl cellosolve are 3: 1;
(3) speed of the precursor liquid after the dilution in the step (2) with 5000 rev/mins is spun on YSZ (zirconia that yttrium the is stable) monocrystal chip with the acetone ultrasonic cleaning; The spin coating time is 60s; Then the YSZ single-crystal substrate behind the spin coating precursor liquid is placed tube furnace, in quality purity is 99.999% high-purity Ar atmosphere, temperature in the stove is incubated 0.1h after room temperature is heated to 1000 ℃ with the heating rate of 300 ℃/min; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains SrTiO
3The forming core layer film;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2000 rev/mins speed
3On the forming core layer film, the spin coating time is 60s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace; In quality purity is 99.999% high-purity Ar atmosphere; Heating rate with 300 ℃/min is incubated 0.5h with temperature in the stove after room temperature is heated to 1000 ℃; Rate of temperature fall with 2 ℃/min is cooled to room temperature again, obtains having the Ca-Ti ore type SrTiO of good c axle texture and less surface roughness (RMS is less than 5nm)
3Resilient coating.
Present embodiment adopts the precursor liquid after the spin-coating method spin coating dilution to prepare SrTiO
3The forming core layer film; The precursor liquid of spin coating not diluted again prepares Ca-Ti ore type SrTiO3 resilient coating; Simplified the preparation technology of resilient coating, and can realize low cost, the mass preparation of SrTiO3 resilient coating, the Ca-Ti ore type SrTiO3 resilient coating of preparation has good c axle texture and flat surface.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every according to inventing technical spirit to any simple modification, change and equivalent structure variation that above embodiment did, all still belong in the protection range of technical scheme of the present invention.
Claims (5)
1. the preparation method of a perovskite type buffer layer is characterized in that, this method may further comprise the steps:
(1) be that 1: 1 ratio is carried out weighing with acetylacetone,2,4-pentanedione oxygen titanium and the strontium acetate that contains 1/2 crystallization water according to mol ratio; The mixed solvent that in strontium acetate, adds volume ratio then and be 1～10: 1 propionic acid and acetylacetone,2,4-pentanedione dissolves and makes solution A; In acetylacetone,2,4-pentanedione oxygen titanium, add the 2-methyl cellosolve dissolving and make solution B; Above-mentioned solution A and solution B are mixed, the molar concentration that is mixed with acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate is the precursor liquid of 0.1mol/L～1.0mol/L again;
(2) get precursor liquid described in the part steps (1); In precursor liquid, add volume ratio and be 1～10: 1 the propionic acid and the mixed solvent of acetylacetone,2,4-pentanedione; Add 2-methyl cellosolve again and dilute, the molar concentration that obtains acetylacetone,2,4-pentanedione oxygen titanium and strontium acetate after stirring is the precursor liquid of 0.003mol/L～0.05mol/L;
(3) speed of the precursor liquid after the dilution in the step (2) with 2000 rev/mins～5000 rev/mins is spun in the substrate with the acetone ultrasonic cleaning; The spin coating time is 10s～60s; Then the substrate behind the spin coating precursor liquid is placed tube furnace, in low-oxygen environment, temperature in the stove is incubated 0.1h～1h after room temperature is heated to 850 ℃～1100 ℃ with the heating rate that is not less than 50 ℃/min; Be cooled to room temperature with the rate of temperature fall that is not less than 2 ℃/min again, obtain SrTiO
3The forming core layer film; Said low-oxygen environment is that quality purity is 99.999% high-purity Ar, or for the oxygen mass content be 10
-10Ppm～10
-3The Ar-H of ppm
2Mixed atmosphere, or for the oxygen mass content be 10
-10Ppm～10
-3The N of ppm
2-H
2Mixed atmosphere;
(4) precursor liquid described in the step (1) is spun on SrTiO described in the step (3) with 2000 rev/mins～5000 rev/mins speed
3On the forming core layer film, the spin coating time is 10s～60s, then with the SrTiO behind the spin coating precursor liquid
3The forming core layer film places tube furnace; In low-oxygen environment; Heating rate to be not less than 50 ℃/min is incubated 0.5h～3h with temperature in the stove after room temperature is heated to 900 ℃～1100 ℃, be cooled to room temperature with the rate of temperature fall that is not less than 2 ℃/min again, obtains Ca-Ti ore type SrTiO
3Resilient coating; Said low-oxygen environment is that quality purity is 99.999% high-purity Ar, or for the oxygen mass content be 10
-10Ppm～10
-3The Ar-H of ppm
2Mixed atmosphere, or for the oxygen mass content be 10
-10Ppm～10
-3The N of ppm
2-H
2Mixed atmosphere.
2. the preparation method of a kind of perovskite type buffer layer according to claim 1 is characterized in that, described in the step (1) in the mixed solvent volume ratio of propionic acid and acetylacetone,2,4-pentanedione be 2～5: 1.
3. the preparation method of a kind of perovskite type buffer layer according to claim 1 is characterized in that, described in the step (2) in the mixed solvent volume ratio of propionic acid and acetylacetone,2,4-pentanedione be 2～5: 1.
4. the preparation method of a kind of perovskite type buffer layer according to claim 1 is characterized in that, the volume ratio of mixed solvent and 2-methyl cellosolve is 3: 1 described in the step (2).
5. the preparation method of a kind of perovskite type buffer layer according to claim 1 is characterized in that, substrate described in the step (3) is NiW base band, NdGaO
3Monocrystal chip, LaAlO
3Monocrystal chip or YSZ single-crystal substrate, wherein YSZ is meant the zirconia that yttrium is stable.
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| CN101419855A (en) * | 2008-12-05 | 2009-04-29 | 西北有色金属研究院 | Producing process for double perovskite type cushion layer used for coating conductor |
| CN101587763A (en) * | 2009-06-26 | 2009-11-25 | 西北有色金属研究院 | Method for preparing buffer layers of high-temperature superconducting coating conductors |
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| CN101587763A (en) * | 2009-06-26 | 2009-11-25 | 西北有色金属研究院 | Method for preparing buffer layers of high-temperature superconducting coating conductors |
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| 张文魁等.溶胶-凝胶法制备钙钛矿型纳米钛酸锶.《中国有色金属学报》.2005,第15卷(第4期),全文. |
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