CN100538445C - Extension strontium barium niobate film and preparation method that electrically conducting transparent lithium nickelate hearth electrode is arranged - Google Patents
Extension strontium barium niobate film and preparation method that electrically conducting transparent lithium nickelate hearth electrode is arranged Download PDFInfo
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- CN100538445C CN100538445C CNB2007101564783A CN200710156478A CN100538445C CN 100538445 C CN100538445 C CN 100538445C CN B2007101564783 A CNB2007101564783 A CN B2007101564783A CN 200710156478 A CN200710156478 A CN 200710156478A CN 100538445 C CN100538445 C CN 100538445C
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Abstract
The invention discloses a kind of extension strontium barium niobate film and preparation method with electrically conducting transparent lithium nickelate hearth electrode.At MgO substrate one side epitaxial deposition LNO lithium nickelate transparency conducting layer LNO film, extension prepares the SBN film on the LNO film again.Its preparation process is as follows: at first with lithium carbonate, and nickel oxide, niobium oxide, strontium carbonate, barium carbonate are raw material, prepare lithium nickelate target and strontium barium niobate target respectively with solid sintering technology; Secondly put into reaction chamber after (001) MgO substrate being cleaned, reaction chamber vacuumizes, and heated substrates, is blanket gas with oxygen, introduces in the reaction chamber pulsed laser deposition target, priority epitaxial deposition lithium nickelate conductive electrode and strontium barium niobate film on substrate.Preparation method of the present invention is simple, and the strontium barium niobate film that makes is (001) direction epitaxial growth, and thin film epitaxy is good, the quality height, and electrooptical coefficient is big, and (r33 can reach 180～230pm/V), has a good application prospect.
Description
Technical field
The present invention relates to the technology of preparing of optical waveguide film on (001) MgO substrate, specially refer to PLD and prepare electrically conducting transparent extension lithium nickelate bottom electrode layer, the high electrooptical coefficient strontium barium niobate of extension film and preparation method thereof then.
Background technology
Optical waveguide material is a kind of electrooptical material with broad prospect of application, and it is a kind of light wave can being strapped in the medium of optical wavelength magnitude size, the material of the radiationless transmission of long distance.Common fiber waveguide device comprises (1). optical interconnection device (linear pattern, S flexure type) (2). and power divider (1 fen 2:Y type and MMI type) (3). optical waveguide reverberator (catoptron and grating) (4). bidirectional coupler (5). the polarizer (6). polarization beam apparatus (anisotropic polarization beam splitter) (7). phase-modulator (E-O phase-modulator) (8). intensity modulator (M-Z interferometer) (9) .TE/TM converter (electric light TE/TM converter) (10). frequency shifter (A-O frequency shifter).And integrated optoelectronic device is meant one or more is integrated in the device that constitutes light path on semiconductor or the medium substrate by discrete photovalve that these elements comprise light source, optical filter, photodetector and thin film optical wave-guide etc.
Strontium barium niobate (Sr
xBa
1-xNb
2O
6, 0.2＜x＜0.8, be called for short SBN:
100X) crystal is a kind of electro-optic crystal of tungsten bronze structure, have good piezoelectric property and electrooptical effect, its effective linear electro-optic coefficient is 10～100 times of electrooptical material lithium columbate crystal commonly used, but its half-wave voltage has only 1/10～1/100 of lithium columbate crystal half-wave voltage.Therefore, utilize its good linear electrooptic performance, can prepare various electrooptic modulators.Experiment showed, that the SBN film has very high light and sells off sensitivity.For the SBN film, generally we are modal four kinds: SBN25, SBN60, SBN50 and SBN75.Be characterized in that pyroelectric coefficient is bigger, dielectric loss is less, and permittivity is very big, so be applicable to the small size detector in the detector array.On this material, form small-sized optical waveguide, both can utilize the special construction of waveguide to improve the optical property of crystal, also can constitute the part of integrated optical device.
By methods such as orientation and extensions, can prepare the epitaxial orientation material, realize growth of single crystal, defective control and the crystal property improvement etc. of material, reach the purpose of optimizing material property.Existing monocrystal material substrate such as upward direct deposition preparation such as MgO, the Si extension SBN membraneous material of being reported in obtains result highly significant.Wherein, because the MgO substrate is transparent, needing can be used for the electrooptical material field of transparency carrier.And it has less specific inductive capacity and dielectric loss, can reduce the loss between film and the substrate greatly, is regarded as one of optimal baseplate material.Yet because the MgO baseplate material is non-conductive, and practical application needs the hearth electrode of one deck conduction usually, therefore must solve the problem of introducing one deck conductive electrode between MgO substrate and SBN.Simultaneously, the grating constant of this conductive electrode material should be complementary with the grating constant of MgO substrate and SBN membraneous material, to reach the purpose that epitaxial growth is transmitted.In order to guarantee that film can be applied to transparent electrooptical material field, this hearth electrode also will have certain transmitance in visible-range.And in order to guarantee the conduction of light in film, the refractive index of the hearth electrode of introducing should be less than the refractive index of SBN.Existing a kind of hearth electrode material is a nickel acid lanthanum material at present, and it has electric conductivity and transmitance preferably.Yet the epitaxial growth direction of nickel acid lanthanum material on the MgO substrate is (110) direction, thereby do not possess the effect that (001) direction epitaxial growth is transmitted.The SBN film of considering (001) direction extension has better crystal structure and electro-optical properties, so must develop a kind ofly new both have preferably electric conductivity, than high permeability and less refractive index, have the hearth electrode material of (001) direction epitaxial growth transfer function again.The present invention adopts lithium nickelate as transparency conductive electrode, has successfully prepared the SBN film of (001) direction extension.And every dielectric properties of this extension SBN material are all very excellent, and especially the electrooptical coefficient of material can reach 180～230pm/V, have goodish using value.
Summary of the invention
The object of the present invention is to provide with the PLD method and prepare a kind of extension strontium barium niobate film and preparation method with electrically conducting transparent lithium nickelate hearth electrode.
The step of the technical solution used in the present invention is as follows:
1, a kind of extension strontium barium niobate film with electrically conducting transparent lithium nickelate hearth electrode:
At MgO substrate one side epitaxial deposition LNO lithium nickelate transparency conducting layer LNO film, extension prepares the SBN film on the LNO film again.
The transmitance of described LNO film is 30%～60%, and conductivity is between 2 * 10
-3～3 * 10
-3Ω m.
2, a kind of preparation method with extension strontium barium niobate film of electrically conducting transparent lithium nickelate hearth electrode, the step of this method is as follows:
1) be raw material with lithium carbonate and nickel oxide, by the quality percentage composition 10%～20% lithium carbonate with after 80%～90% nickel oxide mixes, ground 3～5 hours, with pressure is 2～10MPa compression moulding, and in air sintering, sintering range is 800～900 ℃, the heating rate range of control is 100～600 ℃/h, temperature retention time is controlled at 1～3h, obtains the lithium nickelate target after dropping to room temperature;
2) be raw material with strontium carbonate, barium carbonate and niobium oxide, it by the quality percentage composition 25%～30% strontium carbonate, with 10%～30% barium carbonate with after 45%～60% niobium oxide mixes, grinding 3～5 hours, is 2～10MPa compression moulding with pressure, and in air sintering, sintering range is 900～1100 ℃, the heating rate range of control is 100～600 ℃/h, and temperature retention time is controlled at 1～3h, obtains the strontium barium niobate target after dropping to room temperature;
4) adopt the above-mentioned lithium nickelate target that has prepared, utilize pulsed laser deposition, epitaxial deposition lithium nickelate film on (001) MgO substrate, the depositing temperature scope is 500～600 ℃;
5) adopt the strontium barium niobate target prepared, utilize pulsed laser deposition, deposit in extension on (001) MgO substrate of lithium nickelate electrode layer and continue epitaxial deposition strontium barium niobate film, the depositing temperature scope is 800～1000 ℃.
Wherein strontium barium niobate and lithium nickelate film all have good epitaxial nature, and the extension direction is (001) direction.X ray PHI scans demonstration, and strontium barium niobate and lithium nickelate lattice all satisfy the outer matching relationship of accurate face between lithium nickelate and the magnesium oxide-based lath lattice, and the rocking curve value is 0.5 °～0.9 °.The strontium barium niobate film that makes has higher electrooptical coefficient, and electrooptical coefficient is between 180～230pm/V.
The present invention compares with background technology, and the useful effect that has is:
1, adopt the strontium barium niobate ferroelectric thin film of conduction extension lithium nickelate hearth electrode preparation, the film quality of preparation is better, and the thin film crystallization performance can increase under the effect of epitaxial loayer;
2, adopt the strontium barium niobate ferroelectric thin film of conduction extension lithium nickelate hearth electrode preparation, have the good transparency, the transmitance in visible-range can reach 30%～60%, thereby can be used for optical waveguide material;
3, adopt the strontium barium niobate ferroelectric thin film of conduction extension lithium nickelate hearth electrode preparation, have higher photoelectric coefficient.Experiment shows that when the quality percentage composition of Sr was 30%, the electrooptical coefficient value of strontium barium niobate film was 230pm/V;
4, adopt the high electrooptical coefficient strontium barium niobate of the extension ferroelectric thin film of extension lithium nickelate conductive electrode layer preparation, preparing technique process is simple, and is with low cost, has good market outlook.
Description of drawings
Fig. 1 is a structure principle chart of the present invention.
Fig. 2 is the XRD curve and the rocking curve of transparent lithium nickelate conductive electrode membraneous material of the present invention.
Fig. 3 is XRD curve and the rocking curve that utilizes lithium nickelate to prepare the high electrooptical coefficient strontium barium niobate of extension membraneous material for transparency conductive electrode of the present invention.
Fig. 4 is the PHI scanning curve that utilizes lithium nickelate to prepare the high electrooptical coefficient strontium barium niobate of extension membraneous material for transparency conductive electrode of the present invention;
Fig. 5 is the surface topography of lithium nickelate transparency conductive electrode of the present invention, and utilizes lithium nickelate to prepare the surface topography and the sectional drawing of the high electrooptical coefficient strontium barium niobate of extension membraneous material for transparency conductive electrode.
Fig. 6 is the conductivity and the transmittance curve of extension lithium nickelate transparency conductive electrode membraneous material of the present invention;
Embodiment
Embodiment 1:
With lithium carbonate and nickel oxide is raw material, by the quality percentage composition 15% lithium carbonate with after 85% nickel oxide mixes, ground 4 hours, with pressure is 5MPa compression moulding, and in air sintering, sintering temperature is 850 ℃, heating rate is controlled to be 300 ℃/h, temperature retention time is controlled at 2h, obtains the lithium nickelate target after the cooling; With strontium carbonate, barium carbonate and niobium oxide is raw material, it by the quality percentage composition 25% strontium carbonate, 30% barium carbonate is with after 45% niobium oxide mixes, grinding 4 hours, is 6MPa compression moulding with pressure, and in air sintering, sintering temperature is 880 ℃, heating rate is controlled to be 400 ℃/h, and temperature retention time is controlled at 2.5h, obtains the strontium barium niobate target after the cooling; Adopt the lithium nickelate target that has prepared, utilize pulsed laser deposition, deposition lithium nickelate film on (001) MgO substrate, substrate temperature is 550 ℃; Adopt the strontium barium niobate target that has prepared, utilize pulsed laser deposition, be coated with deposition strontium barium niobate film on (001) MgO substrate of lithium nickelate hearth electrode, substrate temperature is 800 ℃, obtains the strontium barium niobate film.The XRD curve and the rocking curve of lithium nickelate film are seen accompanying drawing 2, and the electrooptical coefficient of the strontium barium niobate film of (001) orientation that generates under this example condition is 180pm/v.
Embodiment 2:
With lithium carbonate and nickel oxide is raw material, by the quality percentage composition 10% lithium carbonate with after 90% nickel oxide mixes, ground 3 hours, with pressure is 2MPa compression moulding, and in air sintering, sintering temperature is 800 ℃, heating rate is controlled to be 100 ℃/h, temperature retention time is controlled at 1h, obtains the lithium nickelate target after the cooling; With strontium carbonate, barium carbonate and niobium oxide is raw material, it by the quality percentage composition 30% strontium carbonate, 10% barium carbonate is with after 60% niobium oxide mixes, grinding 5 hours, is 10MPa compression moulding with pressure, and in air sintering, sintering temperature is 900 ℃, heating rate is controlled to be 600 ℃/h, and temperature retention time is controlled at 3h, obtains the strontium barium niobate target after the cooling; Adopt the lithium nickelate target that has prepared, utilize pulsed laser deposition, deposition lithium nickelate film on (001) MgO substrate, substrate temperature is 600 ℃; Adopt the strontium lead titanate target that has prepared, utilize pulsed laser deposition, be coated with deposition strontium barium niobate film on (001) MgO substrate of lithium nickelate hearth electrode, substrate temperature is 1000 ℃, obtains the strontium barium niobate film.Its XRD scanning curve and rocking curve are seen accompanying drawing 3, and the electrooptical coefficient of the strontium barium niobate film of (001) orientation that generates under this example condition is 230pm/v.
Embodiment 3:
With lithium carbonate and nickel oxide is raw material, by the quality percentage composition 17% lithium carbonate with after 83% nickel oxide mixes, ground 3 hours, with pressure is 5MPa compression moulding, and in air sintering, sintering temperature is 850 ℃, the heating rate range of control is 300 ℃/h, temperature retention time is controlled at 1h, obtains the lithium nickelate target after the cooling; With strontium carbonate, barium carbonate and niobium oxide is raw material, it by the quality percentage composition 26% strontium carbonate, 16% barium carbonate is with after 58% niobium oxide mixes, grinding 3 hours, is 5MPa compression moulding with pressure, and in air sintering, sintering temperature is 850 ℃, heating rate is controlled to be 300 ℃/h, and temperature retention time is controlled at 2h, obtains the strontium barium niobate target after the cooling; Adopt the lithium nickelate target that has prepared, utilize pulsed laser deposition, deposition lithium nickelate film on (001) MgO substrate, substrate temperature is 600 ℃; Adopt the strontium lead titanate target that has prepared, utilize pulsed laser deposition, be coated with deposition strontium barium niobate film on (001) MgO substrate of lithium nickelate hearth electrode, the substrate temperature scope is 960 ℃, obtains the strontium barium niobate film.The PHI scanning curve of the extension strontium barium niobate film that generates under this example condition is seen accompanying drawing 4 (a), and the PHI scanning curve of lithium nickelate hearth electrode is seen accompanying drawing 4 (b), and the rocking curve of magnesium oxide substrate is seen accompanying drawing 4 (c).As seen from the figure, the strontium barium niobate film and the lithium nickelate epitaxial loayer of (001) orientation that generates under this example condition are epitaxially grown film, and the electrooptical coefficient of strontium barium niobate film is 210pm/v.
Embodiment 4:
With lithium carbonate and nickel oxide is raw material, by the quality percentage composition 20% lithium carbonate with after 80% nickel oxide mixes, ground 5 hours, with pressure is 10MPa compression moulding, and in air sintering, sintering temperature is 900 ℃, heating rate is controlled to be 600 ℃/h, temperature retention time is controlled at 3h, obtains the lithium nickelate target after the cooling; With strontium carbonate, barium carbonate and niobium oxide is raw material, it by the quality percentage composition 25% strontium carbonate, 30% barium carbonate is with after 45% niobium oxide mixes, grinding 3 hours, is 2MPa compression moulding with pressure, and in air sintering, sintering temperature is 800 ℃, the heating rate range of control is 100 ℃/h, and temperature retention time is controlled at 1～3h, obtains the strontium barium niobate target after the cooling; Adopt the lithium nickelate target that has prepared, utilize pulsed laser deposition, deposition lithium nickelate film on (001) MgO substrate, substrate temperature is 500 ℃; Adopt the strontium barium niobate target that has prepared, utilize pulsed laser deposition, be coated with deposition strontium barium niobate film on (001) MgO substrate of lithium nickelate hearth electrode, the substrate scope is 850 ℃, obtains the strontium barium niobate film.The surface topography of the lithium nickelate film that generates under this example condition is seen accompanying drawing 5 (a), and the surface topography of strontium barium niobate film is seen accompanying drawing 5 (b), and the strontium barium niobate thin-membrane section is seen accompanying drawing 5 (c).The electrooptical coefficient of the strontium barium niobate film of (001) orientation that generates under this example condition is 195pm/v.
Embodiment 5:
With lithium carbonate and nickel oxide is raw material, by the quality percentage composition 18% lithium carbonate with after 82% nickel oxide mixes, ground 3.5 hours, with pressure is 7MPa compression moulding, and in air sintering, sintering range is 820 ℃, the heating rate range of control is 300 ℃/h, temperature retention time is controlled at 1.5h, obtains the lithium nickelate target after the cooling; With strontium carbonate, barium carbonate and niobium oxide is raw material, it by the quality percentage composition 23% strontium carbonate, 20% barium carbonate is with after 57% niobium oxide mixes, grinding 5 hours, is 6MPa compression moulding with pressure, and in air sintering, sintering temperature is 900 ℃, heating rate is controlled to be 500 ℃ of h, and temperature retention time is controlled at 1h, obtains the strontium barium niobate target after the cooling; Adopt the lithium nickelate target that has prepared, utilization/pulsed laser deposition, deposition lithium nickelate film on (001) MgO substrate, substrate temperature is 590 ℃; Adopt the strontium barium niobate target that has prepared, utilize pulsed laser deposition, be coated with deposition strontium barium niobate film on (001) MgO substrate of lithium nickelate hearth electrode, substrate temperature is 900 ℃, obtains the strontium barium niobate film.The current-voltage curve of the lithium nickelate film that can generate under this example condition is seen accompanying drawing 6 (a), and its transmitance at visible-range is seen accompanying drawing 6 (b), and as seen from the figure, the conductivity of the lithium nickelate film that can generate under this example condition is 2.5 * 10
-3Ω m, transmitance is 35%.The electrooptical coefficient of the strontium barium niobate film of (001) orientation that generates under this example condition is 210pm/v.
Embodiment 6:
With lithium carbonate and nickel oxide is raw material, by the quality percentage composition 12% lithium carbonate with after 88% nickel oxide mixes, ground 4.5 hours, with pressure is 7MPa compression moulding, and in air sintering, sintering temperature is 870 ℃, heating rate is controlled to be 400 ℃/h, temperature retention time is controlled at 2h, obtains the lithium nickelate target after the cooling; With strontium carbonate, barium carbonate and niobium oxide is raw material, it by the quality percentage composition 23% strontium carbonate, 20% barium carbonate is with after 57% niobium oxide mixes, grinding 5 hours, is 6MPa compression moulding with pressure, and in air sintering, sintering temperature is 900 ℃, heating rate is controlled to be 500 ℃ of h, and temperature retention time is controlled at 1h, obtains the strontium barium niobate target after the cooling; Adopt the lithium nickelate target that has prepared, utilization/pulsed laser deposition, deposition lithium nickelate film on (001) MgO substrate, substrate temperature is 600 ℃; Adopt the strontium barium niobate target that has prepared, utilize pulsed laser deposition, be coated with deposition strontium barium niobate film on (001) MgO substrate of lithium nickelate hearth electrode, substrate temperature is 920 ℃, obtains the strontium barium niobate film.The electrooptical coefficient of the strontium barium niobate film of (001) orientation that generates under this example condition is 215pm/v.
Claims (3)
1, a kind of extension strontium barium niobate film that electrically conducting transparent lithium nickelate hearth electrode is arranged is characterized in that:
At magnesium oxide substrate (1) one side epitaxial deposition transparency conducting layer lithium nickelate film (2), go up extension at transparency conducting layer lithium nickelate film (2) again and prepare strontium barium niobate film (3).
2, a kind of extension strontium barium niobate film that electrically conducting transparent lithium nickelate hearth electrode is arranged according to claim 1, it is characterized in that: the transmitance of described transparency conducting layer lithium nickelate film (2) is 30%～60%, and conductivity is between 2 * 10
-3～3 * 10
-3Ω m.
3, a kind of preparation method that the extension strontium barium niobate film of electrically conducting transparent lithium nickelate hearth electrode is arranged is characterized in that the step of this method is as follows:
1) be raw material with lithium carbonate and nickel oxide, by the quality percentage composition 10%～20% lithium carbonate with after 80%～90% nickel oxide mixes, ground 3～5 hours, with pressure is 2～10MPa compression moulding, and in air sintering, sintering range is 800～900 ℃, the heating rate range of control is 100～600 ℃/hour, temperature retention time was controlled at 1～3 hour, obtained the lithium nickelate target after dropping to room temperature;
2) be raw material with strontium carbonate, barium carbonate and niobium oxide, it by the quality percentage composition 25%～30% strontium carbonate, with 10%～30% barium carbonate with after 45%～60% niobium oxide mixes, grinding 3～5 hours, is 2～10MPa compression moulding with pressure, and in air sintering, sintering range is 900～1100 ℃, the heating rate range of control is 100～600 ℃/hour, and temperature retention time was controlled at 1～3 hour, obtains the strontium barium niobate target after dropping to room temperature;
3) adopt the above-mentioned lithium nickelate target that has prepared, utilize pulsed laser deposition, epitaxial deposition lithium nickelate film on (001) magnesium oxide substrate, the depositing temperature scope is 500～600 ℃;
4) adopt the strontium barium niobate target prepared, utilize pulsed laser deposition, deposit in extension on (001) magnesium oxide substrate of lithium nickelate electrode layer and continue epitaxial deposition strontium barium niobate film, the depositing temperature scope is 800～1000 ℃.
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|---|---|---|---|
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