GB2399340A - Preparing Rare Earth Doped LiNbO3 and LiTaO3 Films and Powders - Google Patents
Preparing Rare Earth Doped LiNbO3 and LiTaO3 Films and Powders Download PDFInfo
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- GB2399340A GB2399340A GB0305818A GB0305818A GB2399340A GB 2399340 A GB2399340 A GB 2399340A GB 0305818 A GB0305818 A GB 0305818A GB 0305818 A GB0305818 A GB 0305818A GB 2399340 A GB2399340 A GB 2399340A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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Abstract
A method of preparing a rare earth doped LiMO3 film, wherein M is Nb or Ta, comprises the steps of applying a rare earth doped LiMO3 sol coating onto a substrate, and annealing the substrate. A method of preparing a rare earth doped LiMO3 powder, comprises the steps of precipitating a rare earth doped LiMO3 sol, and sintering the precipitate. The rare earth metal may be Nd or Er. The substrate may be glass, SiO2/Si, Pt/Ti/SiO2/Si or Sr TiO3. The doped LiMO3 sol may be prepared by reacting LiM(OC2H5)6 with an acetic acid solution of a rare earth acetate.
Description
Method of Preparing Rare Earth Doped LiNbO and LiTaO Films and Powders The
invention relates to a method of preparing rare earth doped LiNbO3 and LiTaO3 films and powders, and to rare earth doped LiNbO3 and LiTaO3 films and powders prepared by that method. The invention also relates to a method of preparing rare earth doped LiNbO3 and LiTO3 sole, and to rare earth doped sots prepared by that method.
Lithium niobate (LN) and lithium tantalate (LT) are attractive candidates for integrated optics (IO), because of their excellent electro-optical, acousto- optical, and nonlinear optical properties. Rare earth doping will further increase the potential of these materials, allowing the integration of optical amplifiers, lasers, modulators and other active and passive devices on the same substrate. Among the rare earth ions, neodymium (Nd) and erbium (Er) are of great importance in optical communications, as they can provide optical amplification or lasing at 1.3pm and l.Sm respectively, which corresponds to the two low loss bands of silica glass fibres.
So far, Nd3+ has been introduced into LiNbO3 by direct crystal growth by the Czochralski (CZ) method from doped melt, ion implantation and indiffusion, and recently pulsed laser deposition. Recently, attention has also been paid to Nd3±doped LiTaO3 (Nd3+:LT) material systems. Up to now, lasing in Nd3+:LT crystals and simultaneous quasi-phase-matched second harmonic generation and lasing have been demonstrated. In addition, a new photorefractive effect has also been observed in Nd3+:LT. These Nd3+:LT crystals are also prepared by the CZ method in which Nd2O3 is doped in LT through melting.
The sol-gel technique is a technique that allows mixing of the liquid starting materials, and consequently, it is very suitable for introducing dopants. Nd3+ and Er3+ ions have been successfully introduced into various glass matrixes, such as silica and silica aluminia. However, little work has been done on sol- gel processed rare earth doped lithium niobate and lithium tantalate.
It is an object of the invention to provide a new method for preparing rare earth doped LiNbO3 and LiTaO3 films, powders and sots.
According to a first aspect, the invention provides a method of preparing a rare earth doped LiMO3 film, wherein M is Nb or Ta, the method comprising the steps of applying a rare earth doped LiMO3 sol coating onto a substrate, and annealing the substrate.
The substrate may be pre-heated before it is annealed.
The steps of applying a rare earth doped LiMO3 sol coating onto the substrate, and then pre-heating the substrate, may be repeated before annealing the substrate.
The rare earth doped LiMO3 sol may be applied by spin coating.
The spin coating may be carried out at a speed in the range 2500 to 3500 rpm, preferably at about 3000 rpm.
The pre-heating step may be carried out at a temperature in the range 200 to 400 C, preferably at about 300 C.
The substrate may be pre-heated for at least two minutes, preferably for about minutes.
The annealing step may be carried out at a temperature in the range 400 to 700 C, preferably 500 to 600 C, more preferably at about 500 C when M is Nb and about 600 C when M is Ta.
The substrate may be annealed for at least 20 minutes, preferably for about 30 minutes.
The substrate may be selected from the group consisting of glass, SiOJSi, Pt/Ti/SiOJSi and SrTiO3 The rare earth may be Nd or Er.
According to a second aspect, the invention provides a method of preparing a rare earth doped LiMO3 powder, wherein M is Nb or Ta comprising the steps of precipitating a rare earth doped LiMiO3 sol, and sintering the precipitate.
The sintering step may be carried out at a temperature in the range 400 to 700 C, preferably 500 to 600 C, more preferably at about 500 C when M is Nb, and about 600 when M is Ta.
The rare earth may be Nd or Er.
According to a third aspect of the invention, the invention provides a method of preparing a rare earth doped LiMO3 sol, comprising the steps of i) mixing X (CH3CO0)3 and CH3COOH to form an acetic solution of X ions; and ii) reacting the acetic solution with LiM(OC2H5)6, wherein M is Nb or Ta, and X is a rare earth The LiM(OC2H5)6 may be prepared by reacting LiOC2Hs and M(OC2Hs)s.
The LiOC2Hs and M(OC2Hs)s may be reacted in ethanol.
The molar concentration of X in the rare earth doped LiMO3 sol may be in the range 1 to 3%.
X may be Nd or Er.
The rare earth doped LiMO3 sol according to the invention may be used to prepare the films and powders according to the invention.
Two examples of a method of preparing a rare earth doped LiMO3 sol according to the invention will now be described, by way of illustration, as well as two examples of a method of preparing a rare earth doped LiMO3 film and powder according to the invention, with reference to the following drawings, of which: Fig. 1 shows a flow chart for the preparation of Nd3+: LT sots, films and powders; Fig. 2 shows the experimental set-up for measuring the PL characteristics of the powders; Fig. 3a shows the XRD of Nd3+:LT films according to the invention having different Nd3+ concentrations; Fig. 3b shows the XRD of Nd3+:LT powders according to the invention having different Nd3+ concentrations; Fig. 4a shows an AFM image of a Nd3+:LT film according to the invention, captured on a 2.0mol /O Nd3±doped sample; Fig. 4b shows a SEM image of a Nd3+:LT powder according to the invention, captured on a 3.0% Nd3±doped sample; Fig. 5 shows the PL characteristic of Nd3+:LT powders according to the invention having different Nd3+ concentrations, corresponding to the 4F3/2 _4I '/2 transition of Nd3+; Fig. 6 shows a Micro-Raman study of a Nd3+:LT powder according to the invention.
Fig. 7 shows the XRD of Nd3+:LN films according to the invention having different Nd3+ concentrations; Fig. 8 shows the energy level scheme of the four 4f-electrons in Nd3+:LN; and Fig. 9 shows the photoluminescence at 1.06pm observed in Nd3+:LN powders according to the invention having different Nd3+ concentrations.
Example 1 - Nd3+: LiTaOa Fig. 1 shows a flowchart for the preparation of a Nd3+:LT sol, and for the preparation of films and powders from that sol.
The sol was prepared by mixing LiOC2H,, Ta(OC2H5) and ethanol at a molar concentration of 0.40M. The acetic solution for the introduction of the Nd3+ dopant (0.01M) was prepared by dissolving Nd(CH3COO)3-H2O in acetic acid at an elevated temperature of about 80 C. Different molar concentrations of 1.0%, 2.0%, and 3.0% of Nd3+ were introduced into the sol.
A thin film was deposited on the substrates by spin coating with preheat treatment at 300 C for 5 minutes after the spinning. For annealing, each film sample was directly put into a furnace at a fixed annealing temperature for 30 minutes. The sample was then removed from the furnace and cooled in air.
Multi-layer films may be prepared, if desired, by repetitive spin coating with a pre-heating treatment at 300 C for 5 minutes in between each spinning.
Since the LiTaO3 films crystallize at about 600 C, the annealing temperature for the Nd3+:LT films was selected to be 600 C.
The powders were prepared by sintering the precipitation at 600 C for 60 minutes.
The Nd3+:LT films were studied by X-ray diffraction (XRD, Rigaku RINT2000) and atomic force microscopy (AFM, Digital instrument). The crystallinity of the Nd3+:LT powders was studied by XRD and Micro-Raman, and the surface morphology was observed under a scanning electron microscope (SEM) . The PL characteristics of the powders were studied by a PL setup using an Ar±laser at the wavelength of 488nm as shown in Figure 2.
A long pass filter was used to eliminate the excitation wavelength and a computer was used for control and data acquisition.
Figs. 3a and 3b show the XRD of Nd3+:LT films and powders respectively having different molar concentrations of Nd3+ obtained at a glancing angle of 1 .
The bars stand for the position and the relative X-ray diffraction intensity of the standard powder sample (PDF#29-836). As can be seen from the figure, the films with different Nd3+ concentrations crystallize into the pure trigonal phase of LiTaO3. Meanwhile, the ratio of the X-ray diffraction intensities of the thin films is quite similar to that of the standard powder sample, which means that the crystallites in the films are randomly oriented. This is quite different from undoped LiTaO3 films on the same substrates which show some degree of c-axis orientation. The applicant believes that the reason for this difference is the introduction of the acetic solution of Nd3+ into the sol, which leads to a new molecularly modified organic precursor and an alteration of the molecular make-up of the original alkoxide. As the introduction of Nd3+ solution decreases the molar concentration of LT in the final sol, this results in a thinner film, and consequently, the peak intensities of the diffraction decrease with the increase of the Nd3+ concentration.
The XRD results for the powders were obtained with a standard attachment.
Again, it can be seen that the phase is very pure. No evidence of Nd-LiTa oxides, such as NdTaO4, Nd3TaO7 or Nd2O3 can be found.
Figure 4(a) shows a typical AFM image of a Nd3+:LT film, which was captured on the 2.0mol%-Nd-3±doped sample. The nanocrystalline nature of the film is revealed in the figure. The size of the crystals is about several tens of nanometers, and the maximum crystalline size as can be observed from the image is about 58nm. The film is rather flat, as represented by the RMS roughness of about l.9nm. Figure 7(b) is an SEM image of a Nd3+:LT powder which was captured on the 3.0mol%-Nd3±doped sample. Nanoclusters, with a crystalline size of about a few hundred nanometers, can be found in the powders. In comparison with the thin films, the crystalline size is increased, which may be caused by the relatively long sintering time and the different crystallization condition for powders and thin films.
Photoluminescence was observed in all of the Nd3+:LT powder samples with different dopant concentrations and Figure 5 shows their PL characteristics.
The peak fluorescence occurs at 1.06pm, corresponding to the transition of the Nd3+ ion from the 4F3/2 state to the 4I/2 state. In comparison with the peak fluorescence wavelength value of the single crystal which is about 1.082 m, the value of the Nd3+:LT powder is slightly shifted toward the short wavelength side. This phenomenon has also been observed in Nd-doped LiNbO3 films prepared by pulsed laser deposition, and is perhaps caused by the small crystalline size and/or the relatively low crystallinity. The full-width at half maximum (FWHM) is about 40nm for the samples. The most intense PL is observed in the 1.0 mol%ND3+:LT powder sample. Due to the fact that the thickness of the films is quite small (<800nm), no PL can be observed in the film samples.
The phonon energy was also studied by a micro-Reman, and a typical result is shown in Figure 6. The Raman peaks are in good agreement with those of the commercial LiTaO3 crystal, which again indicates the pure trigonal phase of LiTaO3.
The phonon energy was also studied by a micro-Reman, and a typical result is shown in Figure 6. The Raman peaks are in good agreement with those of the commercial LiTaO3 crystal, which again indicates the pure trigonal phase of LiTaO3.
Example 2 - Nd3+ LiNbO The same process was used for the preparation of Nd3+:LN films and powders, except Nb(OC2H5)s was used instead of Ta(OC2H5) 5, and the annealing temperature was 500 C.
Similar studies were carried out on the Nd3+ LN films and powders as were carried out on the Nd3+:LT films and powders.
Fig. 7 shows an XRD of Nd3+:LN films having different molar concentrations of Nd3+ obtained at a glancing angle of 1 . The trigonal phase of LiNbO3 was identified.
Atomic force microscopy (AFM) and scanning electron microscopy (SEM) studies reveal the polycrystalline nature of the films and the powders, with a crystalline size of about several tens of nanometers. An argon ion laser operating at the wavelength of 488nm was used to excite the photoluminescence (PL) of the powders. The photoluminescence at the wavelength of 1.06pm, corresponding to the 4F3/2.4I/2 transition of Nd-3+ (Figure 8), was observed in all of the studied powder samples (Figure 9) and the full width at half maximum (FWHM) was about 40nm.
In summary, the Examples show that Nd3±doped LiNbO3 and LiTaO3 have been successfully prepared by the sol-gel method. The crystalline size is about several tens of nanometers for the films and a few hundred nanometers for the powders after an annealing at 600 C. Photoluminescence is observed at 1.06pm in the powder samples and the most intense PL is observed in the 2. 0 mol% Nd3+ LN and 1.0 mol%Nd3+:LT samples. The methods of the invention may also be used with other rare earths, Er being particularly useful.
Claims (36)
1. A method of preparing a rare earth doped LiMO3 film, wherein M is Nb or Ta, the method comprising the steps of applying a rare earth doped LiMO3 sol coating onto a substrate, and annealing the substrate.
2. A method according to Claim 1, wherein the substrate is pre-heated before it is annealed.
3. A method according to Claim 2, wherein the steps of applying a rare earth doped LiMO3 sol coating onto the substrate, and then pre-heating the substrate, are repeated before annealing the substrate.
4. A method according to any preceding claim, wherein the rare earth doped LiMO3 sol is applied by spin coating.
5. A method according to Claim 4, wherein the spin coating is carried out at a speed in the range 2500 to 3500 rpm.
6. A method according to Claim 5, wherein the spin coating is carried out at about 3000 rpm.
7. A method according to any of Claims 2 to 6, wherein the pre-heating step is carried out at a temperature in the range 200 to 400 C.
8. A method according to Claim 7, wherein the pre-heating step is carried out at about 300 C.
9. A method according to any of Claims 2 to 8, wherein the substrate is pre-heated for at least 2 minutes.
10. A method according to Claim 9, wherein the substrate is pre-heated for about 5 minutes.
11. A method according to any preceding claim, wherein the annealing step is carried out at a temperature in the range 400 to 700 C.
12. A method according to Claim 11, wherein the annealing step is carried out at a temperature in the range 500 to 600 C.
13. A method according to Claim 12, wherein the annealing step is carried out at about 500 C when M is Nb, and about 600 C when M is Ta.
14. A method according to any preceding claim, wherein the substrate is annealed for at least 20 minutes.
15. A method according to Claim 14, wherein the substrate is annealed for about 30 minutes.
16. A method according to any preceding claim, wherein the substrate is selected from the group consisting of glass, SiOJSi, Pt/Ti/SiO2/Si and SrTiO3.
17. A method according to any preceding claim, wherein the rare earth is Nd or Er.
18. A method according to any preceding claim, wherein the rare earth doped LiMO3 sol is prepared by a method according to any of Claims 29to34.
19. A method of preparing a rare earth doped LiMO3 film substantially as described herein with reference to the Examples, wherein M is Nb or Ta.
20. A rare earth doped LiMO3 film when prepared by a method according to any of Claims I to 19.
21. A method of preparing a rare earth doped LiMO3 powder, wherein M is Nb or Ta, comprising the steps of precipitating a rare earth doped! LiMO3 sol, and sintering the precipitate.
22. A method according to Claim 21, wherein the sintering step is carried out at a temperature in the range 400 to 700 C. I
23. A method according to Claim 22, wherein the sintering step is carried out at a temperature in the range 500 to 600 C.
24. A method according to Claim 23, wherein the sintering step is carried out at about 500 C when M is Nb, and about 600 C when M is Ta I
25. A method according to any one of Claims 21 to 24, wherein the rare earth is Nd or Er.
26. A method according to any one of Claims 21 to 25, wherein the rare earth doped LiMO3 sol is prepared by a method according to any of Claims 29 to 34.
27. A method of preparing a rare earth doped LiMO3 powder, wherein M is Nb or Ta, substantially as described herein with reference to the
Examples.
28. A rare earth doped LiMO3 powder when prepared by a method according to any of Claims 21 to 27.
29. A method of preparing a rare earth doped LiMO3 sol, comprising the steps of i) mixing X (CH3CO0)3 and CH3COOH to form an acetic solution of X ions; and ii) reacting the acetic solution with LiM(OC2H5)6, wherein M is Nb or Ta, and X is a rare earth.
30. A method according to Claim 29, wherein the LiM(OC2H5)6 is prepared by reacting LiOC2H5 and M(OC2H5)5.
31. A method according to Claim 30, wherein the LiOC2H5 and M(OC2H5)5 are reacted in ethanol.
32. A method according to any of Claims 28 to 30, wherein the molar concentration of X in the rare earth doped LiMO3 sol is in the range 1 to3%.
33. A method according to any of Claims 29 to 32, wherein X is Nd or Er.
34. A method of preparing a rare earth doped LiMO3 sol, wherein M is Nb or Ta, substantially as described herein with reference to the Examples.
35. A rare earth doped LiMO3 sol when prepared by a method according to any of Claims 29 to 34.
36. A rare earth doped LiMO3 sol substantially as described herein with reference to the Examples.
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| Application Number | Priority Date | Filing Date | Title |
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| GB0305818A GB2399340A (en) | 2003-03-13 | 2003-03-13 | Preparing Rare Earth Doped LiNbO3 and LiTaO3 Films and Powders |
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| GB0305818A GB2399340A (en) | 2003-03-13 | 2003-03-13 | Preparing Rare Earth Doped LiNbO3 and LiTaO3 Films and Powders |
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| GB2399340A true GB2399340A (en) | 2004-09-15 |
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| CN118663251A (en) * | 2024-08-20 | 2024-09-20 | 电子科技大学长三角研究院(湖州) | Rare earth element doped niobium pentoxide photocatalyst, preparation method and application thereof in reduction of carbon dioxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05327107A (en) * | 1992-05-22 | 1993-12-10 | Matsushita Electric Ind Co Ltd | Optical waveguide type optical amplifire and its forming mehtod |
| JPH1168206A (en) * | 1997-08-27 | 1999-03-09 | Oki Electric Ind Co Ltd | Manufacture of waveguide type optical amplification element |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05327107A (en) * | 1992-05-22 | 1993-12-10 | Matsushita Electric Ind Co Ltd | Optical waveguide type optical amplifire and its forming mehtod |
| JPH1168206A (en) * | 1997-08-27 | 1999-03-09 | Oki Electric Ind Co Ltd | Manufacture of waveguide type optical amplification element |
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