CN101560680A - Terbium-doped gadolinium oxide green light luminescent film and preparation method thereof - Google Patents
Terbium-doped gadolinium oxide green light luminescent film and preparation method thereof Download PDFInfo
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- CN101560680A CN101560680A CNA2009100980032A CN200910098003A CN101560680A CN 101560680 A CN101560680 A CN 101560680A CN A2009100980032 A CNA2009100980032 A CN A2009100980032A CN 200910098003 A CN200910098003 A CN 200910098003A CN 101560680 A CN101560680 A CN 101560680A
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Abstract
The invention discloses a terbium-doped gadolinium oxide green light luminescent film and a preparation method thereof. A layer of terbium-doped gadolinium oxide green light luminescent film is deposited on a conductive glass substrate. The preparation method comprises the following steps: selecting a soluble gadolinium salt solution and a soluble terbium salt as raw materials; carrying out thin film deposition on the conductive glass substrate by an electrochemical method; inserting a three-electrode into an evenly mixed solution of a gadolinium salt and the terbium salt, and depositing the mixture in a constant temperature water bath at a temperature of between 50 and 70 DEG C, wherein regulation voltage is between -0.90 and -1.4V (vs an SCE saturation calomel reference electrode), and the deposition time is 15 to 60 minutes; washing and drying the obtained film; and then carrying out rapid annealing on the film for 3 to 5 minutes at a temperature of between 400 and 700 DEG C under the protection of argon gas. The prepared luminescent film is even and compact and has no cracking; the film material has a sharp green light emission spectrum at 545 nanometers and 491 nanometers; the luminescent film has the advantages of simple technique, easily-obtained raw materials, low cost, low energy consumption and no toxicity; and the formed film is even and compact and has no cracking.
Description
Technical field
The present invention relates to a kind of terbium-doped gadolinium oxide green light luminescent film and preparation method thereof.
Background technology
Rear-earth-doped luminous be the 4f inner electron transition luminescence of rare earth ion, the 4f inner electron of rare earth ion is because the shielding effect of out-shell electron is subjected to the external environment factor affecting little, monochromaticity is good, brightness is high, the life-span is long, efficient is high.Luminous spectral range from ultraviolet, can see near infrared, have in fields such as optical communication, plane demonstration, illumination, optical storages widely and to use.[Zhang Zhen is emerging for Wang Tao, Pan Xiaojun, Li Hui, Xie Erqing, the Room-Temperature Visible Luminescence of terbium doped nanocrystalline GaN film, Chinese rare-earth journal 26 (2008): 244-247].Because ree content is limited, for the performance that makes rare earth element obtains better application, [Zhou Jianguo, Li Zhenquan, Zhao Fengying, Xia Shuping, Gao Shiyang, nanometer Y are reported in the research that has recently begun to occur relevant rare earth ion doped nano luminescent material ten or twenty year
2O
3: Eu
3+The Review Study of luminescent material, chemical industry progress, 6 (2003): 573-577].
Along with the high speed development of information technology, people are more and more higher to the requirement of standard of living, and the demand of large-screen high-resolution degree colour TV, high resolution display, projection TV, energy-efficient lamp etc. is increased rapidly.The proposition that requires along with friendly society and energy saving society etc. simultaneously, people require the variation except function such as indicating meter, wish that also it has slim, lightweight, low voltage drive, low in power consumption, this just requires fluorescent material to have characteristics such as many performances, strong luminous, high-color rendering, high life.
Tb
3+The luminous spectrum main peak of intrinsic is about 550nm, green corresponding with standard colorimetric system (CIE) just, so terbium-doped gadolinium oxide is the green glow fluorescent material of excellent property, it is widely used in colour television set picture tube, three-color fluorescent lamp and stained glass etc.Tb
3+Doping is subjected to people's attention.The gadolinium sesquioxide film that the electrochemical filming method prepares the doping terbium is a kind of brand-new preparation method, and can prepare the film of excellent property.By the adjusting of reaction parameter, can evenly grow on substrate material gadolinium sesquioxide and terbium sesquioxide codeposition film both can reduce the reaction materials, saved follow-up coated technique again, reduced production costs greatly.In addition, the electrochemical method film forming is even, and deposit thickness is controlled, equipment and simple to operate, reaction conditions is gentle, environmental pollution is little, is a kind of brand-new, clean, gentle, eco-friendly method.
Summary of the invention
The objective of the invention is to propose a kind of terbium-doped gadolinium oxide green light luminescent film and preparation method thereof, with solubility gadolinium salt and terbium salts solution is raw material, on Conducting Glass, deposit the terbium-doped gadolinium oxide film by electrochemical method, obtain terbium-doped gadolinium oxide green light luminescent film through high temperature rapid thermal annealing.
The technical solution used in the present invention step is as follows:
One, a kind of terbium-doped gadolinium oxide green light luminescent film:
The green light-emitting film of deposition gadolinium sesquioxide and terbium sesquioxide on face of Conducting Glass.
The chemical formula of described light-emitting film is Gd
2O
3: Tb
3+, there is sharp-pointed green emission spectrum in this thin-film material in 545 nanometers and 491 nanometers.
Two, a kind of preparation method of terbium-doped gadolinium oxide green light luminescent film, the step of this method is as follows:
1) respectively with solubility gadolinium salt and terbium salt, is dissolved in the deionized water, stirs, all be made into gadolinium salts solution and the terbium salts solution of volumetric molar concentration 0.05～0.2mol/L;
2) get above-mentioned gadolinium salt and terbium salts solution and form the solution that mixes, control solution temperature at 50 ℃～70 ℃ by water bath with thermostatic control;
3) utilize the three-electrode electro Chemical pond of forming by working electrode, counter electrode and reference electrode to carry out thin film deposition on the Conducting Glass, three electrodes are inserted in the mixing solutions of gadolinium salt and terbium salts solution composition, regulate between working electrode and SCE saturated calomel reference electrode voltage-0.9V～-1.4V between, depositing time was controlled at 15 minutes～60 minutes;
4) will deposit good film, use washed with de-ionized water, and drying, subsequently, with film short annealing 3 minutes～5 minutes under 400 ℃～700 ℃ argon shields.
In the described three-electrode electro Chemical pond, working electrode is a Conducting Glass, and counter electrode is platinum electrode, gold electrode or Graphite Electrodes, and reference electrode is the SCE saturated calomel reference electrode.
Described solubility gadolinium salt and terbium salt are nitrate.
The chemical formula of described light-emitting film is Gd
2O
3: Tb
3+, this forming thin film even compact does not have cracking, has sharp-pointed green emission spectrum in 546 nanometers and 491 nanometers.The beneficial effect that the present invention has is:
The present invention makes a kind of novel terbium-doped gadolinium oxide green light luminescent film by simple electrochemical deposition method and follow-up high-temperature annealing process, and this thin-film material even compact does not have cracking, has sharp-pointed green emission spectrum in 546 nanometers and 491 nanometers.Processing method of the present invention is simple, raw material is easy to get, cost is low, and energy consumption is low, and is nontoxic, and the film forming even compact does not have cracking.
Description of drawings
Fig. 1 is a terbium-doped gadolinium oxide green light luminescent film structural representation on the Conducting Glass
Among Fig. 1: 1 terbium-doped gadolinium oxide green light luminescent film, 2. Conducting Glass.
Fig. 2 is the energy spectrogram of embodiment 1 products therefrom.
Fig. 3 is the XRD spectra of embodiment 1 products therefrom.
Fig. 4 is electromicroscopic photograph (low power) figure of embodiment 1 products therefrom.
Fig. 5 is electromicroscopic photograph (high power) figure of embodiment 1 products therefrom.
Fig. 6 is the photoluminescence emmission spectrum of embodiment 1 products therefrom.
Embodiment
As shown in Figure 1, the present invention deposits one deck terbium-doped gadolinium oxide green light luminescent film 1 on Conducting Glass 2.The chemical formula of described this light-emitting film is Gd
2O
3: Tb
3+, there is sharp-pointed green emission spectrum in this thin-film material in 546 nanometers and 491 nanometers.
Embodiment 1:
Terbium-doped gadolinium oxide green light luminescent film and synthetic is dissolved in 4.513g six nitric hydrate gadoliniums in the 100mL deionized water, stirs, and is made into the gadolinium salts solution of volumetric molar concentration 0.1mol/L; 4.529g six nitric hydrate terbiums are dissolved in the 100mL deionized water, stir, be made into the terbium salts solution of volumetric molar concentration 0.1mol/L.
Get above-mentioned gadolinium salt and terbium salt and mix by a certain percentage, mixing solutions is 12mL altogether, controls solution temperature at 60 ℃ by water bath with thermostatic control.Utilize the three-electrode electro Chemical pond to carry out the terbium-doped gadolinium oxide depositing of thin film.Working electrode is a conductive glass.Counter electrode is highly purified platinum electrode.Reference electrode is the SCE saturated calomel reference electrode.Three electrodes are inserted gadolinium salt and terbium mixed salt solution, constant temperature 30 minutes.Regulating voltage is at-1.20V (vs SCE saturated calomel reference electrode), and depositing time was controlled at 30 minutes.The film that deposition is good is used washed with de-ionized water, and dry.Subsequently, with film short annealing 3 minutes under 700 ℃ of argon shields.Fig. 2 is the EDS collection of illustrative plates of this film product, shows on the collection of illustrative plates mainly to have oxygen, gadolinium and three kinds of elements of terbium.The atomic quantity ratio of yttrium and terbium is about 10.2: 1:, illustrate that the film that obtains is a terbium-doped gadolinium oxide.Fig. 3 is the XRD spectra of film, and the standard card (JCPDS#43-1014) of this spectrogram and cubic phase oxygen gadolinium fits like a glove.Fig. 4 is the low power electromicroscopic photograph of this routine products therefrom.As can be seen from the figure film particles is even, the fine and close nothing cracking of film.Fig. 5 is the high power electromicroscopic photograph of this routine products therefrom.This routine product has stronger photoluminescence emmission spectrum as seen from Figure 6, has sharp-pointed green emission spectrum in 546 nanometers and 491 nanometers.
Embodiment 2:
Terbium-doped gadolinium oxide green light luminescent film and synthetic is dissolved in 2.2565g six nitric hydrate gadoliniums in the 100mL deionized water, stirs, and is made into the gadolinium salts solution of volumetric molar concentration 0.05mol/L; 2.2645g six nitric hydrate terbiums are dissolved in the 100mL deionized water, stir, be made into the terbium salts solution of volumetric molar concentration 0.05mol/L.
Get above-mentioned gadolinium salt and terbium salt and mix by a certain percentage, mixing solutions is 12mL altogether, controls solution temperature at 70 ℃ by water bath with thermostatic control.Utilize the three-electrode electro Chemical pond to carry out the terbium-doped gadolinium oxide depositing of thin film.Working electrode is a conductive glass.Counter electrode is highly purified platinum electrode.Reference electrode is the SCE saturated calomel reference electrode.Three electrodes are inserted gadolinium salt and terbium mixed salt solution.Regulating voltage is at-1.4V (vs SCE saturated calomel reference electrode), and depositing time was controlled at 30 minutes.The film that deposition is good is used washed with de-ionized water, and dry.Subsequently, with film short annealing 5 minutes under 700 ℃ of argon shields.The concrete test result of prepared terbium-doped gadolinium oxide film is similar to the test effect of embodiment 1.
Embodiment 3:
Terbium-doped gadolinium oxide green light luminescent film and synthetic is dissolved in 9.0260g six nitric hydrate gadoliniums in the 100mL deionized water, stirs, and is made into the gadolinium salts solution of volumetric molar concentration 0.20mol/L; 9.0580g six nitric hydrate terbiums are dissolved in the 100mL deionized water, stir, be made into the terbium salts solution of volumetric molar concentration 0.20mol/L.
Get above-mentioned gadolinium salt and terbium salt and mix by a certain percentage, mixing solutions is 12mL altogether, controls solution temperature at 50 ℃ by water bath with thermostatic control.Utilize the three-electrode electro Chemical pond to carry out the terbium-doped gadolinium oxide depositing of thin film.Working electrode is a conductive glass.Counter electrode is highly purified platinum electrode.Reference electrode is the SCE saturated calomel reference electrode.Three electrodes are inserted gadolinium salt and terbium mixed salt solution.Regulating voltage is at-0.9V (vs SCE saturated calomel reference electrode), and depositing time was controlled at 15 minutes.The film that deposition is good is used washed with de-ionized water, and dry.Subsequently, with film short annealing 3 minutes under 400 ℃ of argon shields.The concrete test result of prepared terbium-doped gadolinium oxide film is similar to the test effect of embodiment 1.
Claims (6)
1, a kind of terbium-doped gadolinium oxide green light luminescent film is characterized in that: the green light-emitting film (1) of deposition gadolinium sesquioxide and terbium sesquioxide on (2) faces of Conducting Glass.
2, a kind of terbium-doped gadolinium oxide green light luminescent film according to claim 1 is characterized in that: the chemical formula of described light-emitting film is Gd
2O
3: Tb
3+, there is sharp-pointed green emission spectrum in this thin-film material in 545 nanometers and 491 nanometers.
3, a kind of preparation method of terbium-doped gadolinium oxide green light luminescent film is characterized in that the step of this method is as follows:
1) respectively with solubility gadolinium salt and terbium salt, is dissolved in the deionized water, stirs, all be made into gadolinium salts solution and the terbium salts solution of volumetric molar concentration 0.05～0.2mol/L;
2) get above-mentioned gadolinium salt and terbium salts solution and form the solution that mixes, control solution temperature at 50 ℃～70 ℃ by water bath with thermostatic control;
3) utilize the three-electrode electro Chemical pond of forming by working electrode, counter electrode and reference electrode to carry out thin film deposition on the Conducting Glass, three electrodes are inserted in the mixing solutions of gadolinium salt and terbium salts solution composition, regulate between working electrode and SCE saturated calomel reference electrode voltage-0.9V～-1.4V between, depositing time was controlled at 15 minutes～60 minutes;
4) will deposit good film, use washed with de-ionized water, and drying, subsequently, with film short annealing 3 minutes～5 minutes under 400 ℃～700 ℃ argon shields.
4, the preparation method of a kind of terbium-doped gadolinium oxide green light luminescent film according to claim 3, it is characterized in that: in the described three-electrode electro Chemical pond, working electrode is a Conducting Glass, counter electrode is platinum electrode, gold electrode or Graphite Electrodes, and reference electrode is the SCE saturated calomel reference electrode.
5, the preparation method of a kind of terbium-doped gadolinium oxide green light luminescent film according to claim 3 is characterized in that: described solubility gadolinium salt and terbium salt are nitrate.
6, the preparation method of a kind of terbium-doped gadolinium oxide green light luminescent film according to claim 3 is characterized in that: the chemical formula of described light-emitting film is Gd
2O
3: Tb
3+, this forming thin film even compact does not have cracking, has sharp-pointed green emission spectrum in 546 nanometers and 491 nanometers.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115247064A (en) * | 2021-01-18 | 2022-10-28 | 浙江理工大学 | Terbium-doped tin oxide film and preparation method thereof |
| CN115895649A (en) * | 2022-12-30 | 2023-04-04 | 桂林电子科技大学 | Rare earth terbium and rare earth gadolinium codoped gallium oxide fluorescent material and preparation method and application thereof |
-
2009
- 2009-04-23 CN CNA2009100980032A patent/CN101560680A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115247064A (en) * | 2021-01-18 | 2022-10-28 | 浙江理工大学 | Terbium-doped tin oxide film and preparation method thereof |
| CN115895649A (en) * | 2022-12-30 | 2023-04-04 | 桂林电子科技大学 | Rare earth terbium and rare earth gadolinium codoped gallium oxide fluorescent material and preparation method and application thereof |
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Open date: 20091021 |