CN100572326C - Nano Ge particle dispersion ceramic basal body photoluminescence material and preparation method thereof - Google Patents
Nano Ge particle dispersion ceramic basal body photoluminescence material and preparation method thereof Download PDFInfo
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- CN100572326C CN100572326C CNB2007100519583A CN200710051958A CN100572326C CN 100572326 C CN100572326 C CN 100572326C CN B2007100519583 A CNB2007100519583 A CN B2007100519583A CN 200710051958 A CN200710051958 A CN 200710051958A CN 100572326 C CN100572326 C CN 100572326C
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Abstract
The invention belongs to inorganic nano embedded photoluminescent material field.A kind of nano Ge particle dispersion ceramic basal body photoluminescence material is characterized in that it is formed by aluminium source, silicon source and germanium source feedstock production, in the aluminium source in Al, the silicon source in Si, the germanium source Ge meet chemical formula Al
12(Si
4-xGe
x) O
26, 0＜x≤1 wherein; Described aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is a tetraethoxy; The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester.The chemical stability of the material that this method obtains is good, and this method has the advantages that technology is simple, cost is low.
Description
Technical field
The invention belongs to inorganic nano embedded photoluminescent material field, be specifically related to a kind of nano Ge particle dispersion ceramic basal body photoluminescence material and preparation method thereof.
Background technology
Body phase Ge is an indirect band-gap semiconductor, has less optical band gap width (0.66eV) and low-down optical radiation efficient, generally can only produce extremely weak photoluminescence phenomenon and can not visible emitting in infrared light region.But when the size of semi-conductor Ge particle reaches below several nanometers and is embedded in the dielectric equably, owing to there is quantum size effect, small-size effect, stronger visible region photoluminescence phenomenon can be at room temperature observed in effects such as macro quanta tunnel effect.Its luminescence spectrum scope is very abundant, comprises multiple bands of a spectrum such as infrared, red, yellow, green, blue, purple, ultraviolet, this for its application in field of optoelectronic devices provides may.The method for preparing nano Ge particle dispersion dielectric embedded photoluminescent material so far mainly contains wet chemical methods such as physical methods such as magnetron sputtering, vapour deposition, ion implantation, electron beam evaporation and sol-gel.Wherein to have equipment simple, easy to operate for wet chemistry method, and raw material can mix on molecular level equably, ge content is easy to advantages such as control, is convenient to the laboratory and carries out.Up to the present, in the dielectric matrix research of inlaying for the Ge nanoparticle, mainly concentrate on amorphous SiO
2Matrix, these materials avoid oxidation and ability such as resistance to wear poor, limited the application of such material to a certain extent.And stupalith has very good mechanical properties and good characteristic such as high temperature resistant, anti-oxidant, wear-resistant, and stable environment and guarantee can be provided for the photoluminescence of disperse Ge particle therein, and more wide application prospect is arranged.
Summary of the invention
The object of the present invention is to provide a kind of nano Ge particle dispersion ceramic basal body photoluminescence material and preparation method thereof, the chemical stability of the material that this method obtains is good, and this method has the advantages that technology is simple, cost is low.
To achieve these goals, technical scheme of the present invention is: a kind of nano Ge particle dispersion ceramic basal body photoluminescence material, it is characterized in that it is formed by aluminium source, silicon source and germanium source feedstock production, in the aluminium source in Al, the silicon source in Si, the germanium source Ge meet chemical formula Al
12(Si
4-xGe
x) O
26, 0＜x≤1 wherein;
Described aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is a tetraethoxy; The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester.
The preparation method of above-mentioned a kind of nano Ge particle dispersion ceramic basal body photoluminescence material (utilizing sol-gel to become glue) is characterized in that it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein aluminium source, silicon source and germanium source raw material for standby are chosen in 0＜x≤1; Wherein, the aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is tetraethoxy (TEOS); The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester (TEOG);
2), the aluminium source is dissolved in distilled water or the dehydrated alcohol, add NH after being heated with stirring to 70 ℃～90 ℃
3H
2O regulator solution pH value to 7.5～8.5; The dropping mass concentration is 5%～15% HNO behind solution stirring 1～3h
3, 1～3h is continued to stir in regulator solution pH value to 2.5～3.5 backs; Dropwise add silicon source and germanium source in above-mentioned solution, the regulator solution pH value is to move in 60 ℃～90 ℃ waters bath with thermostatic control until forming xerogel after 3～5h is stirred in 7.5～8.5 continuation;
3), xerogel 1300 ℃～1400 ℃ thermal treatment 1～5 hour in air; Powder H after the thermal treatment
2, H
2-Ar, H
2-N
2Perhaps gac gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 500 ℃～700 ℃ reduction 1～9 hour.
The preparation method of above-mentioned a kind of nano Ge particle dispersion ceramic basal body photoluminescence material (utilizing co-precipitation to become glue) is characterized in that it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein aluminium source, silicon source and germanium source raw material for standby are chosen in 0＜x≤1; Wherein, the aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is a tetraethoxy; The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester;
2), with the aluminium source, silicon source and germanium source are dispersion agent with distilled water or dehydrated alcohol, drip NH in 60 ℃～90 ℃ waters bath with thermostatic control
3H
2O, stirred 2-6 hour regulator solution pH value to 6.5～7.5 backs, and the gained slip is poured in the Rotary Evaporators and is carried out drying under 60 ℃～90 ℃, obtains xerogel;
3), xerogel 1300 ℃～1400 ℃ thermal treatment 1～5 hour in air; Powder H after the thermal treatment
2, H
2-Ar, H
2-N
2Perhaps gac gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 500 ℃～700 ℃ reduction 1～9 hour.
It is that feedstock production has obtained a kind of nano Ge particle dispersion ceramic basal body photoluminescence material that the present invention adopts aluminium source, silicon source and germanium source, and the chemical stability of this square bar material is good, nontoxic, radiationless, belongs to the environmental type luminescent material.This method has that technology is simple, safety, flow process are short, be easy to control, characteristics with low cost.This method is easy to suitability for industrialized production, can be widely used in luminous and the demonstration field.
The D/Max-RB type X-ray diffractometer that adopts Japanese Rigaku company to produce carries out X-ray diffraction (XRD) analysis to sample.Use CuK α target, operating voltage is 40kV, and working current is 50mA, 4 °/min of sweep velocity.Light at room temperature photoluminescence (PL) spectrum adopts the InVia type confocal microscopy Raman spectrometer of Britain Renishaw company to analyze, with Ar
+The 514.5nm of laser apparatus is an exciting light, and the laser intensity of sample surfaces is about 3.2 * 10 in the photoluminescence spectrum
-4Mw/ μ m
2
Description of drawings
Fig. 1 is a material heat treatment x-ray diffractogram of powder (XRD) among the embodiment 1
Fig. 2 is the photoluminescence spectrogram (PL) of material among the embodiment 1
Embodiment
The following examples are in order further to illustrate technological process feature of the present invention and unrestricted the present invention, and wherein embodiment 1～7th, adopt sol-gel to become glue, and embodiment 8～13rd, utilize co-precipitation to become glue.Annotate: the amount of getting of aluminium source, silicon source, germanium source raw material only is accurate to the back double figures of radix point in the embodiments of the invention, can realize the present invention in the experiment; The general technology person in present technique field can be accurate to higher by the technical scheme of summary of the invention part.
Embodiment 1:
According to chemical formula Al
12(Si
3.75Ge
0.25) O
26, with 43.71g Al (NO
3)
39H
2O is dissolved in the 600ml distilled water, dropwise adds NH after being heated with stirring to 90 ℃
3H
2O regulator solution pH value to 8; The dropping mass concentration is 10% HNO behind the solution stirring 3h
3, 3h is continued to stir in regulator solution pH value to 3 back; Add 36.41mmol tetraethoxy (TEOS) and 2.43mmol 3-trichlorine germanium propionic acid, regulator solution pH value to 8 moves in 80 ℃ of waters bath with thermostatic control until forming xerogel after continuing to stir 5h.Xerogel 1300 ℃ of thermal treatment 4 hours in air; Powder H after the thermal treatment
2-Ar mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 500 ℃ of reduction 3 hours.This luminescent material maximum intensity is 8185.
Fig. 1 is material heat treatment powder x-ray diffraction (XRD) figure among this embodiment, and Fig. 2 is photoluminescence spectrum (PL) figure of material among this embodiment.
Embodiment 2:
According to chemical formula Al
12(Si
3Ge) O
26, with 28.13g AlCl
36H
2O is dissolved in the 500ml dehydrated alcohol, dropwise adds NH after being heated with stirring to 70 ℃
3H
2O regulator solution pH value to 7.5; The dropping mass concentration is 5% HNO behind the solution stirring 2h
3, 2h is continued to stir in regulator solution pH value to 3.5 back; Add 29.14mmol tetraethoxy (TEOS) and 9.71mmol germanic acetoacetic ester (TEOG), regulator solution pH value to 8 moves in 60 ℃ of waters bath with thermostatic control until forming xerogel after continuing to stir 3h.Xerogel 1400 ℃ of thermal treatment 1 hour in air; Powder H after the thermal treatment
2-N
2Mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 500 ℃ of reduction 9 hours.This luminescent material maximum intensity is 4154.
Embodiment 3:
According to chemical formula Al
12(Si
3.25Ge
0.75) O
26, with 43.71g Al (NO
3)
39H
2O is dissolved in the 600ml distilled water, dropwise adds NH after being heated with stirring to 90 ℃
3H
2O regulator solution pH value to 8.5; The dropping mass concentration is 15% HNO behind the solution stirring 3h
3, 3h is continued to stir in regulator solution pH value to 3 back; Add 31.56mmolTEOS and 7.28mmolTEOG, regulator solution pH value to 8.5 moves in 70 ℃ of waters bath with thermostatic control until forming xerogel after continuing to stir 5h.Xerogel 1400 ℃ of thermal treatment 6 hours in air; Powder H after the thermal treatment
2-N
2Mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 500 ℃ of reduction 1 hour.This luminescent material maximum intensity is 5438.
Embodiment 4:
According to chemical formula Al
12(Si
3Ge) O
26, the 23.80g aluminum isopropylate is dissolved in the 500ml dehydrated alcohol, dropwise add NH after being heated with stirring to 70 ℃
3H
2O regulator solution pH value to 8; The dropping mass concentration is 10% HNO behind the solution stirring 3h
3, 3h is continued to stir in regulator solution pH value to 3 back; Add 29.11mmolTEOS and 9.70mmol 3-trichlorine germanium propionic acid, regulator solution pH value to 8 moves in 80 ℃ of waters bath with thermostatic control until forming xerogel after continuing to stir 5h.Xerogel 1300 ℃ of thermal treatment 6 hours in air; Powder H after the thermal treatment
2-Ar mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 700 ℃ of reduction 9 hours.This luminescent material maximum intensity is 807.
Embodiment 5:
According to chemical formula Al
12(Si
3.99Ge
0.01) O
26, with 43.71g Al (NO
3)
39H
2O is dissolved in the 600ml distilled water, dropwise adds NH after being heated with stirring to 90 ℃
3H
2O regulator solution pH value to 7.5; The dropping mass concentration is 5% HNO behind the solution stirring 1h
3, 1h is continued to stir in regulator solution pH value to 2.5 back; Add 38.74mmolTEOS and 0.97mmol 3-trichlorine germanium propionic acid, the regulator solution pH value is to move in 60 ℃ of waters bath with thermostatic control until forming xerogel after 3h is stirred in 7.5 continuation; Xerogel 1300 ℃ of thermal treatment 1 hour in air; Powder H after the thermal treatment
2-Ar mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 700 ℃ of reduction 3 hours.This luminescent material maximum intensity is 4732.
Embodiment 6:
A kind of preparation method of nano Ge particle dispersion ceramic basal body photoluminescence material, it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein x=0.8 chooses aluminium source, silicon source and germanium source raw material for standby; Wherein, the aluminium source is an aluminum nitrate; The silicon source is tetraethoxy (TEOS); The germanium source is a 3-trichlorine germanium propionic acid;
2), the aluminium source is dissolved in the distilled water, add NH after being heated with stirring to 70 ℃
3H
2O regulator solution pH value to 7.5; The dropping mass concentration is 5% HNO behind the solution stirring 1h
3, 1h is continued to stir in regulator solution pH value to 2.5 back; Dropwise add silicon source and germanium source in above-mentioned solution, the regulator solution pH value is to move in 60 ℃ of waters bath with thermostatic control until forming xerogel after 3h is stirred in 7.5 continuation;
3), xerogel 1300 ℃ of thermal treatment 1 hour in air; Powder after the thermal treatment 500 ℃ of reduction 1 hour, gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) with gac.
Embodiment 7:
A kind of preparation method of nano Ge particle dispersion ceramic basal body photoluminescence material, it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein x=0.1 chooses aluminium source, silicon source and germanium source raw material for standby; Wherein, the aluminium source is an aluminum isopropylate; The silicon source is tetraethoxy (TEOS); The germanium source is germanic acetoacetic ester (TEOG);
2), the aluminium source is dissolved in the dehydrated alcohol, add NH after being heated with stirring to 90 ℃
3H
2O regulator solution pH value to 8.5; The dropping mass concentration is 15% HNO behind the solution stirring 3h
3, 3h is continued to stir in regulator solution pH value to 3.5 back; Dropwise add silicon source and germanium source in above-mentioned solution, the regulator solution pH value is to move in 90 ℃ of waters bath with thermostatic control until forming xerogel after 5h is stirred in 8.5 continuation;
3), xerogel 1400 ℃ of thermal treatment 5 hours in air; Powder H after the thermal treatment
2-N
2700 ℃ of reduction 9 hours, get product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material).
Embodiment 8:
According to chemical formula Al
12(Si
3.75Ge
0.25) O
26, with 43.71g Al (NO
3)
39H
2O is dissolved in the 300ml dehydrated alcohol, adds 36.41mmol TEOS and 2.43mmol 3-trichlorine germanium propionic acid, dropwise adds NH in 60 ℃ of following waters bath with thermostatic control
3H
2O, stirred 3 hours regulator solution pH value to 7 back; The gained slip is poured into and is carried out drying in the Rotary Evaporators under 80 ℃, obtains xerogel, xerogel 1300 ℃ of thermal treatment 1 hour in air; Powder H after the thermal treatment
2-Ar mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 500 ℃ of reduction 1 hour.This luminescent material maximum intensity is 5821.
Embodiment 9:
According to chemical formula Al
12(Si
3.5Ge
0.5) O
26, with 28.13g AlCl
36H
2O is dissolved in the 500ml distilled water, adds 34.00mmolTEOS and 4.86mmolTEOG, dropwise adds NH in 80 ℃ of following waters bath with thermostatic control
3H
2O, stirred 4 hours regulator solution pH value to 7.5 back; The gained slip is poured into and is carried out drying in the Rotary Evaporators under 90 ℃, obtains xerogel; Xerogel 1300 ℃ of thermal treatment 4 hours in air; Powder H after the thermal treatment
2-Ar mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 700 ℃ of reduction 3 hours.This luminescent material maximum intensity is 1372.
Embodiment 10:
According to chemical formula Al
12(Si
3Ge) O
26, the 23.80g aluminum isopropylate is dissolved in the 300ml dehydrated alcohol, add 29.11mmolTEOS and 9.70mmolTEOG, in 65 ℃ of following waters bath with thermostatic control, dropwise add NH
3H
2O, stirred 5 hours regulator solution pH value to 7 back, and the gained slip is poured into and is carried out drying in the Rotary Evaporators under 70 ℃, and 1400 ℃ of thermal treatment is 1 hour in the air; Powder H after the thermal treatment
2-N
2Mixed gas gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) 700 ℃ of reduction 1 hour.This luminescent material maximum intensity is 3169.
Embodiment 11:
According to chemical formula Al
12(Si
3.99Ge
0.01) O
26, with 43.71g Al (NO
3)
39H
2O is dissolved in the 500ml distilled water, adds 38.74mmolTEOS and 0.97mmol 3-trichlorine germanium propionic acid, dropwise adds NH in 80 ℃ of following waters bath with thermostatic control
3H
2O, stirred 3 hours regulator solution pH value to 7 back; The gained slip is poured into and is carried out drying in the Rotary Evaporators under 70 ℃, and 1400 ℃ of thermal treatment is 5 hours in the air; Powder H after the thermal treatment
2700 ℃ of reduction 3 hours, get product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material).This luminescent material maximum intensity is 1964.
Embodiment 12:
A kind of preparation method of nano Ge particle dispersion ceramic basal body photoluminescence material, it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein x=0.8 chooses aluminium source, silicon source and germanium source raw material for standby; Wherein, the aluminium source is an aluminum chloride; The silicon source is a tetraethoxy; The germanium source is a 3-trichlorine germanium propionic acid;
2), with the aluminium source, silicon source and germanium source are dispersion agent with distilled water, drip NH in 60 ℃ of waters bath with thermostatic control
3H
2O, stirred 2 hours regulator solution pH value to 6.5 back, and the gained slip is poured into and is carried out drying in the Rotary Evaporators under 60 ℃, obtains xerogel;
3), xerogel 1300 ℃ of thermal treatment 1 hour in air; Powder after the thermal treatment 500 ℃ of reduction 1 hour, gets product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material) with gac.
Embodiment 13:
A kind of preparation method of nano Ge particle dispersion ceramic basal body photoluminescence material, it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein x=0.1 chooses aluminium source, silicon source and germanium source raw material for standby; Wherein, the aluminium source is an aluminum isopropylate; The silicon source is a tetraethoxy; The germanium source is the germanic acetoacetic ester;
2), with the aluminium source, silicon source and germanium source are dispersion agent with the dehydrated alcohol, drip NH in 90 ℃ of waters bath with thermostatic control
3H
2O, stirred 6 hours regulator solution pH value to 7.5 back, and the gained slip is poured into and is carried out drying in the Rotary Evaporators under 90 ℃, obtains xerogel;
3), xerogel 1400 ℃ of thermal treatment 5 hours in air; Powder H after the thermal treatment
2-N
2700 ℃ of reduction 9 hours, get product (a kind of nano Ge particle dispersion ceramic basal body photoluminescence material).
Claims (3)
1. a nano Ge particle dispersion ceramic basal body photoluminescence material is characterized in that it is formed by aluminium source, silicon source and germanium source feedstock production, in the aluminium source in Al, the silicon source in Si, the germanium source Ge meet chemical formula Al
12(Si
4-xGe
x) O
26, 0＜x≤1 wherein;
Described aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is a tetraethoxy; The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester.
2. the preparation method of nano Ge particle dispersion ceramic basal body photoluminescence material as claimed in claim 1 is characterized in that it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) O
26, wherein aluminium source, silicon source and germanium source raw material for standby are chosen in 0＜x≤1; Wherein, the aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is a tetraethoxy; The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester;
2), the aluminium source is dissolved in distilled water or the dehydrated alcohol, add NH after being heated with stirring to 70 ℃～90 ℃
3H
2O regulator solution pH value to 7.5～8.5; The dropping mass concentration is 5%～15% HNO behind solution stirring 1～3h
3, 1～3h is continued to stir in regulator solution pH value to 2.5～3.5 backs; Dropwise add silicon source and germanium source in above-mentioned solution, the regulator solution pH value is to move in 60 ℃～90 ℃ waters bath with thermostatic control until forming xerogel after 3～5h is stirred in 7.5～8.5 continuation;
3), xerogel 1300 ℃～1400 ℃ thermal treatment 1～5 hour in air; Powder H after the thermal treatment
2, H
2-Ar, H
2-N
2Perhaps gac gets product 500 ℃～700 ℃ reduction 1～9 hour.
3. the preparation method of nano Ge particle dispersion ceramic basal body photoluminescence material as claimed in claim 1 is characterized in that it comprises the steps:
1), meets chemical formula Al by Ge in Si, the germanium source in Al, the silicon source in the aluminium source
12(Si
4-xGe
x) 0
26, wherein aluminium source, silicon source and germanium source raw material for standby are chosen in 0＜x≤1; Wherein, the aluminium source is aluminum nitrate, aluminum isopropylate or aluminum chloride; The silicon source is a tetraethoxy; The germanium source is 3-trichlorine germanium propionic acid or germanic acetoacetic ester;
2), with the aluminium source, silicon source and germanium source are dispersion agent with distilled water or dehydrated alcohol, drip NH in 60 ℃～90 ℃ waters bath with thermostatic control
3H
2O, stirred 2-6 hour regulator solution pH value to 6.5～7.5 backs, and the gained slip is poured in the Rotary Evaporators and is carried out drying under 60 ℃～90 ℃, obtains xerogel;
3), xerogel 1300 ℃～1400 ℃ thermal treatment 1～5 hour in air; Powder H after the thermal treatment
2, H
2-Ar, H
2-N
2Perhaps gac gets product 500 ℃～700 ℃ reduction 1～9 hour.
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| 镶嵌型纳米锗的制备新方法及其光致发光研究. 徐骏等.发光学报，第20卷第3期. 1999 |
| 镶嵌型纳米锗的制备新方法及其光致发光研究. 徐骏等.发光学报，第20卷第3期. 1999 * |
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