CN110156021A - A kind of SiNWS:Eu3+,Lu3+Fluorescent nano material preparation method - Google Patents
A kind of SiNWS:Eu3+,Lu3+Fluorescent nano material preparation method Download PDFInfo
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- CN110156021A CN110156021A CN201910468367.9A CN201910468367A CN110156021A CN 110156021 A CN110156021 A CN 110156021A CN 201910468367 A CN201910468367 A CN 201910468367A CN 110156021 A CN110156021 A CN 110156021A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The present invention provides a kind of novel SiNWS:Eu3+,Lu3+The preparation method of fluorescent nano material includes the following steps: S1, uses monocrystalline silicon piece for substrate, is cleaned by ultrasonic with diluted HF；The monocrystalline silicon piece after S2, cleaning is boiled 3-5 minutes with the concentrated sulfuric acid, is rinsed with deionized water, drying, spare；S3, the metal Al layer that 4-8nm is grown on the substrate of the step S2 spare monocrystalline silicon piece, the metallic catalyst as growth Si nano wire；S4, under the protection of argon gas, temperature be 1150-1200 DEG C, Si substrate surface grow diameter be 50-100nm, length be 10-100um Si nano wire；S5, with rare earth Eu2O3And Lu2O3Powder is impurity source, and the surface for the Si nano wire that the step S4 is generated proportionally is uniformly mixed and be coated in for 10:1-20:1；S6, temperature be 1200-1300 DEG C, N2Throughput is 1500-1800sccm and growth time is to carry out Eu to the silicon nanowires under the technological parameters such as 30-90min3+And Lu3+Fluorescent nano material SiNWs:Eu is completed in doping, preparation3+,Lu3+。
Description
Technical field
The present invention relates to nano material production technical field more particularly to a kind of novel SiNWS:Eu3+,Lu3+Fluorescence nano
The preparation method of material.
Background technique
Fluorescent nano material had not only remained the advantage of nano material itself, but also had unique optical property, made it glimmering
Light immunoassay, ion identification, protein active measurement, fluorescent marker, optical imagery and medical diagnosis etc. have extensively
And important application prospect.Therefore, carry out preparation, structural characterization, the characteristics of luminescence and the stability etc. of fluorescent nano material
Research have great importance.Wherein Eu3+Red emission have that stable physical property, monochromaticjty is good, quantum efficiency is high etc.
Feature is widely used in the luminescent material in the various fields such as illumination, medicine, military affairs, nuclear physics and radiation field.
In the prior art, often with rare earth Eu2O3Powder is impurity source, is 1000-1200 DEG C, N in temperature2Throughput is
Under the process conditions such as 1000sccm, Eu is carried out to Si nano wire (SiNWs)3+Doping prepares SiNWs:Eu3+Down-conversion fluorescent is received
Rice material.But under above-mentioned process conditions, Eu3+Red light emitting intensity is lower.
Therefore, a kind of novel SiNWS:Eu is needed3+,Lu3+The preparation method of fluorescent nano material, the Lai Gaishan prior art
Middle Eu3+The lower problem of red light emitting intensity is the problem that those skilled in the art need to capture.
Summary of the invention
In view of this, the present invention provides a kind of novel SiNWS:Eu3+,Lu3+The preparation method of fluorescent nano material, tool
Body scheme is as follows:
A kind of novel SiNWS:Eu3+,Lu3+The preparation method of fluorescent nano material, which comprises the steps of:
S1, it uses monocrystalline silicon piece for substrate, is cleaned by ultrasonic with diluted HF；
The monocrystalline silicon piece after S2, cleaning is boiled 3-5 minutes with the concentrated sulfuric acid, is rinsed with deionized water, drying, spare；
S3, the metal Al layer that 4-8nm is grown on the substrate of the step S2 spare monocrystalline silicon piece, receive as growth Si
The metallic catalyst of rice noodles；
S4, under the protection of argon gas, temperature is 1150-1200 DEG C, and it is 50-100nm that Si substrate surface, which grows diameter, long
Degree is the Si nano wire of 10-100um；
S5, with rare earth Eu2O3And Lu2O3Powder is impurity source, is proportionally uniformly mixed and is coated in for 10:1-20:1
The surface for the Si nano wire that the step S4 is generated；
S6, temperature be 1200-1300 DEG C, N2Throughput is 1500-1800sccm and growth time is 30-90min etc.
Under technological parameter, Eu is carried out to the silicon nanowires3+And Lu3+Fluorescent nano material SiNWs:Eu is completed in doping, preparation3+,Lu3+。
Specifically, the equipment used in the step S3 is magnetron sputtering coater.
Specifically, completed in tube type high-temperature furnace in the step S4.
Specifically, the step S6 is completed in tubular type high-temperature heater.
Specifically, the diluted HF concentration proportioning is HF:H2O=1:10.
Specifically, deionized water temperature used in the step S2 is 80-100 DEG C.
Specifically, the Lu:Eu3+Doping ratio be 2.5-10%.
SiNWS:Eu provided by the invention3+,Lu3+The preparation method of fluorescent nano material, having the advantages that can
Improve Eu3+Red light emitting intensity 33.3%, can further improve the sensitivity and resolution ratio of sample in the application.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is required attached drawing in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the SiNWs:Eu under different doping ratios3+,Lu3+Intensity profile of light emission figure；
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of novel SiNWS:Eu is claimed in the present invention3+,Lu3+The preparation method of fluorescent nano material, including walk as follows
It is rapid:
S1, it uses monocrystalline silicon piece for substrate, is cleaned by ultrasonic with diluted HF；
The monocrystalline silicon piece after S2, cleaning is boiled 3-5 minutes with the concentrated sulfuric acid, is rinsed with deionized water, drying, spare；
S3, the metal Al layer that 4-8nm is grown on the substrate of the step S2 spare monocrystalline silicon piece, receive as growth Si
The metallic catalyst of rice noodles；
S4, under the protection of argon gas, temperature is 1150-1200 DEG C, and it is 50-100nm that Si substrate surface, which grows diameter, long
Degree is the Si nano wire of 10-100um；
S5, with rare earth Eu2O3And Lu2O3Powder is impurity source, is proportionally uniformly mixed and is coated in for 10:1-20:1
The surface for the Si nano wire that the step S4 is generated；
S6, temperature be 1200-1300 DEG C, N2Throughput is 1500-1800sccm and growth time is 30-90min etc.
Under technological parameter, Eu is carried out to the silicon nanowires3+And Lu3+Fluorescent nano material SiNWs:Eu is completed in doping, preparation3+,Lu3+。
Specifically, the Lu:Eu3+Doping ratio be 2.5-10%.
Specifically, the equipment used in the step S3 is magnetron sputtering coater.
Specifically, completed in tube type high-temperature furnace in the step S4.
Specifically, the step S6 is completed in tubular type high-temperature heater.
Specifically, the diluted HF concentration proportioning is HF:H2O=1:10.
Specifically, deionized water temperature used in the step S2 is 80-100 DEG C.
Experimental result is referring to shown in attached drawing 1:
It is 1200 DEG C, N in temperature2Throughput is 1500sccm and growth time is 60min, and dopant Lu:Eu is 0-
SiNWs:Eu is prepared under 50% equal technological parameters3+,Lu3+。
With the increase of Lu doping, sample luminous intensity occurs first increasing the trend reduced afterwards, is in the content of Lu
When 5% or so, the luminous intensity of sample has reached maximum value.
The embodiment of the present invention is described with above attached drawing, but the invention is not limited to above-mentioned specific
Embodiment, the above mentioned embodiment is only schematical, rather than restrictive, those skilled in the art
Under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, it can also make very much
Form, all of these belong to the protection of the present invention.
Claims (7)
1. a kind of novel SiNWS:Eu3+,Lu3+The preparation method of fluorescent nano material, which comprises the steps of:
S1, it uses monocrystalline silicon piece for substrate, is cleaned by ultrasonic with diluted HF；
The monocrystalline silicon piece after S2, cleaning is boiled 3-5 minutes with the concentrated sulfuric acid, is rinsed with deionized water, drying, spare；
S3, the metal Al layer that 4-8nm is grown on the substrate of the step S2 spare monocrystalline silicon piece, as growth Si nano wire
Metallic catalyst；
S4, under the protection of argon gas, temperature is 1150-1200 DEG C, and it is 50-100nm that Si substrate surface, which grows diameter, and length is
The Si nano wire of 10-100um；
S5, with rare earth Eu2O3And Lu2O3Powder is impurity source, is proportionally uniformly mixed for 10:1-20:1 and is coated in the step
The surface for the Si nano wire that rapid S4 is generated；
S6, temperature be 1200-1300 DEG C, N2Throughput is 1500-1800sccm and growth time is the techniques such as 30-90min ginseng
Under several, Eu is carried out to the silicon nanowires3+And Lu3+Fluorescent nano material SiNWs:Eu is completed in doping, preparation3+,Lu3+。
2. a kind of novel SiNWS:Eu according to claim 13+,Lu3+The preparation method of fluorescent nano material, feature exist
In the Lu:Eu3+Doping ratio be 2.5-10%.
3. a kind of novel SiNWS:Eu according to claim 23+,Lu3+The preparation method of fluorescent nano material, feature exist
With: the equipment used in the step S3 is magnetron sputtering coater.
4. a kind of novel SiNWS:Eu according to claim 33+,Lu3+The preparation method of fluorescent nano material, feature exist
With: it is to be completed in tube type high-temperature furnace in the step S4.
5. a kind of novel SiNWS:Eu according to claim 43+,Lu3+The preparation method of fluorescent nano material, feature exist
With: the step S6 is completed in tubular type high-temperature heater.
6. a kind of novel SiNWS:Eu according to claim 1-53+,Lu3+The preparation method of fluorescent nano material,
Its feature is being HF:H with: the diluted HF concentration proportioning2O=1:10.
7. a kind of novel SiNWS:Eu according to claim 63+,Lu3+The preparation method of fluorescent nano material, feature exist
With: deionized water temperature used in the step S2 is 80-100 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858150A (en) * | 2006-06-09 | 2006-11-08 | 中国科学院上海硅酸盐研究所 | X-ray excited rare-earth ion blended tungstate flash luminous material and its preparing method |
| CN101270283A (en) * | 2008-04-30 | 2008-09-24 | 中国计量学院 | Gadolinium lutetium oxide fluorescent powder and preparation method thereof |
| US20100164110A1 (en) * | 2006-08-17 | 2010-07-01 | Song Jin | Metal silicide nanowires and methods for their production |
| JP2015067530A (en) * | 2013-10-01 | 2015-04-13 | 日本電信電話株式会社 | Method for manufacturing nanowire |
-
2019
- 2019-05-31 CN CN201910468367.9A patent/CN110156021A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858150A (en) * | 2006-06-09 | 2006-11-08 | 中国科学院上海硅酸盐研究所 | X-ray excited rare-earth ion blended tungstate flash luminous material and its preparing method |
| US20100164110A1 (en) * | 2006-08-17 | 2010-07-01 | Song Jin | Metal silicide nanowires and methods for their production |
| CN101270283A (en) * | 2008-04-30 | 2008-09-24 | 中国计量学院 | Gadolinium lutetium oxide fluorescent powder and preparation method thereof |
| JP2015067530A (en) * | 2013-10-01 | 2015-04-13 | 日本電信電話株式会社 | Method for manufacturing nanowire |
Non-Patent Citations (2)
| Title |
|---|
| 杨景和等: "稀土元素的共发光效应", 《山东大学学报（自然科学版）》 * |
| 范志东: "基于Si纳米线表面SiO2包覆稀土颗粒的上/下转换荧光纳米材料的研究", 《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑》 * |
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