CN103553003A - Preparation method of lanthanum/yttrium-doped silicon nitride nanowire - Google Patents
Preparation method of lanthanum/yttrium-doped silicon nitride nanowire Download PDFInfo
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Abstract
The invention relates to a preparation method of a lanthanum/yttrium-doped silicon nitride nanowire. The preparation method concretely comprises the following steps of: preparing doping controllable nanocrystalline silicon powder through liquid nitrogen low-temperature ball milling by taking high-purity Si powder and high-purity metal lanthanum (La) powder or metal yttrium (Y) powder as initial raw materials; carrying out subsequent nitridation process treatment to obtain a high-purity doping controllable alpha-phase silicon nitride nanowire. According to the invention, the wavelength range of the emission spectrum of the silicon nitride nanowire is 350-500 nanometers. The preparation method disclosed by the invention has the advantages of simple process, low cost and good repeatability; the prepared silicon nitride nanowire has excellent properties of high purity, doping controllability, shortwave light emission, good monochromaticity, high light-emitting intensity, and the like, and can be widely applied to the technical fields of photoelectronic information and nanometer.
Description
Technical field
The present invention relates to nano luminescent material, be specially a kind of preparation method of lanthanum/yttrium beta-silicon nitride nanowire that adulterates, prepared doping lanthanum/yttrium beta-silicon nitride nanowire, can be applicable to the fields such as optoelectronic information and nanotechnology.
Background technology
Along with scientific and technical development, one dimension Nano structure receives increasing concern and attention with its excellent performance, and monodimension nanometer material mainly comprises nanotube, nanometer rod, coaxial nano cable, nano belt etc.
Along with the fast development of China's opto-electronic information technology industry in national defense construction and productive life, people have proposed harsher and urgent requirement to storage with the critical material-semiconductor material of communicating by letter.Nitride nanowires semiconductor material, if gan, indium nitride, beta-silicon nitride nanowire are the third generation semiconductor materials after silicon and gallium arsenide.Wherein, In and Ga are scarce resources, and poisonous, and this class nitride cost is higher; Comparatively speaking, silicon accounts for 26.30% of earth's lithosphere quality, nontoxic, and silicon nitride be again a kind of have high than the good structured material of the over-all propertieies such as strong, Gao Bimo, high temperature resistant, anti-oxidant, wear-resistant and anti-thermal shock.Therefore, beta-silicon nitride nanowire semiconductor material be storage and the communications field there is one of material of application prospect most.
In recent years, increasing investigator has started the research of semiconductor light emitting performance.Semi-conductive physicals and its bandgap structure are closely related, and bandgap structure can be adjusted by doping, therefore by introducing suitable doping, can regulate semi-conductive luminescent properties.Silicon nitride is a kind of broad stopband (～5.0eV) semi-conductor, because obtaining the potentiality that possess good host material compared with high doping content, can be widely used in optoelectronic information and field of nanometer technology.
The method of preparing at present doped silicon nitride nano wire mainly comprises: organic precursor pyrolysis method, self propagating high temperature synthesis method, microwave plasma heating method, laser calcination method etc.There is following deficiency or defect in the doped silicon nitride nano wire that aforesaid method is prepared: the difficult control of yardstick of (1) beta-silicon nitride nanowire mostly; (2) in preparation process, oxidative phenomena is serious, and nano wire production efficiency is low, purity is low, have more lattice imperfection; (3) cost is high, and complex process is not suitable for being applied to industrial production; (4) doping poor controllability, cannot effectively improve silicon nitride luminescent properties etc.
By existing technology, be difficult to realize the doping control of beta-silicon nitride nanowire, the luminescent properties of the beta-silicon nitride nanowire of preparation is weak and unstable, and beta-silicon nitride nanowire is restricted in the application of field of optoelectronic devices.Therefore, simple in the urgent need to finding a kind of technique, with low cost, be applicable to suitability for industrialized production, and can prepare high purity, high yield, yardstick homogeneous, the novel method controlled, that there is shortwave luminescent properties, monochromaticity is good, luminous intensity is high beta-silicon nitride nanowire of adulterating.
Summary of the invention
Technical problem to be solved by this invention is: according to deficiency of the prior art, provide a kind of preparation method of beta-silicon nitride nanowire of rare earth doped lanthanum/yttrium.The method adopts the preparation of liquid nitrogen cryogenics ball milling containing the nanocrystalline silica flour of doped element, by follow-up nitriding treatment, can prepare high-purity, yardstick homogeneous, adulterate controlled, there is shortwave luminescent properties, monochromaticity is good, luminous intensity is high, principal phase is α-Si
3n
4beta-silicon nitride nanowire.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of doping lanthanum/yttrium beta-silicon nitride nanowire provided by the invention, specifically adopts the method for following steps:
(1) high-purity Si powder and metal powder are mixed for 99:1～9:1 in molar ratio, make original powder, described metal powder is high pure metal La powder or high pure metal Y powder;
(2) diameter 5～15mm Stainless Steel Ball and original powder are joined in the ball grinder of liquid nitrogen cryogenics ball mill by ball material mass ratio 8:1～128:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 100～1000r/min, Ball-milling Time 6～48h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, then corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into nitrogen or ammonia, atmosphere flow 100～1000ml/min; Heat-up rate with 10～20 ℃/min rises to 1200～1600 ℃ by temperature, naturally cools to room temperature after being incubated 1～48h, and collecting the product making is doping lanthanum/yttrium beta-silicon nitride nanowire with shortwave luminescent properties.
The purity of described Si powder is 99.99%, and granularity can be 50～400 orders.
The purity of described metal La powder is 99.99%, and granularity can be 50～400 orders.
The purity of described metal Y powder is 99.99%, and granularity can be 50～400 orders.
Doping lanthanum/yttrium beta-silicon nitride nanowire that the present invention makes, its principal phase is α-Si
3n
4, its emmission spectrum wavelength region is 350～500nm.
Doping lanthanum/yttrium beta-silicon nitride nanowire that the present invention makes, can be used as short-wavelength laser material and is applied in optoelectronic information and field of nanometer technology.
The controlled beta-silicon nitride nanowire of doping prepared by the present invention, has the high-performance that shortwave is luminous and luminous intensity is high, can be widely used in the fields such as microelectronics, optics, illumination.The method of preparing beta-silicon nitride nanowire provided by the invention is to obtain content evenly and the controlled nanocrystalline silica flour that adulterates by liquid nitrogen cryogenics ball-milling technology, and the follow-up nitrogenizing reaction of process is prepared high purity, phase is single, controlled beta-silicon nitride nanowire adulterates.The present invention has advantages of following with respect to other method:
(1) technique, equipment are simple, easy to operate, can be applicable to industrially scalable and produce continuously;
(2) the beta-silicon nitride nanowire productive rate making is high, and in product, the content of oxygen element, lower than 0.5%, has effectively been avoided oxidative phenomena in building-up process;
(3) the doping controllability of the beta-silicon nitride nanowire making is good, and the mol ratio of element silicon and doped element can accurately be controlled between 99:1～9:1; Monochromaticity is good, and emmission spectrum wavelength region is 350～500nm; Luminous intensity is significantly increased with beta-silicon nitride nanowire prepared by existing technique relatively, can be widely used in the fields such as optoelectronic information and nanotechnology;
(4) in preparation process, do not produce objectionable impurities, non-environmental-pollution, energy consumption is low, with low cost.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the beta-silicon nitride nanowire that makes of embodiment 1.
Fig. 2 is the SEM picture of the beta-silicon nitride nanowire that makes of embodiment 2.
Fig. 3 is the photoluminescence spectrum of the beta-silicon nitride nanowire that makes of embodiment 3.
Fig. 4 is the photoluminescence spectrum of the beta-silicon nitride nanowire that makes of embodiment 4.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but do not limit to described content below.
Embodiment 1:
(1) 300 order high-purity Si powder and 300 height of eye pure metal La powder are mixed by mole ratio 27:1, make original powder;
(2) the stainless steel abrading-ball that is 5mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 32:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 400r/min, Ball-milling Time 10h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping La making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into nitrogen, atmosphere flow is 100ml/min, temperature rise rate with 10 ℃/min rises to 1300 ℃, after insulation 6h, naturally cool to room temperature, collect the doping La beta-silicon nitride nanowire making.
Fig. 1 is the XRD figure spectrum of the doping La beta-silicon nitride nanowire that makes of the present embodiment, with α-Si
3n
4standard diffraction card (NO.09-0250) conform to, illustrate that the doping La beta-silicon nitride nanowire principal phase of preparing in the present embodiment is α-Si
3n
4.
Embodiment 2:
(1) 200 order high-purity Si powder and 200 height of eye pure metal La powder are mixed by mole ratio 42:1, make original powder;
(2) the stainless steel abrading-ball that is 10mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 8:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 600r/min, Ball-milling Time 12h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping La making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into ammonia, atmosphere flow is 500ml/min, temperature rise rate with 20 ℃/min rises to 1500 ℃, after insulation 24h, naturally cool to room temperature, collect the doping La beta-silicon nitride nanowire making.
Fig. 2 is the SEM picture of the doping La beta-silicon nitride nanowire that makes of the present embodiment, and the silicon nitride nano length-to-diameter ratio that as can be seen from the figure makes is large and yardstick is even.
Embodiment 3:
(1) 50 order high-purity Si powder and 50 height of eye pure metal La powder are mixed by mole ratio 57:1, make original powder;
(2) the stainless steel abrading-ball that is 5mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 32:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 600r/min, Ball-milling Time 18h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping La making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into ammonia, atmosphere flow is 600ml/min, temperature rise rate with 15 ℃/min rises to 1600 ℃, after insulation 12h, naturally cool to room temperature, collect the doping La beta-silicon nitride nanowire making.
Fig. 3 is the photoluminescence spectrum of the doping La beta-silicon nitride nanowire that makes of the present embodiment, and excitation wavelength is 325nm, and as can be seen from the figure the emmission spectrum wavelength region of beta-silicon nitride nanowire is 350～500nm, and glow peak is positioned at 390nm.
Embodiment 4:
(1) 100 order high-purity Si powder and 100 height of eye pure metal Y powder are mixed by mole ratio 60:1, make original powder;
(2) the stainless steel abrading-ball that is 15mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 16:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 800r/min, Ball-milling Time 36h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping Y making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into nitrogen, atmosphere flow is 300ml/min, temperature rise rate with 20 ℃/min rises to 1350 ℃, after insulation 12h, naturally cool to room temperature, collect the doping Y beta-silicon nitride nanowire making.
Fig. 4 is the photoluminescence spectrum of the doping Y beta-silicon nitride nanowire that makes of the present embodiment, and excitation wavelength is 325nm, and as can be seen from the figure the emmission spectrum wavelength region of beta-silicon nitride nanowire is 350～500nm, and glow peak is positioned at 410nm.
Embodiment 5:
(1) 300 order high-purity Si powder and 300 height of eye pure metal Y powder are mixed by mole ratio 42:1, make original powder;
(2) the stainless steel abrading-ball that is 10mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 128:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 100r/min, Ball-milling Time 16h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping Y making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into ammonia, atmosphere flow is 1000ml/min, temperature rise rate with 10 ℃/min rises to 1550 ℃, after insulation 6h, naturally cool to room temperature, collect the doping Y beta-silicon nitride nanowire making.
Embodiment 6:
(1) 100 order high-purity Si powder and 100 height of eye pure metal Y powder are mixed by mole ratio 9:1, make original powder;
(2) the stainless steel abrading-ball that is 15mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 64:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out with rotating speed 600r/min, Ball-milling Time 48h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping Y making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into nitrogen, atmosphere flow is 1000ml/min, temperature rise rate with 15 ℃/min rises to 1200 ℃, after insulation 48h, naturally cool to room temperature, collect the doping Y beta-silicon nitride nanowire making.
Embodiment 7:
(1) 400 order high-purity Si powder and 400 height of eye pure metal La powder are mixed by mole ratio 99:1, make original powder;
(2) the stainless steel abrading-ball that is 5mm by diameter and original powder join in the ball grinder of liquid nitrogen cryogenics ball mill by ball material weight ratio 64:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 1000r/min, Ball-milling Time 6h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour of doping La making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, again corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into nitrogen, atmosphere flow is 500ml/min, temperature rise rate with 10 ℃/min rises to 1400 ℃, after insulation 6h, naturally cool to room temperature, collect the doping La beta-silicon nitride nanowire making.
In above-described embodiment, can adopt liquid nitrogen cryogenics ball mill to carry out ball milling.
Doping lanthanum/yttrium beta-silicon nitride nanowire prepared by above-described embodiment, can be used as short-wavelength laser material and is applied in optoelectronic information and field of nanometer technology.
Claims (6)
1. the adulterate preparation method of lanthanum/yttrium beta-silicon nitride nanowire, is characterized in that adopting the method for following steps:
(1) high-purity Si powder and metal powder are mixed for 99:1～9:1 in molar ratio, make original powder, described metal powder is high pure metal La powder or high pure metal Y powder;
(2) diameter 5～15mm Stainless Steel Ball and original powder are joined in the ball grinder of liquid nitrogen cryogenics ball mill by ball material mass ratio 8:1～128:1;
(3) in ball grinder, pass into liquid nitrogen, make original powder and stainless steel abrading-ball all be immersed in liquid nitrogen;
(4) ball mill carries out ball milling with rotating speed 100～1000r/min, Ball-milling Time 6～48h;
(5) ball milling is complete, and ball grinder is moved to vacuum glove box, is naturally warming up to room temperature, collects the nanocrystalline silica flour making;
(6) the ultrasonic dispersion of nanocrystalline silica flour is placed in corundum Noah's ark, then corundum Noah's ark is placed in to vertical high-temperature tube furnace, pass into nitrogen or ammonia, atmosphere flow 100～1000ml/min; Heat-up rate with 10～20 ℃/min rises to 1200～1600 ℃ by temperature, naturally cools to room temperature after being incubated 1～48h, and collecting the product making is doping lanthanum/yttrium beta-silicon nitride nanowire with shortwave luminescent properties.
2. the preparation method of doping lanthanum/yttrium beta-silicon nitride nanowire according to claim 1, is characterized in that: the purity of described Si powder is 99.99%, and granularity is 50～400 orders.
3. the preparation method of doping lanthanum/yttrium beta-silicon nitride nanowire according to claim 1, is characterized in that: the purity of described metal La powder is 99.99%, and granularity is 50～400 orders.
4. the preparation method of doping lanthanum/yttrium beta-silicon nitride nanowire according to claim 1, is characterized in that: the purity of metal Y powder is 99.99%, and granularity is 50～400 orders.
5. the preparation method of doping lanthanum/yttrium beta-silicon nitride nanowire according to claim 1, is characterized in that: the doping lanthanum/yttrium beta-silicon nitride nanowire principal phase making is α-Si
3n
4, its emmission spectrum wavelength region is 350～500nm.
6. doping lanthanum/yttrium beta-silicon nitride nanowire that in claim 1 to 5, described in arbitrary claim, method makes, can be used as short-wavelength laser material and is applied in optoelectronic information and field of nanometer technology.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477538A (en) * | 2016-11-03 | 2017-03-08 | 清华大学 | Beta-silicon nitride nanowire preparation method, beta-silicon nitride nanowire, beta-silicon nitride powder and silicon nitride submicron powder |
| CN114517091A (en) * | 2022-03-09 | 2022-05-20 | 渤海大学 | Rare earth ion doped silicon nitride nanowire and preparation method thereof |
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| CN101979317A (en) * | 2010-10-09 | 2011-02-23 | 武汉理工大学 | Low-temperature ball milling preparation method for nano crystal silicon powder |
| CN102328919A (en) * | 2011-07-06 | 2012-01-25 | 武汉理工大学 | Preparation method for scale-controllable silicon nitride nano wire short-wavelength light emitting material |
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| CN101613856A (en) * | 2009-07-16 | 2009-12-30 | 中国科学院上海硅酸盐研究所 | A kind of aluminium doped alpha phase silicon nitride (α-Si 3N 4) sill and preparation method thereof |
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Cited By (3)
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| CN106477538A (en) * | 2016-11-03 | 2017-03-08 | 清华大学 | Beta-silicon nitride nanowire preparation method, beta-silicon nitride nanowire, beta-silicon nitride powder and silicon nitride submicron powder |
| CN114517091A (en) * | 2022-03-09 | 2022-05-20 | 渤海大学 | Rare earth ion doped silicon nitride nanowire and preparation method thereof |
| CN114517091B (en) * | 2022-03-09 | 2023-09-12 | 渤海大学 | Rare earth ion doped silicon nitride nanowire and preparation method thereof |
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Application publication date: 20140205 |