CN101613092A - A kind of nanometer samarium nitride powder and preparation method - Google Patents
A kind of nanometer samarium nitride powder and preparation method Download PDFInfo
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- CN101613092A CN101613092A CN200810012079A CN200810012079A CN101613092A CN 101613092 A CN101613092 A CN 101613092A CN 200810012079 A CN200810012079 A CN 200810012079A CN 200810012079 A CN200810012079 A CN 200810012079A CN 101613092 A CN101613092 A CN 101613092A
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Abstract
The invention discloses a kind of nano-scale nitride metal samarium and preparation method thereof.Have not yet to see nano rare earth metal or nano rare earth metal hydride respectively with N
2The report of prepared in reaction nano rare earth metal nitride.The present invention (is lower than 400 ℃) at a lower temperature through 1-24 hour, prepares the nano rare earth nitride powder.Product belongs to face-centred cubic structure through the XRD diffraction analysis; Transmissioning electric mirror test shows particle diameter less than 100nm, and minimum diameter is 1nm.The nano metal samarium nitride can make benzene selective hydrogenation generate tetrahydrobenzene.Nano rare earth nitride metal samarium chemical reactivity is than its corresponding commercial goods high 2-4 order of magnitude, and they will have important use to be worth in fields such as material, the energy, chemical industry.This invention equipment is simple, operational condition is easy to control, low production cost, the nano silicon nitride samarium powder good dispersion degree that obtains, active high.
Description
Technical field
The present invention relates to nano-scale metal nitride and preparation method, particularly relate to nano-scale rare earth metal nitride and preparation method.
Background technology
Nanoscale science and technology is a kind of new and high technology that grows up the end of the eighties.The chemical reactivity of nano rare earth metallic substance is than its corresponding commercial goods high 2-4 order of magnitude, and they will have important application value in fields such as material, the energy, chemical industry, produce direct economic benefit.The preparation of nano material is the basis of nanosecond science and technology, is divided into physical method and chemical process usually.Chemical method is mainly by suitable chemical reaction, from molecule, atom preparation nano material.China has advantageous rare earth resources, and rare earth nitride is widely used at aspects such as material, electronics, chemical industry.Common rare earth metal and nitrogen direct reaction generate the exigent temperature of reaction of corresponding rare earth nitride, and generally more than 800 ℃, and particle is the micron number magnitude.Have not yet to see the relevant bibliographical information for preparing nano rare earth nitride metal samarium with chemical method.
Summary of the invention
The purpose of this invention provides a kind of product and preparation method and its application of nano rare earth nitride.
Present method utilize nano rare earth samarium metal or nano rare earth metal hydride samarium respectively with N
2Direct reaction is prepared nano rare earth samarium nitride powder, and particle diameter is less than 100nm.
Utilizing the nano metal samarium to prepare nano silicon nitride samarium method, is under protection of inert gas, under the condition of normal pressure, generates black nano nitride metal samarium powder with nitrogen through 1-24 hour reaction back at 100～400 ℃, and particle diameter is less than 100nm.
Utilize nano metal hydrogenation samarium to prepare nano silicon nitride samarium preparation method; be under protection of inert gas; under the condition of normal pressure, nano metal hydrogenation samarium powder and flowing nitrogen are at 100～400 ℃, process reaction back generation in 1-24 hour black nano nitride metal samarium powder, and particle diameter is less than 100nm.
The nano metal samarium nitride can make benzene selective hydrogenation generate tetrahydrobenzene.
This invention equipment is simple, operational condition is easy to control, low production cost, the nano silicon nitride samarium powder good dispersion degree that obtains and active high, can be applicable to multiple field.
Description of drawings
Fig. 1 is the XRD figure of nano-scale nitride metal samarium.
Fig. 2 is the transmission electron microscope photo of nano-scale nitride metal samarium.
Embodiment
Below by concrete grammar nano-scale nitride metal samarium, preparation method and the application that this invention provides is described further.
Utilize the nano metal samarium to prepare nano metal samarium nitride powder.Under protection of inert gas, take by weighing nano metal samarium (ZL 02144105.7) 3.5g and be put in the Glass tubing, under the condition of normal pressure, generate black nano size nitride metal samarium powder with nitrogen through 1-24 hour reaction back at 100～400 ℃.The standard diffraction data (JCPDS#01-089-3465) that obtains that XRD diffractogram analysed preparation belongs to face-centred cubic structure and database fits like a glove, and the size that the Scherrer formula calculates is 12.0nm; The test result of transmission electron microscope TEM shows particle diameter less than 100nm, and minimum is about 1nm.
Utilize nano metal hydrogenation samarium to prepare nano metal samarium nitride powder.Under protection of inert gas; take by weighing nano metal hydrogenation samarium (ZL 02141735.0) 3.6g and be put in the Glass tubing, under the condition of normal pressure with flowing nitrogen (1-5mL/min) 100～400 ℃, generate black nano size nitride metal samarium powder through 1-24 hour reaction back.XRD diffractogram analysed preparation belongs to face-centred cubic structure (JCPDS#01-089-3465), and the size that the Scherrer formula calculates is 12.0nm; The test result of transmission electron microscope TEM shows particle diameter less than 100nm, and minimum is about 1nm.
The nano metal samarium nitride makes benzene selective hydrogenation generate tetrahydrobenzene.In the small pressure still, put 5mL benzene into, add 0.2g nano metal samarium nitride, under 0.1-0.5MPa hydrogen, heat 80 ℃, 1-4 hour, there is 92% benzene to generate tetrahydrobenzene.
Claims (4)
1. a nano-scale nitride metal samarium powder is characterized in that the basic granules size less than 100nm, and minimum is 1nm.
2. one kind is utilized the nano metal samarium to prepare nano metal samarium nitride method; it is characterized in that under protection of inert gas; under the condition of normal pressure, nano-scale samarium metal powder generates black nano size nitride metal samarium powder at 100～400 ℃ with the nitrogen process after 1-24 hour.
3. one kind is utilized nano metal hydrogenation samarium to prepare nano metal samarium nitride method; it is characterized in that under protection of inert gas; under the condition of normal pressure, nano-scale metal hydride samarium powder generates black nano size nitride metal samarium powder with flowing nitrogen (1-5mL/min) through 1-24 hour reaction back at 100～400 ℃.
4. the nano-scale nitride metal samarium application in selecting hydrogenation is characterized in that putting 5mL benzene in the small pressure axe, adds 0.2g nano metal samarium nitride, under the 0.1-0.5MPa hydrogen, heat 80 ℃, 1-2 hour, 92% benzene generation tetrahydrobenzene.
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| CN200810012079A CN101613092A (en) | 2008-06-27 | 2008-06-27 | A kind of nanometer samarium nitride powder and preparation method |
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| CN200810012079A CN101613092A (en) | 2008-06-27 | 2008-06-27 | A kind of nanometer samarium nitride powder and preparation method |
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| CN101613092A true CN101613092A (en) | 2009-12-30 |
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| CN200810012079A Pending CN101613092A (en) | 2008-06-27 | 2008-06-27 | A kind of nanometer samarium nitride powder and preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102971256A (en) * | 2010-08-11 | 2013-03-13 | 太平洋水泥株式会社 | Method for producing metal nitride |
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2008
- 2008-06-27 CN CN200810012079A patent/CN101613092A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102971256A (en) * | 2010-08-11 | 2013-03-13 | 太平洋水泥株式会社 | Method for producing metal nitride |
| CN102971256B (en) * | 2010-08-11 | 2016-03-02 | 太平洋水泥株式会社 | The manufacture method of metal nitride |
| US9302913B2 (en) | 2010-08-11 | 2016-04-05 | Taiheiyo Cement Corporation | Method for producing metal nitride |
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Open date: 20091230 |