CN1109022A - Synthesis of nm-sized magnesium nitride - Google Patents
Synthesis of nm-sized magnesium nitride Download PDFInfo
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- CN1109022A CN1109022A CN 94110129 CN94110129A CN1109022A CN 1109022 A CN1109022 A CN 1109022A CN 94110129 CN94110129 CN 94110129 CN 94110129 A CN94110129 A CN 94110129A CN 1109022 A CN1109022 A CN 1109022A
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- magnesium
- reaction
- magnesium nitride
- normal pressure
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Abstract
The nm-sized magnesium nitride may be prepared through reaction of high-activity magnesium powder on nitrogen at 300-600 deg.C and ordinary pressure or the pressure less than 5 MPa. It is possible to add in compound of transition metal such as Ni, Ti, or Co during reaction for speeding-up. The synthesis process features simple equipment, easy control of reaction condition, high yield rate and 3-30 nm diameter of magnesium nitride particles.
Description
The present invention relates to a kind of nm-sized magnesium nitride (Mg
3N
2) synthetic method.Specifically, be exactly (under 0.1～5MPa), 300～600 ℃ of condition, to use the reaction of high-activity magnesium powder Mg and nitrogen, the magnesium nitride of synthesis of nano size at normal pressure or pressurization.
Mg
3N
2Be of wide application, can be used for 1. preparing high rigidity, high thermal conductance, anticorrosive, resistance to wear and the nitride of resistant to elevated temperatures other element; 2. prepare special stupalith; 3. make the whipping agent of specific alloy; 4. make specific glass; 5. catalytic polymer commissure and 6. reclaim nuke rubbish or the like.Relevant synthetic Mg
3N
2The more existing patent reports of reaction, as USSR (Union of Soviet Socialist Republics) patent (1961, U.S.S.R. 141,854) with metal magnesium powder Mg its fusing point (648.8 ℃) more than with the nitrogen reaction, and reactor imposed vibration in vertical direction, synthesize granular Mg
3N
2; German Patent (1958, Ger.1,034,594) uses magnesium oxide and coal, under hot conditions with N
2Reaction, synthetic Mg
3N
2; French Patent (nineteen fifty-one, Fr.996,658) is used anhydrous magnesium sulfate, in the presence of 700 ℃, iron powder with N
2Reaction, synthetic Mg
3N
2Though document reported once that (specific surface was 0.9m to metal magnesium powder
2/ g) under the ionizing rays condition, can be in 450 ℃ and N
2Reaction, but reaction 18h, Mg
3N
2Yield has only 14%(Fomin, O.K.; Et al., High Energy Chem., 1985,19,406).The synthetic Mg that reports in the recent document
3N
2Temperature of reaction be more than 600 ℃.Have not yet to see synthetic Mg with high-activity magnesium powder Mg
3N
2Bibliographical information.Do not see synthesis of nano size Mg yet
3N
2Bibliographical information.
The purpose of this invention is to provide a kind of can normal pressure or pressurization (0.1～5MPa) or than 300～600 ℃ of conditions of low reaction temperatures under, the method for the magnesium nitride of synthesis of nano size.
The available reaction formula of reaction of synthesis of nano size magnesium nitride of the present invention is expressed as:
Mg
*Be to adopt the high-activity magnesium powder, can obtain, also can adopt synthesizing hydrogenated magnesium of catalysis or anthracene magnesium pyrolysated product (chemical journal, 1988,46,612 under normal pressure or vacuum condition by the known method for preparing the high-activity magnesium powder; ).Above-mentioned building-up reactions also can be carried out under normal pressure and 300～450 ℃ of conditions.In above-mentioned building-up reactions, by the containing transition metal compound, as contain Ni, Ti, the compound of elements such as Co can make the speed of response of above-mentioned reaction significantly accelerate, and dopant species difference, the degree that speed of response improves are also different.Dopant species is at synthetic MgH
2The time or synthetic MgH
2After mix; Can when elbs reaction magnesium or behind the elbs reaction magnesium, mix transistion metal compound equally; Doping is 0.1～20mol% of reactant magnesium.When doping less than 0.1% the time, the doping DeGrain; Doping was greater than 20% o'clock, and the doping effect is also not good, and too much, the synthetic cost of foreign matter content increases.Below by example synthetic method provided by the invention is described further.
The reaction of example 1 synthesis of nano size magnesium nitride
Under protection of inert gas, take by weighing 0.46g high-activity magnesium powder Mg and pack in the exsiccant reaction flask that links to each other with eudiometer, be heated to 450 ℃ with the heat preserving type electric furnace, under normal pressure, synthesize Mg
3N
2Reaction; By inhaling N
2Amount (volume change of eudiometer) is calculated Mg
3N
2Yield.Reaction 8h, Mg
3N
2Yield is 69%; Reaction 18h, Mg
3N
2Yield is 81%.Utilize transmission electron microscope to measure product Mg
3N
2The particle diameter scope be 3～30nm.
Example 2 is by doped with Mg
*System is synthesized Mg
3N
2
Press example 1 described experiment condition and step, carry out the experiment of example 2, the results are shown in Table 1.
Table 1 is by different Mg
*System is synthesized Mg
3N
2Reaction result
| Example | Dopant species | Mg 3N 2Yield (%) | |||
| Reaction times (h) | |||||
| 1?????2???????4????????6??????8????????18 | |||||
| 1 | Do not have | ???37????46??????56???????65?????69????????81 | |||
| 2 | NiCl 2 | ???54????64??????73???????79?????83????????92 | |||
| 3 | Cp 2TiCl 2 * | ???65????77??????86???????91?????94????????99 | |||
| 4 | CoCl 2 | ???48????56??????64???????70?????76????????87 | |||
*: cyclopentadienyl titanium dichloride.Reaction conditions: normal pressure (nitrogen atmosphere), 450 ℃.Doping is 2.5mol.%.
The influence of example 3 temperature of reaction
Press example 1 described experiment condition and step, carry out the experiment of example 3, the results are shown in Table 2.
Comparative example 1 is by the synthetic Mg of commercial magnesium powder
3N
2
Take by weighing certain amount of industrial magnesium powder (100～200 orders, MAGNESIUM METAL content are 99%), press example 1 described experiment condition and step, synthesize Mg
3N
2Reaction.Reaction 23h, Mg
3N
2Yield is 1%.
According to above-mentioned example and comparative example, as seen adopt synthetic method of the present invention, under normal pressure, 450 ℃ of conditions, by Mg
*Energy is the magnesium nitride (Mg of synthesis of nano size quantitatively
3N
2).The present invention proposes high-activity magnesium powder Mg
*An important new purposes.Method of the present invention is less demanding to conversion unit, easily-controlled reaction conditions, and raw material is easy to get, and method is simple.
Table 2 temperature of reaction is to synthetic Mg
3N
2The influence of reaction
| Example | Temperature of reaction (℃) | Mg 3N 2Yield (%) | |||
| Reaction times (h) | |||||
| 1?????2???????4????????6??????8????????18 | |||||
| 2 | 450 | ???54????64??????73???????79?????83????????92 | |||
| 5 | 400 | ???20????27??????35???????42?????48????????56 | |||
| 6 | 300 | ????1????2????????4???????5.5????6.3???????10 | |||
Reaction conditions: normal pressure (nitrogen atmosphere).Dopant species is NiCl
2, doping is 2.5mol.%.
Claims (4)
1, a kind of preparation method of synthesis of nano size magnesium nitride is characterized in that reactant magnesium powder adopts the high-activity magnesium powder, and building-up reactions can be at normal pressure or 5MPa with under the overdraft, and temperature of reaction is carried out under 300～600 ℃ condition.
2, according to the preparation method of the described nm-sized magnesium nitride of claim 1, it is characterized in that building-up reactions can be at normal pressure, carry out under 300～450 ℃ of the temperature of reaction.
3,, it is characterized in that reactant high-activity magnesium powder can adopt the product of the synthesizing hydrogenated magnesium of catalysis or anthracene magnesium thermolysis gained under normal pressure or vacuum condition according to the preparation method of the described nm-sized magnesium nitride of claim 1.
4, according to the preparation method of the described nm-sized magnesium nitride of claim 1, but it is characterized in that containing transition metal compound in the reaction, as contain Ni, Ti, the compound of Co element significantly improves speed of response, and the amount of hotchpotch is 0.1～20mol.% of reactant magnesium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94110129A CN1044355C (en) | 1994-03-21 | 1994-03-21 | Synthesis of nm-sized magnesium nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94110129A CN1044355C (en) | 1994-03-21 | 1994-03-21 | Synthesis of nm-sized magnesium nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1109022A true CN1109022A (en) | 1995-09-27 |
| CN1044355C CN1044355C (en) | 1999-07-28 |
Family
ID=5034117
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94110129A Expired - Fee Related CN1044355C (en) | 1994-03-21 | 1994-03-21 | Synthesis of nm-sized magnesium nitride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1044355C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491289A (en) * | 2011-12-09 | 2012-06-13 | 上海交通大学 | Method for preparing nanoscale magnesium nitride powder |
| CN102971256A (en) * | 2010-08-11 | 2013-03-13 | 太平洋水泥株式会社 | Method for producing metal nitride |
| WO2015134578A1 (en) * | 2014-03-04 | 2015-09-11 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2487474A (en) * | 1945-01-02 | 1949-11-08 | Permanente Metals Corp | Preparation of magnesium nitride |
| US2497583A (en) * | 1945-02-12 | 1950-02-14 | Permanente Metals Corp | Preparation of magnesium nitride |
| US2488054A (en) * | 1945-04-17 | 1949-11-15 | Metal Hydrides Inc | Production of magnesium nitride |
| SU788621A1 (en) * | 1979-05-11 | 1984-06-07 | Предприятие П/Я А-7924 | Method of preparing magnesium nitride |
-
1994
- 1994-03-21 CN CN94110129A patent/CN1044355C/en not_active Expired - Fee Related
Cited By (9)
| 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 |
| CN102491289A (en) * | 2011-12-09 | 2012-06-13 | 上海交通大学 | Method for preparing nanoscale magnesium nitride powder |
| CN102491289B (en) * | 2011-12-09 | 2014-02-19 | 上海交通大学 | Method for preparing nanoscale magnesium nitride powder |
| WO2015134578A1 (en) * | 2014-03-04 | 2015-09-11 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
| US10343219B2 (en) | 2014-03-04 | 2019-07-09 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
| US10654107B2 (en) | 2014-03-04 | 2020-05-19 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
| US11618077B2 (en) | 2014-03-04 | 2023-04-04 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
| US11781199B2 (en) | 2014-03-04 | 2023-10-10 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1044355C (en) | 1999-07-28 |
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