CN105271138A - Preparation method of alkaline earth metal nitride - Google Patents
Preparation method of alkaline earth metal nitride Download PDFInfo
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- CN105271138A CN105271138A CN201510667411.0A CN201510667411A CN105271138A CN 105271138 A CN105271138 A CN 105271138A CN 201510667411 A CN201510667411 A CN 201510667411A CN 105271138 A CN105271138 A CN 105271138A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a preparation method of an alkaline earth metal nitride. The method comprises steps as follows: alkaline earth metal is placed in a metal tantalum crucible, the crucible is placed in a carbon tube furnace, vacuum pumping is performed, the furnace is washed for more than three times, nitrogen is charged until the pressure is 0.1-0.3 MPa, heating and temperature holding are performed at the temperature of 400-800 DEG C for 2-6 h, and the nitride is obtained after natural cooling and crushing. No additive is required to be added, the operation is convenient, and the product purity is guaranteed; the synthesis efficiency is higher, the nitrogen consumption is low, and the production efficiency is higher; the technology is easy to control, the nitridation time is short, energy consumption is low, and the production period is short.
Description
Technical field
The present invention relates to a kind of preparation method of alkaline-earth nitride.
Background technology
The research work of Henridemoissan (ComptesRendusa1 ' AcademiedesSciences, 18981, Vol.127, PaGES497-503), alkaline-earth nitride is placed in nickel crucible by the preparation method disclosing traditional alkaline-earth nitride, heats and obtain in pure stream of nitrogen gas.The molecular formula that he gives CaCl2 is: Ca3N2.In patent CN03815383.1, Buddhist Lang Keyisi René Lacoste provides the synthesis technique of CaCl2 to be utilize calcium zinc alloy, in reaction vessel, the nitrogen of preheating is passed into, utilize calcium and nitrogen to react liberated heat zinc is evaporated and obtains CaCl2, the CaCl2 purity arrived of this technique is not high enough.
General alkaline-earth metal and nitrogen react and just start at the temperature of 200 DEG C, but the increase of weight is by a small margin, late phase reaction will stop by the time, makes reaction be difficult to carry out this is because reaction generates one deck N-Ca film s, even if at 600 DEG C, more than 50 hours, reaction is also difficult to carry out.Only reach more than 650 DEG C in temperature and again could start reaction, and pass into a large amount of stream of nitrogen gas, if at this moment the purity of nitrogen is not very high, the product oxygen level obtained can be very high, and the reaction times that will make to react completely needs lasting more than 10 hours.
The subject matter that above technique exists is: 1, the nitrogen of reaction needed ultra-high purity; 2, react and carry out in nitrogen gas stream, the nitrogen that reaction needed is a large amount of; 3, the reaction times is longer more than 50 hours.4, this technique is mostly only for the production of CaCl2, and the technique of other alkaline-earth nitrides does not provide.
Summary of the invention
The invention discloses a kind of preparation method of alkaline-earth nitride, the method, without the need to adding any additive, both ensure that the purity of product and nitrogen use level is few, and production efficiency is high.
For this reason, the technical scheme adopted is:
A kind of preparation method of alkaline-earth nitride, be placed in carbon tube furnace again after alkaline-earth metal is placed in metal tantalum crucible, carbon tube furnace is vacuumized, nitrogen prepurging more than three times, inflated with nitrogen pressure is to 0.1-0.3MPa, heating and thermal insulation temperature 400-800 DEG C, soaking time 2-6 hour, pulverize after naturally cooling and obtain nitride.
Described alkaline-earth metal refers to: a kind of simple substance in Mg, Ca, Sr, Ba or two or more alloys.
The present invention is that nitrogen and alkaline-earth metal react in the reactor, and without the need to reacting in stream of nitrogen gas, nitrogen use level is few, and product purity is high.And technique easily controls, nitridation time is short, less energy consumption, with short production cycle.Compared to CaCl2 synthesis technique and the preparation technology of other alkaline-earth nitrides reports less, present method is applicable to the production of magnesium nitride, strontium nitride, nitrogenize barium.
Nitrogen and alkaline-earth metal at high temperature easily react, Surface Creation nitride is carried out along with what react under normal pressure, the nitride coating formed can be more and more thicker, and the chance of nitrogen contacting metal diminishes reduction speed of reaction, and speed of reaction can diminish gradually and even stop.If continuation raised temperature, significant reaction can be accelerated, but raises the coating that the fusing point reaching nitride will form one deck liquid along with temperature, and reaction will stop.And the molecular motion increasing the various raw materials of pressure participation reaction can increase, atomic vibration also can strengthen, the activity of thus reacting can increase, particularly the motion of nitrogen-atoms strengthens, the probability internally spread increases, and reaction can be carried out to metal blocks inside, forms chain reaction, externally to internal divergence, reaction more fully completely.In addition metal blocks is broken into the generation that metal-powder is also conducive to product.
Embodiment
embodiment 1
Take calcium metal (Ca:99.99%) 50.0g and be placed in tantalum crucible with cover, carbon tube furnace is put in sealing, uncaps.Vacuumize, after the air inside nitrogen (99.99%) prepurging three emptyings, stamping press 700 DEG C of insulations 2 hours, cools to room temperature to 0.15Mpa with the furnace.Take out tantalum crucible and take out material in nitrogen protection atmosphere glove box.Material is garnet material, weighs as 61.78g
embodiment 2
Take Preparation of Metallic Strontium (Sr:99.9%) 50.0g and be placed in tantalum crucible with cover, carbon tube furnace is put in sealing.Vacuumize, uncap, after the air inside nitrogen (99.99%) prepurging three emptyings, stamping press 750 DEG C of insulations 4 hours, cools to room temperature to 0.1Mpa with the furnace.Take out tantalum crucible and take out material in nitrogen protection atmosphere glove box.Material is atrament, weighs as 54.01g
embodiment 3
Take MAGNESIUM METAL (Mg:99.99%) 50.0g and be placed in tantalum crucible with cover, carbon tube furnace is put in sealing, uncaps.Vacuumize, after the air inside nitrogen (99.99%) prepurging three emptyings, stamping press 800 DEG C of insulations 6 hours, cools to room temperature to 0.3Mpa with the furnace.Take out tantalum crucible and take out material in nitrogen protection atmosphere glove box.Material is yellow-green colour material, weighs as 69.21g
embodiment 4
Take barium metal (Ba:99.9%) 50.0g and be placed in tantalum crucible with cover, carbon tube furnace is put in sealing.Vacuumize, after the air inside nitrogen (99.99%) prepurging three emptyings, stamping press 400 DEG C of insulations 6 hours, cools to room temperature to 0.3Mpa with the furnace.Take out tantalum crucible and take out material in nitrogen protection atmosphere glove box.Material is atrament, weighs as 53.41g.
embodiment 5
Take calcium-magnesium alloy (Mg:Ca=75:25% weight ratio) 50.0g and be placed in tantalum crucible with cover, carbon tube furnace is put in sealing, uncaps.Vacuumize, after the air inside nitrogen (99.99%) prepurging three emptyings, stamping press 720 DEG C of insulations 5 hours, cools to room temperature to 0.2Mpa with the furnace.Take out tantalum crucible and take out material in nitrogen protection atmosphere glove box.Material is brown-green material, weighs as 67.33g.
embodiment 6
Take calcium-magnesium alloy (Mg:Ca=75:25% weight ratio) 80g and be ground into the strontium powder that powder adds 20g again, mix and be placed in tantalum crucible with cover, carbon tube furnace is put in sealing.Vacuumize, after the air inside argon gas (99.99%) prepurging three emptyings, after 750 DEG C of insulation 2h, cooling is taken out, the broken alloy block obtaining three in glove box, take alloy sample 50g be placed in tantalum crucible with cover sealing put into carbon tube furnace, stamping press of uncapping is incubated 5 hours to 0.2Mpa at 720 DEG C, cools to room temperature with the furnace.Take out tantalum crucible and take out material in nitrogen protection atmosphere glove box.Material is grey matter, weighs as 64.91g.
Embodiment record is as follows:
From upper table, the Data Comparison of products weight and theoretical value is found out, the oxygen level of the inventive method products therefrom is extremely low.
Claims (2)
1. the preparation method of an alkaline-earth nitride, it is characterized in that: be placed in carbon tube furnace again after alkaline-earth metal is placed in metal tantalum crucible, carbon tube furnace is vacuumized, nitrogen prepurging more than three times, inflated with nitrogen pressure is to 0.1-0.3MPa, heating and thermal insulation temperature 400-800 DEG C, soaking time 2-6 hour, pulverize after naturally cooling and obtain nitride.
2. the preparation method of a kind of alkaline-earth nitride according to claim 1, is characterized in that: described alkaline-earth metal refers to: a kind of simple substance in Mg, Ca, Sr, Ba or two or more alloys.
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| CN201510667411.0A CN105271138A (en) | 2015-10-16 | 2015-10-16 | Preparation method of alkaline earth metal nitride |
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| CN201510667411.0A CN105271138A (en) | 2015-10-16 | 2015-10-16 | Preparation method of alkaline earth metal nitride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111170288A (en) * | 2020-02-07 | 2020-05-19 | 吉林大学 | High-temperature high-pressure preparation method of monoclinic phase barium diazenium |
| CN112441610A (en) * | 2020-11-24 | 2021-03-05 | 兰州冉华实德新材料有限公司 | High-purity strontium calcium europium nitride solid solution powder and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU788621A1 (en) * | 1979-05-11 | 1984-06-07 | Предприятие П/Я А-7924 | Method of preparing magnesium nitride |
| CN102241393A (en) * | 2010-09-28 | 2011-11-16 | 南昌大学 | Process for preparing magnesium nitride through airflow method |
| CN102491289A (en) * | 2011-12-09 | 2012-06-13 | 上海交通大学 | Method for preparing nanoscale magnesium nitride powder |
| CN104843657A (en) * | 2015-04-24 | 2015-08-19 | 武汉科技大学 | Alkali metal based aluminum nitride nano-material and preparation method thereof |
-
2015
- 2015-10-16 CN CN201510667411.0A patent/CN105271138A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU788621A1 (en) * | 1979-05-11 | 1984-06-07 | Предприятие П/Я А-7924 | Method of preparing magnesium nitride |
| CN102241393A (en) * | 2010-09-28 | 2011-11-16 | 南昌大学 | Process for preparing magnesium nitride through airflow method |
| CN102491289A (en) * | 2011-12-09 | 2012-06-13 | 上海交通大学 | Method for preparing nanoscale magnesium nitride powder |
| CN104843657A (en) * | 2015-04-24 | 2015-08-19 | 武汉科技大学 | Alkali metal based aluminum nitride nano-material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张冠涛等: "《化学 第二册》", 30 April 1983 * |
| 曹文焕等: "静态氮气氛中合成金属氮化物", 《材料导报: 研究篇》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111170288A (en) * | 2020-02-07 | 2020-05-19 | 吉林大学 | High-temperature high-pressure preparation method of monoclinic phase barium diazenium |
| CN112441610A (en) * | 2020-11-24 | 2021-03-05 | 兰州冉华实德新材料有限公司 | High-purity strontium calcium europium nitride solid solution powder and preparation method thereof |
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Application publication date: 20160127 |