CN115403043B - Preparation method of rare earth element carbide, nitride or carbonitride powder - Google Patents
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Abstract
The invention provides a preparation method of rare earth element carbide, nitride or carbonitride powder, belonging to the technical field of rare earth compound preparation. Firstly mixing rare earth element oxide, carbon black and a liquid medium, then sequentially carrying out ball milling, drying and hydrogenation treatment to obtain hydrogenated powder, and then carrying out carbothermic reduction reaction on the hydrogenated powder under the atmosphere condition to obtain rare earth element carbide, nitride or carbonitride powder. The rare earth element carbide, nitride or carbonitride powder prepared by the method is high-purity spherical-like nanoscale powder, the carbothermal reduction reaction temperature is low, the reaction time is short, and the energy is saved.
Description
Technical Field
The invention relates to the technical field of rare earth compound preparation, in particular to a preparation method of rare earth element carbide, nitride or carbonitride powder.
Background
Rare earth is mainly applied to the fields of advanced technology and military industry, is praised as industrial monosodium glutamate, industrial vitamins and new material, and is an extremely important strategic resource. Therefore, the method has very important practical significance for researching the rare earth compound.
The carbide, nitride and carbonitride of rare earth elements not only play an important role in the fields of electrocatalysis, electromagnetism and the like, but also can be used for preparing various inorganic composite materials, such as rare earth permanent magnet materials, high-performance ceramic materials, luminescent materials and the like. However, the purity of rare earth carbide and nitride is required to be high.
In the prior art, the preparation of rare earth carbide mainly comprises two modes: the rare earth oxide and carbon react at high temperature under the argon atmosphere to generate carbide; rare earth hydrides and graphite form carbides under vacuum conditions. Likewise, the preparation of rare earth nitrides mainly includes two modes: direct combination of rare earth metal and nitrogen; the rare earth hydride reacts with nitrogen. However, the rare earth metal is very easy to oxidize in the air due to the chemical nature, and the rare earth hydride has strong activity, so that the preparation of carbide and nitride by directly using metal elements or hydrides has great difficulty.
From experimental experience, carbothermal reduction and carbothermal reduction nitridation are the main process routes for preparing rare earth element carbide, rare earth element nitride and rare earth element carbonitride powder, but the process routes have high reaction temperature (1800-2400 ℃), the purity of the reaction products is low, and rare earth carbide, nitride or carbonitride powder with higher purity is basically not obtained. Therefore, the development of a preparation method of single-phase nano rare earth carbide, nitride or carbonitride powder with low reaction temperature and high purity has important significance.
Disclosure of Invention
The invention aims to provide a preparation method of rare earth element carbide, nitride or carbonitride powder, which solves the technical problems of high carbothermal reduction reaction temperature and low purity of reaction products in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of rare earth element carbide, nitride or carbonitride powder, which comprises the following steps:
(1) Mixing rare earth element oxide, carbon black and a liquid phase medium, and sequentially performing ball milling, drying and hydrogenation treatment to obtain hydrotreated powder;
(2) Carrying out carbothermic reduction reaction on the hydrotreated powder under the atmosphere condition to obtain rare earth element carbide, nitride or carbonitride powder;
the temperature of the carbothermic reaction in the step (2) is 1300-2200 ℃, and the carbothermic reaction time is 2-6 h.
Further, in the step (1), the molar ratio of the rare earth element oxide to the carbon black is 1:3-10, and the rare earth element oxide comprises cerium oxide, yttrium oxide or lanthanum oxide.
Further, the liquid phase medium in the step (1) comprises water, absolute ethyl alcohol, acetone or cyclohexane, wherein the ratio of the volume of the liquid phase medium to the mass sum of the rare earth element oxide and the carbon black is 7-10 ml/1-3 g.
Further, the ball-material ratio in the ball milling treatment in the step (1) is 5-20:1, the ball milling rotating speed is 200-400 r/min, and the ball milling time is 2-24 h.
Further, the temperature of the drying treatment in the step (1) is 60-100 ℃ and the time is 2-10 h.
Further, the hydrotreating in the step (1) is performed under a hydrogen atmosphere, the hydrotreating temperature is 500-1200 ℃, the hydrotreating time is 1-4 hours, and the gas flow rate during the hydrotreating is 100-1000 ml/min.
Further, the flow rate of the gas in the carbothermic reaction in the step (2) is 100-1000 ml/min.
Further, the carbothermic reduction reaction of step (2) is performed under an argon atmosphere when preparing the rare earth element carbide.
Further, the carbothermic reduction reaction of step (2) is performed under a nitrogen atmosphere in the preparation of the rare earth element nitride.
Further, the carbothermal reduction reaction of the step (2) is performed under an atmosphere of argon and nitrogen in which the flow rate ratio of the argon to the nitrogen is 1:0.1 to 10 when preparing the rare earth element carbonitride.
The invention has the beneficial effects that:
(1) The preparation method of the rare earth element carbide, nitride or carbonitride powder provided by the invention has the advantages of simple process, low requirement on equipment, safety and reliability.
(2) The preparation method provided by the invention reduces the temperature of carbothermic reaction from 1800-2400 ℃ to 1300-2200 ℃ in the conventional method, shortens the time of carbothermic reaction from 8-15 h to 2-6 h in the conventional method, reduces the carbothermic reaction temperature, shortens the reaction time, saves energy sources and reduces the manufacturing cost of rare earth element carbide, nitride or carbonitride powder.
(3) The rare earth element carbide, nitride or carbonitride powder prepared by the invention is high-purity sphere-like nano-scale powder.
Drawings
FIG. 1 is a flow chart of a process for preparing rare earth carbide, nitride, carbonitride powders of the present invention;
FIG. 2 is CeC prepared in example 1 2 XRD pattern of the powder;
FIG. 3 is CeC prepared in example 1 2 SEM image of powder;
FIG. 4 is an XRD pattern of CeN powder prepared in example 2;
fig. 5 is an SEM image of CeN powder prepared in example 2.
Detailed Description
The invention provides a preparation method of rare earth element carbide, nitride or carbonitride powder, which comprises the following steps:
(1) Mixing rare earth element oxide, carbon black and a liquid phase medium, and sequentially performing ball milling, drying and hydrogenation treatment to obtain hydrotreated powder;
(2) And carrying out carbothermic reduction reaction on the hydrotreated powder under the atmosphere condition to obtain rare earth carbide, nitride or carbonitride powder.
In the present invention, the molar ratio of the rare earth element oxide to the carbon black in the step (1) is 1:3 to 10, preferably 1:4 to 9, and more preferably 1:5 to 8; the rare earth element oxide contains cerium oxide, yttrium oxide, or lanthanum oxide, preferably cerium oxide, yttrium oxide, and more preferably cerium oxide.
In the present invention, the liquid phase medium in the step (1) comprises water, absolute ethanol, acetone or cyclohexane, preferably water, absolute ethanol or acetone, and more preferably water or absolute ethanol; wherein the ratio of the volume of the liquid phase medium to the mass sum of the rare earth element oxide and the carbon black is 7-10 ml:1-3 g, preferably 8-9 ml:2g.
In the invention, the ball-material ratio in the ball milling treatment in the step (1) is 5-20:1, preferably 10-15:1, and more preferably 12:1; the rotation speed of the ball milling is 200-400 r/min, preferably 250-350 r/min, and more preferably 300r/min; the ball milling time is 2 to 24 hours, preferably 6 to 20 hours, more preferably 10 to 16 hours.
In the present invention, the temperature of the drying treatment in the step (1) is 60 to 100 ℃, preferably 70 to 90 ℃, and more preferably 80 ℃; the time is 2 to 10 hours, preferably 4 to 8 hours, more preferably 6 hours.
In the present invention, the hydrogenation treatment in the step (1) is performed under a hydrogen atmosphere, and the temperature of the hydrogenation treatment is 500 to 1200 ℃, preferably 600 to 1100 ℃, and more preferably 700 to 1000 ℃; the hydrogenation treatment time is 1 to 4 hours, preferably 2 to 3 hours, and more preferably 2.5 hours; the flow rate of the gas during the hydrogenation treatment is 100 to 1000ml/min, preferably 200 to 900ml/min, and more preferably 300 to 800ml/min.
In the present invention, the flow rate of the gas at the time of carbothermic reaction in the step (2) is 100 to 1000ml/min, preferably 200 to 900ml/min, and more preferably 300 to 800ml/min.
In the present invention, the carbothermic reaction in the step (2) has a temperature of 1300 to 2200 ℃, preferably 1400 to 2100 ℃, and more preferably 1500 to 2000 ℃; the carbothermic reaction time is 2 to 6 hours, preferably 2.5 to 5.5 hours, and more preferably 3 to 5 hours.
The carbothermic reduction reaction of the step (2) is carried out under an argon atmosphere when preparing the rare earth carbide.
The carbothermic reduction reaction of the step (2) is carried out under nitrogen atmosphere when preparing the rare earth element nitride.
The carbothermal reduction reaction in the step (2) is carried out in an atmosphere of argon and nitrogen in the preparation of rare earth element carbonitride, wherein the flow rate ratio of the argon to the nitrogen is 1:0.1-10, preferably 1:1-9, and more preferably 1:2-8.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
9.566g of nano cerium oxide powder and 4.095g of nano carbon black powder are weighed, 80ml of deionized water is measured, the nano powder and deionized water are put into a ball milling tank for ball milling treatment, wherein the ball material ratio is 10:1 during ball milling treatment, the rotating speed is 300r/min, and the ball milling is carried out for 12 hours. Pouring out the mixture after ball milling treatment, and drying at 80 DEG C4h, grinding for 10min again, putting the mixed powder into an alumina crucible, putting the crucible into a BTF-1200C tubular furnace, and introducing 99.999% high-purity hydrogen at a gas flow rate of 400ml/min for hydrogenation treatment, wherein the hydrogenation treatment temperature is 900 ℃ for 1h, so as to obtain the hydrogenated powder. Then placing the hydrotreated powder into a BTF-1600C high-temperature tube furnace, introducing 99.999% high-purity argon gas at a gas flow rate of 800ml/min to perform carbothermic reaction, wherein the carbothermic reaction temperature is 1550 ℃ and the time is 6h, thus obtaining high-purity single-phase nanoscale CeC 2 And (3) powder.
FIG. 2 is CeC 2 XRD pattern of powder, FIG. 3 is CeC 2 SEM image of powder, ceC prepared in example 1 2 The carbon content in the powder is 25.09wt% and the oxygen content is 0.8972wt%, so that the powder is spherical-like nano-scale powder with regular morphology.
Example 2
20.010g of nano cerium oxide powder and 8.383g of nano carbon black powder are weighed, 90ml of deionized water is measured, the nano powder and deionized water are put into a ball milling tank for ball milling treatment, wherein the ball material ratio is 5:1 during ball milling treatment, the rotating speed is 400r/min, and the ball milling is carried out for 6 hours. Pouring out the mixture after ball milling treatment, drying for 8 hours at 100 ℃, manually grinding for 20 minutes, putting the mixed powder into an alumina crucible, putting the crucible into a BTF-1200C tubular furnace, and introducing 99.999% high-purity hydrogen at a gas flow rate of 600ml/min for hydrogenation treatment, wherein the hydrogenation treatment temperature is 1000 ℃ and the time is 2 hours, thus obtaining the hydrogenated powder. And placing the hydrogenated powder into a high-temperature tube furnace with BTF-1600C, and introducing 99.999% high-purity nitrogen at a gas flow rate of 600ml/min to perform carbothermal reduction nitridation reaction, wherein the carbothermal reduction nitridation reaction is performed at a temperature of 1500 ℃ for 4 hours, so as to obtain high-purity single-phase nano-scale CeN powder.
FIG. 4 shows the XRD pattern of CeN powder and FIG. 5 shows the SEM pattern of CeN powder, and CeN powder prepared in example 2 has nitrogen content of 5.340wt% and oxygen content of 1.225wt% and is a morphology-regular, spheroid-like nanoscale powder.
Example 3
17.198g of nano cerium oxide powder and 6.006g of nano carbon black powder were weighed,100ml of deionized water is measured, nano powder and deionized water are put into a ball milling tank for ball milling treatment, wherein the ball material ratio is 12:1 during ball milling treatment, the rotating speed is 200r/min, and the ball milling is carried out for 12 hours. Pouring out the mixture after ball milling treatment, drying for 10 hours at 60 ℃, manually grinding for 15 minutes, putting the mixed powder into an alumina crucible, putting the crucible into a BTF-1200C tubular furnace, and introducing 99.999% high-purity hydrogen at a gas flow rate of 1000ml/min for hydrogenation treatment, wherein the hydrogenation treatment temperature is 800 ℃ for 4 hours, thus obtaining the hydrogenated powder. Then placing the hydrotreated powder into a high-temperature tube furnace with BTF-1600℃, introducing 99.999% of high-purity nitrogen gas and 99.999% of high-purity argon gas at a gas flow rate of 1000ml/min for carbothermic reduction nitridation reaction, wherein the gas flow rate ratio of the nitrogen gas to the argon gas is 1:6, and the carbothermic reduction nitridation reaction is carried out at a temperature of 1600 ℃ for 2 hours to obtain nanoscale CeN 0.59 C 0.10 A spheroid-like powder.
From the above examples, the present invention provides a method for preparing rare earth element carbide, nitride or carbonitride powder, comprising mixing rare earth element oxide, carbon black and a liquid medium, sequentially performing ball milling, drying and hydrogenation treatment to obtain hydrotreated powder, and performing carbothermal reduction reaction on the hydrotreated powder under an atmosphere condition to obtain rare earth element carbide, nitride or carbonitride powder. The rare earth element carbide, nitride or carbonitride powder prepared by the method is high-purity spherical-like nanoscale powder, the carbothermal reduction reaction temperature is low, the reaction time is short, and the energy is saved.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. A method for preparing rare earth carbide, nitride or carbonitride powder, comprising the steps of:
(1) Mixing rare earth element oxide, carbon black and a liquid phase medium, and sequentially performing ball milling, drying and hydrogenation treatment to obtain hydrotreated powder;
(2) Carrying out carbothermic reduction reaction on the hydrotreated powder under the atmosphere condition to obtain rare earth element carbide, nitride or carbonitride powder;
the hydrogenation treatment in the step (1) is carried out under the hydrogen atmosphere, the temperature of the hydrogenation treatment is 500-1200 ℃, the time of the hydrogenation treatment is 1-4 h, and the flow rate of gas during the hydrogenation treatment is 100-1000 ml/min;
the temperature of the carbothermic reaction in the step (2) is 1300-1600 ℃, and the carbothermic reaction time is 2-6 h.
2. The method for producing a rare earth element carbide, nitride or carbonitride powder according to claim 1, wherein the molar ratio of the rare earth element oxide to the carbon black in the step (1) is 1: 3-10, wherein the rare earth element oxide comprises cerium oxide, yttrium oxide or lanthanum oxide.
3. The method for producing a rare earth element carbide, nitride or carbonitride powder according to claim 2, wherein the liquid-phase medium in the step (1) comprises water, absolute ethyl alcohol, acetone or cyclohexane, and wherein the ratio of the volume of the liquid-phase medium to the mass sum of the rare earth element oxide and carbon black is 7 to 10ml: 1-3 g.
4. The method for preparing rare earth element carbide, nitride or carbonitride powder according to claim 3, wherein the ball-milling treatment in the step (1) is carried out at a ball-milling speed of 200-400 r/min and a ball-milling time of 2-24 h, wherein the ball-material ratio is 5-20:1.
5. The method for producing a rare earth element carbide, nitride or carbonitride powder according to any one of claims 1 to 4, wherein the drying treatment in step (1) is carried out at a temperature of 60 to 100℃for a period of 2 to 10 hours.
6. The method for producing a rare earth element carbide, nitride or carbonitride powder according to claim 1, wherein the flow rate of the gas at the time of carbothermal reduction in the step (2) is 100 to 1000ml/min.
7. The method for producing a rare earth element carbide, nitride or carbonitride powder according to claim 6, wherein said step (2) of carbothermal reduction reaction is carried out under an argon atmosphere in producing a rare earth element carbide.
8. The method for producing a rare earth element carbide, nitride or carbonitride powder according to claim 6, wherein the carbothermal reduction reaction in the step (2) is carried out under a nitrogen atmosphere in the production of the rare earth element nitride.
9. The method for producing a rare earth element carbide, nitride or carbonitride powder according to claim 6, wherein the carbothermal reduction reaction in step (2) is performed under an atmosphere of argon and nitrogen, wherein the flow rate ratio of argon to nitrogen is 1:0.1 to 10.
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