CN117735494A - Preparation method of high-purity submicron lanthanum nitride powder - Google Patents
Preparation method of high-purity submicron lanthanum nitride powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 69
- QCLQZCOGUCNIOC-UHFFFAOYSA-N azanylidynelanthanum Chemical compound [La]#N QCLQZCOGUCNIOC-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 57
- 239000011733 molybdenum Substances 0.000 claims abstract description 57
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 34
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000004321 preservation Methods 0.000 claims abstract description 15
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 abstract description 12
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000000975 dye Substances 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 238000002844 melting Methods 0.000 description 14
- 230000008018 melting Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- 239000012535 impurity Substances 0.000 description 12
- 238000005121 nitriding Methods 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910000497 Amalgam Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001640 fractional crystallisation Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- NUXZAAJDCYMILL-UHFFFAOYSA-K trichlorolanthanum;hydrate Chemical compound O.Cl[La](Cl)Cl NUXZAAJDCYMILL-UHFFFAOYSA-K 0.000 description 1
Abstract
The invention provides a preparation method of high-purity submicron lanthanum nitride powder, which comprises the following steps: putting metal lanthanum powder particles into a molybdenum boat, putting the molybdenum boat into sintering equipment, heating to 1000 ℃ under the condition of vacuumizing, and preserving heat for 2-3 hours; then cooling to 300-400 ℃, preserving heat for 1-2 hours, and introducing H in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, in circulation N 2 Heating to 850-1100 ℃ under the atmosphere condition, and preserving heat for 2-8 hours; and after the heat preservation is finished, naturally cooling to room temperature, taking out the product, crushing and sieving to obtain the high-purity submicron lanthanum nitride powder. The invention has simple preparation process, low operation cost and wide process window, the particle size of the obtained powder is 0.01-1 mu m, the purity is more than 99.99 percent, and the invention is suitable for large-scale industrial production, and the prepared lanthanum nitride powder is used in magnetic materials, hydrogen energy catalysts, semiconductor devices, electronic products, dyes and steelAnd the like.
Description
Technical Field
The invention relates to lanthanum nitride and a preparation method thereof, in particular to a preparation method of high-purity submicron lanthanum nitride powder.
Background
Rare earth elements are praised as a new material treasury in the 21 st century, and the application is relatively wide. Rare earth elements generally have similar electron structures and characteristics with 4f orbitals, whereas lanthanum is different from other rare earth elements, with zero electrons in the 4f orbitals. Therefore, lanthanum has stronger affinity to hydrogen, oxygen and nitrogen than rare earth elements such as cerium, europium and the like, and is not easy to separate and purify. The main impurities in lanthanum are: o, fe, si, ni, mn, al, among others, the O and Fe content is the largest. The rare earth elements are separated by the methods of fractional crystallization and fractional precipitation, but the separation method needs 15 times of recrystallization to ensure that the purity of the lanthanum metal reaches 99.98 percent, has low production efficiency, is difficult to realize continuous operation and is not suitable for industrial production. At present, the common separation process of lanthanum metal in China is a sulfuric acid method and an extraction separation method, and although the operation is simpler, the purity of the lanthanum metal obtained by the method is generally higher, the content of Fe impurities is higher, and the special requirements of high-performance rare earth functional materials are difficult to meet.
Lanthanum nitride is an inorganic compound, has a chemical formula of Lan, has a particle size mostly of the order of microns, is stable at high temperature, and can be used as a high-temperature structural material. The submicron lanthanum nitride powder has higher optical and electronic properties and thermal stability compared with micron lanthanum nitride powder due to larger specific surface area and dispersibility, and is widely applied in the fields of magnetic materials, hydrogen energy catalysts, semiconductor devices, electronic products, dyes, steel and the like.
The common lanthanum chloride hydrate for industrially preparing lanthanum nitride is reduced by using metal calcium after dehydration, or is prepared by melting anhydrous lanthanum chloride and then electrolyzing, or is prepared by mixing lanthanum and mercury to prepare amalgam, and then nitriding reaction is carried out after the amalgam is obtained to obtain lanthanum nitride; or direct nitrogen in an ammonia atmosphereAnd (5) lanthanum metal is subjected to lanthanum melting to obtain lanthanum nitride. However, these preparation methods are complicated in process and are not suitable for large-scale industrial production. Chinese patent CN 101618865a discloses a metal lanthanum nitride powder and a preparation method thereof, which uses nano rare earth dysprosium or nano rare earth metal to hydrogenate macum and N respectively 2 The lanthanum nitride powder is prepared by direct reaction, however, the lanthanum nitride powder obtained by the method has higher requirements on raw materials, and the obtained lanthanum nitride has poorer crystallinity.
Disclosure of Invention
The invention aims to provide high-purity submicron lanthanum nitride powder and a preparation method thereof, so as to solve the problems of low purity and complex process of the lanthanum nitride powder prepared by the prior art.
The invention aims at realizing the following technical scheme:
the invention provides submicron lanthanum nitride powder, the particle size of the powder is 0.01-1 mu m, and the purity is more than or equal to 99.99%.
The preparation method of the high-purity submicron lanthanum nitride powder comprises the following steps:
putting metal lanthanum powder particles into a molybdenum boat, putting the molybdenum boat into sintering equipment, vacuumizing to-0.1 Mpa, heating to 1000 ℃, and preserving heat for 2-3h; then cooling to 300-400 ℃, preserving heat for 1-2 hours, and introducing H in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, in circulation N 2 Heating to 850-1100 ℃ under the atmosphere condition, and preserving heat for 2-8 hours; and after the heat preservation is finished, naturally cooling to room temperature, taking out the product, crushing and sieving to obtain the high-purity submicron lanthanum nitride powder.
The molybdenum boat is a three-layer molybdenum boat, the uppermost layer and the lowermost layer of the molybdenum boat are both molybdenum plates, the molybdenum plates on the uppermost layer are provided with uniform holes, and the middle layer is a screen; the lanthanum metal powder particles are positioned at the uppermost layer of the molybdenum boat.
Further, the particle size of the lanthanum metal powder particles is 3-10mm.
Further, the diameter of the hole on the molybdenum plate at the uppermost layer of the molybdenum boat is 0.1-2mm; the screen mesh of the middle layer consists of molybdenum wires, and the aperture is 200-500 meshes.
Further, the heating rate of the temperature to 1000 ℃ is 30-50 ℃/min; the cooling rate for cooling to 300-400 ℃ is 10-30 ℃/min; the heating rate to 850-1100 ℃ is 5 ℃/min.
Further, the H 2 And NH 3 In the mixed gas of (2), H 2 With NH 3 The volume ratio of (1-5): (5-9), the flow rate is controlled to be 0.5-1.5L/min.
Further, the N is 2 The flow rate of the catalyst is controlled to be 5-10L/h.
Further, the crushing is performed in a vacuum vibration mill.
The invention has the beneficial effects that:
the invention provides a preparation method of high-purity submicron lanthanum nitride powder, which is simple, easy to operate, low in cost, wide in process window and suitable for large-scale industrial production. The lanthanum nitride powder prepared by the method has the particle size of 0.01-1 mu m and the purity of more than 99.99 percent, and can be widely applied to the fields of magnetic materials, hydrogen energy catalysts, semiconductor devices, electronic products, dyes, steel and the like.
The method has no strict requirement on the grain size of the raw materials, and the metal lanthanum powder with the grain size of 3-10mm can be used. In the preparation process, high-temperature sintering at 1000 ℃ is firstly carried out after vacuumizing, so that impurities such as oxygen, greasy dirt and the like attached to the surface of the raw material are effectively removed. The high-temperature sintering process at 1000 ℃ is creatively selected to be carried out in the three-layer molybdenum crucible, because the upper layer and the middle layer of the three-layer molybdenum crucible are provided with holes or screens, molten lanthanum ingots (because the melting point of metal lanthanum is 920 ℃, the sintering temperature is 1000 ℃ and exceeds the melting point of the lanthanum ingots, the lanthanum ingots are molten to form molten state) can be filtered from the upper layer to the lower layer of the molybdenum crucible in a fluid form, fe impurities (melting point 1535 ℃), si impurities (melting point 1410 ℃), mn impurities (1246 ℃) and the like with higher melting points are retained in the upper layer of the crucible, so that the impurities such as Fe, si, mn and the like with higher melting points are effectively removed, and the purity of the final product lanthanum nitride powder is improved to a certain extent. In addition, after high-temperature sintering, the method of the invention also carries out cooling, and mixed gas of hydrogen and ammonia is introduced in the sintering process, the cooling process can cause the aggregation of molten lanthanum metal, and along with the introduction of the mixed gas of hydrogen and ammonia, the aggregated lanthanum metal can react with the hydrogen and the ammonia to generate hydrogen crushing phenomenon, so that the raw materials are more beneficial to the later nitridation, the nitridation rate and the purity of lanthanum nitride powder are improved, and the ductility of the metal block after hydrogen crushing is reduced, the brittleness is increased, the later crushing treatment is more beneficial to the reduction of the particle size of the powder, and the powder particles reach submicron level.
Drawings
Fig. 1 is an XRD pattern of lanthanum nitride prepared in example 1.
Fig. 2 is an SEM image of lanthanum nitride prepared in example 1.
Detailed Description
The following examples serve to further illustrate the invention in detail, but do not limit it in any way.
Example 1
The preparation method of the high-purity submicron lanthanum nitride powder comprises the following steps:
putting 3-10mm metal lanthanum powder particles into a three-layer molybdenum boat (the uppermost layer and the lowermost layer of the molybdenum boat are molybdenum plates, the uppermost layer molybdenum plates are provided with holes with the diameter of 2mm; the screen mesh of the middle layer is composed of molybdenum wires, the aperture is 200 meshes), putting the molybdenum boat into sintering equipment, vacuumizing to-0.1 Mpa, heating to 1000 ℃ at the speed of 50 ℃/min, and preserving heat for 3 hours; then cooling to 400 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and introducing H with the volume ratio of 3:7 at the air flow of 1L/min in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, at N 2 Heating to 900 ℃ at a speed of 5 ℃/min under the atmosphere condition with the flow of 8L/h, and sintering for 4 hours; and after sintering, naturally cooling to room temperature, taking out a product, putting the product into a vacuum vibration mill for crushing, and sieving to obtain the high-purity submicron lanthanum nitride powder.
Nitriding ratio = actual weight gain/theoretical weight gain.
The nitriding rate of the lanthanum nitride powder prepared by the method is calculated to be 100 percent according to the formula, XRD of the lanthanum nitride powder is tested, and XRD test results are compared with lanthanum nitride standard cards, and the results are shown in figure 1, so that the lanthanum nitride powder is pure-phase LaN. As can be seen from the ICP test results in table 1, the purity of the lanthanum nitride powder was 99.99%. As shown in FIG. 2, which is an SEM image of lanthanum nitride powder, it can be seen that the particle size of the lanthanum nitride powder is 0.01-1. Mu.m.
Example 2
The preparation method of the high-purity submicron lanthanum nitride powder comprises the following steps:
putting 3-10mm metal lanthanum powder particles into a three-layer molybdenum boat (the uppermost layer and the lowermost layer of the molybdenum boat are molybdenum plates, the uppermost layer molybdenum plates are provided with holes with the diameter of 2mm; the screen mesh of the middle layer is composed of molybdenum wires, the aperture is 200 meshes), putting the molybdenum boat into sintering equipment, vacuumizing to-0.1 Mpa, heating to 1000 ℃ at the speed of 30 ℃/min, and preserving heat for 2 hours; then cooling to 300 ℃ at a speed of 30 ℃/min, preserving heat for 1 hour, and introducing H with a volume ratio of 1:5 at a gas flow of 0.5L/min in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, at N 2 Heating to 850 ℃ at a speed of 5 ℃/min under the atmosphere condition with the flow of 10L/h, and preserving heat for 8 hours; and after the heat preservation is finished, naturally cooling to room temperature, taking out a product, putting the product into a vacuum vibration mill for crushing, and sieving to obtain the high-purity submicron lanthanum nitride powder. The detection shows that the particle size of the lanthanum nitride powder is 0.01-1 mu m, the nitriding rate is 99%, and the purity is 99.5%.
Example 3
The preparation method of the high-purity submicron lanthanum nitride powder comprises the following steps:
putting 3-10mm metal lanthanum powder particles into a three-layer molybdenum boat (the uppermost layer and the lowermost layer of the molybdenum boat are molybdenum plates, the uppermost layer molybdenum plates are provided with holes with the diameter of 2mm; the screen mesh of the middle layer is composed of molybdenum wires, the aperture is 200 meshes), putting the molybdenum boat into sintering equipment, vacuumizing to-0.1 Mpa, heating to 1000 ℃ at the speed of 30 ℃/min, and preserving heat for 2 hours; then cooling to 300 ℃ at a speed of 30 ℃/min, preserving heat for 1 hour, and introducing H with a volume ratio of 5:9 at a gas flow of 1.5L/min in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, at N 2 Under the atmosphere condition with the flow of 5L/h, heating to 1100 ℃ at the speed of 5 ℃/min, and preserving heat for 2 hours; and after the heat preservation is finished, naturally cooling to room temperature, taking out a product, putting the product into a vacuum vibration mill for crushing, and sieving to obtain the high-purity submicron lanthanum nitride powder. Through the detection, the detection results show that,the grain diameter of the lanthanum nitride powder is 0.01-1 mu m, the nitriding rate is 100%, and the purity is 99.96%.
Example 4
Putting 3-10mm metal lanthanum powder particles into a three-layer molybdenum boat (the uppermost layer and the lowermost layer of the molybdenum boat are molybdenum plates, the uppermost layer molybdenum plates are provided with holes with the diameter of 0.1mm, a screen mesh of the middle layer is composed of molybdenum wires, the aperture is 500 meshes), putting the molybdenum boat into sintering equipment, vacuumizing to-0.1 Mpa, heating to 1000 ℃ at the speed of 50 ℃/min, and preserving heat for 3 hours; then cooling to 400 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and introducing H with the volume ratio of 3:7 at the air flow of 1L/min in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, at N 2 Heating to 900 ℃ at a speed of 5 ℃/min under the atmosphere condition with the flow of 8L/h, and sintering for 4 hours; and after sintering, naturally cooling to room temperature, taking out a product, putting the product into a vacuum vibration mill for crushing, and sieving to obtain the high-purity submicron lanthanum nitride powder. The detection shows that the particle size of the lanthanum nitride powder is 0.01-0.05 mu m, the nitriding rate is 100%, and the purity is 99.995%.
Comparative example 1
The preparation method of the high-purity submicron lanthanum nitride powder is the same as that of the embodiment 1, except that the three-layer molybdenum boat in the embodiment 1 is replaced by a common crucible.
The nitriding rate of lanthanum nitride prepared by the method of this example was calculated to be 97% by the same method.
Comparative example 2
Placing 3-10mm metal lanthanum powder particles into a common crucible, placing the crucible into sintering equipment, heating to 400 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and introducing H with the volume ratio of 3:7 at the air flow of 1L/min in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, at N 2 Heating to 900 ℃ at a speed of 5 ℃/min under the atmosphere condition with a flow of 5L/h, and preserving heat for 4 hours; and after the heat preservation is finished, naturally cooling to room temperature, taking out a product, and crushing and sieving under an inert gas environment to obtain the high-purity submicron lanthanum nitride powder.
The lanthanum nitride prepared by the method of this example was calculated as in example 1 to have a nitriding rate of 95%.
Comparative example 3
Placing 3-10mm metal lanthanum powder particles into a three-layer molybdenum boat, placing the molybdenum boat into sintering equipment, vacuumizing to 0.1Mpa, heating to 1000 ℃ at a speed of 50 ℃/min, and preserving heat for 3 hours; then cooling to 400 ℃ at a speed of 10 ℃/min, and preserving heat for 2 hours; thereafter, at N 2 Heating to 900 ℃ at a speed of 5 ℃/min under the atmosphere condition with the flow rate of 8L/h, and preserving heat for 4 hours; and after the heat preservation is finished, naturally cooling to room temperature, taking out a product, putting the product into a vacuum vibration mill for crushing, and sieving to obtain the high-purity submicron lanthanum nitride powder.
The lanthanum nitride prepared by the method of this example was calculated as in example 1 to have a nitriding rate of 85%.
ICP testing was performed on example 1, comparative example 1 and comparative example 2, respectively, and the test results are shown in table 1.
TABLE 1 ICP detection results
As can be seen from the ICP test results shown in table 1, the O content and the Fe content in the lanthanum nitride powder prepared in example 1 were significantly lower than those in the lanthanum nitride powders prepared in comparative examples 1 and 2. This is because in the preparation method of example 1, high temperature sintering at 1000 ℃ is performed after evacuation, and the process is performed in a three-layer molybdenum crucible, on the one hand, the high temperature sintering can effectively remove oxygen impurities contained in lanthanum ingots; on the other hand, as the melting point of lanthanum is 920 ℃ and the sintering temperature is 1000 ℃ exceeds the melting point of lanthanum ingot, the lanthanum ingot is melted to form a molten state, holes or screens are formed in the upper layer and the middle layer of the three-layer molybdenum crucible, and the molten state lanthanum ingot is filtered from the upper layer to the lower layer of the molybdenum crucible in a fluid form, so that Fe impurities (melting point 1535 ℃) Si impurities (melting point 1410 ℃) Mn impurities (1246 ℃) with higher melting point are retained in the upper layer of the crucible, the effect of effectively removing Fe/Si/Mn impurities with higher melting point and the like is achieved, and high-purity lanthanum nitride powder is obtained.
Claims (8)
1. The high-purity submicron lanthanum nitride powder is characterized in that the particle size is 0.01-1 mu m, and the purity is more than or equal to 99.99%.
2. The preparation method of the high-purity submicron lanthanum nitride powder is characterized by comprising the following steps of:
putting metal lanthanum powder particles into a molybdenum boat, putting the molybdenum boat into sintering equipment, vacuumizing to-0.1 Mpa, heating to 1000 ℃, and preserving heat for 2-3h; then cooling to 300-400 ℃, preserving heat for 1-2 hours, and introducing H in the heat preservation process 2 And NH 3 Is a mixed gas of (a) and (b); thereafter, in circulation N 2 Heating to 850-1100 ℃ under the atmosphere condition, and preserving heat for 2-8 hours; after the heat preservation is completed, naturally cooling to room temperature, taking out the product, crushing and sieving to obtain high-purity submicron lanthanum nitride powder;
the molybdenum boat is a three-layer molybdenum boat, the uppermost layer and the lowermost layer of the molybdenum boat are both molybdenum plates, the molybdenum plates on the uppermost layer are provided with uniform holes, and the middle layer is a screen; the lanthanum metal powder particles are positioned at the uppermost layer of the molybdenum boat.
3. The method for preparing high-purity submicron lanthanum nitride powder according to claim 1, wherein the particle size of the lanthanum metal powder particles is 3-10mm.
4. The method for preparing high-purity submicron lanthanum nitride powder according to claim 1, wherein the diameter of the holes on the molybdenum plate on the uppermost layer of the molybdenum boat is 0.1-2mm; the screen mesh of the middle layer consists of molybdenum wires, and the aperture is 200-500 meshes.
5. The method for preparing high-purity submicron lanthanum nitride powder according to claim 1, characterized in that the heating rate to 1000 ℃ is 30-50 ℃/min; the cooling rate for cooling to 300-400 ℃ is 10-30 ℃/min; the heating rate to 850-1100 ℃ is 5 ℃/min.
6. The method for preparing high-purity submicron lanthanum nitride powder according to claim 1, wherein the H 2 And NH 3 In the mixed gas of (2), H 2 With NH 3 The volume ratio of (1-5): (5-9), the flow rate is controlled to be 0.5-1.5L/min.
7. The method for preparing high-purity submicron lanthanum nitride powder according to claim 1, wherein the N is 2 The flow rate of the catalyst is controlled to be 5-10L/h.
8. The method for preparing high-purity submicron lanthanum nitride powder according to claim 1, wherein the crushing is performed in a vacuum vibration mill.
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