CN113564690A - Method for purifying lanthanum hexaboride - Google Patents
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- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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Abstract
The invention provides a method for purifying lanthanum hexaboride, which comprises the following steps: (1) purifying lanthanum hexaboride raw material powder for the first time in induction plasma spheroidizing equipment; (2) placing the powder obtained in the step (1) in a discharge plasma furnace, uniformly discharging among powder particles by using pulse current, and carrying out secondary purification on the lanthanum hexaboride powder to obtain a lanthanum hexaboride material rod; (3) and (3) placing the lanthanum hexaboride bar obtained in the step (2) into an optical zone melting furnace, locally melting the material, cutting off two ends after zone melting, and carrying out zone melting for one or more times to obtain the high-purity lanthanum hexaboride cathode material. The thermal emission performance of the lanthanum hexaboride cathode material obtained after purification by the method is obviously improved, so that the application of the cathode material in future vacuum devices with high power and long service life becomes possible.
Description
Technical Field
The invention belongs to the technical field of preparation of thermode materials. In particular to a method for purifying lanthanum hexaboride by combining an induction plasma technology, a discharge plasma technology and a zone melting technology.
Background
Lanthanum hexaboride has CsCl structure, La atom is cubic-symmetric eight B6The octahedron is tightly surrounded. This structure makes LaB6The cathode material has the characteristics of high melting point, high conductivity, good chemical stability, low work function, large emission current density, good ion bombardment resistance and the like, is an excellent cathode material, and is widely applied to the national defense and civil high-technology fields of satellites, deep space exploration, electron beam processing, 3D printing, nuclear energy, plasma sources, electron microscopes and the like. With the rapid development of large-scale precise electronic analysis instruments, cathodes are required to have higher brightness and longer service life. This requires the development of lanthanum hexaboride cathode materials with high current densities. Research shows that the most effective way to improve the material performance is to continuously improve the purity of lanthanum hexaboride. Currently commercially available LaB6The powder is generally prepared by adopting a boron thermal reduction method and a boron carbide reduction method, however, the powder obtained by the two techniques inevitably contains impurities such as Fe, Ca, BO and the like, and even if the impurities are subjected to acid-base cleaning, the effect is still not obvious. The presence of the above impurities greatly weakens LaB6The cathode has mechanical property and emission property, so that lanthanum hexaboride needs to be purified, the performance of the lanthanum hexaboride is improved, and a foundation is laid for the development of high-power and long-life vacuum devices in China.
CN108048907A discloses a preparation method of a large-size and high-performance lanthanum hexaboride single crystal, which combines a spark plasma sintering technology and an optical zone melting technology. Although lanthanum hexaboride prepared in CN108048907A has a large size, some impurities that are difficult to remove still exist in the prepared lanthanum hexaboride crystal, thereby affecting the physical properties and emission properties of lanthanum hexaboride.
Therefore, a technique capable of further purifying lanthanum hexaboride crystals is in demand.
The induction plasma spheroidizing technology is a new technology for forming spherical powder in recent years, and the principle of the technology is as follows: the powder is fed into a plasma torch through a carrier gas, powder particles are rapidly heated in a plasma high-temperature area, the surface (or the whole) of the powder particles is instantly melted to form liquid drops after the powder particles rapidly absorb heat, the liquid drops shrink into spheres under the action of surface tension, and the spheres are fixed after the liquid drops enter a cooling chamber and are rapidly condensed and solidified, so that the spherical powder is obtained. Induction plasma spheronization is considered one of the most effective means to obtain dense, regular spherical particles. An important application area of induction plasma spheronization technology is metal 3D printing.
The inventor creatively discovers that lanthanum hexaboride and impurity elements can be effectively stripped in the process of the induction plasma spheroidization technology due to different surface tensions of different materials. In addition, the ultra-high temperature generated by the plasma torch can also volatilize impurity elements with low melting points, thereby achieving the effect of powder purification.
The present invention has been made based on the above findings.
Disclosure of Invention
Technical problem
The invention aims to solve the problem of the existing LaB6The problem that the purity of cathode material is not high so as to influence the thermal emission performance is solved, and the preparation of high-purity LaB6Cathode material method.
Technical scheme
The invention specifically provides a method for purifying lanthanum hexaboride, which is characterized by comprising the following steps:
(1) purifying lanthanum hexaboride raw material powder for the first time in induction plasma spheroidizing equipment;
(2) placing the powder obtained in the step (1) in a discharge plasma furnace, uniformly discharging among powder particles by using pulse current (direct current), and carrying out secondary purification on lanthanum hexaboride powder under vacuum to obtain a lanthanum hexaboride material rod;
(3) and (3) placing the lanthanum hexaboride bar obtained in the step (2) into an optical zone melting furnace, locally melting the material, cutting off two ends after zone melting, and carrying out zone melting for one or more times to obtain the lanthanum hexaboride cathode material.
In the step (1), the purification in the induction plasma spheroidizing device means that powder particles are melted by using a plasma torch, and the particles are spheroidized by using the surface tension of the material after being melted; because the surface tension of different materials is different, lanthanum hexaboride and impurity elements can be effectively stripped in the induction plasma spheroidizing process. In addition, the ultra-high temperature generated by the plasma torch can also volatilize impurity elements with low melting points, so that the effect of purifying lanthanum hexaboride raw material powder is achieved;
in the step (2), the pulse wave generated by the discharge can break down the oxide thin film formed on the surface of the powder particle;
in the step (3), since the solute distribution coefficients of different materials are different in the floating-zone process, the impurity elements in lanthanum hexaboride can be intensively distributed at two ends of the sample in the floating-zone process, and the impurity elements can be removed by cutting off the two ends.
Preferably, the process parameters of the induction plasma spheroidizing device in the step (1) are as follows: the heating power is 10.0-16.0 kW; carrier gas flow: 2-5 slpm; the powder feeding speed is 4.0 g/min-7.33 g/min; the hydrogen pressure was 1.5X 104Pa, argon pressure 8.5X 104Pa; the powder feeding speed has obvious influence on the powder purification effect, and the spheroidization rate of the powder is gradually increased along with the reduction of the powder feeding speed, which means that the effect of plasma on the powder is enhanced, namely the purification effect of the powder is continuously improved.
However, when the powder feeding rate is higher than the above upper limit, the cleaning effect is not good; when the powder feeding rate is lower than the above lower limit, the increase of the purifying effect is not significant, and there is a problem that the production rate is decreased.
Preferably, the process parameters of the discharge plasma furnace in the step (2) are as follows: discharge current: 2000-5000A; voltage: 3-6V; time: 0.1-2 hours;
preferably, the process parameters of the optical zone melting furnace in the step (3): heating power: 10-15 kW, operation rate: 1-300 mm/h; flow rate of shielding gas: 2-8L/min; the gas pressure is: 0.1-1 MPa; number of zone-melting times: 2-3 times; more preferably, the shielding gas is one or more selected from the group consisting of argon, nitrogen and helium;
in the step (3), the heating source of the optical zone melting furnace may be a laser, a xenon lamp, an electron beam, an arc, or the like.
Wherein, the purity of the lanthanum hexaboride raw material powder is more than 98 wt%, preferably more than 99 wt%, and the purity of the lanthanum hexaboride cathode material obtained in the step (3) is more than 99.9 wt%, preferably more than 99.91 wt%.
Particularly preferably, the impurity Fe content in the lanthanum hexaboride cathode material obtained in step (3) is 0.0015 wt% or less and the Ca content is 0.0009 wt% or less, based on 100 wt% of the lanthanum hexaboride cathode material.
According to a second aspect of the present invention, there is provided a lanthanum hexaboride cathode material prepared by the method of purifying lanthanum hexaboride according to the present invention.
Preferably, the purity of the lanthanum hexaboride cathode material is 99.9 wt% or more, preferably 99.91 wt% or more.
Preferably, the impurity Fe content in the lanthanum hexaboride cathode material is less than 0.0015 wt%, and the Ca content is less than 0.0009 wt%.
Advantageous effects
(1) The invention applies the induction plasma spheroidization technology to the removal of impurity elements in powder, and realizes the purification of materials from the source; and the discharge plasma technology and the optical zone melting technology are combined in the preparation process of the cathode material, so that further purification is realized;
(2) the thermal emission performance of the purified lanthanum hexaboride cathode material is obviously improved, so that the application of the cathode material in future high-power and long-life vacuum devices becomes possible.
Drawings
Figure 1 is a graph showing XRD patterns in powders of lanthanum hexaboride starting material, lanthanum hexaboride prepared according to example 1 of the present invention, and a standard PDF card.
Fig. 2 is an SEM picture showing the microstructure of lanthanum hexaboride prepared in example 1.
Fig. 3 is a graph showing the thermal emission current density of lanthanum hexaboride single crystals prepared according to example 1 and comparative example 1 of the present invention, respectively.
Detailed Description
The present invention is further illustrated by the following specific examples. The following examples are intended only to illustrate the present invention and should not be construed as limiting the scope of the present invention.
Example 1
The lanthanum hexaboride is purified by using an induction plasma spheroidizing technology in combination with a discharge plasma technology and a zone melting technology, and the method comprises the following specific steps:
(1) about 200g of lanthanum hexaboride raw material powder (purchased from the rare earth research institute of Hunan, with a purity of 99.0 wt%) was weighed into a powder feeder of an induction plasma spheroidizing apparatus (TekNano 15kW, Canada), and the pressure of hydrogen and argon was adjusted, wherein the hydrogen pressure was 1.5X 104Pa, argon pressure 8.5X 104And Pa, turning on the radio frequency plasma and igniting, wherein the flow of the carrier gas is 4.0slpm, the power is increased to 14.1kW, and the powder feeding is started, and the powder feeding rate is 4.5 g/min. And after the powder feeding is finished, closing the plasma, introducing argon, cooling and taking out the powder.
(2) Putting the powder obtained in the step (1) into a graphite mold (the inner diameter: 25mm and the height: 80mm) in a discharge plasma furnace (LABOX-360, Japan), vacuumizing to below 5Pa, gradually increasing the current at the rate of 100A/min, keeping the voltage at 5V when the current reaches 2700A, keeping the temperature for 10min, then closing the current and the voltage, and cooling along with the furnace to obtain a material rod.
(3) Performing first zone melting purification by adopting an optical zone melting furnace, fixing the prepared material rods on an upper drawing rod and a lower drawing rod, ensuring that the upper material rod and the lower material rod are coaxial during fixing, installing a high-temperature-resistant and high-pressure-resistant quartz tube after the upper material rod and the lower material rod are fixed, and introducing and circulating high-purity argon as working gas, wherein the argon can play a role in protection and can inhibit volatilization of elements, the gas flow rate is 4.5L/min, and the gas pressure is 0.15 MPa; heating power: 12.5kW, the primary zone-melting speed of 20mm/h, the upper and lower charging bars rotate reversely at the rotating speed of 30 rpm; after zone-melting, the sample was cut at both ends.
(4) And (3) performing secondary zone melting purification by adopting an optical zone melting furnace, performing secondary zone melting purification by taking the material rod obtained by the primary zone melting purification as a feeding rod, wherein the secondary zone melting speed is 10mm/h, the feeding rod and the discharging rod rotate reversely at the rotating speed of 15rpm, and performing zone melting to obtain the high-purity lanthanum hexaboride cathode material.
High purity LaB prepared according to example 16The XRD spectrum of the compound is shown in figure 1. As can be seen from fig. 1: LaB prepared according to example 1 of the invention6The position of the diffraction peak is consistent with the XRD pattern of the standard PDF card, no shift and no new diffraction peak appear, which indicates that LaB before and after plasma spheroidization6All show pure LaB6And (4) phase(s). From fig. 2, it can be seen that no trace impurities were found under more microscopic vision.
The results of fig. 1 and 2 show that no new impurities are introduced by the purification carried out by the process of the invention.
Example 2
Lanthanum hexaboride was purified in the same manner as in example 1 except that the powder feeding rate in step (1) was adjusted to 7.00 g/min. The obtained LaB6The impurity contents of (a) are shown in table 1.
Comparative example 1
Lanthanum hexaboride was produced in the same manner as in example 1 except that the step (1) was omitted, and its impurity content was as shown in table 1.
Comparative example 2
LaB was purified in the same manner as in example 1, except that the feed rate in step (1) was 2.0g/min6Wherein the impurity content is shown in table 1.
TABLE 1 impurity content of lanthanum hexaboride single crystal
FIG. 3 shows a graph prepared according to example 1 and comparative example 1 of the present invention, respectivelyLaB6Thermal emission current density plot of single crystal. It can be seen that the reduction of Fe and Ca impurities can effectively promote LaB6Thermal emission properties of the single crystal.
Claims (10)
1. A method for purifying lanthanum hexaboride, which is characterized by comprising the following steps:
(1) purifying lanthanum hexaboride raw material powder for the first time in induction plasma spheroidizing equipment;
(2) placing the powder obtained in the step (1) in a discharge plasma furnace, uniformly discharging among powder particles by using pulse current, and carrying out secondary purification on the lanthanum hexaboride powder to obtain a lanthanum hexaboride material rod;
(3) and (3) placing the lanthanum hexaboride bar obtained in the step (2) into an optical zone melting furnace, locally melting the material, cutting off two ends after zone melting, and carrying out zone melting for one or more times to obtain the lanthanum hexaboride cathode material.
2. The method of claim 1,
the technological parameters of the induction plasma spheroidizing device in the step (1) are as follows: the heating power is 10.0-16.0 kW; carrier gas flow: 2-5 slpm; the powder feeding speed is 4.0 g/min-7.33 g/min.
3. The method according to claim 1 or 2,
the technological parameters of the discharge plasma furnace in the step (2) are as follows: discharge current: 2000-5000A; voltage: 3-6V; time: 0.1 to 2 hours.
4. The method according to any one of claims 1 to 3,
the process parameters of the optical zone melting furnace in the step (3) are as follows: heating power: 10-15 kW, operation rate: 1-300 mm/h; flow rate of shielding gas: 2-8L/min; number of zone-melting times: 2-3 times; preferably, the protective gas is one or more selected from the group consisting of argon, nitrogen and helium.
5. The method according to any one of claims 1 to 4,
in the step (3), the heating source of the optical zone melting furnace is selected from the group consisting of a laser, a xenon lamp, an electron beam, and an arc.
6. The method according to any one of claims 1 to 5,
the purity of the lanthanum hexaboride raw material powder is 98.0 wt% or more, preferably 99.0 wt% or more.
7. The method according to any one of claims 1 to 5,
the purity of the lanthanum hexaboride cathode material is more than 99.9 wt%, preferably more than 99.91 wt%.
8. The method according to any one of claims 1 to 6,
the impurity Fe content in the lanthanum hexaboride cathode material is less than 0.0015 wt% and the Ca content is less than 0.0009 wt% based on 100 wt% of the lanthanum hexaboride cathode material.
9. A lanthanum hexaboride cathode material prepared according to the method of any one of claims 1 to 8.
10. The lanthanum hexaboride cathode material of claim 9 wherein the lanthanum hexaboride cathode material has a purity of 99.9 wt.% or greater; preferably, the impurity Fe content in the lanthanum hexaboride cathode material is 0.0015 wt% or less and the Ca content is 0.0009 wt% or less, based on 100 wt% of the lanthanum hexaboride cathode material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394604A (en) * | 2022-01-20 | 2022-04-26 | 上海海事大学 | Preparation method of superhard spherical tungsten boride powder |
| CN114908422A (en) * | 2022-06-29 | 2022-08-16 | 合肥工业大学 | Strontium-doped lanthanum hexaboride single crystal and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61168597A (en) * | 1985-01-23 | 1986-07-30 | Hitachi Ltd | Method of growing single crystal of lanthanum hexaboride |
| JP2001002496A (en) * | 1999-06-17 | 2001-01-09 | Denki Kagaku Kogyo Kk | Single crystal of hexaboride of rare earth element and its preparation |
| CN108048907A (en) * | 2017-12-14 | 2018-05-18 | 合肥工业大学 | A kind of preparation method of large-size and high performance lanthanum hexaboride monocrystalline |
| CN112301412A (en) * | 2020-09-28 | 2021-02-02 | 湖南稀土金属材料研究院 | Rare earth boride single crystal preparation equipment and method |
-
2021
- 2021-07-08 CN CN202110774066.6A patent/CN113564690B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61168597A (en) * | 1985-01-23 | 1986-07-30 | Hitachi Ltd | Method of growing single crystal of lanthanum hexaboride |
| JP2001002496A (en) * | 1999-06-17 | 2001-01-09 | Denki Kagaku Kogyo Kk | Single crystal of hexaboride of rare earth element and its preparation |
| CN108048907A (en) * | 2017-12-14 | 2018-05-18 | 合肥工业大学 | A kind of preparation method of large-size and high performance lanthanum hexaboride monocrystalline |
| CN112301412A (en) * | 2020-09-28 | 2021-02-02 | 湖南稀土金属材料研究院 | Rare earth boride single crystal preparation equipment and method |
Non-Patent Citations (1)
| Title |
|---|
| 张宁等: "悬浮区域熔炼法制备REB6（LaB6、CeB6）单晶体及其表征", 《功能材料》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394604A (en) * | 2022-01-20 | 2022-04-26 | 上海海事大学 | Preparation method of superhard spherical tungsten boride powder |
| CN114394604B (en) * | 2022-01-20 | 2024-04-02 | 上海海事大学 | Preparation method of superhard spherical tungsten boride powder |
| CN114908422A (en) * | 2022-06-29 | 2022-08-16 | 合肥工业大学 | Strontium-doped lanthanum hexaboride single crystal and preparation method thereof |
| CN114908422B (en) * | 2022-06-29 | 2024-06-14 | 合肥工业大学 | Strontium doped lanthanum hexaboride monocrystal and preparation method thereof |
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