CN112974812B - High-combustion low-sensitivity rare earth alloy hydride material and preparation method thereof - Google Patents
High-combustion low-sensitivity rare earth alloy hydride material and preparation method thereof Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract
The invention discloses a high-combustion low-sensitivity rare earth alloy hydride material and a preparation method thereof, belonging to the technical field of energetic materials. The rare earth alloy hydride material is of a core-shell structure, the shell is a metal layer, and the core is rare earth alloy hydride; and the rare earth hydride in the rare earth aluminum alloy hydride is dispersed and distributed in the rare earth aluminum alloy. The invention does not need special process flow and complex treatment process, the light rare earth metal hydride is dispersed and distributed in the rare earth alloy second phase and is coated with the high combustion heat metal layer, and the invention has the characteristics of simple operation, easy reaching of experimental conditions, safety and reliability, and is convenient for later use.
Description
Technical Field
The invention belongs to the technical field of energetic materials, and particularly relates to a high-combustion low-sensitivity rare earth alloy hydride material and a preparation method thereof.
Background
The rare earth metal has strong chemical activity, and the application range of the rare earth metal is wider and wider from discovery to the present along with the development of scientific technology, and the rare earth metal is applied to various aspects of scientific research, daily life and the like. The rare earth metal can be used as a permanent magnet material with good performance, a catalyst in the processes of petroleum cracking and automobile exhaust treatment and an electric light source with good performance. The excellent characteristics and functions of rare earth metals are one of important research directions in the 21 st century, and the rare earth metal has good development and application prospects.
The rare earth metal hydride is widely applied to various fields of military affairs, civil use and energy and chemical industry due to the excellent performance of the rare earth metal hydride. The light rare earth metal hydride has extremely high energy, typically represents about 217.6MJ/kg of the energy of cerium hydride, is 40 times of the energy of cyclotetramethylenetetranitramine (HMX), and belongs to an ultra-high explosive additive. The light rare earth metal hydride is applied to the active material, so that the combustion heat energy of the active material can be improved, in addition, the cerium hydride has very high chemical reaction activity, ignition and detonation are easy to occur, and the energy density of the cerium hydride is high, so that the cerium hydride can be used as a high-energy additive in the explosion process of a better energetic material. Light rare earth metal hydrides are also one of the important additives for future new active materials.
Friction of energetic materials on hard surfaces is one of the major factors leading to their accidental explosions. Therefore, the friction sensitivity test is an essential part for optimizing the formula of the novel energetic material and improving the production environment, and is an important link for determining the influence of impurities or aging on the performance of the novel energetic material. The current methods for reducing the sensitivity of materials mainly comprise: the surface of the metal hydride is modified by adopting a special production process to reduce the sensitivity of the material (Liu Ji Ping, xiao Lu, metal hydride stability processing scheme, CN 201310293795.5); organic glue solution coating method (Zhang Weishan, research on preparation of light rare earth metal hydride active fragment and damage experiment, great thesis of Beijing university of science and technology). In order to prevent the light rare earth hydride from accidental spontaneous combustion, the conventional storage mode is that the light rare earth hydride is stored in a closed container in a sealed manner so as to isolate air and water.
Although the sensitivity of the light rare earth metal hydride can be reduced by the measures and the methods, the treatment process is complicated, the light rare earth metal hydride is still required to be taken out from a vessel or inert gas in later use, and the risk of oxidation and even spontaneous combustion caused by instantaneous contact with air still exists, so a series of problems of safety, use and the like are brought.
Disclosure of Invention
The invention aims to provide a high-combustion low-sensitivity rare earth alloy hydride material and a preparation method thereof, and the specific technical scheme is as follows:
a high-combustion low-sensitivity rare earth alloy hydride material is in a core-shell structure, wherein a shell is a metal layer, and a core is a rare earth alloy hydride; and the rare earth hydride in the rare earth aluminum alloy hydride is dispersed in the rare earth aluminum alloy.
Furthermore, the metal layer is made of a metal with high combustion heat, preferably Al, mg, cu, ni, ti, zr, cr or B; the thickness of the metal layer is 1-1000nm.
Furthermore, the metal material is coated on the surface of the rare earth aluminum alloy hydride by a physical vapor deposition method.
Wherein, the physical vapor deposition method comprises any one of magnetron sputtering and electron beam evaporation; the deposition process of magnetron sputtering is characterized in that the pre-vacuum degree is less than 5 multiplied by 10 -3 Pa, sputtering pressure of 0.1-1.0 Pa, sputtering power of 1-20 kW and deposition time of 0.1-10 h.
Further, the rare earth aluminum alloy hydride used as the core material is obtained by hydrogen disproportionation reaction of the rare earth aluminum alloy by hydrogen absorption.
Wherein, the rare earth aluminum alloy is powder with the grain diameter of-20 to +800 meshes; the hydrogen absorption condition is 0.1-5.0 MPa and 0-200 ℃.
The rare earth aluminum alloy is obtained by smelting rare earth and aluminum, wherein the rare earth is any one or more of La, ce, Y, dy, er, yb and Sm. The molar ratio of rare earth to aluminum in the rare earth aluminum alloy is 5:1 to 1:10, the smelting method is medium-frequency induction smelting, suspension smelting or electron beam smelting.
The preparation method of the rare earth alloy hydride material comprises the following steps:
(1) Smelting rare earth and aluminum to obtain rare earth aluminum alloy;
(2) Crushing the rare earth aluminum alloy obtained in the step (1) to-20- +800 meshes to obtain rare earth aluminum alloy powder;
(3) Absorbing hydrogen by the rare earth aluminum alloy powder obtained in the step (2) until the rare earth aluminum alloy powder is saturated, and carrying out hydrogen induced disproportionation reaction to obtain rare earth aluminum alloy hydride powder; wherein the judgment standard of hydrogen absorption saturation is as follows: the material absorbs hydrogen until the hydrogen pressure no longer changes, at which point the material is saturated with hydrogen.
(4) And (4) coating a metal layer on the surface of the rare earth aluminum alloy hydride obtained in the step (3) by adopting a physical vapor deposition method.
In the step (2), the rare earth aluminum alloy is crushed to-20- +800 meshes by a crusher or gas atomization to obtain the rare earth aluminum alloy powder.
The step (3) aims to effectively reduce the contact between the high-activity rare earth hydride and the external oxidation environment and reduce the sensitivity of the rare earth hydride.
Dispersing rare earth aluminum alloy hydride powder in advance by adopting high-frequency vibration or ultrasonic vibration before coating in the step (4); the step (4) aims to form a complete and uniform metal coating layer on the surface of the rare earth aluminum alloy hydride so as to reduce the thorough isolation of the high-activity rare earth aluminum alloy hydride from the external oxidation environment and effectively reduce the sensitivity of the rare earth alloy hydride. According to GB/T21566 friction sensitivity test method for hazardous explosive, a friction sensitivity instrument is used for testing, and the powder subjected to stabilizing treatment by adopting the technical scheme has the friction sensitivity exceeding 360N, so that the subsequent use requirements can be met.
The beneficial effects of the invention are as follows: the invention does not need special process flow and complex treatment process, the light rare earth metal hydride is dispersed and distributed in the rare earth alloy second phase and is coated with the high combustion heat metal layer, and the invention has the characteristics of simple operation, easy reaching of experimental conditions, safety and reliability, and is convenient for later use.
Drawings
Figure 1 XRD pattern of CeAl alloy hydride after hydrogen sorption in example 1.
FIG. 2 is a microstructure view of the hydride coated aluminum of the CeAl alloy in example 1; FIG. 2-a is the microscopic morphology of the powder at low magnification, and FIG. 2-b is the microscopic morphology of the powder at high magnification.
FIG. 3 is a microstructure of YAl alloy hydride coated copper in example 2; FIG. 3-a is the micro-morphology of the powder at low magnification, and FIG. 3-b is the micro-morphology of the powder at high magnification.
Detailed Description
The present invention provides a high-combustion, low-sensitivity rare earth alloy hydride material and a method for preparing the same, which will be further described with reference to the following examples, but the present invention is not intended to be limited thereto, and can be suitably modified within the scope of the claims without changing the scope of the present invention.
Specifically, the preparation method of the rare earth alloy hydride material provided by the invention comprises the following steps:
(1) Smelting rare earth and aluminum to obtain rare earth aluminum alloy; wherein, the rare earth is one or more of La, ce, Y, dy, er, yb and Sm, the mol ratio of the rare earth to the aluminum is 5:1 to 1:10, the smelting method is medium-frequency induction smelting, suspension smelting or electron beam smelting.
(2) And (2) crushing the rare earth aluminum alloy obtained in the step (1) to-20- +800 meshes by adopting a crusher or gas atomization to obtain rare earth aluminum alloy powder.
(3) And (3) placing the rare earth aluminum alloy powder obtained in the step (2) into hydrogenation equipment to absorb hydrogen until saturation, and performing hydrogen-induced disproportionation reaction to form a structure with high-activity rare earth hydride dispersed and distributed in the rare earth aluminum alloy, so as to obtain the rare earth aluminum alloy hydride powder. Wherein the hydrogen absorption condition is 0.1-5.0 MPa and 0-200 ℃.
The step (3) aims to effectively reduce the contact between the high-activity rare earth hydride and the external oxidation environment and reduce the sensitivity of the rare earth hydride.
(4) Dispersing the rare earth aluminum alloy hydride powder in the step (3) by adopting high-frequency vibration or ultrasonic vibration, and then coating a metal layer on the surface of the dispersed rare earth aluminum alloy hydride powder by adopting a physical vapor deposition method such as magnetron sputtering, electron beam evaporation and the like to obtain the rare earth alloy hydride material with a core-shell structure taking the metal layer as a shell and the rare earth aluminum alloy hydride as a core. Wherein, the metal layer is made of metal with high combustion heat, preferably Al, mg or B; the thickness of the metal layer is 1-1000nm. The deposition process of magnetron sputtering in the physical vapor deposition method is characterized in that the pre-vacuum degree is less than 5 multiplied by 10 -3 Pa, sputtering pressure of 0.1-1.0 Pa, sputtering power of 1-20 kW and deposition time of 0.1-10 h.
The step (4) aims to form a complete and uniform metal coating layer on the surface of the rare earth aluminum alloy hydride so as to reduce the thorough isolation of the high-activity rare earth aluminum alloy hydride from the external oxidation environment and effectively reduce the sensitivity of the rare earth alloy hydride.
Example 1
(1) Respectively weighing 280g of pure cerium and 81g of pure aluminum, and smelting by using a suspension smelting furnace at the heating temperature of 1000 ℃ to obtain the CeAl alloy.
(2) The CeAl alloy powder is prepared by adopting a mechanical powder preparation method.
(3) Absorbing hydrogen in the environment of 1.0MPa and 100 ℃ to generate hydrogen induced disproportionation reaction to form CeH x Dispersed and distributed in the CeAl alloy matrix. And screening the powder by using a grading screening technology to obtain alloy hydride powder with-20 to +800 meshes.
(4) Coating metal Al on the surface of CeAl alloy hydride powder by magnetron sputtering technology, dispersing the powder by a high-frequency vibration device, wherein the vibration frequency is 5kHz, and the pre-vacuumizing degree reaches 3 multiplied by 10 -3 Pa, introducing argon gas with the flow of 60sccm, the sputtering power of 1.5kW and the deposition time of 3h to obtain the core-shell structure powder with the CeAl alloy hydride as the core and the metal Al as the shell.
Fig. 1 is an XRD pattern of the CeAl alloy hydride after hydrogen absorption of example 1. As can be seen from FIG. 1, the disproportionation reaction of the alloy after hydrogen absorption to form CeH 2.53 And CeAl 2 Two-phase, rather than conventional, alloy hydride Ce 3 Al 2 H x 。
FIG. 2 is a micro-morphology of the powder coated by magnetron sputtering in example 1; wherein, fig. 2-a is the micro-morphology of the powder under low power, and fig. 2-b is the micro-morphology of the powder under high power. As can be seen from FIG. 2-b, the surface of the powder is uniformly coated with metal Al, the thickness of the powder is about 68.9nm, and the coating layer effectively isolates the high-activity rare earth hydride from air.
Tests show that the rare earth aluminum alloy hydride product obtained in the example 1 has the combustion heat of 9.98MJ/Kg, can be directly exposed to the atmosphere, has the friction sensitivity of 400N, and obviously reduces the sensitivity of the material.
Comparative example 1
(1) Respectively weighing 280g of pure cerium and 81g of pure aluminum, and smelting by using a suspension smelting furnace at the heating temperature of 1000 ℃ to obtain the CeAl alloy.
(2) The CeAl alloy powder is prepared by a mechanical powder preparation method.
(3) Absorbing hydrogen in the environment of 1.0MPa and 100 ℃ to generate hydrogen induced disproportionation reaction to form CeH x And the dispersed distribution is in the structure of the CeAl alloy matrix. And screening the powder by using a grading screening technology to obtain alloy hydride powder with-20 to +800 meshes.
Tests prove that the combustion heat of the rare earth aluminum alloy hydride product obtained in the comparative example 1 is 9.57MJ/Kg, but the powder cannot be directly exposed in the atmosphere, is extremely easy to spontaneously combust in the atmosphere and cannot meet the use requirement.
Example 2
(1) 216g of pure metal yttrium and 24g of pure metal aluminum are respectively weighed, and a YAl alloy is smelted by using a suspension smelting furnace.
(2) YAl alloy powder is prepared by adopting a gas atomization method.
(3) Absorbing hydrogen in the environment of 2.5MPa and 160 ℃ to generate hydrogen-induced disproportionation reaction to form YH x The material is dispersed in a YAl alloy matrix structure. And screening the powder by using a grading screening technology to obtain alloy hydride powder with-20 to +800 meshes.
(4) Coating metal Cu on the surface of YAl alloy hydride powder by electron beam evaporation, and dispersing the powder by an ultrasonic vibration device, wherein the vibration frequency is 2kHz, and the pre-vacuumizing degree reaches 3 x 10 -3 And Pa, introducing argon gas, wherein the flow rate is 100sccm, the sputtering power is 2.4kW, and the deposition time is 2h to obtain the powder with the core-shell structure, wherein YAl alloy hydride is used as a core, and metal Cu is used as a shell.
FIG. 3 is the micro-morphology of the powder coated by electron beam evaporation in example 2; wherein, fig. 3-a is the micro-morphology of the powder under low power, and fig. 3-b is the micro-morphology of the powder under high power. As can be seen from FIG. 3-b, the surface of the powder is uniformly coated with Cu, and the coating effectively isolates the highly active rare earth hydride from air.
The test shows that the burning heat of the rare earth aluminum alloy hydride is 7.69MJ/Kg, the rare earth aluminum alloy hydride can be directly exposed in the atmosphere, the friction sensitivity of the material is 360N, and the sensitivity of the material is obviously reduced.
Claims (7)
1. The high-combustion low-sensitivity rare earth alloy hydride material is characterized in that the rare earth alloy hydride material is in a core-shell structure, a shell is a metal layer, and a core is rare earth alloy hydride; the rare earth hydride in the rare earth aluminum alloy hydride is dispersed and distributed in the rare earth aluminum alloy; the metal layer is made of Al, mg and Cu, and the rare earth is any one or more of La, ce, Y, dy, er, yb and Sm;
the rare earth aluminum alloy hydride is obtained by hydrogen induced disproportionation reaction of the rare earth aluminum alloy through hydrogen absorption, and the hydrogen absorption conditions are 0.1-5.0 MPa and 0-200 ℃.
2. A rare earth alloy hydride material of claim 1, wherein the metal layer is 1-1000nm thick.
3. The rare earth alloy hydride material of claim 2, wherein the metal material is coated on the surface of the rare earth alloy hydride by physical vapor deposition.
4. The rare earth alloy hydride material of claim 3, wherein the physical vapor deposition method comprises any one of magnetron sputtering, electron beam evaporation; the deposition process of magnetron sputtering comprises the steps of pre-vacuum degree less than 5 multiplied by 10 < -3 > Pa, sputtering air pressure of 0.1 to 1.0Pa, sputtering power of 1 to 20kW and deposition time of 0.1 to 10 hours.
5. A method of producing a rare earth alloy hydride material as claimed in any one of claims 1 to 4, comprising the steps of:
(1) Smelting rare earth and aluminum to obtain rare earth aluminum alloy;
(2) Crushing the rare earth aluminum alloy obtained in the step (1) to obtain rare earth aluminum alloy powder;
(3) Absorbing hydrogen by the rare earth aluminum alloy powder obtained in the step (2) until the rare earth aluminum alloy powder is saturated, and carrying out hydrogen induced disproportionation reaction to obtain rare earth aluminum alloy hydride powder;
(4) And (4) coating a metal layer on the surface of the rare earth aluminum alloy hydride obtained in the step (3) by adopting a physical vapor deposition method.
6. The method of claim 5, wherein the rare earth aluminum alloy has a molar ratio of rare earth to aluminum of 5:1 to 1:10, the smelting method is medium-frequency induction smelting, suspension smelting or electron beam smelting.
7. The method according to claim 5, wherein in the step (2), the rare earth aluminum alloy is crushed to-20 to +800 meshes by a crusher or gas atomization to obtain rare earth aluminum alloy powder; and (4) dispersing the rare earth aluminum alloy hydride powder in advance by adopting high-frequency vibration or ultrasonic vibration before coating.
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