CN111992725B - Zr 2 Preparation method and application of Fe alloy powder - Google Patents
Zr 2 Preparation method and application of Fe alloy powder Download PDFInfo
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- CN111992725B CN111992725B CN202010759764.4A CN202010759764A CN111992725B CN 111992725 B CN111992725 B CN 111992725B CN 202010759764 A CN202010759764 A CN 202010759764A CN 111992725 B CN111992725 B CN 111992725B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0031—Intermetallic compounds; Metal alloys; Treatment thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C16/00—Alloys based on zirconium
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses Zr 2 A preparation method and application of Fe alloy powder. The method comprises the following steps: weighing raw materials of zirconium and iron according to weight percentage, and cleaning the surface of the raw materials; putting the raw materials into smelting equipment for smelting to obtain an alloy, and cooling, wherein the smelting equipment is a suspension induction smelting furnace or an intermediate frequency furnace; putting the cooled alloy into a crusher, and crushing in vacuum, inert atmosphere or organic solvent; sieving Zr 2 Fe alloy powder. Zr prepared by the invention 2 The Fe alloy powder has high purity and low oxygen content; the method improves production efficiency and reduces production cost; the alloy powder is more stable in use and more obvious in effect, and has high hydrogen absorption rate and difficult pulverization when being used as a metal hydrogen absorption material.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to Zr 2 A preparation method and application of Fe alloy powder.
Background
Zr 2 The Fe alloy is used as a metal hydrogen absorption material, and has the use advantages of rapid hydrogen absorption, high absorption thorough efficiency, difficult pulverization and the like compared with other hydrogen absorption materials; at the same time, zr 2 The Fe alloy raw material and the production cost are lower than those of other hydrogen absorption materials, and the Fe alloy is more suitable to be used as a hydrogen isotope gas recovery material in large-scale industrial production. However, the current preparation methodObtained Zr 2 The Fe alloy has the problems of low alloy purity, high oxygen content, instability in the using process, unobvious effect and the like.
Disclosure of Invention
The invention aims to provide Zr 2 Preparation method and application of Fe alloy powder to solve the problem of Zr in the prior art 2 The Fe alloy has the problems of low purity, incapability of meeting the requirement of oxygen content and using, low production efficiency, high production cost, poor stability in use, unobvious effect and the like.
The above purpose is realized by the following technical scheme:
according to one aspect of the invention, the invention provides Zr 2 The preparation method of the Fe alloy powder comprises the following steps:
s10, weighing raw materials of zirconium and iron according to weight percentage, and cleaning the surface of the raw materials, wherein the weight ratio of zirconium: 76.5%, iron: 23.5 percent;
s20, putting the raw materials into a smelting device for smelting to obtain an alloy, and then cooling, wherein the smelting device is a suspension induction smelting furnace or an intermediate frequency furnace;
s30, putting the cooled alloy into a crusher, and crushing in vacuum, inert atmosphere or organic solvent;
step S40, sieving Zr 2 Fe alloy powder.
Preferably, the purity of the zirconium is more than or equal to 99.99 percent, and the purity of the iron is more than or equal to 99.99 percent.
Preferably, step S20 includes:
step S21, vacuumizing the smelting equipment to 2 multiplied by 10 -2 Pa～6×10 -2 Pa；
S22, filling argon until the vacuum reaches 0.01-0.1 MPa;
and S23, heating for 5-40 min, keeping the temperature for 1-30 min, casting the alloy into a cast iron mould in an electrified way, cooling and taking out the alloy.
Further, in step S23,
when the smelting equipment is a suspension induction smelting furnace, heating for 5-15 min at 550V and 100-200A current, and keeping the temperature for 1-10 min;
when the smelting equipment is a 10Kg intermediate frequency furnace, the power is increased to 8-25 Kw, the heating is carried out for 10-40 min, and the heat preservation is carried out for 5-30 min;
when the smelting equipment is an intermediate frequency furnace of 25Kg, the power is increased to 8-25 Kw, the heating is carried out for 10-40 min, and the heat preservation is carried out for 5-30 min.
Preferably, in step S30, the mixture is crushed to a particle size of 0.27 to 0.025mm.
Preferably, step S30 further includes: performing primary crushing on the cooled alloy before crushing by a crusher; and crushing again after crushing with the crusher.
Preferably, zr with the grain diameter of 0.048-0.075 mm is sieved out in the step S40 2 Fe alloy powder.
Preferably, zr obtained in step S40 2 In the Fe alloy powder, the impurity content is less than or equal to 0.01 percent, and the oxygen content is less than or equal to 0.02 percent.
According to another aspect of the invention, the invention provides Zr 2 Use of Fe alloy powder in hydrogen absorbing material, wherein said Zr 2 The Fe alloy powder is prepared according to the preparation method.
Compared with the prior art, the Zr in the invention 2 The preparation method of the Fe alloy powder comprises the steps of obtaining an alloy block through one-time smelting, and crushing to obtain Zr with uniform components 2 The Fe alloy powder has high alloy purity and low oxygen content, and specifically, the impurity content in the alloy powder is lower than 0.01 percent, and the oxygen content in the alloy powder is lower than 0.02 percent.
The invention improves Zr 2 The preparation efficiency of the Fe alloy powder reduces the production cost, and the equipment required in the preparation process is simple and has little pollution; the alloy powder obtained by the preparation method meets the requirement of oxygen content, is more stable in the using process and has more obvious effect; zr of the invention 2 When the Fe alloy powder is used as a metal hydrogen absorption material, the Fe alloy powder has the advantages of high hydrogen absorption rate and difficult pulverization.
Drawings
FIG. 1 shows Zr according to the present invention 2 XRD detection results of the Fe alloy powder are shown schematically.
Detailed Description
The technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiment of the present invention:
the invention provides Zr 2 The preparation method of the Fe alloy powder comprises the following steps:
step S10, using metal zirconium and metal iron with the purity of more than or equal to 99.99% as raw materials according to Zr 2 Weighing raw materials of Fe alloy components, and cleaning the surfaces of metal zirconium and metal iron. Wherein, zr 2 The Fe alloy comprises the following components in percentage by weight: zirconium: 76.5%, iron: 23.5 percent.
And step S20, mixing the raw materials, and putting the mixture into smelting equipment for smelting to obtain the alloy. The smelting equipment can be a suspension induction smelting furnace and an intermediate frequency furnace.
In an alternative embodiment, during smelting, the smelting equipment is firstly vacuumized to 2 x 10 -2 Pa～6 ×10 - 2 Pa, then closing the valve; filling high-purity argon until the vacuum in the smelting equipment reaches 0.03-0.05 MPa; and then heating for 5-40 min, preserving heat for 1-30 min, casting into a cast iron mould in an electrified way, and taking out the alloy after cooling. In the smelting process, the oxygen content in the alloy can be reduced to a greater extent by pumping to a higher vacuum, and then the oxygen content in the smelting process can be further reduced by filling high-purity argon into the smelting equipment (and reaching the vacuum extent), so that the splashing of liquid metal in the smelting process can be prevented, and the purity of the alloy is effectively protected.
Further, when the smelting equipment is a suspension induction smelting furnace, the furnace is heated for 5-15 min under the voltage of 550V and the current of 100-200A, and the temperature is kept for 1-10 min. When the smelting equipment is a 10Kg intermediate frequency furnace, the power is increased to 8-25 Kw, the heating is carried out for 10-40 min, and the heat preservation is carried out for 5-30 min. When the smelting equipment is a 25Kg intermediate frequency furnace, the power is increased to 8-25 Kw, the heating is carried out for 10-40 min, and the heat preservation is carried out for 5-30 min.
And step S30, putting the cooled alloy into a crusher, and crushing in vacuum, inert atmosphere or organic solvent. The crushing can be carried out, for example, in a container filled with alcohol.
In an alternative embodiment, the method further comprises the step of simply performing primary crushing on the cooled alloy before crushing by using the crusher. Simple primary crushing means that a large ingot is directly physically crushed, for example, by being broken with a hammer or by an oil press, and there is no particular requirement for the particle size as long as it can be placed in a container of a crusher. Then a crusher is adopted for crushing, the crusher can beat powder with different grain diameters according to different time, and then the powder is continuously (re) crushed until the grain diameter is 0.025-0.27 mm after being screened and the grain diameter is still too large.
Step S40, sieving Zr 2 Fe alloy powder. Sieving out Zr with the diameter of 0.048-0.075 mm 2 Fe alloy powder. Through detection, the impurity content in the screened alloy powder is less than or equal to 0.01 percent, and the oxygen content is less than or equal to 0.02 percent.
The invention also provides Zr 2 The application of Fe alloy powder in hydrogen absorption material. Wherein, said Zr 2 The Fe alloy powder was prepared according to the above preparation method. Zr in the reaction solution 2 The Fe alloy powder is used as a hydrogen absorption material and has the advantages of high hydrogen absorption rate and difficult pulverization.
The following examples are given for the detailed implementation and the specific operation procedures, but the scope of the present invention is not limited to the following examples.
Example 1
Taking 2.296kg of metal zirconium (the purity is more than or equal to 99.99 percent) and 0.704kg of metal iron (the purity is more than or equal to 99.99 percent) as raw materials, and cleaning the surface; then adding the mixture into a crucible of a suspension induction melting furnace, starting a mechanical pump and a molecular pump to begin to pump vacuum until the vacuum of the suspension induction melting furnace reaches 5 multiplied by 10 -2 Pa, after a valve is closed, filling high-purity argon into the suspension induction smelting furnace until the vacuum of the suspension induction smelting furnace reaches 0.04MPa; heating for 8min under 550V and 160A current, keeping the temperature for 2min, casting into a cast iron mould with the diameter of 140mm and the height of 40mm in an electrified way, and taking out the alloy after cooling; zr after cooling 2 The Fe alloy is simply crushed initially and then filled with alcoholPutting the container into a crusher for crushing; finally, screening out Zr with different thicknesses by using a sieve 2 Fe alloy powder. Zr with the diameter of 0.048-0.075 mm can be screened out 2 Fe alloy powder.
The alloy powder obtained by the above method has an impurity content (0.00843%) of less than 0.01% and an oxygen content of less than 0.02%, see table 1 for details.
Example 2
Taking 5.355kg of metal zirconium (the purity is more than or equal to 99.99%) and 1.645kg of metal iron (the purity is more than or equal to 99.99%) as raw materials, and cleaning the surface; then adding the mixture into a 10Kg intermediate frequency furnace crucible, starting a mechanical pump and a diffusion pump to vacuumize until the vacuum of the 10Kg intermediate frequency furnace reaches 5 multiplied by 10 -2 Pa, closing a valve, and then filling high-purity argon into the 10Kg of intermediate frequency furnace until the vacuum of the 10Kg of intermediate frequency furnace reaches 0.04MPa; increasing the power to 16Kw, heating for 25min, keeping the temperature for 10min, carrying out charged casting to a cast iron mould with the diameter of 180mm and the height of 80mm, and taking out the alloy after cooling; zr after cooling 2 Simply and primarily crushing the Fe alloy, then putting the Fe alloy into a container filled with alcohol, and putting the container into a crusher for crushing; finally, screening out Zr with different thicknesses 2 Fe alloy powder.
The alloy powder obtained by the above method has an impurity content (0.00878%) of less than 0.01% and an oxygen content of less than 0.02%, see table 1 for details.
Example 3
Taking 15.3kg of metal zirconium (the purity is more than or equal to 99.99%) and 4.7kg of metal iron (the purity is more than or equal to 99.99%) as raw materials, and cleaning the surface; then adding the mixture into a crucible of an intermediate frequency furnace of 25Kg, and opening a mechanical pump and a diffusion pump to pump the mixture until the vacuum of the intermediate frequency furnace of 25Kg reaches 5 multiplied by 10 -2 Pa, closing a valve, and then filling high-purity argon into the 25Kg of intermediate frequency furnace until the vacuum of the 25Kg of intermediate frequency furnace reaches 0.04MPa; increasing the power to 16Kw, heating for 25min, preserving heat for 10min, casting into a cast iron mould with the diameter of 180mm and the height of 200mm in an electrified way, and taking out the alloy after cooling; zr after cooling 2 Simply and primarily crushing the Fe alloy, then putting the Fe alloy into a container filled with alcohol, and putting the container into a crusher for crushing; finally, screening out Zr with different thicknesses 2 Fe alloy powder.
The alloy powder obtained by the method has the impurity content (0.00934%) of less than 0.01% and the oxygen content of less than 0.01%, see table 1 specifically.
Zr obtained in examples 1 to 3 2 The results of the composition analysis of the Fe alloy powder are shown in table 1:
TABLE 1 Zr 2 Detection result of Fe alloy powder composition (%)
The invention adopts an intermediate frequency furnace or a suspension induction melting furnace to obtain alloy blocks by one-time melting, and then adopts a crusher to crush the alloy blocks to obtain Zr with uniform components 2 Fe alloy powder; wherein the preparation efficiency of the suspension induction melting furnace is higher. The invention is about the Zr obtained by preparation 2 The phase analysis of the Fe alloy powder showed Zr in FIG. 1 2 Phase composition of Fe.
Claims (6)
1. Zr 2 The preparation method of the Fe alloy powder is characterized by comprising the following steps of:
s10, weighing raw materials of zirconium and iron according to weight percentage, and cleaning the surface of the raw materials, wherein the weight ratio of zirconium: 76.5%, iron: 23.5 percent; the purity of the zirconium is more than or equal to 99.99 percent, and the purity of the iron is more than or equal to 99.99 percent;
s20, putting the raw materials into a smelting device for primary smelting, wherein in the smelting process, the smelting device is vacuumized to 2 x 10 -2 Pa～6×10 -2 Pa, then closing a valve, introducing high-purity argon until the vacuum in the smelting equipment reaches 0.03-0.05 MPa, then heating for 5-40 min, preserving the heat for 1-30 min, casting the alloy into a cast iron mould in an electrified way, and taking out the alloy after cooling; the smelting equipment is a suspension induction smelting furnace or an intermediate frequency furnace;
s30, putting the cooled alloy into a crusher, and crushing in vacuum, inert atmosphere or organic solvent;
step S40, sieving Zr 2 Fe alloy powder with impurity content less than or equal to0.01 percent and the oxygen content is less than or equal to 0.02 percent.
2. The production method according to claim 1, wherein, in step S23,
when the smelting equipment is a suspension induction smelting furnace, heating for 5-15 min at 550V and 100-200A current, and keeping the temperature for 1-10 min;
when the smelting equipment is a 10Kg intermediate frequency furnace, the power is increased to 8-25 Kw, the heating is carried out for 10-40 min, and the heat preservation is carried out for 5-30 min;
when the smelting equipment is a 25Kg intermediate frequency furnace, the power is increased to 8-25 Kw, the heating is carried out for 10-40 min, and the heat preservation is carried out for 5-30 min.
3. The method according to claim 1, wherein the step S30 is carried out by crushing the mixture to a particle size of 0.27 to 0.025mm.
4. The method according to claim 3, wherein the step S30 further comprises: performing primary crushing on the cooled alloy before crushing by a crusher; and crushing again after crushing with the crusher.
5. The method according to claim 1, wherein Zr having a particle size of 0.048-0.075 mm is sieved in step S40 2 Fe alloy powder.
6. Zr 2 Use of Fe alloy powder in hydrogen absorbing material, zr as said 2 Fe alloy powder produced by the production method according to any one of claims 1 to 5.
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