CN102528066B - Superfine high-purity hafnium powder as well as preparation method and application thereof - Google Patents
Superfine high-purity hafnium powder as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to superfine high-purity hafnium powder as well as a preparation method and an application thereof. The grain size of the superfine high-purity hafnium powder is less than 1 micron; the purity reaches above 99.99%; the total content of metal impurities is less than 100ppm; and the oxygen content is less than 0.2%. The preparation method comprises the following steps: a) uniformly mixing hafnium oxide powder with reducing agent powder at a molar ratio of 1:1 to 1:6, and filling a mixture into a crucible; b) placing the crucible into a reaction tank, covering with a cover, then vacuumizing, filling argon for washing, heating and reducing, and performing constant-temperature insulation reduction; c) vacuumizing, filling argon again, and cooling under the argon protection; and d) washing: firstly, washing with an acid, then washing with deionized water, and screening and drying the obtained product, thereby obtaining the product of the superfine high-purity hafnium powder. The oxide generated by the method provided by the invention is capable of protecting hafnium powder, is anti-explosion and is safe and controllable.
Description
Technical field
The present invention relates to a kind of superfine high-purity hafnium powder and its preparation method and application, particularly a kind of preparation method who is widely used in the fields such as atomic energy industry, information industry, bioengineering, military science, medical field, petrochemical industry, space flight and aviation superfine high-purity hafnium powder.
Background technology
Hafnium is bright silvery white metal, and pure hafnium tool plasticity, easily processing, high temperature resistant, anticorrosive, be atomic energy industry important materials.The thermal neutron capture cross section of hafnium large (115b), can absorb the thermal neutron of nuclear reactor and control the reaction speed of reactor, for control rod and the protective device of atomic pile.Hafnium powder can be made the propeller of rocket; In electrical equipment industry, hafnium powder can be manufactured the negative electrode of X-ray tube, can be used as the getter in electric lamp filament and electron tube; Hafnium powder is the raw material of the high-purity hafnium ingot of melting, is the raw material that powder metallurgy is prepared hafnium part.The alloy of hafnium can be made the forward position protective layer of the aircraft that rocket nozzle and gliding type reentry, and Hf-Ta alloy can fabrication tool steel and resistance material.Hafnium is also applied to metallurgy, chemical industry, gunpowder and special refractories.
Superfine high-purity hafnium powder requires purity up to 99.99%, and metal impurities total content is less than 100ppm, and oxygen content is less than 0.2%, and granularity is less than 1 μ m, and technology of preparing does not have bibliographical information, adopts common experimental technique to be difficult to reach above-mentioned requirements.Therefore, preparing superfine high-purity hafnium powder is the very large and challenging work of a difficulty.
Summary of the invention
The object of this invention is to provide a kind of purity up to 99.99%, metal impurities total content is less than 100ppm, and oxygen content is less than 0.2%, and granularity is less than hafnium metal powder of 1 μ m and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions:
A kind of superfine high-purity hafnium powder, is characterized in that: the granularity of hafnium powder is less than 1 μ m, purity is up to more than 99.99%, and metal impurities total content is less than 100ppm, and oxygen content is less than 0.2%.The preparation method of above-mentioned superfine high-purity hafnium powder, its preparation process comprises the steps:
A. the hafnium oxide powder and the reducing agent powder that by mol ratio are 1: 1～1: 6 mix, and pack in crucible;
B. crucible is put into retort, build after lid and vacuumize, be filled with argon gas washing, heat reduction, then carries out constant temperature insulation reduction;
C. then vacuumize, be filled with again afterwards argon gas, cooling under argon shield;
D. washing: first adopt pickling, then adopt deionized water washing, the product obtaining is sieved, dried, be superfine high-purity hafnium powder product.
A kind of preferred technical scheme, is characterized in that: in step a, the purity of described hafnium oxide powder is greater than 99.9%, and granularity is less than 1mm.
A kind of preferred technical scheme, is characterized in that: described reducing agent powder is CaH
2, LiH, Ca or their mixture powder, the granularity of described powder is less than 2mm.
A kind of preferred technical scheme, is characterized in that: described mixing adopts the mixing method of reactant blend.
A kind of preferred technical scheme, is characterized in that: the material of described crucible is Mo, Ta, Hf, W or Nb metal.
A kind of preferred technical scheme, is characterized in that: in step b, the temperature of described heat reduction is 800～1400 DEG C, and the heating-up time is 0.5～10 hour.
A kind of preferred technical scheme, is characterized in that: in step b, the temperature of described constant temperature insulation reduction is 800～1400 DEG C, and temperature retention time is 0.5～10 hour.
A kind of preferred technical scheme, is characterized in that: in step b, described heat reduction and constant temperature insulation reduction are all carried out under argon shield.
A kind of preferred technical scheme, is characterized in that: in step c, described vacuumizes as vacuumize 0.5～10 hour at 800～1400 DEG C.To control the hydrogen content in hafnium powder.
A kind of preferred technical scheme, is characterized in that: in steps d, described pickling be at room temperature to 70 DEG C, adopts hydrochloric acid, sulfuric acid, nitric acid or their mixed acid of 0.2M～10M to wash, and pickling number of times is 1-15 time.Take acid washing method imurity-removal.
A kind of preferred technical scheme, is characterized in that: in steps d, described deionized water washing is at room temperature to 100 DEG C, and with deionized water washing, number of times is 1-15 time.
A kind of preferred technical scheme, it is characterized in that: the purity of described superfine high-purity hafnium powder is up to more than 99.99%, and metal impurities total content is less than 100ppm, and oxygen content is less than 0.2%, granularity is less than 1 μ m, and the hafnium Powder Particle Size that hydrogenation and dehydrogenization method obtains is much larger than 1 μ m.
Another object of the present invention is to provide the prepared purity of said method up to 99.99%, and metal impurities total content is less than 100ppm, and oxygen content is less than 0.2%, and granularity is less than the application of the hafnium metal powder of 1 μ m.
Superfine high-purity hafnium powder prepared by the inventive method, directly manufactures high pure metal hafnium target and powder metallurgy section bar applicable to powder metallurgy process; Can be used as iodide process and prepare hafnium crystal bar high-purity, low gap constituent content; Can be used as direct melting and prepare the raw material of high-purity hafnium ingot.
Method of the present invention, adopts argon shield, and 800～1400 DEG C of constant temperature 0.5～10 hour, can ensure that hafnium oxide reacts completely; Employing is heated to 800～1400 DEG C of techniques that vacuumize, and can reduce the hydrogen content in hafnium metal powder.
The invention has the advantages that:
(1) pickling of the present invention, washing impurity removal process, can effectively remove the metal impurities in product, is met the high pure metal hafnium powder of requirement.
(2) method of the present invention, the oxide of generation can be protected hafnium powder, prevent exploding, safety is controlled.
Below by detailed description of the invention, the present invention will be further described, but and do not mean that limiting the scope of the invention.
Detailed description of the invention
Embodiment 1
Purity 99.9%, granularity are less than to the reducing agent powder CaH that the hafnium oxide of 1mm and purity are greater than 98.9%, granularity is less than 2mm
2, mix according to the mol ratio ratio of 1: 1, pack in molybdenum crucible.Crucible is put into retort, build after lid and be evacuated to 0.01Pa, argon gas washing, within 0.5 hour, be heated to 800 DEG C, argon shield.950 DEG C of constant temperature are after 5 hours, and 800 DEG C vacuumize 10 hours, are filled with afterwards argon gas to pressure-fired again, cooling under argon shield.By product with the hydrochloric acid of 0.2M room temperature washing 15 times, then in deionized water washing 1 time for room temperature, the product obtaining is sieved, finally obtaining hafnium opaque amount is: the purity of hafnium powder is 99.99%, metal impurities total content is less than 100ppm, oxygen content is less than 0.2%, particle mean size 0.2 μ m.
Embodiment 2
Purity is greater than to the reducing agent LiH that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 98.9%, granularity is less than 2mm, mixes according to the mol ratio ratio of 1: 1, pack in tantalum crucible.Crucible is put into retort, build after lid and be evacuated to 0.03Pa, argon gas washing, within 10 hours, be heated to 1400 DEG C, argon shield.1400 DEG C of constant temperature are after 0.5 hour, and 1400 DEG C vacuumize 0.5 hour, are filled with afterwards argon gas to pressure-fired again, cooling under argon shield.Product is washed 15 times at 70 DEG C with the hydrochloric acid of 10M, then 100 DEG C of deionized waters washing 15 times, will obtain product and sieve, and finally obtain hafnium opaque amount and be: the purity of hafnium powder will be 99.99%, metal impurities total content 95ppm, oxygen content 0.2%, granularity are less than 0.8 μ m.
Embodiment 3
Purity is greater than to the Ca reducing agent powder that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 2mm, mixes according to the mol ratio ratio of 1: 6, pack in hafnium crucible.Crucible is put into retort, build after lid and be evacuated to 0.05Pa, argon gas washing, within 10 hours, be heated to 1000 DEG C, argon shield.At 1000 DEG C, constant temperature, after 0.5 hour, vacuumizes 10 hours afterwards, is filled with afterwards argon gas to pressure-fired again, cooling under argon shield.By product with the nitric acid of 0.2M room temperature washing 10 times, then 50 DEG C of deionized waters are washed 15 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 80ppm, oxygen content is less than 0.2%, particle mean size 0.9 μ m.
Embodiment 4
Purity is greater than to the CaH that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 1mm
2reducing agent powder, mixes according to the mol ratio ratio of 1: 1.5, packs in hafnium crucible.Crucible is put into retort, build after lid and be evacuated to 0.06Pa, argon gas washing, within 10 hours, be heated to 1000 DEG C, argon shield.At 1000 DEG C, constant temperature, after 2 hours, vacuumizes 2 hours at 1000 DEG C afterwards, is filled with afterwards argon gas to pressure-fired again, cooling under argon shield.The hydrochloric acid that is 0.5M by acidity by product and the mixed acid of nitric acid wash 8 times at 40 DEG C, then 50 DEG C of deionized waters are washed 10 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 70ppm, oxygen content is less than 0.2%, particle mean size 0.2 μ m.
Embodiment 5
Purity is greater than to the CaH that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 1mm
2reducing agent powder, mixes according to the mol ratio ratio of 1: 1.5, packs in tungsten crucible.Crucible is put into retort, build after lid and be evacuated to 0.07Pa, argon gas washing, within 10 hours, be heated to 1000 DEG C, argon shield.At 1000 DEG C, constant temperature, after 2 hours, vacuumizes 2 hours at 1000 DEG C afterwards, is filled with afterwards argon gas to pressure-fired again, cooling under argon shield.The sulfuric acid that is 0.2M by acidity by product washs 15 times at 70 DEG C, then 50 DEG C of deionized waters are washed 15 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 85ppm, oxygen content is less than 0.2%, particle mean size 0.3 μ m.
Embodiment 6
Purity is greater than to the CaH that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 1mm
2reducing agent powder, mixes according to the mol ratio ratio of 1: 2, packs in niobium crucible.Crucible is put into retort, build after lid and be evacuated to 0.08Pa, argon gas washing, within 4 hours, be heated to 1000 DEG C, argon shield.At 1000 DEG C, constant temperature, after 2 hours, vacuumizes 2 hours at 1000 DEG C afterwards, is filled with afterwards argon gas to pressure-fired again, cooling under argon shield.The hydrochloric acid that is 0.2M by acidity by product washs 15 times at 40 DEG C, then 50 DEG C of deionized waters are washed 15 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 80ppm, oxygen content is less than 0.2%, particle mean size 0.35 μ m.
Embodiment 7
Purity is greater than to the CaH that the hafnium oxide of 99.99% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 1mm
2, Ca, LiH mixing reducing agent powder (three's mol ratio is 1: 1: 1), mix according to the mol ratio ratio of 1: 1.5, pack in hafnium crucible.Crucible is put into retort, build after lid and be evacuated to 0.09Pa, argon gas washing, within 10 hours, be heated to 1100 DEG C, argon shield.At 1100 DEG C, constant temperature, after 2 hours, vacuumizes 2 hours at 1100 DEG C afterwards, is filled with afterwards argon gas again, cooling under argon shield.The hydrochloric acid that is 0.2M by acidity by product and the mixed acid of nitric acid wash 15 times at 30 DEG C, then 100 DEG C of deionized waters are washed 15 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 50ppm, oxygen content is less than 0.2%, particle mean size 0.2 μ m.
Embodiment 8
Purity is greater than to the CaH that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 1mm
2reducing agent powder, mixes according to the mol ratio ratio of 1: 1.5, packs in high temperature alloy 4169 crucibles.Crucible is put into retort, build after lid and be evacuated to 0.1Pa, argon gas washing, within 10 hours, be heated to 950 DEG C, argon shield.At 950 DEG C, constant temperature, after 2 hours, vacuumizes 2 hours at 950 DEG C afterwards, is filled with afterwards argon gas again, cooling under argon shield.The mixed acid of the hydrochloric acid, nitric acid and the sulfuric acid that are 0.5M by acidity by product is room temperature washing 8 times, then 50 DEG C of deionized waters are washed 10 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 950ppm, oxygen content is less than 0.2%, particle mean size 0.2 μ m.
Embodiment 9
Purity is greater than to the CaH that the hafnium oxide of 99.9% (granularity is less than 1mm) and purity are greater than 99%, granularity is less than 1mm
2reducing agent powder, mixes according to the mol ratio ratio of 1: 1.6, packs in high temperature alloy 4169 crucibles.Crucible is put into retort, build after lid and be evacuated to 0.1Pa, argon gas washing, within 10 hours, be heated to 800 DEG C, argon shield.At 800 DEG C, constant temperature, after 10 hours, vacuumizes 2 hours at 800 DEG C afterwards, is filled with afterwards argon gas again, cooling under argon shield.The mixed acid of the hydrochloric acid, nitric acid and the sulfuric acid that are 10M by acidity by product is room temperature washing 1 time, then 60 DEG C of deionized waters are washed 10 times, the product obtaining is sieved, the quality that finally obtains metal hafnium is: the purity of hafnium powder is 99.99%, metal impurities total content 950ppm, oxygen content is less than 0.2%, particle mean size 0.2 μ m.
Claims (6)
1. a superfine high-purity hafnium powder, is characterized in that: the granularity of hafnium powder is less than 1 μ m, and purity is up to more than 99.99%, and metal impurities total content is less than 100ppm, and oxygen content is less than 0.2%; Its preparation method, hafnium oxide powder and reducing agent powder that to comprise the steps: mol ratio be 1:1～1:6 mix, and pack in crucible; The purity of described hafnium oxide powder is greater than 99.9%, and granularity is less than 1mm; Described reducing agent powder is CaH
2, LiH, Ca or their mixture powder, the granularity of powder is less than 2mm; Described mixing adopts the mixing method of reactant blend; The material of described crucible is Mo, Ta, Hf, W or Nb; Crucible is put into retort, build after lid and vacuumize, be filled with argon gas washing, heat reduction, then carries out constant temperature insulation reduction; The temperature of described heat reduction is 800～1400 DEG C, and the heating-up time is 0.5～10 hour; The temperature of described constant temperature insulation reduction is 800～1400 DEG C, and temperature retention time is 0.5～10 hour; Described heat reduction and constant temperature insulation reduction are all carried out under argon shield; Then vacuumize, be filled with again afterwards argon gas, cooling under argon shield; Washing: first adopt pickling, then adopt deionized water washing, the product obtaining is sieved, dried, be superfine high-purity hafnium powder product.
2. a preparation method for superfine high-purity hafnium powder, comprises the steps:
A. the hafnium oxide powder that is 1:1～1:6 by mol ratio and reducing agent powder mix, and pack in crucible; The purity of described hafnium oxide powder is greater than 99.9%, and granularity is less than 1mm; Described reducing agent powder is CaH
2, LiH, Ca or their mixture powder, the granularity of powder is less than 2mm; Described mixing adopts the mixing method of reactant blend; The material of described crucible is Mo, Ta, Hf, W or Nb;
B. crucible is put into retort, build after lid and vacuumize, be filled with argon gas washing, heat reduction, then carries out constant temperature insulation reduction; The temperature of described heat reduction is 800～1400 DEG C, and the heating-up time is 0.5～10 hour; The temperature of described constant temperature insulation reduction is 800～1400 DEG C, and temperature retention time is 0.5～10 hour; Described heat reduction and constant temperature insulation reduction are all carried out under argon shield;
C. then vacuumize, be filled with again afterwards argon gas, cooling under argon shield;
D. washing: first adopt pickling, then adopt deionized water washing, the product obtaining is sieved, dried, be superfine high-purity hafnium powder product.
3. the preparation method of superfine high-purity hafnium powder according to claim 2, is characterized in that: in step c, described vacuumizes as vacuumize 0.5～10 hour at 800～1400 DEG C.
4. the preparation method of superfine high-purity hafnium powder according to claim 2, is characterized in that: described pickling, at room temperature to 70 DEG C, adopts hydrochloric acid, sulfuric acid, nitric acid or the washing of their mixed acid of 0.2M～10M, and pickling number of times is 1-15 time.
5. the preparation method of superfine high-purity hafnium powder according to claim 2, is characterized in that: the washing of described deionized water is at room temperature to 100 DEG C, and with deionized water washing, number of times is 1-15 time.
Superfine high-purity hafnium powder claimed in claim 1 powder metallurgy process directly manufacture high pure metal hafnium target and powder metallurgy section bar, iodide process prepare the hafnium crystal bar of high-purity, low gap constituent content and directly melting prepare the application in high-purity hafnium ingot.
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| CN103862059B (en) * | 2012-12-07 | 2016-07-06 | 北京有色金属研究总院 | A kind of method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate |
| CN104096847A (en) * | 2013-04-03 | 2014-10-15 | 北京有色金属研究总院 | Preparing method of low-oxygen large-dimension high-purity hafnium powder |
| CN104439262A (en) * | 2013-09-22 | 2015-03-25 | 北京有色金属研究总院 | Large-sized metal zirconium powder low in oxygen content and preparation method of zirconium powder |
| CN104451317A (en) * | 2013-09-22 | 2015-03-25 | 北京有色金属研究总院 | Hafnium-base mixed metal material and iodination preparation method thereof |
| CN104646659B (en) * | 2013-11-22 | 2017-06-20 | 北京有色金属研究总院 | A kind of manufacture method of hypoxemia high pure metal hafnium powder |
| CN110129588A (en) * | 2019-06-03 | 2019-08-16 | 南通晶朋新材料科技有限公司 | A kind of preparation method of high purity metal hafnium |
| CN112095022B (en) * | 2020-01-21 | 2022-06-17 | 有研资源环境技术研究院(北京)有限公司 | Method for deeply removing oxygen in metal hafnium by using super-oxophilic metal-calcium synergistic method |
| CN113073211A (en) * | 2021-03-17 | 2021-07-06 | 西安交通大学 | Method for directly reducing powder into magnesium metal under inert gas carrying |
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