CN103862059B - A kind of method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate - Google Patents
A kind of method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate Download PDFInfo
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Abstract
The present invention relates to a kind of method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate, comprise the steps: that a. is by hafnium potassium fluorozirconate that mol ratio is 1:1 ~ 1:10 and reducing agent powder mix homogeneously, loads in crucible；B. crucible is put in retort, evacuation after building lid, be re-filled with argon washing, heat reduction, then carry out constant temperature insulation reduction；C. then heating up, evacuation carries out vacuum distilling；D. it is re-filled with argon, cools down under argon shield；E. washing: first adopt pickling, then adopt deionized water wash, undertaken the product obtained sieving, drying, the purity of the hafnium powder prepared is more than 83wt%, even may be up to more than 98wt%, and granularity is micron order, oxygen content is less than 0.2%, and other metals and gas impurity content are low.The present invention prepares the new method of high-purity hafnium powder, and it can effectively reduce the oxygen content in hafnium powder, and granularity is micron order, safely controllable, it is prevented that blast.
Description
Technical field
The present invention relates to a kind of method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate, the preparation method belonging to high-purity hafnium.Preparation method for high-purity hafnium powder in the fields such as atomic energy industry, information industry, petrochemical industry, Aero-Space.
Background technology
Hafnium has the nuclearity energy of excellence, and its thermal-neutron capture cross-section is up to 115b (1b=10-28m2), it is possible to absorb the thermal neutron of nuclear reactor, be used as the protection coating controlled in material and reactor and the flux decline device of nuclear reactor.Metal hafnium is because having good decay resistance, and the corrosion resistance in hot water and steam mixture is higher than titanium, zirconium, it is possible to as the special construction material of chemical industry.It addition, hafnium also has high antioxidant, good electrical and thermal conductivity and relatively low electron work functon, it is used as the plasma emission body of plasma cutting electrode.With the addition of the alloy of hafnium element, its strength of materials, corrosion resistance etc. can be significantly improved, as can be used for resisting the aircraft of 1650 DEG C of high temperature containing the hafnium base alloy of tantalum, molybdenum；Niobium-hafnium-tungsten alloy can be used for rocket and combustion gas turbine.Hafnium or a kind of well getter, hafnium titanium alloy is applied in the electric product such as bulb, electron tube as getter.
Due to developing rapidly of nuclear industry, metal hafnium has important and potential using value, and the preparation therefore studying metal hafnium has important theory and realistic meaning.Since eighties of last century the fifties, the preparation of metal hafnium becomes the focus of countries in the world research in succession, and especially atomic energy level hafnium requires hafnium material containing zirconium less than 2.1%, but prepares the task that the metal hafnium meeting technology requirement remains current more difficult.Kroll process is the main production process preparing metal hafnium at present.Namely with high-purity molten magnesium reduction hafnium tetrachloride.Due to the method, to there is production efficiency low, and equipment investment is big, the problems such as environmental pollution is serious, and the hafnium produced by the method is contained too many oxygen and not easily forges.Have studied both at home and abroad at present can the metallothermic processes of Kroll method as an alternative.Sharmaetal. have studied calciothermics and prepare hafnium metal powder, at 960 DEG C of hafnium powder (oxygen-containing 6000ppm and nitrogenous 147ppm) prepared with the calcium reduction hafnium oxide of excessive 70wt%.JuneJaetal. have studied aluminium reducing its metal of Group IV metal Preparation and alloy.Sharmaetal. it is investigated aluminothermic process and prepares some metal hafnium alloys.But, all there is some problems in the technique of the hafnium that said method is produced, or technique is too complicated, or production efficiency is low, or in product, impurity content is high.The present invention prepares the new method of high-purity hafnium powder, due to oxygen-free element in the raw material of hafnium potassium fluorozirconate own, more superior than hafnium oxide, hafnium potassium fluorozirconate is not volatile simultaneously, can overcome the drawback of hafnium chloride, and it can effectively reduce the oxygen content in hafnium powder, granularity is micron order, safely controllable, it is prevented that blast.
Summary of the invention
It is an object of the invention to provide a kind of high purity 98wt%, particle diameter is micron-sized, the preparation method of the oxygen content hafnium metal powder less than 0.2wt%.
It is an object of the invention to be achieved through the following technical solutions:
A kind of method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate, its preparation process comprises the steps:
A. by hafnium potassium fluorozirconate that mol ratio is 1:1 ~ 1:10 and reducing agent powder mix homogeneously, load in crucible；
B. crucible is put in retort, evacuation after building lid, be re-filled with argon washing, heat reduction, then carry out constant temperature insulation reduction；
C. then heating up, evacuation carries out vacuum distilling；
D. it is re-filled with argon, cools down under argon shield；
E. washing: first adopt pickling, then adopt deionized water wash, undertaken the product obtained sieving, drying, be high-purity hafnium powder product.
In step a, the purity of described hafnium potassium fluorozirconate is more than 98wt%, and granularity is about less than 1mm.
In step a, described reducing agent powder is Mg, Ca, Al, Al+Zn or the powder of their mixture, and the purity of described reducing agent powder is more than 98wt%, and the granularity of powder is less than 1mm.
In step a, described mixing adopts the mixing method that reactant is blended；The material of described crucible is Mo, Ta, Hf, W or Nb metal.
In step b, being evacuated to 0.01Pa ~ 0.1Pa, being namely filled with the vacuum before argon washing is 0.01Pa ~ 0.1Pa, and described heat reduction and constant temperature insulation reduction all carry out under argon shield.
In step b, the temperature of described heat reduction is 800 ~ 1450 DEG C, and the heating-up time is 0.5 ~ 20 hour.
In step b, the temperature of described constant temperature insulation reduction is 800 ~ 1450 DEG C, and temperature retention time is 0.5 ~ 20 hour.
In step c, being warming up to 850 ~ 1500 DEG C, namely the temperature of vacuum distilling is 850 ~ 1500 DEG C.Described evacuation is evacuation 0.5 ~ 10 hour after reduction terminates, before vacuum distilling, and vacuum is less than 0.1Mpa.
In step d, described cooling atmosphere under the protection of argon, must be cooled to room temperature.
Pickling described in step e is at room temperature to 70 DEG C, adopts the hydrochloric acid of 0.2 ~ 10M, sulphuric acid, nitric acid or their mixed acid, and pickling number of times is 1 ~ 15 time.
In step e, described deionized water wash is at room temperature to 100 DEG C, and with deionized water wash, number of times is 1 ~ 15 time.
The present invention passes through metallothermic reduction hafnium potassium fluorozirconate and vacuum distilling, and the purity preparing hafnium powder is more than 83wt%, even may be up to more than 98wt%, and particle diameter is micron-sized, and oxygen content is below 0.2wt%, and other metals and gas impurity content are low.
It is an advantage of the current invention that:
(1) present invention adopts hafnium potassium fluorozirconate to be raw material, and itself is oxygen-free, more superior than hafnium oxide, and the oxygen content in hafnium powder can be made to reduce.The present invention prepares the new method of high-purity hafnium powder, and it can effectively reduce the oxygen content in hafnium powder, and granularity is micron order, safely controllable, it is prevented that blast.
(2) present invention adopts hafnium potassium fluorozirconate to be raw material, and its volatility does not have hafnium fluoride, hafnium chloride strong, can effectively overcome the problem that hafnium fluoride, hafnium chloride make feed operation aspect.
(3) present invention adopts metallothermic reduction hafnium potassium fluorozirconate, adopts multiple reducing agent, such as the powder of Mg, Ca, Al, Zn, Al+Zn or their mixture, specify that the probability of above-mentioned reducing agent reduction hafnium potassium fluorozirconate.
(4) method of the present invention, adopts vacuum distilling can effectively remove volatile impurity in product, such as NaF, KF, AlF after the reduction3Deng.
(5) technique of the hafnium that the present invention prepares simply adopts reduction, distillation integration, and technique is simple.
(6) hafnium that the present invention prepares after vacuum distillation again pickling washing can effectively remove impurity, the purity making the final hafnium powder prepared is higher.
(7) the hafnium powder prepared may finally remove impurity further by electronic torch melting, final prepared ultra-pure metal hafnium.
Detailed description of the invention
Below by specific embodiment, the present invention will be further described, but is not meant to limiting the scope of the invention.
Embodiment 1
It is 98wt%, the granularity reducing agent powder Ca less than 1mm by purity 98wt%, the hafnium potassium fluorozirconate of granularity 1mm and purity, according to the ratio mix homogeneously of mol ratio 1:1, loads in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.01Pa after building lid, being filled with argon and wash, heating was warming up to 800 DEG C to 0.5 hour, argon shield.800 DEG C of constant temperature, after 0.5 hour, are warming up to 850 DEG C, evacuation 0.5 hour, and vacuum is 0.01Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.At room temperature being washed by the hydrochloric acid of product 0.2M 1 time, then at room temperature use deionized water wash 1 time, sieved by the product obtained, the hafnium opaque amount finally given is: the purity of hafnium powder is 85wt%.
Embodiment 2
By purity more than 98%, the granularity hafnium potassium fluorozirconate less than 1mm and purity is more than 98%, granularity is less than 1mm reducing agent powder Mg, according to the ratio mix homogeneously of mol ratio 1:2, load in tungsten crucible.Being put into by crucible in retort, after being evacuated to 0.03Pa after building lid, being filled with argon and wash, heating was warming up to 900 DEG C to 1 hour, argon shield.900 DEG C of constant temperature, after 2 hours, are warming up to 950 DEG C, evacuation 1 hour, and vacuum is 0.03Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.At room temperature being washed by the hydrochloric acid of product 1M 3 times, then at room temperature use deionized water wash 3 times, sieved by the product obtained, the hafnium opaque amount finally given is: the purity of hafnium powder is 84wt%.
Embodiment 3
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity is more than 98%, granularity is less than 1mm reducing agent powders A l, according to the ratio mix homogeneously of mol ratio 1:4, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.06Pa after building lid, being filled with argon and wash, heating was warming up to 1100 DEG C to 3 hours, argon shield.1100 DEG C of constant temperature, after 8 hours, are warming up to 1200 DEG C, evacuation 5 hours, and vacuum is 0.07Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.The hydrochloric acid of product 3M is at room temperature washed 2 times, then at room temperature use deionized water wash 7 times, the product obtained is sieved, the hafnium opaque amount finally given is: hafnium powder purity reaches 98.75wt%, particle diameter is about 3 μm, and oxygen content is less than 0.2wt%, and impurity content is relatively low.
Embodiment 4
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity more than reducing agent powders A l+Zn less than 1mm of 98wt%, granularity, according to the ratio mix homogeneously of mol ratio 1:5, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.07Pa after building lid, being filled with argon and wash, heating was warming up to 1050 DEG C to 4 hours, argon shield.1050 DEG C of constant temperature, after 10 hours, are warming up to 1250 DEG C, evacuation 6 hours, and vacuum is 0.02Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.At room temperature being washed by the hydrochloric acid of product 5M 7 times, then at room temperature use deionized water wash 8 times, sieved by the product obtained, the hafnium opaque amount finally given is: the purity of hafnium powder is 83wt%.
Embodiment 5
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity more than reducing agent powders A l less than 1mm of 98wt%, granularity, according to the ratio mix homogeneously of mol ratio 1:6, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.06Pa after building lid, being filled with argon and wash, heating was warming up to 1100 DEG C to 7 hours, argon shield.1100 DEG C of constant temperature, after 12 hours, are warming up to 1000 DEG C, evacuation 5 hours, and vacuum is 0.09Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.At room temperature being washed by the hydrochloric acid of product 6M 8 times, then at room temperature use deionized water wash 9 times, sieved by the product obtained, the hafnium opaque amount finally given is: the purity of hafnium powder is 90wt%.
Embodiment 6
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity more than reducing agent powders A l less than 1mm of 98wt%, granularity, according to the ratio mix homogeneously of mol ratio 1:7, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.07Pa after building lid, being filled with argon and wash, heating was warming up to 1150 DEG C to 8 hours, argon shield.1150 DEG C of constant temperature, after 14 hours, are warming up to 1200 DEG C, evacuation 7 hours, and vacuum is 0.06Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.At room temperature being washed by the hydrochloric acid of product 7M 10 times, then at room temperature use deionized water wash 12 times, sieved by the product obtained, the hafnium opaque amount finally given is: the purity of hafnium powder is 86wt%.Containing a small amount of Al in hafnium powder, it is to exist with the form of hafnium aluminium alloy.
Embodiment 7
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity more than reducing agent powder Ca less than 1mm of 98wt%, granularity, according to the ratio mix homogeneously of mol ratio 1:8, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.08Pa after building lid, being filled with argon and wash, heating was warming up to 1200 DEG C to 5 hours, argon shield.1200 DEG C of constant temperature, after 16 hours, are warming up to 1300 DEG C, evacuation 8 hours, and vacuum is 0.08Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.The hydrochloric acid of product 8M is at room temperature washed 12 times, then at room temperature use deionized water wash 10 times, the product obtained is sieved, the hafnium powder purity finally given reaches 95wt%, particle diameter is about 2 μm, and oxygen content is less than 0.2wt%, and impurity content is relatively low.
Embodiment 8
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity more than reducing agent powder Ca less than 1mm of 98wt%, granularity, according to the ratio mix homogeneously of mol ratio 1:9, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.09Pa after building lid, being filled with argon and wash, heating was warming up to 1300 DEG C to 9 hours, argon shield.1300 DEG C of constant temperature, after 18 hours, are warming up to 1400 DEG C, evacuation 9 hours, and vacuum is 0.05Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.The hydrochloric acid of product 9M is at room temperature washed 13 times, then at room temperature use deionized water wash 7 times, the product obtained is sieved, the hafnium opaque amount finally given is: the purity of hafnium powder is 99wt%, particle diameter is about 5 μm, and oxygen content is less than 0.2wt%, and impurity content is relatively low.
Embodiment 9
By purity more than hafnium potassium fluorozirconate less than 1mm of 98wt%, granularity and purity more than reducing agent powder Ca less than 1mm of 98wt%, granularity, according to the ratio mix homogeneously of mol ratio 1:10, load in molybdenum crucible.Being put into by crucible in retort, after being evacuated to 0.1Pa after building lid, being filled with argon and wash, heating was warming up to 1450 DEG C to 10 hours, argon shield.1450 DEG C of constant temperature, after 20 hours, are warming up to 1500 DEG C, evacuation 10 hours, and vacuum is 0.1Mpa, carries out vacuum distilling, is re-filled with argon to pressure-fired, cool down under argon shield.The hydrochloric acid of product 10M is washed 15 times at 70 DEG C, then at 100 DEG C with deionized water wash 15 times, the product obtained is sieved, the hafnium opaque amount finally given is: the purity of hafnium powder is 98.9wt%, particle diameter is that oxygen content is less than 0.2wt%, and impurity content is relatively low less than 1 μm.
The purity of the hafnium powder that the present invention prepares is more than 83wt%, even may be up to more than 98wt%, and granularity is micron order, and oxygen content is less than 0.2%, and other metals and gas impurity content are low.Preparation method of the present invention can effectively reduce the oxygen content in hafnium powder, and granularity is micron order, safely controllable, it is prevented that blast.
Claims (10)
1. the method preparing high-purity hafnium with hafnium potassium fluorozirconate for raw material, comprises the steps:
A. by hafnium potassium fluorozirconate that mol ratio is 1:1 ~ 1:10 and reducing agent powder mix homogeneously, load in crucible；
B. crucible is put in retort, evacuation after building lid, be re-filled with argon washing, heat reduction, then carry out constant temperature insulation reduction；
C. then heating up, evacuation carries out vacuum distilling；
D. it is re-filled with argon, cools down under argon shield；
E. washing: first adopt pickling, then adopt deionized water wash, undertaken the product obtained sieving, drying, be high-purity hafnium powder.
2. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: described reducing agent powder is Mg, Ca, Al, Al+Zn or the powder of their mixture.
3. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 2, it is characterised in that: the purity of described reducing agent powder is more than 98wt%, and the granularity of powder is less than 1mm；The purity of described hafnium potassium fluorozirconate is more than 98wt%, and granularity is less than 1mm.
4. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: described mixing adopts the mixing method that reactant is blended；The material of described crucible is Mo, Ta, Hf, W or Nb.
5. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: the described vacuum before argon washs that is filled with is 0.01Pa ~ 0.1Pa.
6. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: the temperature of described heat reduction is 800 ~ 1450 DEG C, and the heating-up time is 0.5 ~ 20 hour；The temperature of described constant temperature insulation reduction is 800 ~ 1450 DEG C, and temperature retention time is 0.5 ~ 20 hour.
7. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: the temperature of described vacuum distilling is 850 ~ 1500 DEG C.
8. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 7, it is characterised in that: before described vacuum distilling, the time of evacuation is 0.5 ~ 20 hour.
9. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: described pickling is at room temperature to 70 DEG C, adopts the hydrochloric acid of 0.2 ~ 10M, sulphuric acid, nitric acid or their mixed acid, and pickling number of times is 1 ~ 15 time；Described deionized water wash is at room temperature to 100 DEG C, and with deionized water wash, number of times is 1 ~ 15 time.
10. the method preparing high-purity hafnium for raw material with hafnium potassium fluorozirconate according to claim 1, it is characterised in that: the purity of the high-purity hafnium powder of gained is more than 83wt%, and oxygen content is below 0.2wt%, and particle diameter is micron order.
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| RU2002838C1 (en) * | 1991-07-11 | 1993-11-15 | Всероссийский научно-исследовательский институт химической технологии | Method of separation of zirconium and hafnium close in properties of elements |
| CN1751990A (en) * | 2005-11-03 | 2006-03-29 | 武汉科技大学 | Preparation method of transition metal carbide material |
| CN102528066A (en) * | 2010-12-16 | 2012-07-04 | 北京有色金属研究总院 | Superfine high-purity hafnium powder as well as preparation method and application thereof |
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- 2012-12-07 CN CN201210526237.4A patent/CN103862059B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4127409A (en) * | 1975-10-17 | 1978-11-28 | Teledyne Industries, Inc. | Method of reducing zirconium |
| EP0134643A2 (en) * | 1983-07-08 | 1985-03-20 | Solex Research Corporation of Japan | Preparing metallic zirconium, hafnium or titanium |
| RU2002838C1 (en) * | 1991-07-11 | 1993-11-15 | Всероссийский научно-исследовательский институт химической технологии | Method of separation of zirconium and hafnium close in properties of elements |
| CN1751990A (en) * | 2005-11-03 | 2006-03-29 | 武汉科技大学 | Preparation method of transition metal carbide material |
| CN102528066A (en) * | 2010-12-16 | 2012-07-04 | 北京有色金属研究总院 | Superfine high-purity hafnium powder as well as preparation method and application thereof |
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