CN111926282A - Hydrogenation method for tantalum material and niobium material - Google Patents
Hydrogenation method for tantalum material and niobium material Download PDFInfo
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- CN111926282A CN111926282A CN202010604803.3A CN202010604803A CN111926282A CN 111926282 A CN111926282 A CN 111926282A CN 202010604803 A CN202010604803 A CN 202010604803A CN 111926282 A CN111926282 A CN 111926282A
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- niobium
- tantalum
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- alkaline earth
- earth metal
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- 239000000463 material Substances 0.000 title claims abstract description 74
- 239000010955 niobium Substances 0.000 title claims abstract description 70
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 70
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 64
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 53
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 53
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 26
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 26
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 21
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 239000002253 acid Substances 0.000 description 6
- 238000007664 blowing Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000004913 activation Effects 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002821 niobium Chemical class 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- -1 niobium metal oxide Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000004071 soot Substances 0.000 description 2
- 150000003481 tantalum Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- WTKKCYNZRWIVKL-UHFFFAOYSA-N tantalum Chemical compound [Ta+5] WTKKCYNZRWIVKL-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to a method for hydrogenating a tantalum material and a niobium material. The method is characterized by comprising the following steps: taking a tantalum material or a niobium material with a clean surface; charging the obtained tantalum material or niobium material into a crucible of a hydrogenation furnace, and adding a certain amount of alkali metal or alkaline earth metal around the crucible, wherein Be is not included in the alkaline earth metal; vacuumizing the hydrogenation furnace for the first time, filling high-purity hydrogen until the pressure reaches 0.1-2MPa, heating to 300-plus-one temperature for 600 ℃ and preserving heat for 2-6h, vacuumizing for the second time, continuously heating to 600-plus-one temperature for 1000 ℃ and preserving heat for 2-6h, filling high-purity hydrogen until the pressure reaches 0.1-2MPa, then powering off and cooling, and after the temperature is reduced to less than 60 ℃, evacuating and replacing to discharge redundant hydrogen and then discharging the hydrogen out of the furnace. The method adds a strong reducing agent in the conventional process, does not need early-stage chemical corrosion, and economically and environmentally improves the hydrogenation effect of tantalum/niobium ingots, sintered rods, blocks and the like.
Description
Technical Field
The present invention relates to a method for hydrogenating a tantalum material and a niobium material.
Background
The hydrogen brittleness of tantalum/niobium metal after hydrogen absorption is utilized, and tantalum/niobium powder with a certain particle size range and purity can be prepared through crushing, dehydrogenation and purification. The surface of the compact metal such as the tantalum/niobium sintered rod and the smelting ingot can be oxidized when the compact metal is crystallized or placed in the air for a long time to generate a protective oxide film, the oxide film can prevent hydrogen from permeating into the metal and reduce the hydrogen absorption amount, so that the hydrogenation effect of the final metal is influenced, and the tantalum/niobium ingot after hydrogenation can show the phenomena of blocky crystals, unobvious layering, insufficient intermediate hydrogenation and the like, so that the subsequent powder preparation is hindered.
In the prior art, activation treatment needs to be carried out before hydrogenation, one is vacuum high-temperature activation treatment, namely, before hydrogenation, a material to be hydrogenated is firstly in a hydrogen atmosphere or is heated to high temperature (1200-1500 ℃) in vacuum, so that an oxide film on the surface of a metal has defects, and hydrogen is favorably diffused into the metal; the other is chemical treatment, namely soaking in acid solution such as HF with certain concentration, thereby removing or reducing the oxide film on the surface of the metal to increase the hydrogen absorption amount of the metal. The first treatment method has higher requirements on equipment, consumes more energy and is not economical; the second treatment method uses HF acid with a certain concentration, is not environment-friendly, and is easy to generate a new oxide film on the surface of the niobium ingot due to different acid corrosion degrees or different corrosion times and the like, so that the permeation of hydrogen is prevented in the temperature-rising hydrogenation process, and the hydrogenation effect is not ideal. In order to ensure the hydrogenation effect, in chinese patent CN103147050B, the tantalum ingot needs to be cut into 5-10 mm blocks by 5-10 mm in advance, and then hydrogenated; chinese patent CN106216695A is to crush tantalum rods into 2-5mm fragments by a crusher and then carry out dehydrogenation powder preparation. The above-mentioned operations of cutting or crushing beforehand introduce new impurities and increase the loss of material.
Disclosure of Invention
The invention aims to provide a method for hydrogenating a tantalum material and a niobium material, which can economically and environmentally improve the hydrogenation effect of the tantalum material and the niobium material without early-stage chemical corrosion.
A method for hydrogenating a tantalum material and a niobium material, comprising the steps of:
(1) taking a tantalum material or a niobium material with a clean surface;
(2) charging the obtained tantalum material or niobium material into a crucible of a hydrogenation furnace, and adding a certain amount of alkali metal or alkaline earth metal around the crucible, wherein Be is not included in the alkaline earth metal;
(3) vacuumizing the hydrogenation furnace for the first time, filling high-purity hydrogen until the pressure reaches 0.1-2MPa, heating to 300-plus-one temperature for 600 ℃ and preserving heat for 2-6h, vacuumizing for the second time, continuously heating to 600-plus-one temperature for 1000 ℃ and preserving heat for 2-6h, filling high-purity hydrogen until the pressure reaches 0.1-2MPa, then powering off and cooling, and after the temperature is reduced to less than 60 ℃, evacuating and replacing to discharge redundant hydrogen and then discharging the hydrogen out of the furnace.
In the step (2), the form of the alkali metal or the alkaline earth metal is in a stable state at normal temperature, and the addition amount of the alkali metal or the alkaline earth metal is 0.02 to 0.1 percent of the weight of the tantalum material or the niobium material.
In the step (2), the alkali metal is potassium or sodium, and the alkaline earth metal is magnesium, calcium, strontium or barium.
And (4) vacuumizing the first time and the second time in the step (3) to 0-100 MPa.
A method for hydrogenating a tantalum material and a niobium material, comprising the steps of:
(1) taking a tantalum material or a niobium material with a clean surface;
(2) charging the obtained tantalum material or niobium material into a crucible of a hydrogenation furnace, and adding a certain amount of alkali metal or alkaline earth metal around the crucible, wherein Be is not included in the alkaline earth metal;
(3) heating the hydrogenation furnace to 600-plus-1000 ℃, vacuumizing the hydrogenation furnace, preserving heat for 2-6h at the temperature of 600-plus-1000 ℃, then filling high-purity hydrogen with 0.1-2MPa, continuously preserving heat for 2-6h at the temperature of 600-plus-1000 ℃, then cutting off power and reducing temperature, after the temperature is reduced to less than 60 ℃, evacuating and replacing to discharge redundant hydrogen, and discharging the hydrogen out of the furnace.
In the step (2), the form of the alkali metal or the alkaline earth metal is in a stable state at normal temperature, and the addition amount of the alkali metal or the alkaline earth metal is 0.02 to 0.1 percent of the weight of the tantalum material or the niobium material.
In the step (2), the alkali metal is potassium or sodium, and the alkaline earth metal is magnesium, calcium, strontium or barium.
And (3) vacuumizing to 0-100 MPa.
The hydrogenation method solves the problem of poor hydrogenation effect of the tantalum/niobium material on the premise of not needing activation treatment. The hydrogenation method is applied to the hydrogenation treatment of tantalum/niobium/titanium ingots, tantalum/niobium/titanium sintered rods and tantalum/niobium/titanium billets. The hydrogenation method reduces the prior activation treatment, not only avoids the use of HF acid in the prior period, but also avoids high-temperature heating treatment, so the hydrogenation method is more environment-friendly and economic. The method adds a strong reducing agent in the conventional process, does not need early-stage chemical corrosion, and economically and environmentally improves the hydrogenation effect of tantalum/niobium ingots, sintered rods, blocks and the like.
Detailed Description
The prior art has the following defects: the activation treatment before hydrogenation has high requirements on equipment, large energy consumption and poor economical efficiency on one hand, and uses HF which is not environment-friendly on the other hand; the cutting and crushing treatment before hydrogenation not only increases the impurity content of the raw materials, but also increases the loss of the materials. The method solves the problem of poor hydrogenation effect of the tantalum/niobium material in the prior art. In order to improve the hydrogenation effect of tantalum/niobium materials in practical operation, it is necessary to activate the valve metal surface or perform multiple hydrogenations before hydrogenating the tantalum/niobium material.
The surface purification treatment of the tantalum/niobium material in the step (1) of the method is a treatment mode which is automatically selected according to the surface cleanliness of the tantalum/niobium material, if the surface cleanliness is high, the treatment can be omitted or only the soot blowing of the surface is carried out by using compressed air, and if impurities such as oil stains and the like exist on the surface, the treatment can be carried out by using HCL or nitric acid with certain concentration and the flushing and drying are carried out by using pure water, which belong to the conventional technologies in the field.
When the hydrogen is added in the step (3) and the temperature is raised to 600 ℃ of 300-x(M ═ alkali metal, x ═ 1; M ═ alkaline earth metal, x;, 2;), and MHxHas strong reducibility, and MH is vacuumized and at the temperature of 600-1000 DEG CxIn the gaseous state, MHxCan reduce tantalum/niobium metal oxide, thus destroying oxide film on the surface of tantalum/niobium material, promoting hydrogen to permeate into metal in the power-off and temperature-reducing process, enhancing hydrogen absorption effect of tantalum/niobium metal, and further reducing oxygen content of hydrogenated tantalum/niobium material.
Example 1:
blowing dust on the surface of 1 cylindrical niobium ingot with the diameter of 120mm and the weight of 100kg by using compressed air, then loading the niobium ingot into a crucible of a hydrogenation furnace, adding 100g of sodium blocks around the crucible, evacuating the hydrogenation furnace (-2MPa), then filling high-purity hydrogen with the pressure of 1.0MPa (actually filling the hydrogen until the pressure reaches 1.0MPa), raising the temperature to 600 ℃, keeping the temperature for 2 hours, then evacuating the hydrogenation furnace again (-40MPa), continuing to raise the temperature to 950 ℃, keeping the temperature for 4 hours, then filling the high-purity hydrogen with the pressure of 1.2MPa (actually filling the hydrogen until the pressure reaches 1.2MPa), then stopping the power, naturally cooling to ensure that the niobium ingot can fully absorb the hydrogen and react with the hydrogen, evacuating the hydrogen in the hydrogenation furnace after the temperature is reduced to less than 60 ℃, finally obtaining the hydrogenated niobium ingot which is obvious in layering, easy to peel and has no sandwich phenomenon.
The invention also relates to a method step (3), under the conditions of vacuum pumping and temperature of 600-1000 ℃, alkali metal or alkaline earth metal (except Be) is evaporated and is attached to materials needing hydrogenation, such as tantalum/niobium ingot, sintered rod and the like, when hydrogen is added, the corresponding alkali metal or alkaline earth metal (except Be) reacts with the hydrogen to produce ionic hydride MHx (M ═ alkali metal, x ═ 1; M ═ alkaline earth metal, x ═ 2;) with strong reducibility, hydride generated at the temperature of 600-1000 ℃ can reduce tantalum/niobium metal oxide, thereby destroying the oxidation film on the surface of the tantalum/niobium material, promoting the hydrogen to permeate into the metal in the power failure cooling process, enhancing the hydrogen absorption effect of the tantalum/niobium metal, and further reducing the oxygen content of the tantalum/niobium material after hydrogenation.
Example 2:
blowing dust on the surface of 1 cylindrical niobium ingot with the diameter of 120mm and the weight of 100kg by using compressed air, then loading the niobium ingot into a crucible of a hydrogenation furnace, adding 100g of sodium blocks around the crucible, heating the hydrogenation furnace to 900 ℃, vacuumizing to the pressure less than-60 MPa, preserving heat for 2 hours at the temperature of 900 ℃, then introducing high-purity hydrogen with the pressure of 1.0MPa into the hydrogenation furnace (actually introducing the hydrogen to the pressure of 1.0MPa), continuing preserving heat for 6 hours at the temperature of 900 ℃, then naturally cooling by power failure, evacuating and discharging the hydrogen in the hydrogenation furnace after the temperature is reduced to the temperature of less than 60 ℃, and finally obtaining the hydrogenated niobium ingot which is obvious in layering, easy to peel and free of sandwich phenomenon after being discharged from the furnace.
Example 3:
blowing soot on the surface of 1 cylindrical niobium sintered rod with the diameter of 120mm and the weight of 100kg by using compressed air, then placing the niobium sintered rod into a crucible of a hydrogenation furnace, adding 20g of sodium blocks around the crucible, heating the hydrogenation furnace to 900 ℃, vacuumizing to the pressure less than-60 MPa, preserving heat for 2 hours at the temperature of 900 ℃, then introducing high-purity hydrogen with the pressure of 1.0MPa into the hydrogenation furnace (actually introducing the hydrogen until the pressure reaches 1.0MPa), continuing preserving heat for 6 hours at the temperature of 900 ℃, then naturally cooling by power failure, evacuating and discharging the hydrogen in the hydrogenation furnace after the temperature is reduced to less than 60 ℃, and finally obtaining the hydrogenated niobium rod which is obvious in layering, easy to peel and free of sandwich phenomenon after being discharged from the furnace.
Example 4:
blowing dust on the surfaces of 1 cylindrical tantalum ingot with the diameter of 120mm and the weight of 100kg by using compressed air, then loading the tantalum ingot into a crucible of a hydrogenation furnace, adding 100g of calcium blocks around the crucible, heating the hydrogenation furnace to 950 ℃, vacuumizing to the pressure less than-60 MPa, preserving heat for 2 hours at the temperature of 950 ℃, then introducing high-purity hydrogen with the pressure of 1.0MPa into the hydrogenation furnace (actually introducing the hydrogen to the pressure of 1.0MPa), continuing preserving heat for 6 hours at the temperature of 950 ℃, then naturally cooling by power failure, evacuating and discharging the hydrogen in the hydrogenation furnace after the temperature is reduced to the temperature of less than 60 ℃, and finally obtaining the hydrogenated tantalum ingot which is obvious in layering, easy to peel and free of sandwich phenomenon after being discharged from the furnace.
Example 5:
blowing dust on the surface of 1 cylindrical tantalum rod with the diameter of 120mm and the weight of 100kg by using compressed air, then placing the tantalum rod into a crucible of a hydrogenation furnace, adding 20g of magnesium powder around the crucible, heating the hydrogenation furnace to 900 ℃, vacuumizing to the pressure of less than-60 MPa, preserving heat at the temperature of 900 ℃ for 2 hours, then introducing high-purity hydrogen with the pressure of 1.0MPa into the hydrogenation furnace, continuing preserving heat at the temperature of 900 ℃ for 6 hours, then powering off to reduce the temperature, evacuating and discharging the hydrogen in the hydrogenation furnace after the temperature is reduced to the temperature of less than 60 ℃, and finally discharging the tantalum ingot after hydrogenation from the furnace, wherein the tantalum ingot is obviously layered, easy to peel and free of sandwich phenomenon.
Comparative example 1:
soaking 100kg niobium ingot with the diameter of 120mm by using 30% HF acid for 8 hours to erode the outer surface of the niobium ingot by using acid, then washing the niobium ingot by using pure water and drying the niobium ingot, then loading the niobium ingot into a crucible of a hydrogenation furnace, vacuumizing the hydrogenation furnace to the pressure of less than-60 MPa, heating the niobium ingot to 900 ℃, preserving the heat for 2 hours, then introducing high-purity hydrogen with the pressure of 0.8MPa into the hydrogenation furnace, continuing preserving the heat for 6 hours, then powering off and cooling the niobium ingot, evacuating and discharging the hydrogen in the hydrogenation furnace after the temperature is reduced to the temperature of less than 60 ℃, finally discharging the niobium ingot from the furnace to obtain the hydrogenated niobium ingot, wherein the niobium ingot presents the phenomenon of insufficient hydrogenation such as blocky crystals, unobvious layering and the like.
Claims (8)
1. A method for hydrogenating a tantalum material and a niobium material, comprising the steps of:
(1) taking a tantalum material or a niobium material with a clean surface;
(2) charging the obtained tantalum material or niobium material into a crucible of a hydrogenation furnace, and adding a certain amount of alkali metal or alkaline earth metal around the crucible, wherein Be is not included in the alkaline earth metal;
(3) vacuumizing the hydrogenation furnace for the first time, filling high-purity hydrogen until the pressure reaches 0.1-2MPa, heating to 300-plus-one temperature for 600 ℃ and preserving heat for 2-6h, vacuumizing for the second time, continuously heating to 600-plus-one temperature for 1000 ℃ and preserving heat for 2-6h, filling high-purity hydrogen until the pressure reaches 0.1-2MPa, then powering off and cooling, and after the temperature is reduced to less than 60 ℃, evacuating and replacing to discharge redundant hydrogen and then discharging the hydrogen out of the furnace.
2. A method for hydrogenating a tantalum material and a niobium material in accordance with claim 1, wherein: in the step (2), the form of the alkali metal or the alkaline earth metal is in a stable state at normal temperature, and the addition amount of the alkali metal or the alkaline earth metal is 0.02 to 0.1 percent of the weight of the tantalum material or the niobium material.
3. A method for hydrogenating a tantalum material and a niobium material in accordance with claim 1, wherein: in the step (2), the alkali metal is potassium or sodium, and the alkaline earth metal is magnesium, calcium, strontium or barium.
4. A method for hydrogenating a tantalum material and a niobium material in accordance with claim 1, wherein: and (4) vacuumizing the first time and the second time in the step (3) to 0-100 MPa.
5. A method for hydrogenating a tantalum material and a niobium material, comprising the steps of:
(1) taking a tantalum material or a niobium material with a clean surface;
(2) charging the obtained tantalum material or niobium material into a crucible of a hydrogenation furnace, and adding a certain amount of alkali metal or alkaline earth metal around the crucible, wherein Be is not included in the alkaline earth metal;
(3) heating the hydrogenation furnace to 600-plus-1000 ℃, vacuumizing the hydrogenation furnace, preserving heat for 2-6h at the temperature of 600-plus-1000 ℃, then filling high-purity hydrogen with 0.1-2MPa, continuously preserving heat for 2-6h at the temperature of 600-plus-1000 ℃, then cutting off power and reducing temperature, after the temperature is reduced to less than 60 ℃, evacuating and replacing to discharge redundant hydrogen, and discharging the hydrogen out of the furnace.
6. A method for hydrogenating a tantalum material and a niobium material in accordance with claim 1, wherein: in the step (2), the form of the alkali metal or the alkaline earth metal is in a stable state at normal temperature, and the addition amount of the alkali metal or the alkaline earth metal is 0.02 to 0.1 percent of the weight of the tantalum material or the niobium material.
7. A method for hydrogenating a tantalum material and a niobium material in accordance with claim 1, wherein: in the step (2), the alkali metal is potassium or sodium, and the alkaline earth metal is magnesium, calcium, strontium or barium.
8. A method for hydrogenating a tantalum material and a niobium material in accordance with claim 1, wherein: and (3) vacuumizing to 0-100 MPa.
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| CN201911426274 | 2019-12-30 | ||
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115156542A (en) * | 2022-07-09 | 2022-10-11 | 湖南宏承新材料科技有限公司 | Preparation method of low-oxygen niobium powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1305227A (en) * | 1961-11-13 | 1962-09-28 | Union Carbide Corp | New tantalum powder and its manufacturing process |
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| CN115156542A (en) * | 2022-07-09 | 2022-10-11 | 湖南宏承新材料科技有限公司 | Preparation method of low-oxygen niobium powder |
| CN115156542B (en) * | 2022-07-09 | 2023-09-05 | 湖南宏承新材料科技有限公司 | Preparation method of low-oxygen niobium powder |
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