CN106917028B - Alloy and preparation method are penetrated using the high-performance V base hydrogen of special elements doping - Google Patents
Alloy and preparation method are penetrated using the high-performance V base hydrogen of special elements doping Download PDFInfo
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- CN106917028B CN106917028B CN201710088734.3A CN201710088734A CN106917028B CN 106917028 B CN106917028 B CN 106917028B CN 201710088734 A CN201710088734 A CN 201710088734A CN 106917028 B CN106917028 B CN 106917028B
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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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- C22C30/00—Alloys containing less than 50% by weight of each constituent
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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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- 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
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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Abstract
The present invention provides a kind of high-performance V base hydrogen using special elements doping through alloy and preparation method, chemical general formula V100‑(x+y+z)MxNyPz, wherein a kind or a kind or more of element in M Ti, Zr and Hf；N is a kind or a kind or more of element in Ni or Co；P is a kind or a kind or more of element in Cr, Fe, Cu, Al, Y, Mo, Ru, Rh, W, Si, Mn, Sn, Zn and Mg, and 10≤x≤30,10≤y≤30,5≤z≤20, x, y, z is mole percent.Preparation method includes: Incise the raw material, and clears up raw material surface；Material composition is calculated, and carries out raw material weighing；Carry out electric arc melting.The present invention has prepared the hydrogen with preferably infiltration hydrogen and hydrogen embrittlement energy of addition special elements through alloy film material using vacuum arc melting method.
Description
Technical field
The present invention relates to technical field of alloy material, especially relate to a kind of high-performance V adulterated using special elements
Base hydrogen penetrates alloy and preparation method.
Background technique
Hydrogen Energy have many advantages, such as efficiently, cleaning, renewable, rich reserves, from a wealth of sources, energy density is high, semiconductor,
The numerous areas such as fine chemistry industry, aerospace, fuel cell have broad application prospects, and are a kind of ideal secondary energy sources,
As the new energy system that 21 century holds the balance, many countries will develop hydrogen economy all in active development Hydrogen Energy in the world
As long term object.The sources of hydrogen are very various, other than water electrolysis hydrogen production, extraction industry byproduct (such as chlor-alkali,
Synthesis ammonia, coke-stove gas etc.) in hydrogen be also one of effective way for obtaining hydrogen；Usually industrial especially sophisticated industry is led
It is the high-purity hydrogen after separating-purifying used in domain.Separation Technique of Hydrogen Gas determines whether the hydrogen of acquisition meets industry
The standard for changing application, is the link of most critical in high-purity hydrogen technology of preparing, causes the interest of numerous researchers, which also promotes
The development of hydrogen isolation technics.Compared with pressure-variable adsorption, two kinds of cryogenic separation common hydrogen isolation technics, metal film hydrogen separation material by
In permeability with higher and higher diffusion coefficient, good high high-temp stability and mechanical performance, excellent toughness and
Hydrogen is selective and has broad application prospects.
Currently, palladium and palldium alloy (such as Pd-Ag alloy) are because having high differential permeability, good thermostabilization to hydrogen
Property, mechanical stability and catalytic activity, are widely studied and applied in hydrogen separation field.However, palladium resource is very
It is rare, expensive, it would be highly desirable to which that the New Hydrogen without palladium or few palladium for developing cheap, hypertonic hydrogen performance separates metal membrane material.Research
It was found that 5B race metal (Nb, V, Ta) has hydrogen infiltration coefficient more higher than palladium, and cost is more much lower than palldium alloy, is to have very much
The hydrogen separation membrane material of development prospect, however these pure metal caused hydrogen embrittlement during seeping hydrogen is very serious, can not apply
In actual production；Alloying is to solve the effective way of hydrogen embrittlement harm.
Domestic and foreign scholars develop polynary crystal alloy system mainly around the 5B such as Nb, V, Ta race's metal in recent years, to make
Standby good hydrogen penetrating quality existing out, and the polynary hydrogen of hydrogen embrittlement generation is highly resistant to through alloy film material.Such as Nb-Ni-
Ti system alloy has double structure, by primary phase bcc-Nb (Ti, Ni) solid solution (Primary phase) and eutectic phase { Nb
(Ti, Ni)+TiNi } (Eutectic phase) composition, hydrogen infiltration coefficient and hydrogen embrittlement energy with higher.Bcc primary phase
Nb (Ti, Ni) solid solution mainly serves during seeping hydrogen seeps hydrogen, but hydrogen embrittlement can occur；And eutectic phase Nb (Ti, Ni)+
TiNi } and compound therebetween mutually can effectively improve its hydrogen embrittlement.Some researches show that certain special elements, which are added, to be facilitated
Improve infiltration hydrogen and hydrogen embrittlement energy that hydrogen penetrates alloy.Currently, hydrogen is through alloy, it is still necessary to further increase the infiltration of its hydrogen and resist
Hydrogen embrittlement performance.We have invented a kind of new high-performance V base hydrogen using special elements doping to penetrate alloy and preparation side thus
Method, simple process, reliable performance.
Summary of the invention
An object of the present invention be to provide it is a kind of with high hydrogen permeability, high hydrogen embrittlement, mixed using special elements
Miscellaneous V base crystalline state hydrogen penetrates alloy through the high-performance V base hydrogen using special elements doping of alloy；The second purpose is to provide this
High-performance V base hydrogen penetrates the preparation method of alloy.
An object of the present invention can be achieved by the following technical measures: the high-performance V base adulterated using special elements
Hydrogen penetrates alloy, which penetrates the chemical general formula of alloy as V100-(x+y+z)MxNyPz,
Wherein, the element of a kind in M Ti, Zr and Hf or a kind or more；N is a kind or a kind or more of member in Ni or Co
Element；P be Cr, Fe, Cu, Al, Mo, Ru, Rh, W, Si, Mn, Sn, Zn and Mg in a kind or a kind or more of element, 10≤x≤
30,10≤y≤30,5≤z≤20, x, y, z are mole percent.
An object of the present invention can be also achieved by the following technical measures:
The high-performance V base hydrogen for using special elements to adulterate through alloy it is maximum seep hydrogen coefficient for (9.7~10.2) ×
10-8mol·H2·m-1·s-1·Pa-0.5, 523~673K at a temperature of can seep hydrogen, and there is hydrogen embrittlement energy.
The second object of the present invention can be achieved by the following technical measures: the high-performance V base adulterated using special elements
Hydrogen penetrates the preparation method of alloy, which includes: step through the preparation method of alloy
Rapid 1, Incise the raw material, and clear up raw material surface；
When Incise the raw material, blocky raw material are cut with wire electric discharge cutting instruments, are allowed to form graininess, convenient for mixing
Uniformly, facilitate melting；
When clearing up raw material surface, feed particulate material is successively carried out in chloroazotic acid, deionized water and acetone soln clear
It washes, to remove the oxidation film on raw material surface；
Step 2, material composition is calculated, and carries out raw material weighing；
Quality percentage when calculating material composition, according to alloy atom required for testing than calculating each component in sample
Than obtaining the weighing quality of each component multiplied by refined ingot quality with mass ratio；
When carrying out raw material weighing, service precision is to be uniformly mixed after the electronic balance of a ten thousandth weighs raw material；
Step 3, electric arc melting is carried out, uniformly mixed raw material is fitted into copper crucible, the first pure titanium ingot of melting absorbs remaining
Oxygen, then melting sample；
Electric arc melting is carried out under protection of argon gas, and cooling using water jacketed copper crucible, vacuum degree is 3~6 × 10-3Pa, it is maximum
Melting electric current 1200A, striking mode are high-frequency arc strike, and the melting kettle type of cooling is cooling for water jacket, manufactured button ingot sample
Weight is 20~25g；For ingredient, the even tissue for improving purity He making alloy cast ingot, the fusion process of an alloy sample
It is at least repeated 10 times, by ingot overturning when repeating every time；For containing the sample of certain refractory metals, fusion process is at least heavy
It is 15 times multiple.
The second object of the present invention can be also achieved by the following technical measures:
The preparation method further includes after step 3, after preparing alloy mother's ingot with arc melting method, being cut with line
It cuts instrument and cuts out laminar sample, alloy film thickness 0.7-1.0mm；0.5 μm of alumina particle throwing is polished and passed through with sand paper
After light is at mirror surface, alloy film after palladium is plated in the pure palladium membranes of 180nm~200nm thickness on two surface magnetic control sputterings of sample, test
Infiltration hydrogen performance at different temperatures.
The high-performance V base hydrogen using special elements doping in the present invention penetrates alloy, utilizes vacuum arc melting method system
Standby, used material purity is all larger than 99.9%.Electric arc melting is carried out under protection of argon gas, it is cold using water jacketed copper crucible
But, vacuum degree is 3~6 × 10-3Pa, maximum melting electric current 1200A, striking mode are high-frequency arc strike, the melting kettle type of cooling
Cooling (magnetic stirring) for water jacket, manufactured button ingot example weight is in 20~25g.In order to improve purity and make alloy cast ingot at
Divide, even tissue, the fusion process of a usual alloy sample will be repeated 10 times, by ingot overturning when repeating every time.For
Sample containing certain refractory metals, fusion process are repeated 15 times.A pure titanium ingot is put in stove, is wanted before each molten alloy ingot
The first pure titanium ingot of melting keeps high vacuum state to absorb remnant oxygen a small amount of inside stove.Present invention research has excellent
The alloy film material for seeping hydrogen performance and anti-hydrogen embrittlement ability, has prepared the various special elements of addition using vacuum arc melting method
Alloy film material is penetrated with the preferable hydrogen for seeping hydrogen and hydrogen embrittlement energy,
Detailed description of the invention
Fig. 1 is the high-performance V base hydrogen of the invention using special elements doping through the one specific of the preparation method of alloy
The flow chart of embodiment.
Specific embodiment
To enable above and other objects, features and advantages of the invention to be clearer and more comprehensible, preferably implementation is cited below particularly out
Example, and cooperate shown in attached drawing, it is described in detail below.
The high-performance V base hydrogen for using special elements to adulterate penetrates the chemical general formula of alloy as V100-(x+y+z)MxNyPz；M be Ti,
1 kind or a kind or more of element in Zr and Hf；N is a kind or a kind or more of element in Ni or Co；P be Cr, Fe,
1 kind or a kind or more of element in Cu, Al, Y, Mo, Ru, Rh, W, Si, Mn, Sn, Zn and Mg, 10≤x≤30,10≤y≤
30,5≤z≤20, x, y, z are mole percent.The hydrogen mainly contains hydrogen infiltration phase and resistance to hydrogen embrittlement phase two through alloy
Phase, in addition inevitably containing a small amount of certain intermetallic compound impurity phases.The hydrogen invented penetrates alloy, and maximum seeps hydrogen
Coefficient is (9.7~10.2) × 10-8mol·H2·m-1·s-1·Pa-0.5, 523~673K at a temperature of can seep hydrogen, resistant to hydrogen
It is crisp to work well.
As shown in FIG. 1, FIG. 1 is the preparation sides that the high-performance V base hydrogen of the invention using special elements doping penetrates alloy
The flow chart of method.
Step 101, Incise the raw material: blocky raw material are cut with wire electric discharge cutting instruments, are allowed to form graininess, just
In being uniformly mixed, facilitate melting.
Step 102, raw material removing surface: by feed particulate material successively in chloroazotic acid, deionized water and acetone soln
It is cleaned, to remove the oxidation film on raw material surface.
Step 103, material composition calculates: the quality according to alloy atom required for testing than calculating each component in sample
Percentage obtains the weighing quality of each component multiplied by refined ingot quality with mass ratio.
Step 104, weigh: service precision is to be uniformly mixed after the electronic balance of a ten thousandth weighs raw material.
Step 105, electric arc melting: uniformly mixed raw material is fitted into copper crucible, and the first pure titanium ingot of melting absorbs residual oxygen
Gas, then melting sample.
Step 106, after preparing alloy mother's ingot with arc melting method, laminar sample is cut out with wire cutting instrument.Alloy film
When doing hydrogen permeability test, thickness is generally 0.7-1.0mm；0.5 μm of oxidation is polished and passed through with the sand paper of variable grain degree
After alumina particles are polished to mirror surface, the palladium membranes of 180nm~200nm thickness on two surface magnetic control sputterings of sample, test flake
Infiltration hydrogen performance at different temperatures.
The following are apply several specific embodiments of the invention.
Embodiment 1: a kind of high-performance V base crystalline state hydrogen of special elements doping penetrates alloy, and composition formula is
V49Ti28Ni18Al5.Alloy sample system of the invention is prepared using vacuum arc melting method, and used material purity is big
In 99.9%.Electric arc melting is carried out under protection of argon gas, and cooling using water jacketed copper crucible, vacuum degree is 3 × 10-3Pa, melting electricity
1200A is flowed, striking mode is high-frequency arc strike, and the melting kettle type of cooling is that water jacket is cooling (magnetic stirring), manufactured button ingot sample
Product weight is 25g.The fusion process of one alloy sample will be repeated 10 times, by ingot overturning when repeating every time.Stove interior
A pure titanium ingot is placed, wants the pure titanium ingot of first melting before each molten alloy ingot, to absorb remnant oxygen a small amount of inside stove,
Keep high vacuum state.When doing hydrogen and testing thoroughly, alloy film thickness 0.7mm；It is polished with the sand paper of variable grain degree and passes through 0.5
μm alumina particle be polished to mirror surface after, the palladium membranes of 180nm thickness on two surface magnetic control sputterings of sample, test as cast condition sample
The infiltration hydrogen performance of product at different temperatures.Seeping hydrogen coefficient in 673K maximum is 9.7 × 10-8molH2m-1s-1Pa-0.5, 523K~
Hydrogen can be seeped in 673K temperature range.
Embodiment 2: a kind of high-performance V base crystalline state hydrogen of special elements doping penetrates alloy, composition formula V49Ti13Ni13
(CuSi)10.Alloy sample system of the invention is prepared using vacuum arc melting method, and used material purity is all larger than
99.9%.Electric arc melting is carried out under protection of argon gas, and cooling using water jacketed copper crucible, vacuum degree is 6 × 10-3Pa, melting electric current
1150A, striking mode are high-frequency arc strike, and the melting kettle type of cooling is that water jacket is cooling (magnetic stirring), manufactured button ingot sample
Weight is 20g.The fusion process of one alloy sample will be repeated 10 times, by ingot overturning when repeating every time.Stove interior is put
A pure titanium ingot is set, the pure titanium ingot of first melting is wanted before each molten alloy ingot, to absorb remnant oxygen a small amount of inside stove, is protected
Hold high vacuum state.When doing hydrogen and testing thoroughly, alloy film thickness 1.0mm；It is polished with the sand paper of variable grain degree and passes through 0.5 μm
Alumina particle be polished to mirror surface after, the palladium membranes of 200nm thickness on two surface magnetic control sputterings of sample, test as cast condition sample
Infiltration hydrogen performance at different temperatures.Seeping hydrogen coefficient in 673K maximum is 10.2 × 10-8molH2m-1s-1Pa-0.5, 523K~
Hydrogen can be seeped in 673K temperature range.
Embodiment 3: a kind of high-performance V base crystalline state hydrogen of special elements doping penetrates alloy, composition formula V49Ti22Ni14
(SnWMo)15.Alloy sample system of the invention is prepared using vacuum arc melting method, and used material purity is all larger than
99.9%.Electric arc melting is carried out under protection of argon gas, and cooling using water jacketed copper crucible, vacuum degree is 3.9 × 10-3Pa, melting electricity
1100A is flowed, striking mode is high-frequency arc strike, and the melting kettle type of cooling is that water jacket is cooling (magnetic stirring), manufactured button ingot sample
Product weight is 23g.The fusion process of one alloy sample will be repeated 10 times, by ingot overturning when repeating every time.Stove interior
A pure titanium ingot is placed, wants the pure titanium ingot of first melting before each molten alloy ingot, to absorb remnant oxygen a small amount of inside stove,
Keep high vacuum state.When doing hydrogen and testing thoroughly, alloy film thickness 0.75mm；It is polished and is passed through with the sand paper of variable grain degree
After 0.5 μm of alumina particle is polished to mirror surface, the palladium membranes of 190nm thickness on two surface magnetic control sputterings of sample, test casting
The infiltration hydrogen performance of aspect product at different temperatures.Seeping hydrogen coefficient in 673K maximum is 9.9 × 10-8molH2m-1s-1Pa-0.5,
Hydrogen can be seeped in 523K~673K temperature range.
Claims (4)
1. penetrating alloy using the high-performance V base hydrogen of special elements doping, which is characterized in that this uses the height of special elements doping
Performance V base hydrogen is V through the chemical general formula of alloy100-(x+y+z)MxNyPz, wherein M Ti；N is Ni；P be Al, (Cu, Si) or
(Sn, W, Mo), 10≤x≤30,10≤y≤30,5≤z≤20, x, y, z are mole percent.
2. the high-performance V base hydrogen according to claim 1 using special elements doping penetrates alloy, which is characterized in that should
The high-performance V base hydrogen for using special elements to adulterate seeps hydrogen coefficient through the maximum of alloy for 9.7~10.2 × 10-8mol·H2·
m-1·s-1·Pa-0.5, 523~673K at a temperature of can seep hydrogen, and there is hydrogen embrittlement energy.
3. the high-performance V base hydrogen described in claim 1 using special elements doping penetrates the preparation method of alloy, feature exists
In the preparation method includes:
Step 1, Incise the raw material, and clear up raw material surface；
When Incise the raw material, blocky raw material are cut with wire electric discharge cutting instruments, are allowed to form graininess, it is equal convenient for mixing
It is even, facilitate melting；
When clearing up raw material surface, feed particulate material is successively cleaned in chloroazotic acid, deionized water and acetone soln, with
Remove the oxidation film on raw material surface；
Step 2, material composition is calculated, and carries out raw material weighing；
When calculating material composition, according to mass percent of the required alloy atom than calculating each component in sample is tested, use
Mass ratio obtains the weighing quality of each component multiplied by refined ingot quality；
When carrying out raw material weighing, service precision is to be uniformly mixed after the electronic balance of a ten thousandth weighs raw material；
Step 3, electric arc melting is carried out, uniformly mixed raw material is fitted into copper crucible, the first pure titanium ingot of melting absorbs remnant oxygen,
Melting sample again；
Electric arc melting is carried out under protection of argon gas, and cooling using water jacketed copper crucible, vacuum degree is 3~6 × 10-3Pa, maximum melting
Electric current 1200A, striking mode are high-frequency arc strike, and the melting kettle type of cooling is cooling for water jacket, manufactured button ingot example weight
For 20~25g；For ingredient, the even tissue for improving purity He making alloy cast ingot, the fusion process of an alloy sample is at least
It is repeated 10 times, by ingot overturning when repeating every time；For containing the sample of certain refractory metals, fusion process at least repeats 15
It is secondary.
4. the high-performance V base hydrogen according to claim 3 using special elements doping penetrates the preparation method of alloy, special
Sign is that the preparation method further includes after step 3, after preparing alloy mother's ingot with arc melting method, using wire cutting
Instrument cuts out laminar sample, alloy film thickness 0.7-1.0mm；0.5 μm of alumina particle polishing is polished and passed through with sand paper
After mirror surface, the pure palladium membranes of 180nm~200nm thickness on two surface magnetic control sputterings of sample, alloy film exists after palladium is plated in test
Infiltration hydrogen performance under different temperatures.
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Non-Patent Citations (2)
| Title |
|---|
| Hydrogen transport through V85Ni10M5 alloy membranes;M.D. Dolan，et al;《Journal of Membrane Science》;20110124;14-19页 * |
| V-Ni-Ti multi-phase alloy membranes for hydrogen purification;G Song，et al;《Journal of Alloys and Compounds》;20110802;9322-9328页 * |
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