CN106834854B - Alloy and preparation method are penetrated using rear-earth-doped high-performance Nb base hydrogen - Google Patents
Alloy and preparation method are penetrated using rear-earth-doped high-performance Nb base hydrogen Download PDFInfo
- Publication number
- CN106834854B CN106834854B CN201710091769.2A CN201710091769A CN106834854B CN 106834854 B CN106834854 B CN 106834854B CN 201710091769 A CN201710091769 A CN 201710091769A CN 106834854 B CN106834854 B CN 106834854B
- Authority
- CN
- China
- Prior art keywords
- alloy
- hydrogen
- raw material
- performance
- earth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/20—Arc remelting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The present invention provide it is a kind of using rear-earth-doped high-performance Nb base hydrogen through alloy and preparation method, chemical general formula Nb100‑(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 rare earth element La and Ce, a kind or a kind or more of element in Pr, Sm, Nd, Eu, Gd, Tb, Dy, Ho, Er, Sc, Y；10≤x≤30,10≤y≤30,5≤z≤20, x, y, z are 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, electric arc melting is at alloy cast ingot.The present invention has prepared the hydrogen with preferably infiltration hydrogen and hydrogen embrittlement energy of the various rare earth elements of addition 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 using rear-earth-doped high-performance Nb base hydrogen
Through 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 the rare earth elements such as Y, 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 to penetrate alloy and preparation method using rear-earth-doped high-performance Nb base hydrogen thus,
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, rear-earth-doped crystalline state
Hydrogen penetrates alloy using rear-earth-doped high-performance Nb base hydrogen through alloy；It is saturating that the second purpose is to provide high-performance Nb base hydrogen
Cross the preparation method of alloy.
An object of the present invention can be achieved by the following technical measures:
Alloy is penetrated using rear-earth-doped high-performance Nb base hydrogen, the Nb base hydrogen adulterated using high-performance rare-earth is through conjunction
The chemical general formula of gold is Nb100-(x+y+z)MxNyPz, wherein a kind or a kind or more of element in M Ti, Zr and Hf；N is Ni
The either element of a kind in Co or a kind or more；P be rare earth element La and Ce, Pr, Sm, Nd, Eu, Gd, Tb, Dy, Ho, Er,
1 kind or a kind or more of element in Sc, Y；10≤x≤30,10≤y≤30,5≤z≤20, x, y, z are Mole percent
Number.
An object of the present invention can be also achieved by the following technical measures:
This uses rear-earth-doped high-performance Nb base hydrogen through the maximum hydrogen coefficient that seeps of alloy for 4.1~4.6 × 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 preparation method of alloy is penetrated using the Nb base hydrogen of high-performance rare-earth doping, which 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, 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 raw material weighing is carried out according to stoicheiometry；
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 between 20~25g；For ingredient, the even tissue for improving purity He making alloy cast ingot, the melting of an alloy sample
Process is at least repeated 10 times, by ingot overturning when repeating every time；For containing the sample of certain refractory metals, fusion process is extremely
It is repeated 12 times less.
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.
Alloy is penetrated using rear-earth-doped high-performance Nb base hydrogen in the present invention, is prepared using vacuum arc melting method,
Used material purity is all larger than 99.9%.Electric arc melting is carried out under protection of argon gas, it is cooling using water jacketed copper crucible, very
Reciprocal of duty cycle 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 water jacket
Cooling (magnetic stirring), manufactured button ingot sample maximum weight are 20-25g.In order to improve purity and make alloy cast ingot ingredient,
The fusion process of even tissue, a usual alloy sample will be repeated 10 times, by ingot overturning when repeating every time.For containing
The sample of certain refractory metals, fusion process are repeated 12 times.A pure titanium ingot is put in stove, first to be melted before each molten alloy ingot
Pure titanium ingot is refined, to absorb remnant oxygen a small amount of inside stove, keeps high vacuum state.Present invention research has excellent infiltration hydrogen
The alloy film material of performance and anti-hydrogen embrittlement ability has prepared having for the various rare earth elements of addition using vacuum arc melting method
The hydrogen for preferably seeping hydrogen and hydrogen embrittlement energy penetrates alloy film material.
Detailed description of the invention
Fig. 1 is the specific implementation of the invention using rear-earth-doped high-performance Nb base hydrogen through the preparation method of alloy
The flow chart of example.
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.
Use rear-earth-doped high-performance Nb base hydrogen through the chemical general formula of alloy for Nb100-(x+y+z)MxNyPz；M is Ti, Zr
With a kind or a kind or more of element in Hf；N is a kind or a kind or more of element in Ni or Co；P is rare earth element
1 kind or a kind or more of element in La, Ce, Pr, Sm, Nd, Eu, Gd, Tb, Dy, Ho, Er, Sc, Y, 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 penetrates alloy, and maximum seeps hydrogen coefficient and is
(4.1~4.6) × 10-8mol·H2·m-1·s-1·Pa-0.5, 523~673K at a temperature of can seep hydrogen, anti-hydrogen embrittlement effect
It is good.
As shown in FIG. 1, FIG. 1 is the preparation methods of the invention that alloy is penetrated using rear-earth-doped high-performance Nb base hydrogen
Flow chart.
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
The infiltration hydrogen performance of sample at different temperatures.
The following are apply several specific embodiments of the invention.
Embodiment 1: the rear-earth-doped Nb base crystalline state hydrogen of one kind penetrates alloy, composition formula Nb40Zr25Co25(YSm)10。
Alloy sample system of the invention is prepared using vacuum arc melting method, and used material purity is all larger than 99.9%.In argon
Electric arc melting is carried out under gas shielded, cooling using water jacketed copper crucible, vacuum degree is 3 × 10-3Pa, melting electric current 1200A, striking side
Formula is high-frequency arc strike, and the melting kettle type of cooling is that water jacket is cooling (magnetic stirring), and manufactured button ingot example weight is 25g.One
The fusion process of a alloy sample will be repeated 10 times, by ingot overturning when repeating every time.Stove interior places a pure titanium ingot,
The pure titanium ingot of first melting is wanted before each molten alloy ingot, to absorb remnant oxygen a small amount of inside stove, keeps high vacuum state.
When doing hydrogen and testing thoroughly, alloy film thickness 0.7mm；0.5 μm of alumina particle is polished and passed through with the sand paper of variable grain degree
After being polished to mirror surface, the palladium membranes of 200nm thickness on two surface magnetic control sputterings of sample, test as cast condition sample is at different temperatures
Infiltration hydrogen performance.Seeping hydrogen coefficient in 673K maximum is 4.6 × 10-8molH2m-1s-1Pa-0.5, in 523K~673K temperature range
Hydrogen can be seeped, anti-hydrogen embrittlement effect is good.
Embodiment 2: the rear-earth-doped Nb base crystalline state hydrogen of one kind penetrates alloy, composition formula Nb48Hf21Ni19(DyPr)20。
Alloy sample system of the invention is prepared using vacuum arc melting method, and used material purity is all larger than 99.9%.In argon
Electric arc melting is carried out under gas shielded, cooling using water jacketed copper crucible, vacuum degree is 6 × 10-3Pa, melting electric current 1150A, striking side
Formula is high-frequency arc strike, and the melting kettle type of cooling is that water jacket is cooling (magnetic stirring), and manufactured button ingot example weight is 20g.One
The fusion process of a alloy sample is repeated 10 times, by ingot overturning when repeating every time.Stove interior places a pure titanium ingot, often
The pure titanium ingot of first melting is wanted before secondary molten alloy ingot, to absorb remnant oxygen a small amount of inside stove, keeps high vacuum state.It does
When hydrogen is tested thoroughly, alloy film thickness 1.0mm；0.5 μm of alumina particle throwing is polished and passed through with the sand paper of variable grain degree
After light is at mirror surface, the palladium membranes of 180nm thickness on two surface magnetic control sputterings of sample, test as cast condition sample is at different temperatures
Seep hydrogen performance.Seeping hydrogen coefficient in 673K maximum is 4.1 × 10-8molH2m-1s-1Pa-0.5, in 523K~673K temperature range all
Hydrogen can be seeped, anti-hydrogen embrittlement effect is good.
Embodiment 3: the rear-earth-doped Nb base crystalline state hydrogen of one kind penetrates alloy, composition formula Nb40Zr26Co24(ScGd)10。
Alloy sample system of the invention is prepared using vacuum arc melting method, and used material purity is all larger than 99.9%.In argon
Electric arc melting is carried out under gas shielded, cooling using water jacketed copper crucible, vacuum degree is 4.5 × 10-3Pa, melting electric current 1150A, striking
Mode is high-frequency arc strike, and the melting kettle type of cooling is that water jacket is cooling (magnetic stirring), and manufactured button ingot example weight is 23g.
The fusion process of one alloy sample will be repeated 10 times, by ingot overturning when repeating every time.Stove interior places a pure titanium
Ingot wants the pure titanium ingot of first melting before each molten alloy ingot, to absorb remnant oxygen a small amount of inside stove, keeps high vacuum shape
State.When doing hydrogen and testing thoroughly, alloy film thickness 0.8mm；0.5 μm of aluminium oxide granule is polished and passed through with the sand paper of variable grain degree
After grain is polished to mirror surface, the palladium membranes of 190nm thickness on two surface magnetic control sputterings of sample tests as cast condition sample in different temperatures
Under infiltration hydrogen performance.Seeping hydrogen coefficient in 673K maximum is 4.4 × 10-8molH2m-1s-1Pa-0.5, in 523K~673K temperature range
Interior to seep hydrogen, anti-hydrogen embrittlement effect is good.
Claims (4)
1. penetrating alloy using rear-earth-doped high-performance Nb base hydrogen, which is characterized in that this uses rear-earth-doped high-performance Nb
Base hydrogen is Nb through the chemical general formula of alloy100-(x+y+z)MxNyPz, wherein M is a kind or member of more than two kinds in Zr and Hf
Element；N is a kind or element of more than two kinds in Ni or Co；P be rare earth element La and Ce, Pr, Sm, Nd, Eu, Gd, Tb, Dy,
1 kind in Ho, Er, Sc, Y or element of more than two kinds；10≤x≤30,10≤y≤30,5≤z≤20, x, y, z are mole
Percentage.
2. according to claim 1 penetrate alloy using rear-earth-doped high-performance Nb base hydrogen, which is characterized in that the use
Rear-earth-doped high-performance Nb base hydrogen is (4.1~4.6) × 10 through the maximum hydrogen coefficient that seeps of alloy-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 preparation method described in claim 1 for penetrating alloy using rear-earth-doped high-performance Nb base hydrogen, which is characterized in that
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 raw material weighing is carried out according to stoicheiometry；
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 are molten
Electric current 1200A is refined, striking mode is high-frequency arc strike, and the melting kettle type of cooling is cooling for water jacket, manufactured button ingot sample weight
Amount is between 20~25g；For ingredient, the even tissue for improving purity He making alloy cast ingot, the melting of an alloy sample
Journey 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
It is repeated 12 times.
4. the preparation method according to claim 3 for penetrating alloy using rear-earth-doped high-performance Nb base hydrogen, feature
It is, the preparation method further includes, after step 3, after preparing alloy mother's ingot with arc melting method, with wire cutting instrument
Cut out laminar sample, alloy film thickness 0.7-1.0mm；It is polished with sand paper and passes through 0.5 μm of alumina particle and be polished to
After mirror surface, the pure palladium membranes of 180nm~200nm thickness on two surface magnetic control sputterings of sample, alloy film is not after palladium is plated in test
Infiltration hydrogen performance under synthermal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710091769.2A CN106834854B (en) | 2017-02-21 | 2017-02-21 | Alloy and preparation method are penetrated using rear-earth-doped high-performance Nb base hydrogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710091769.2A CN106834854B (en) | 2017-02-21 | 2017-02-21 | Alloy and preparation method are penetrated using rear-earth-doped high-performance Nb base hydrogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106834854A CN106834854A (en) | 2017-06-13 |
| CN106834854B true CN106834854B (en) | 2019-02-05 |
Family
ID=59134636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710091769.2A Active CN106834854B (en) | 2017-02-21 | 2017-02-21 | Alloy and preparation method are penetrated using rear-earth-doped high-performance Nb base hydrogen |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106834854B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117292852B (en) * | 2023-11-27 | 2024-03-08 | 西安稀有金属材料研究院有限公司 | Zirconium hydride moderating material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006283076A (en) * | 2005-03-31 | 2006-10-19 | Hitachi Metals Ltd | Dual phase alloy for separating/refining hydrogen |
| CN1939576A (en) * | 2005-09-26 | 2007-04-04 | 株式会社日本制钢所 | Hydrogen permeation alloy and a method of manufacturing the same |
| CN102851626A (en) * | 2012-09-21 | 2013-01-02 | 清华大学 | Preparation method of Nb-based amorphous alloy and stripe and hydrogen permeating metal film thereof |
-
2017
- 2017-02-21 CN CN201710091769.2A patent/CN106834854B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006283076A (en) * | 2005-03-31 | 2006-10-19 | Hitachi Metals Ltd | Dual phase alloy for separating/refining hydrogen |
| CN1939576A (en) * | 2005-09-26 | 2007-04-04 | 株式会社日本制钢所 | Hydrogen permeation alloy and a method of manufacturing the same |
| CN102851626A (en) * | 2012-09-21 | 2013-01-02 | 清华大学 | Preparation method of Nb-based amorphous alloy and stripe and hydrogen permeating metal film thereof |
Non-Patent Citations (2)
| Title |
|---|
| Nb-Ni(Co)-Ti(Hf)系合金凝固路径及组织和渗氢性能;闫二虎;《中国博士学位论文全文数据库 工程科技I辑》;20150115(第1期);第1045-1048页 |
| 氢气渗透Nb基合金的涉及及特性表征;罗伟民等;《稀有金属材料与工程》;20100630;第39卷(第6期);第B022-16页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106834854A (en) | 2017-06-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106834855B (en) | Alloy and preparation method are penetrated using the Nb base hydrogen of special elements doping | |
| Pang et al. | Corrosion behavior of Zr–(Nb–) Al–Ni–Cu glassy alloys | |
| Luo et al. | Three-dimensional nanoporous copper with high surface area by dealloying Mg–Cu–Y metallic glasses | |
| JP4756450B2 (en) | Double phase alloy for hydrogen separation and purification | |
| KR20130142467A (en) | Titanium-based bulk amorphous matrix composite and method of fabricating thereof | |
| TW200529920A (en) | Multiphase alloy and metal membrane for hydrogen separation-purification and methods for preparing the alloy and the metal membrane | |
| KR101391500B1 (en) | Hydrogen separation alloy and method for producing same | |
| Li et al. | Fabrication and characterization of bulk nanoporous copper by dealloying Al–Cu alloy slices | |
| Jinhong et al. | Influence of minor addition of In on corrosion resistance of Cu-based bulk metallic glasses in 3.5% NaCl solution | |
| CN106929729B (en) | Alloy and preparation method are penetrated using the Ta base hydrogen of special elements doping | |
| Zuo et al. | Fabrication of three-dimensional nanoporous nickel by dealloying Mg-Ni-Y metallic glasses in citric acid solutions for high-performance energy storage | |
| Jiang et al. | Effect of partial Ni substitution in V85Ni15 by Ti on microstructure, mechanical properties and hydrogen permeability of V-based BCC alloy membranes | |
| CN106834854B (en) | Alloy and preparation method are penetrated using rear-earth-doped high-performance Nb base hydrogen | |
| CN106868371B (en) | Alloy and preparation method are penetrated using rear-earth-doped high-performance Ta base hydrogen | |
| CN106917028B (en) | Alloy and preparation method are penetrated using the high-performance V base hydrogen of special elements doping | |
| Luo et al. | Hydrogen permeability in Nb–Ti–Ni alloys containing much primary (Nb, Ti) phase | |
| CN112095040B (en) | Multi-principal-element high-entropy alloy and preparation method thereof | |
| CN106929730B (en) | Alloy and preparation method are penetrated using rear-earth-doped V base hydrogen | |
| Liu et al. | Fabrication and dealloying behavior of monolithic nanoporous copper ribbons with bimodal channel size distributions | |
| Bölitz et al. | Microstructural study of boron-doped Co–Re–Cr alloys by means of transmission electron microscopy and electron energy-loss spectroscopy | |
| CN108977738A (en) | A kind of hydrogeneous titanium-based block amorphous alloy | |
| Li et al. | Tailored products of dealloying as-sintered Al–Cu alloys in sodium hydroxide solutions | |
| Gao et al. | Nanoporous NiAl Matrix Fabricated through Directional Solidification and Pulsed Electrochemical Dissolution | |
| CN109609880A (en) | A kind of light rare earth base block amorphous alloy and preparation method thereof containing metalloid | |
| Li et al. | Microstructure and phase transformation temperatures of two-phase FeAl (B2)+ FeAl2 alloys |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |