CN108160989A - A kind of preparation method of antitoxinization metal hydrogen-absorbing material - Google Patents
A kind of preparation method of antitoxinization metal hydrogen-absorbing material Download PDFInfo
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- CN108160989A CN108160989A CN201611120517.XA CN201611120517A CN108160989A CN 108160989 A CN108160989 A CN 108160989A CN 201611120517 A CN201611120517 A CN 201611120517A CN 108160989 A CN108160989 A CN 108160989A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/508—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by selective and reversible uptake by an appropriate medium, i.e. the uptake being based on physical or chemical sorption phenomena or on reversible chemical reactions
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1689—After-treatment
- C23C18/1692—Heat-treatment
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/04—Hydrogen absorbing
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Abstract
The invention discloses a kind of preparation methods of antitoxinization metal hydrogen-absorbing material.This method is：Machinery powder is into metallic particles after carrying out part hydrogenation to metal hydrogen-absorbing material, Pd films are coated in surface of metal particles using the method for chemical plating successively and Cu films form Pd Cu composite membranes, then the metallic particles after cladding is heat-treated, makes Pd Cu composite membrane alloyings.The antitoxinization metal hydrogen-absorbing material prepared by this method, the Pd Cu alloy films on its surface, which are not easily broken, during hydrogen is put in suction comes off, it ensure that the stability of material hydrogen storage property in the hydrogen isotope gas of impure gas, i.e. material has higher service life cycle.
Description
Technical field
The present invention relates to a kind of preparation methods of antitoxinization metal hydrogen-absorbing material, and in particular to a kind of in impure gas
The preparation method of metal hydrogen-absorbing material with high circulation service life in hydrogen isotope gas belongs to hydrogen isotope recycling, storage
Transport field of material technology.
Background technology
Hydrogen and its isotope are important energy substance, and in social production and national defense applications, hydrogen and its isotope all account for
There is critical role, hydrogen-absorbing material can realize controlled absorbed and the release to hydrogen and its isotope, meet each hydrogen-like application field
To the safe storage of hydrogen and transport demand.But in the actual application of hydrogen and its isotope, portion is often contained in hydrogen
Divide foreign gas, such as CO, CO2、CH4、O2、N2Deng.These foreign gases are often easier to react with hydrogen-absorbing material, in material
Material surface forms the film layer of fine and close metal carbides, nitride, oxide, and blocking hydrogen makes suction hydrogen to alloy diffusion inside
Material hydrogen-absorbing ability is substantially reduced or even completely loses, that is, is poisoned.Therefore, there is an urgent need for the antitoxinization performances to hydrogen-absorbing material
Improved, to meet efficient suction hydrogen application of the hydrogen-absorbing material in impure hydrogen.
Poison improvement problem for anti-foreign gas of the metal hydrogen-absorbing material in hydrogen application is inhaled, carry out both at home and abroad
Some correlative studys work.It is general to improve the anti-toxicity of material using anti-poisoning modification is carried out to metal hydrogen-absorbing material surface
Energy.Silica gel, metal Pd or the Pd-Ag alloys that there is selectivity to penetrate ability to hydrogen are such as coated on hydrogen-absorbing material surface.But
It is, since gel coated layer is blocked up, to easily lead to material and effectively inhale hydrogen rate and drastically decline.And metal Pd film is inhaled below 300 DEG C and is taken off
During attached hydrogen, it may occur that the phase co-conversion between α phases and β phases, since the lattice constant of two kinds of phases has differences, β phases are in α phases
Nucleation and growth can generate serious stress in the material so that dusting occurs after hydrogenation/dehydrogenation for Pd films experience several times, and then
Its selected area update strategy ability to hydrogen is reduced, so that the service life cycle of material reduces.The hydrogen of Pd-Ag alloy films is saturating
Excessive and mechanical strength is higher than pure Pd films, but Pd-Ag alloy films reduce film layer at high temperature in use, its crystal grain can grow up
Compactness and mechanical strength lead to the reduction of its hydrogen selective permeation so that cycle suction of the hydrogen-absorbing material in foreign gas is put
Hydrogen hydraulic performance decline shows as the reduction of material circulation service life.
Invention content
It is an object of the invention to propose a kind of preparation method of antitoxinization metal hydrogen-absorbing material.It is prepared using this method
Metal hydrogen-absorbing material has high circulation service life, it can be achieved that containing CO, CO in the hydrogen isotope gas of impure gas2、
CH4、O2、N2Etc. repeatedly inhale in the hydrogen isotope gas of foreign gases and put hydrogen.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of antitoxinization metal hydrogen-absorbing material carries out metal hydrogen-absorbing material in machinery powder after the hydrogenation of part
Into metallic particles, Pd films are coated in surface of metal particles using the method for chemical plating successively and Cu films form Pd-Cu composite membranes, so
The metallic particles after cladding is heat-treated afterwards, makes Pd-Cu composite membrane alloyings.
Wherein, the partially hydrogenated method is：Under the conditions of 100~500 DEG C, 0.01~5MPa Hydrogen Vapor Pressures, make gold
Belong to hydrogen-absorbing material and inhale hydrogen, inhale the hydrogen time between 0.5~6 hour, then take off metal material part using vacuum pumping method again
Hydrogen, after being cooled to room temperature, under 0.01~5MPa Hydrogen Vapor Pressures, hydrogen content in metal hydrogen-absorbing material 0.1~200mL/g it
Between.
Wherein, the granularity after the metal hydrogen-absorbing material part hydrogenation after machinery powder processed is 20~300 mesh.
Wherein, the Pd-Cu composite membranes are the composite membrane of Pd-Cu, Pd-Cu-Pd or Pd-Cu-Pd-Cu form.
Wherein, in the plating solution of chemical plating Pd films, pd2+A concentration of 0.005~0.02mol/L, bath temperature be 45~55
DEG C, the amount of alloying pellet is 0.5~30kg/L in plating solution, and the rate of addition of reducing agent is 0.6~500mL/min, plating time
10~30min.
Wherein, in the plating solution of Electroless Cu Plating film, Cu2+A concentration of 0.028~0.11mol/L, bath temperature be 45~55
DEG C, the amount of alloying pellet is 0.5~30kg/L in plating solution, and the rate of addition of reducing agent is 1~1000mL/min, plating time
0.5~50min.
Wherein, heat treatment temperature be 400~800 DEG C, heat treatment time be 4~24 hours, protective atmosphere for high-purity hydrogen,
High-purity argon gas or high-purity helium.
The advantage of the invention is that：
1st, present invention employs partial hydrogenation process, make metal hydrogen-absorbing material that certain journey first occur before Pd-Cu films are coated
The volume expansion of degree so as to reduce the volume expansion degree inhaled after cladding processing during hydrogen, improves hydrogen-absorbing material suction and puts hydrogen and lead
The pulverization situation of cause.
2nd, it present invention employs layering chemical plating cladding Pd-Cu composite membranes, then carries out heat treatment and forms Pd-Cu alloy films
Method has stronger mechanical strength, and the crystal grain being not present under high temperature to be grown up now using Pd-Cu alloy films prepared by this method
As ensure that the compactness of film layer, can realizing that multiple inhale of the metal hydrogen-absorbing material after cladding puts hydrogen recycling.
Description of the drawings
Fig. 1 is Zr0.9Ti0.1Co alloy surfaces coat Pd film patterns.
Fig. 2 is the Zr of Pd claddings0.9Ti0.1Co alloy surfaces coat Cu film patterns.
Fig. 3 is Zr after heat treatment0.9Ti0.1Co alloy surfaces coat Pd-Cu alloy film patterns.
Fig. 4 is the Zr that Pd-Cu alloy films and Pd films coat0.9Ti0.1Co alloy cycle lives compare.
Specific embodiment
To prepare antitoxinization Zr0.9Ti0.1Co alloy materials are embodiment, introduce and carry out part hydrogenation and dehydrogenization, Pd- to alloy
Cu films cladding, the implementation of heat treatment.
Zr prepared by vacuum intermediate-frequency induction melting0.9Ti0.1Co alloys, Mechanical Crushing are less than the bulk of 50mm into diameter.
Then by 30kg Zr0.9Ti0.1Co alloy blocks are encapsulated into hydrogenation furnace, and hydrogenation furnace is evacuated to 10-1Then Pa opens hydrogenation
Stove temperature control system sets heating rate as 4 DEG C/min, and 430 DEG C of target temperature continues after 3 hours are vacuumized to system, will be in stove
Temperature is cooled to 410 DEG C in 2h, and the high-purity hydrogen of 4200L is then filled with into stove, and alloy starts to inhale hydrogen, and furnace pressure starts
Decline, after 4h, treat furnace pressure stabilization in 0.3MPa, in-furnace temperature is reduced to 390 DEG C.400 DEG C are warming up to hydrogenation furnace, during heating
Between 0.5h, be then turned on hydrogenation furnace hydrogen discharging valve, alloy starts dehydrogenation, use hydrogen quality testing flow meter put hydrogen integrated flow for
Thus 3500L is calculated, hydrogen content 23mL/g in alloy.Hydrogenation furnace is cooled to room temperature, takes out alloy block, alloy block is kept not
State before hydrogenation, as shown in Figure 1.By alloy block Mechanical Crushing into 40-100 targeted fine powders, for plated film.
Weigh the Zr of 3kg 40-100 mesh0.9Ti0.1Co alloyed powders after its first perfluorinated and sensitization, activation, pour into chemistry
In the plating solution for plating Pd, plating liquid measure is 40L, Pd in plating solution2+Content for 0.024mol/L, the amount of stabilizer 2Na-EDTA is 50g/
L, buffer NH4The amount of Cl is 50g/L.Before pouring into alloyed powder, plating solution is first warming up to 50 DEG C, heating is carried out at the same time stirring, temperature
After degree is stablized, alloyed powder is poured into plating solution, by a concentration of 8% reducing agent N2N4·H2O solution is dripped with the rate of 50mL/min
Enter and chemical plating is carried out in plating solution, this is in the process persistently stirred plating solution, after 15min, stops instilling reducing agent, completes plated film
Process takes out alloyed powder from plating solution, and is cleaned 3 times with deionized water, then filters, and obtains the alloyed powder of Pd films cladding,
Fig. 1 is Zr0.9Ti0.1Co alloy surfaces coat the pattern photo of Pd films, and Pd films are in the cladding dense uniform of alloy surface.
The 3kg alloyed powders coated through chemical plating are poured into the plating solution of Electroless Cu Plating, plating liquid measure is 9.6L, Cu in plating solution2+
The amount of a concentration of 0.11mol/L, stabilizer 2Na-EDTA are 44g/L, buffer 2, and the amount of 2 '-bipyridyl and potassium ferrocyanide is equal
For 0.01mg/L.Before pouring into alloyed powder, plating solution is first warming up to 50 DEG C, heating is carried out at the same time stirring, after temperature is stablized, by alloy
Powder is poured into plating solution, a concentration of 5% reducing agent glyoxylic acid solution with the rate of 100mL/min is instilled, chemistry is carried out in plating solution
Plating is persistently stirred plating solution during this, after 35min, stops instilling reducing agent, completes coating process, by alloyed powder from
It takes out in plating solution, and is cleaned 3 times with deionized water, then filtered, obtain the alloyed powder of Pd-Cu composite membranes cladding.Fig. 2 is
Zr0.9Ti0.1Co alloy surfaces coat the pattern photo of Cu films, according to scanning electron microscope analysis as a result, ingredient is in Pd-Cu alloy films
60Pd-40Cu。
1kg alloyed powders are encapsulated into quartz ampoule, quartz ampoule is put into heat-treatment furnace by argon gas protection, setting heat treatment
10 DEG C/min of stove heating rate, 450 DEG C of target temperature, soaking time 8h, after the completion of heat treatment, alloyed powder cools to room with the furnace
Temperature takes out alloyed powder.Fig. 3 is Zr after heat treatment0.9Ti0.1Co alloy surfaces coat the pattern photo of Pd-Cu alloy films.
The Zr that Pd-Cu alloy films and Pd films are coated0.9Ti0.1Co alloys are in 1%O2+ 4%N2+ 5%He+90%H2Mark
It carries out inhaling in quasi- gas and puts hydrogen circulation experiment, it is room temperature to inhale hydrogen temperature, and hydrogen discharging temperature is 350 DEG C, system pressure 0.05MPa,
Fig. 4 is the hydrogen-sucking amount under different cycle-indexes of two kinds of samples in standard gas, and as shown in Figure 4, the absorption hydrogen of Pd films cladding holds
Amount is remarkably decreased with the increase of cycle-index, and when recycling for the 10th time, hydrogen absorption capacity is declined by the 1.67wt.% of first time
To 0.87wt.%, 48% is had dropped, and has apparent continuous decrease trend.And the alloy of Pd-Cu films cladding, not only inhale for the first time
Hydrogen capacity is greater than Pd film clad alloys, and in cycle later, hydrogen absorption capacity is gradually stablized in 1.60wt% or so, compared with the
One time hydrogen absorption capacity only has dropped 14%.By comparing alloy anti-poisoning ability and recycling longevity it is found that after Pd-Cu films cladding
The alloy of the purer Pd films cladding of life greatly improves, Pd-Cu films cladding hydrogen-absorbing material tool prepared by method using the present invention
There is preferable service life cycle.
Claims (7)
1. a kind of preparation method of antitoxinization metal hydrogen-absorbing material, which is characterized in that part hydrogenation is carried out to metal hydrogen-absorbing material
Machinery powder coats Pd films in surface of metal particles using the method for chemical plating and Cu films forms Pd- successively into metallic particles afterwards
Then Cu composite membranes are heat-treated the metallic particles after cladding, make Pd-Cu composite membrane alloyings.
2. the preparation method of antitoxinization metal hydrogen-absorbing material according to claim 1, which is characterized in that the part hydrogenation
Method be：Under the conditions of 100~500 DEG C, 0.01~5MPa Hydrogen Vapor Pressures, metal hydrogen-absorbing material is made to inhale hydrogen, the suction hydrogen time exists
Between 0.5~6 hour, metal material part dehydrogenation is then made using vacuum pumping method again, after being cooled to room temperature, metal inhales hydrogen material
Hydrogen content in material is between 0.1~200mL/g.
3. the preparation method of antitoxinization metal hydrogen-absorbing material according to claim 1, which is characterized in that the metal inhales hydrogen
Granularity after material part hydrogenation after machinery powder processed is 20~300 mesh.
4. the preparation method of antitoxinization metal hydrogen-absorbing material according to claim 1, which is characterized in that the Pd-Cu is answered
Close the composite membrane that film is Pd-Cu, Pd-Cu-Pd or Pd-Cu-Pd-Cu form.
5. the preparation method of antitoxinization metal hydrogen-absorbing material according to claim 4, which is characterized in that chemical plating Pd films
In plating solution, pd2+A concentration of 0.005~0.02mol/L, bath temperature be 45~55 DEG C, in plating solution the amount of alloying pellet be 0.5
~30kg/L, the rate of addition of reducing agent is 0.6~500mL/min, 10~30min of plating time.
6. the preparation method of antitoxinization metal hydrogen-absorbing material according to claim 4, which is characterized in that Electroless Cu Plating film
In plating solution, Cu2+A concentration of 0.028~0.11mol/L, bath temperature be 45~55 DEG C, in plating solution the amount of alloying pellet be 0.5
~30kg/L, the rate of addition of reducing agent is 1~1000mL/min, 0.5~50min of plating time.
7. the preparation method of antitoxinization metal hydrogen-absorbing material according to claim 1, which is characterized in that heat treatment temperature is
400~800 DEG C, heat treatment time is 4~24 hours, and protective atmosphere is high-purity hydrogen, high-purity argon gas or high-purity helium.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109848427A (en) * | 2018-12-04 | 2019-06-07 | 有研工程技术研究院有限公司 | A method of it improving palladium and coats zirconium base hydrogen-absorbing material antitoxinization cyclical stability |
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| CN101244376A (en) * | 2007-02-13 | 2008-08-20 | 北京有色金属研究总院 | Method for producing metallic hydrogen absorption material with hydrogen absorption ability in hydrogen gas containing mixed gas |
| CN102179521A (en) * | 2011-04-20 | 2011-09-14 | 北京科技大学 | Preparation method of ultra-fine spherical nickel coated titanium composite powder |
| CN103055795A (en) * | 2013-01-15 | 2013-04-24 | 北京联创宏业真空科技有限公司 | Getter and preparation method thereof |
| JP2016139597A (en) * | 2015-01-26 | 2016-08-04 | 住友金属鉱山株式会社 | Manufacturing method of dendritic silver coated copper powder |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244376A (en) * | 2007-02-13 | 2008-08-20 | 北京有色金属研究总院 | Method for producing metallic hydrogen absorption material with hydrogen absorption ability in hydrogen gas containing mixed gas |
| CN102179521A (en) * | 2011-04-20 | 2011-09-14 | 北京科技大学 | Preparation method of ultra-fine spherical nickel coated titanium composite powder |
| CN103055795A (en) * | 2013-01-15 | 2013-04-24 | 北京联创宏业真空科技有限公司 | Getter and preparation method thereof |
| JP2016139597A (en) * | 2015-01-26 | 2016-08-04 | 住友金属鉱山株式会社 | Manufacturing method of dendritic silver coated copper powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109848427A (en) * | 2018-12-04 | 2019-06-07 | 有研工程技术研究院有限公司 | A method of it improving palladium and coats zirconium base hydrogen-absorbing material antitoxinization cyclical stability |
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