CN107739859A - A kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece - Google Patents
A kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece Download PDFInfo
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- CN107739859A CN107739859A CN201711026835.4A CN201711026835A CN107739859A CN 107739859 A CN107739859 A CN 107739859A CN 201711026835 A CN201711026835 A CN 201711026835A CN 107739859 A CN107739859 A CN 107739859A
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
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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
- 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
Abstract
The invention discloses a kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece, (a) using Titanium, metal zirconium and metallic copper as raw material, according to the proportioning of raw material, zirconium CTB alloy is prepared using the method for water jacketed copper crucible electromagnetic induction vacuum levitation melting；(b) the zirconium CTB alloy ingot that obtains step (a) is shaped and the sample of size, and carries out series of preprocessing to its surface；(c) the zirconium CTB alloy sample for obtaining step (b) carries out hydrogen abstraction reaction, prepares finished product.The present invention's will set about in itself from more essential material, and emphasis develops a kind of alloy material of function admirable, and this alloy material, by some micro- pinning effects, can be reduced because body caused by hydrogenization rises and hydrogen embrittlement effect during hydrogen is inhaled.
Description
Technical field
The present invention relates to metal hydrogen storage material and hydrogen-storage electrode preparing technical field, and in particular to a kind of hydrogen storage flawless zirconium
The preparation technology of CTB alloy electrode source piece.
Background technology
Metal hydride (hydrogen includes all three isotope, i.e. protium, deuterium and tritium) is commonly applied to sparking electrode, such as Vacuum Arc
Ion source electrode.During discharging between the electrodes, abundant hydrogen ion and each valence state metal ion will be produced.Tradition
Metal hydride cell using body material inhale hydrogen method prepare, this method first process certain size metal or alloy electricity
Pole, then inhales hydrogen at high temperature, obtained after cubical expansion needed for size metal hydride cell.Because body rises and hydrogen embrittlement effect, this
Metal hydride prepared by kind method is also easy to produce macroscopic cracking, seriously affects the discharge stability of metal hydride cell source piece
Property.Have some patents of invention in hydrogen-storage electrode preparation field at present, what inventor Peng Yu flew：Metal hydride cell preparation side
Method and device and its a kind of of application method ZL201410241645.4 records prepare metal by the way of powder hot forming
Hydride electrode, there is hydrogen titanium than high and flawless advantage, but there is also it is certain the defects of：Easily occur under flash electric discharge
The phenomenon that the large area spray of electrode source piece surface is split, influence to be greatly reduced the use longevity of electrode source piece while discharge stability
Life.In addition, inventor Wang Tao：A kind of preparation technology ZL201510291419.1 of flawless titantium hydride electrode source piece is detailed
Pure Ti electrode inhales the process of flawless after hydrogen, and this process of preparing can actually substantially reduce macroscopic cracking, but
In the presence of it is certain the defects of：It is that yields under the preparation technology is relatively low first, to the raw material technology controlling and process of different manufacturers lot number
Parameter has marked difference；Second be that this method reduces is the big crackle of macroscopic view, that is, it is obvious to meet that naked eyes can not be observed
Macroscopic cracking, but substantial amounts of macroscopical micro-crack is still had using 100X observation by light microscope；3rd, prepared by this method
Hydrogenation titanium source piece although disclosure satisfy that the requirement of no macroscopic cracking, but do not obtain root the problem of its mechanical property, i.e. hydrogen embrittlement
The solution of person's character.Inventor Song Xiping：A kind of preparation technology 201310143639.0 of flawless zircaloy describes commonly
Industrial zircaloy raw material high temperature inhales the process of formation flawless hydrogen storage high alloy after hydrogen, and this process of preparing is still
The problem of being difficult to avoid that low yields and poor mechanical property.
The content of the invention
It is an object of the invention to provide a kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece, by micro-
The Dispersed precipitate of copper nanocrystallite is measured, strengthens the institutional framework mechanical property of alloy, can be resisted because of hydrogen after alloy high-temp inhales hydrogen
Micro-crack caused by crisp effect, which continues expansion, turns into bigger crackle, greatly solves the metal hydride that current technique productions come out
The problem of thing electrode source piece yields is low, poor mechanical property.
The present invention is achieved through the following technical solutions：
A kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece, comprises the following steps：
(a) using Titanium, metal zirconium and metallic copper as raw material, according to the proportioning of raw material, using water jacketed copper crucible electricity
The method of magnetic induction vacuum smelting in suspension prepares zirconium CTB alloy；
(b) the zirconium CTB alloy ingot that obtains step (a) is shaped and the sample of size, and its surface is entered
Row series of preprocessing；
(c) the zirconium CTB alloy sample for obtaining step (b) carries out hydrogen abstraction reaction, prepares finished product.
The present invention is directed the product that manufactures of existing process its problem of poor mechanical property, prior art be present
In, either common elemental metals such as titanium, or alloy material zircaloy, it can not all avoid macroscopic view during high temperature inhales hydrogen
The problem of crackle and poor mechanical property, hydrogen technological parameter can only be inhaled by adjusting, slow down hydrogen-absorption speed, enable hydrogen atom as far as possible
It is enough uniform at high temperature, slowly penetrate into material, so as to the problem of reducing macroscopic cracking and overcoming mechanical property degradation.
The hydrogen embrittlement effect for having its source in material after hydrogenation of this problem is unavoidable, and the work of early stage concentrates on optimization high temperature hydrogen
Chemical industry skill.And the present invention will set about in itself from more essential material, a kind of emphasis development alloy material of function admirable, this
Kind alloy material, by some micro- pinning effects, can be reduced because of body caused by hydrogenization during hydrogen is inhaled
Rise and hydrogen embrittlement effect.
Described step (a) includes step in detail below：
(a1) surface of Titanium, metal zirconium and metallic copper is polished, removes oxide-film, then crush and form particle, particle
Diameter not less than crucible valve stitch；
(a2) weighed by proportioning, titanium is first placed into crucible bottom, places into copper, is finally putting into zirconium；
(a3) vacuumize, and be passed through argon gas and repeatedly replaced, ultimately form the work atmosphere of argon gas；
(a4) open high frequency electric source and carry out a smelting in suspension, form alloy cast ingot；
(a5) take out alloy cast ingot, and by alloy cast ingot be inverted be reentered into crucible, vacuumize and be passed through argon gas carry out it is more
Secondary displacement, ultimately form the work atmosphere of argon gas；
(a6) open high frequency electric source and carry out secondary smelting in suspension.
Specifically, in step (a) of the present invention, it is more than using Titanium body material of the purity more than 99.7%, purity
Metallic copper body material of the 99.7% metal zirconium body material and purity more than 99.9% is raw material, and polishing grinding body material surface is to remove material
To expect the oxide layer on surface, then carry out cutting and crushing again, particle size not less than crucible valve seam to be defined, with anti-leak, wherein
Titanium matches the 25-70% for accounting for weight alloy, and metal zirconium matches the 25-70% for accounting for weight alloy, and the proportioning of metallic copper accounts for conjunction
The 5-10% of golden weight, after completion proportioning is weighed, according to Titanium is put into crucible bottom first, metallic copper is placed into, finally
The order for being put into metal zirconium is put；Vacuum pump group and vacuum valve are opened to vacuum suspension stove evacuation, when vacuum is higher than 1*
During 10-2Pa, bleed-off passage valve is closed, argon gas is filled with to certain pressure, closes argon filling channel valve.Then reopen and take out
Gas passage takes out argon gas in light stove, and vacuum is higher than 1*10-2During Pa, argon gas is re-filled with to certain pressure, closes argon filling channel valve,
Argon gas displacement is minimum to be carried out twice, to empty the foreign gases such as the oxygen in stove, being finally passed through the argon gas of certain pressure as work
Make gas, prepare melting；Open high frequency electric source and carry out smelting in suspension, be slowly increased electric current from small to large, it is miscellaneous to remove gas
Matter, when gaseous impurity volatilization is obvious, keep heated current observation foreign gas evaporation situation, hence it is evident that lift heating during reduction again
Electric current；Metal constituent element gradually melts, and temperature-rise period pays attention to burn-off rate, prevents top solid metal " avalanche " or fierce deflation,
Melt is set to produce splash；After solid metal all melts, temperature is properly increased, makes alloy melt strengthen stirring and increase to suspend
Height is simultaneously incubated 1 minute or so, then progressively cools, forms alloy cast ingot；After alloy graining, power-off cooling blow-on again in 10 minutes
Door feeding, now pays attention to alloy temperature, prevents from scalding.Alloy cast ingot top-bottom is inverted again and is reentered into again in crucible, shuts stove
Door, repeat step (a3) are vacuumized and are passed through argon gas and repeatedly replaced, and are finally passed through the argon gas of certain pressure as work
Make gas, prepare melting；Repeat step (a3) carries out secondary smelting in suspension, electric current is slowly increased from small to large, in this process
Middle phenomenon of deflation can significantly reduce, and pay attention to the burn-off rate of alloy cast ingot；After alloy cast ingot all melts, temperature is properly increased
Degree, alloy melt is strengthened stirring and increase hoverheight and be incubated 1 minute or so, then slow cooling, solidified in melt
Cheng Zhong, cooling rate is controlled, melt upper surface is kept pattern rule, wall built-up, not skewed.
The step (b) comprises the following steps：
(b1) by alloy cast ingot is shaped and the sample of size；
(b2) mechanical lapping is carried out to sample surfaces using ball mill and polishing, grounds travel uses Al2O3Powder；
(b3) workpiece after polishing is removed into grease first in thermokalite, oxide layer is then removed in weak acid, is then spent
Ionized water is cleaned, and places into and ultrasonic cleaning 5min is carried out in alcohol；
(b4) workpiece is dried and weighed, weighing precision reaches 0.01mg, and zirconium titanium copper sample workpiece is made.
Specifically, the sample of zirconium CTB alloy prepared by step (a) for Raw material processing into definite shape and size is used,
Need to carry out its surface pretreatment so that sample forms smooth surface, by way of polishing, cleaning, the workpiece table of acquisition
Surface evenness is higher, the uniform hydride layer of the more high easier formation of surface smoothness, can so significantly reduce interiors of products
The cracked probability of stress and surface, the effect that workpiece is weighed is to demarcate hydrogen-sucking amount, and required precision reaches
0.01mg。
The step (c) includes step in detail below：
(c1) the zirconium titanium copper sample workpiece that step (b) processing is completed is put into vacuum cavity and vacuumized, in vacuum chamber
Vacuum be less than 2*10-4pa；
(c2) heating curve is set, and workpiece heat to certain temperature deflated according to heating curve；
(c3) after cooling the temperature to 420~520 DEG C and temperature stabilization, quick closedown vavuum pump bleeding point simultaneously pours hydrogen,
Carry out hydrogen abstraction reaction；
(c4) set temperature lowering curve to cause hydrogen abstraction reaction to carry out certain time, the workpiece after suction hydrogen is carried out being cooled to room
Temperature, obtain flawless hydrogen storage zirconium CTB alloy finished product.
Specifically, concretely, (c2) high annealing has both sides effect：First, high annealing can eliminate
The internal stress that sample is brought in process, the release of stress can effectively reduce sample and be split caused by during hydrogen is inhaled
Line；Secondly, high annealing is carried out under vacuum environment to have certain effect to the oxide layer for eliminating sample surfaces, expose with suction
The higher point position of hydrogen activity, the heating rate scope control of heating curve is set in 5~10 DEG C/min, often 100 DEG C of heating, holding
5~20min of temperature stabilization；About 600 DEG C of highest discharge temperature, temperature should not exceed 650 DEG C, and too high temperature can cause in alloy
The precipitation of copper；After cooling the temperature to 420~520 DEG C and temperature stabilization, answer quick closedown vavuum pump bleeding point and be passed through certain gas
The hydrogen of pressure, carry out hydrogen abstraction reaction；Temperature is higher, and hydrogen-absorption speed is faster, but faster hydrogen-absorption speed can cause sample cracking powder
Change and deform, therefore inhale hydrogen temperature to be less than 520 DEG C；Temperature is excessively slow less than 420 DEG C of hydrogen-absorption speeds, is inhaling hydrogen for a long time
During surface oxidation easily occurs, therefore inhale hydrogen temperature control at 420~520 DEG C, the selection of air pressure should coordinate the choosing of suction hydrogen temperature
Select, Hydrogen Vapor Pressure is higher, and hydrogen-absorption speed is faster, and too fast hydrogen-absorption speed can cause sample cracking efflorescence and deformation, Hydrogen Vapor Pressure mistake
It is low that sample hydrogen-sucking amount can be caused not reach requirement, therefore the Hydrogen Vapor Pressure scope control in hydrogen abstraction reaction is between -50~100kPa；
Temperature lowering curve is set to cause hydrogen abstraction reaction to carry out certain time, concretely, 0.5~2 DEG C/min of rate of temperature fall scope.Too fast
Cooling can cause sample interior stress occur, and 0.5~2 DEG C/min scope should be met by considering rate of temperature fall；Often cool 20
~60 DEG C, keeping temperature stablizes 10~20min, it is ensured that has inhaled hydrogen saturation in the temperature spot；Inhale the control of hydrogen time range 100~
180min, inhales that the hydrogen time is unsuitable long, and inhaling hydrogen overlong time can cause sample surfaces to aoxidize, and inhaling the hydrogen time too short can cause to inhale
Hydrogen amount does not reach requirement；The temperature range that hydrogen abstraction reaction terminates is 380~420 DEG C, slowly reduces temperature until 100 DEG C of left sides afterwards
The right side, rate of temperature fall should not be greater than 2 DEG C/min；Temperature can close heater after being down to 100 DEG C, and it is i.e. desirable to naturally cool to room temperature
Go out, obtain flawless hydrogen storage zirconium CTB alloy finished product.
The present invention compared with prior art, has the following advantages and advantages：
The present invention's will set about in itself from more essential material, and emphasis develops a kind of alloy material of function admirable, this
Kind alloy material, by some micro- pinning effects, can be reduced because of body caused by hydrogenization during hydrogen is inhaled
Rise and hydrogen embrittlement effect, the crackle of product under the microscope is less than 100nm.
Brief description of the drawings
Accompanying drawing described herein is used for providing further understanding the embodiment of the present invention, forms one of the application
Point, do not form the restriction to the embodiment of the present invention.In the accompanying drawings：
Fig. 1 is the surface view of sample in the embodiment of the present invention, and wherein a is surface macrograph, and b is under light microscope
Surface, which is situated between, sees figure, and c, d are the surface microscopic figures under SEM；
Fig. 2 is the X ray diffracting spectrum of zirconium CTB alloy and zirconium deuteride CTB alloy in embodiment.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, the present invention is made with reference to embodiment
Further to describe in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment
A kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece of the present invention, using Goodfellow
The pure titanium particles of TI006100, the pure zirconium particles of ZR006100 and CU006100 fine copper particle are carried out as raw material according to following technique
Production：
(a1) it is Titanium particle of the purity more than 99.99%, metal zirconium particle of the purity more than 99.8% and purity is big
In 99.99% metallic copper particle polishing grinding to remove the oxide layer of material surface, then cutting and crushing is carried out, particle size 5-
10mm；
(a2) weighed by proportioning, weigh 5g Titanium, weigh 4.5g metal zirconium, weigh 0.5g metallic copper, according to
Titanium, copper, the order of zirconium are sequentially placed into crucible；
(a3) vacuum pump group and vacuum valve are opened to vacuum suspension stove evacuation, when vacuum is higher than 1*10-2During Pa, close
Bleed-off passage valve is closed, argon gas is filled with until pressure reaches 0.05Mpa or so, closes argon filling channel valve, then reopen
Bleed-off passage takes out argon gas in light stove, and vacuum is higher than 1*10-2During Pa, be re-filled with argon gas until pressure reach 0.05Mpa or so, close
Close argon filling channel valve.Argon gas is replaced three times, to empty the foreign gases such as the oxygen in stove, is finally passed through 0.05Mpa argon gas
As working gas, prepare melting；
(a4) open high frequency electric source and carry out smelting in suspension, be slowly increased electric current from small to large, to remove gaseous impurity, when
When gaseous impurity volatilization is obvious, heated current observation foreign gas evaporation situation is kept, hence it is evident that heated current is lifted during reduction again,
After solid metal all melts, temperature is properly increased, alloy melt is strengthened stirring and increase hoverheight and is incubated 1 minute
Left and right, then progressively cool, form alloy cast ingot；
(a5) alloy cast ingot is taken out, and is inverted and is reentered into crucible, (a3) step is repeated, is passed through argon gas and is put three times
Change, final work atmosphere is argon gas；
(a6) open high frequency electric source and carry out secondary smelting in suspension, be slowly increased electric current from small to large, when alloy cast ingot is whole
After fusing, temperature is properly increased, alloy melt is strengthened stirring and increase hoverheight and is incubated 1 minute or so, then slowly
Cooling, in melt process of setting, cooling rate is controlled, melt upper surface is kept pattern rule, wall built-up, not skewed；
(b1) alloy cast ingot is processed into disc-shaped diameter 6.05mm, thickness 0.58mm；
(b2) mechanical lapping and polishing are carried out to the alloy disk machined, using Al2O3 powder as grounds travel in reality
Test in the small grinder of room and be ground 20min；
(b3) the alloy disk for grinding completion is cleaned with deionized water, is put into 60 DEG C of sodium hydroxide solution and soaks
5min, taking-up is put into hydrofluoric acid solution after being cleaned again with deionized water soaks 5min, and taking-up is put after being cleaned again with deionized water
Enter ultrasonic 5min in alcohol；
(b4) last taking-up is put into dryer to be dried, using METTLER TOLEDO XS205 balances to electrode source
Piece is weighed, and measurement result 73.26mg, the weighing precision of the balance reaches 0.01mg；
(c1) zirconium CTB alloy disk is put into vacuum cavity and vacuumized, the vacuum in vacuum chamber is less than 2*10- 4pa；
(c2) setting heating curve, heating curve are as follows：Room temperature is heated uniformly to 100 DEG C by 10min, and keeping should
Temperature 10min, then it is heated uniformly to 200 DEG C by 10min and keeps temperature 10min, then uniformly heated by 10min
To 300 DEG C and temperature 10min is kept, then 400 DEG C is heated uniformly to by 10min and keeps the temperature 10min, Ran Houjing
Cross 10min to be heated uniformly to 500 DEG C and keep temperature 10min, be then heated uniformly to 600 DEG C by 10min and keep being somebody's turn to do
Temperature 10min, then it is heated uniformly to 650 DEG C by 10min and keeps temperature 30min, according to heating curve by zirconium titanium copper
Alloy disk is deflated after being heated to 650 DEG C；
(c3) complete deflation process after, set temperature be down to 520 DEG C, when vacuum cavity temperature is down to 520 DEG C, first to
30kPa deuterium is poured in recorder jar, turns off vavuum pump bleeding point, finally opens the valve between recorder jar and vacuum cavity
Door, now vacuum cavity air pressure is down to 10kPa；
(c4) set temperature lowering curve to cause hydrogen abstraction reaction to carry out certain time, the alloy disk after suction hydrogen is cooled to
Room temperature, obtain finished product zirconium deuteride CTB alloy electrode source piece；Temperature-fall period is as follows：It is equal by 20min after 520 DEG C keep 20min
It is even to be cooled to 500 DEG C and keep 20min, to 460 DEG C and 20min then is kept by 40min uniform decrease in temperature, is then passed through
40min uniform decrease in temperature is to 420 DEG C and keeps 20min, real finally by 160min uniform decrease in temperature to closing heater after 100 DEG C
Now natural stove is cold, and hydrogen storage flawless zirconium CTB alloy electrode source piece is made.
Take out the zirconium deuteride CTB alloy electrode source piece that preparation is completed to be weighed, quality 77.42mg, by calculating
To D：M (Ti+Zr+Cu)=1.759 (at.%), electrode source piece deuterium storage quantity are 5.373% (mass%).Fig. 1 is the surface of sample
Macrograph, surface, which are situated between, sees figure and surface microscopic figure, and picture shows sample surfaces without macroscopic cracking；Light microscope enlargement ratio is about
The surface Jie's sight figure shot at 200 times shows that sample has the crackle of sub-micrometer scale；25k times of times magnification of SEM
The microscopic appearance figure of the non-slit region of sample surfaces is observed under rate, it can be seen that regular crystal grain is densely arranged；Scanning electron shows
The microscopic appearance figure in sample surfaces micro-crack region is observed under 25k times of enlargement ratio of micro mirror, the size of micro-crack is below
100nm, Fig. 2 are the X ray diffracting spectrum of zirconium CTB alloy and zirconium deuteride CTB alloy, and display alloy is after deuterate in diffraction maximum
Substantially there is the diffraction maximum of titanium deuteride and zirconium deuteride.
Above-described embodiment, the purpose of the present invention, technical scheme and beneficial effect are carried out further
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., all should include
Within protection scope of the present invention.
Claims (4)
1. a kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece, it is characterised in that comprise the following steps：
(a) using Titanium, metal zirconium and metallic copper as raw material, according to the proportioning of raw material, using water jacketed copper crucible electromagnetism sense
The method of vacuum levitation melting is answered to prepare zirconium CTB alloy；
(b) the zirconium CTB alloy ingot that obtains step (a) is shaped and the sample of size, and carries out one to its surface
Series pretreatment；
(c) the zirconium CTB alloy sample for obtaining step (b) carries out hydrogen abstraction reaction, prepares finished product.
2. a kind of preparation technology of hydrogen storage flawless zirconium CTB alloy electrode source piece according to claim 1, its feature exist
In described step (a) includes step in detail below：
(a1) surface of Titanium, metal zirconium and metallic copper is polished, removes oxide-film, then it is broken form particle, particle it is straight
Stitched not less than crucible valve in footpath；
(a2) weighed by proportioning, titanium is first placed into crucible bottom, places into copper, is finally putting into zirconium；
(a3) vacuumize, and be passed through argon gas and repeatedly replaced, ultimately form the work atmosphere of argon gas；
(a4) open high frequency electric source and carry out a smelting in suspension, form alloy cast ingot；
(a5) alloy cast ingot is taken out, and alloy cast ingot is inverted and is reentered into crucible, vacuumizes and is passed through argon gas and repeatedly put
Change, ultimately form the work atmosphere of argon gas；
(a6) open high frequency electric source and carry out secondary smelting in suspension.
A kind of 3. preparation technology of flawless hydrogen storage zirconium CTB alloy according to claim 1, it is characterised in that the step
Suddenly (b) comprises the following steps：
(b1) by alloy cast ingot is shaped and the sample of size；
(b2) mechanical lapping is carried out to sample surfaces using ball mill and polishing, grounds travel uses Al2O3Powder；
(b3) workpiece after polishing is removed into grease first in thermokalite, oxide layer is then removed in weak acid, then uses deionization
Water is cleaned, and places into and ultrasonic cleaning 5min is carried out in alcohol；
(b4) workpiece is dried and weighed, weighing precision reaches 0.01mg, and zirconium titanium copper sample workpiece is made.
A kind of 4. preparation technology of flawless hydrogen storage zirconium CTB alloy according to claim 1, it is characterised in that the step
Suddenly (c) includes step in detail below.
(c1) the zirconium titanium copper sample workpiece that step (b) processing is completed is put into vacuum cavity and vacuumized, it is true in vacuum chamber
Reciprocal of duty cycle is less than 2*10-4pa；
(c2) heating curve is set, and workpiece heat to certain temperature deflated according to heating curve；
(c3) after cooling the temperature to 420~520 DEG C and temperature stabilization, quick closedown vavuum pump bleeding point simultaneously pours hydrogen, carries out
Hydrogen abstraction reaction；
(c4) set temperature lowering curve to cause hydrogen abstraction reaction to carry out certain time, the workpiece after suction hydrogen is carried out being cooled to room temperature, obtained
To flawless hydrogen storage zirconium CTB alloy finished product.
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| GB2219948B (en) * | 1988-06-27 | 1992-09-30 | Japan Metals & Chem Co Ltd | A method for refining hydrogen gas |
| CN104726745A (en) * | 2013-12-20 | 2015-06-24 | 北京有色金属研究总院 | Ti-Zr based light-weight high-capacity hydrogen absorption material, and preparation method and application method thereof |
| CN104944375A (en) * | 2015-06-01 | 2015-09-30 | 中国工程物理研究院流体物理研究所 | Preparation technology of crack-free titanium hydride electrode source sheet |
| CN105568110A (en) * | 2016-03-17 | 2016-05-11 | 中国工程物理研究院材料研究所 | AB type hydrogen storage alloy used for storing tritium and preparation method of AB type hydrogen storage alloy |
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