CN104325150A - Preparation process for metal hydride powder - Google Patents
Preparation process for metal hydride powder Download PDFInfo
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- CN104325150A CN104325150A CN201410626755.2A CN201410626755A CN104325150A CN 104325150 A CN104325150 A CN 104325150A CN 201410626755 A CN201410626755 A CN 201410626755A CN 104325150 A CN104325150 A CN 104325150A
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- metal hydride
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Abstract
The invention discloses a preparation process for metal hydride powder. The preparation process comprises the following steps of a preparing step of adding a grinding aid into crushing equipment; a crushing step of adding a metal hydride into the crushing equipment and starting the crushing equipment to crush and sieve the metal hydride to obtain the metal hydride powder. The preparation process has the advantages that the grinding aid is introduced, so that impurity drag-in amount is less, the working efficiency is greatly improved, and the metal hydride powder obtained through the process has high purity, good powder dispersity and good mobility.
Description
Technical field
The present invention relates to field of metallurgy, be specifically related to a kind of metal hydride preparation technique.
Background technology
In powder metallurgy industry, the performance of material powder decides the performance of product.Along with the development of modern industry, the kind of sintered metal product and output are also come greatly, also more and more higher to the requirement of high-purity former powder.
Due to the characteristic of metal, the preparation of metal powder material is different from the preparation process of the powders such as other powder such as ceramic powder.Metal is plasticity, is difficult to carry out powder process by the method for common broken ball milling.Prepare high pure metal powder at present and mainly contain powder by atomization method and hydrogenation and dehydrogenization technique (Hydrogenation-Dehydrogenation) two kinds of methods, powder by atomization method equipment costly, cost is higher, it is low that hydrogenation and dehydrogenization method prepares powder cost compare, is a kind of common method that high pure metal powder is produced.
It is aobvious fragility after utilizing metal to inhale hydrogen that hydrogenation and dehydrogenization technique prepares metal powder material, and intensity is lower, be easy to the characteristic of fragmentation to make metal hydride powder, and then Oxidative Dehydrogenation obtains metal dust in a vacuum furnace.
Summary of the invention
Namely object of the present invention is to provide a kind of metal hydride preparation technique, and this process contaminants amount of bringing into is few, and the working time is short, and the metal hydride Purity of Coke Powder obtained by this technique is high, and powder dispersity is good, good fluidity.
Object of the present invention is achieved through the following technical solutions:
A kind of metal hydride preparation technique, comprises the following steps:
Preparation process: add grinding aid in disintegrating apparatus;
Destruction step: metal hydride is added disintegrating apparatus, starts disintegrating apparatus and carries out fragmentation, screening to metal hydride, obtain metal hydride powder.
It is aobvious fragility after utilizing metal to inhale hydrogen that hydrogenation and dehydrogenization technique prepares metal powder material, and intensity is lower, be easy to the characteristic of fragmentation to make metal hydride powder, and then Oxidative Dehydrogenation obtains metal dust in a vacuum furnace.Wherein, the step preparing metal hydride powder is particularly crucial, and the fineness of metal hydride powder determines the fineness of the metal dust finally obtained.
Current, prepare in the step of metal hydride powder, adopt and metal hydride block is placed in disintegrating apparatus, by the operation of disintegrating apparatus, metal hydride is pulverized, finally obtain metal hydride powder.The fineness of metal hydride powder diminishes along with the increase of broken time.That is to say, in the prior art, reducing the fineness of metal hydride powder by increasing the broken time, to obtain thinner metal hydride powder.
Inventor is studied rear discovery to the existing method preparing metal hydride powder, and existing method exists following problem:
1. inventor finds through research, and metal hydride easily absorbs oxygen in air and nitrogen in shattering process, thus affects the purity of metal hydride.Follow-up dehydration processes, cannot remove and the oxygen of corrupt split and nitrogen, causes the purity of the metal powder material obtained to decline.
Metal hydride is in shattering process, and disintegrating apparatus does work to material, and the temperature of material is raised, and the broken time is longer, and the temperature of material is also higher.And inventor finds after further research, along with the rising of temperature, the absorption of metal hydride to oxygen and nitrogen is also more violent.
Can find out, in the prior art, wish to get thinner metal powder material, the inevitable reduction along with metal powder material purity.
2. inventor also finds, metal hydride is easily reunited in the process of fragmentation, and the mobility of powder is not good, thus adds the difficulty of Crushing and screening.
Based on above-mentioned understanding newly, inventor, in the process of metal hydride fragmentation, introduces grinding aid.Material is in fine grinding process, and particle is refinement progressively, and specific area increases, and particle mutually adsorbs and occurs reuniting, and crush efficiency is declined.And grinding aid can be adsorbed on the surface of metal hydride, the surface energy of powder can be effectively reduced, stop the reunion of powder, make the mobility of powder better, improve Crushing and screening efficiency.
Adopt the present invention, wish to get the metal hydride powder of identical fineness, the time of cost will be less than existing method, simultaneously because spended time is few, the temperature of material is low, and the purity of the metal hydride powder finally obtained is by the purity higher than the metal hydride powder adopting existing method to obtain.
Further, in described preparation process, described grinding aid is gaseous state.The grinding aid dispersion of gaseous state evenly, consumption is less, there will not be grinding aid to pile up phenomenon on powder surface, thus decreases bringing into of impurity, further increase the purity of metal hydride powder.
Further, the concentration of the grinding aid of described gaseous state in protective atmosphere is 0.1-10g/m
3.
Further, in described preparation process, grinding aid and the inert protective gas of described gaseous state together add disintegrating apparatus.Inert protective gas contributes to discharging the oxygen in disintegrating apparatus and nitrogen, and the absorption oxygen making metal hydride less and nitrogen, can improve the purity of metal hydride powder.Meanwhile, grinding aid and the inert protective gas of gaseous state together add disintegrating apparatus, contribute to the dispersed of grinding aid, further reduce the consumption of grinding aid, decrease bringing into of impurity.
Further, before described preparation process, also comprise scrubbing procedure: in disintegrating apparatus, repeatedly pass into inert gas, discharge the foreign gas in disintegrating apparatus.Repeatedly pass into inert gas, be mainly used for discharging the oxygen in disintegrating apparatus and nitrogen, the absorption oxygen making metal hydride less and nitrogen, can improve the purity of metal hydride powder.
Further, described grinding aid is boiling point lower than at least one in the ketone of 150 DEG C and alcohols.
Further, described grinding aid is at least one in methyl alcohol, ethanol or acetone.
Inventor finds through research, and metal hydride has fabulous compatibility to hydroxyl isopolarity group, and the strong bonded that even reacts is on metal hydride surface.
Based on above-mentioned cognition, inventor selects at least one in methyl alcohol, ethanol or acetone as grinding aid.In methyl alcohol, ethanol or acetone, hydroxyl, carbonyl are as polar group, and methyl, ethyl are non-polar group.Polar group can be good at combining with metal hydride, and non-polar group is outside, and formation aligns.These grinding aids reduce the surface energy of powder after being adsorbed onto powder surface, and can stop the reunion of powder, improve the preparation efficiency of powder, reduce the temperature of powder in equipment, decrease the uptake of oxygen nitrogen impurity, make the mobility of powder better.
Inventor selects methyl alcohol, ethanol or acetone to be as another factor of grinding aid: the grinding aid of introducing is also objectively belong to a kind of impurity, just grinding aid is on the impact of metal hydride purity much smaller than the oxygen in air and nitrogen, therefore just uses grinding aid to improve the purity of metal hydride.Since grinding aid belongs to a kind of impurity, so, how reducing the impact of grinding aid on metal hydride purity is to the full extent problem to be solved.Based on the understanding that this is new, inventor selects the simple methyl alcohol of molecular structure, ethanol or acetone as grinding aid, compared to the long strand compound that dipole moment is larger, effectively can reduce the introducing of impurity.In addition, these grinding aids possess lower boiling point, have higher saturated vapor pressure under normal temperature, are easy to gasification, can ensure to be uniformly dispersed in protective atmosphere, and be adsorbed on powder surface uniformly.And the larger long strand compound of dipole moment can only exist with liquid or solid-state form at normal temperatures.Methyl alcohol, ethanol or acetone compared with the large molecule grinding aid of liquid state, dispersion evenly, consumption is less, there will not be grinding aid to pile up phenomenon on powder surface, thus decreases bringing into of impurity.
Further, described metal hydride is the neodymium iron boron after hydrogenated niobium, zircoium hydride or hydrogenation.
In sum, advantage of the present invention and beneficial effect are:
1. introduce grinding aid, make the impurity amount of bringing into of the present invention few, the working time is short, and the metal hydride Purity of Coke Powder obtained by this technique is high;
2. grinding aid is gaseous state, dispersion evenly, consumption is less, there will not be grinding aid to pile up phenomenon on powder surface, thus decreases bringing into of impurity, further increase the purity of metal hydride powder;
3. the grinding aid of gaseous state and inert protective gas together add disintegrating apparatus, contribute to the purity improving metal hydride powder, reduce Grinding aid dosage;
4. increase scrubbing procedure, contribute to the purity improving metal hydride powder;
5. select methyl alcohol, ethanol or acetone as grinding aid, greatly reduce the introducing of impurity, improve the purity of metal hydride powder;
6. selection methyl alcohol, ethanol or acetone are as grinding aid, improve dispersiveness and the mobility of powder.
Detailed description of the invention
In order to make those skilled in the art understand the present invention better, below in conjunction with in the embodiment of the present invention, clear, complete description is carried out to technical scheme of the present invention.Apparent, embodiment described below is only the part in the embodiment of the present invention, instead of all.Based on the embodiment that the present invention records, other all embodiment that those skilled in the art obtain when not paying creative work, all in the scope of protection of the invention.
Embodiment 1:
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Preparation process: be mixed in high-purity argon gas by gaseous state ethanol and spray in glove box, the consumption of ethanol in glove box is 10g/m
3;
Destruction step: after ethanol is uniformly dispersed in glove box, puts in disintegrating machine by 1 kilogram of zircoium hydride block, starts disintegrating machine, closes disintegrating machine, obtain zircoium hydride powder after 4 minutes.
Zircoium hydride powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 75% of zircoium hydride powder gross mass, the not sticky sieve of zircoium hydride powder, the angle of repose of zircoium hydride powder is 41 degree, zircoium hydride powder temperature raises 10 degree, zircoium hydride powder nitrogen content 100ppm, zircoium hydride powder oxygen content 3000ppm.
Embodiment 2:
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Preparation process: be mixed into by gaseous methanol in high-purity argon gas and spray in glove box, the consumption of methyl alcohol in glove box is 5g/m
3;
Destruction step: after methyl alcohol is uniformly dispersed in glove box, puts in disintegrating machine by 1 kilogram of zircoium hydride block, starts disintegrating machine, closes disintegrating machine, obtain zircoium hydride powder after 4 minutes.
Zircoium hydride powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 75% of zircoium hydride powder gross mass, the not sticky sieve of zircoium hydride powder, the angle of repose of zircoium hydride powder is 41 degree, zircoium hydride powder temperature raises 10 degree, zircoium hydride powder nitrogen content 110ppm, zircoium hydride powder oxygen content 3000ppm.
Embodiment 3:
Embodiment 3 is the comparative example of embodiment 1 and embodiment 2.
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Destruction step: put in disintegrating machine by 1 kilogram of zircoium hydride block, starts disintegrating machine, closes disintegrating machine, obtain zircoium hydride powder after 10 minutes.
Zircoium hydride powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 70% of zircoium hydride powder gross mass, the sticky sieve of zircoium hydride powder, the angle of repose of zircoium hydride powder is 47 degree, zircoium hydride powder temperature raises 20 degree, zircoium hydride powder nitrogen content 140ppm, zircoium hydride powder oxygen content 3500ppm.
The percentage that the quality of minus sieve material accounts for zircoium hydride powder gross mass is lower, illustrates that the fineness of powder is not enough.Angle of repose is comparatively large, and the illiquidity of powder is described.Powder nitrogen content and oxygen content higher, illustrate that the purity of powder is lower.
Embodiment 4:
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Preparation process: be mixed in high-purity argon gas by gaseous state ethanol and spray in glove box, the consumption of ethanol in glove box is 10g/m
3;
5 kilograms of hydrogenated niobium blocks are put in disintegrating machine by destruction step: after ethanol is uniformly dispersed in glove box, start disintegrating machine, close disintegrating machine, obtain hydrogenated niobium powder after 4 minutes.
Hydrogenated niobium powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 50% of zircoium hydride powder gross mass, the not sticky sieve of hydrogenated niobium powder, the angle of repose of hydrogenated niobium powder is 43 degree, hydrogenated niobium powder temperature raises 10 degree, hydrogenated niobium powder nitrogen content 80ppm, hydrogenated niobium powder oxygen content 2000ppm.
Embodiment 5:
The present embodiment is the comparative example of embodiment 4.
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Destruction step: put in disintegrating machine by 5 kilograms of hydrogenated niobium blocks, starts disintegrating machine, closes disintegrating machine, obtain hydrogenated niobium powder after 10 minutes.
Hydrogenated niobium powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 50% of hydrogenated niobium powder gross mass, the sticky sieve of hydrogenated niobium powder, the angle of repose of hydrogenated niobium powder is 48 degree, hydrogenated niobium powder temperature raises 14 degree, hydrogenated niobium powder nitrogen content 120ppm, zircoium hydride powder oxygen content 2600ppm.
Can find out, embodiment 4 is compared with the present embodiment, and the fineness of the hydrogenated niobium powder obtained is identical, but broken time decreased 60%, and the sticky sieve of powder, angle of repose reduces by 5 degree, and purity increases substantially.
Embodiment 6:
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Preparation process: be mixed in high-purity argon gas by gaseous state acetone and spray in glove box, the consumption of acetone in glove box is 1g/m
3;
Destruction step: after acetone is uniformly dispersed in glove box, puts in disintegrating machine by 1 kilogram of titantium hydride block, starts disintegrating machine, closes disintegrating machine, obtain zircoium hydride powder after 3 minutes.
Titantium hydride powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 60% of titantium hydride powder gross mass, the not sticky sieve of titantium hydride powder, the angle of repose of titantium hydride powder is 41 degree, hydride powder material temperature degree raises 15 degree, titantium hydride powder nitrogen content 80ppm, titantium hydride powder oxygen content 2000ppm.
Embodiment 7:
The present embodiment is the comparative example of embodiment 6.
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Destruction step: put in disintegrating machine by 1 kilogram of titantium hydride block, starts disintegrating machine, closes disintegrating machine, obtain zircoium hydride powder after 6 minutes.
Titantium hydride powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 60% of titantium hydride powder gross mass, the sticky sieve of titantium hydride powder, the angle of repose of titantium hydride powder is 47 degree, hydride powder material temperature degree raises 20 degree, titantium hydride powder nitrogen content 125ppm, titantium hydride powder oxygen content 2700ppm.
Can find out, embodiment 6 is compared with the present embodiment, and the fineness of the titantium hydride powder obtained is identical, but broken time decreased 50%, and the sticky sieve of powder, angle of repose reduces by 6 degree, and purity increases substantially.
Embodiment 8:
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Preparation process: be mixed in high-purity argon gas by gaseous state acetone and spray in glove box, the consumption of methyl alcohol in glove box is 0.1g/m
3;
Destruction step: after methyl alcohol is uniformly dispersed in glove box, puts in disintegrating machine by 1 kilogram through the neodymium iron boron block that hydrogen is quick-fried, starts disintegrating machine, closes disintegrating machine, obtain neodymium-iron-boron powder after 4 minutes.
Neodymium-iron-boron powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 30% of neodymium-iron-boron powder gross mass, the not sticky sieve of neodymium-iron-boron powder, the angle of repose of neodymium-iron-boron powder is 42 degree, neodymium-iron-boron powder temperature raises 5 degree, neodymium-iron-boron powder nitrogen content 70ppm, neodymium-iron-boron powder oxygen content 1500ppm.
Embodiment 9:
The present embodiment is the comparative example of embodiment 8.
Scrubbing procedure: pass into high-purity argon gas in the glove box that disintegrating machine is housed, through 5 gas washings, reduces the oxygen and nitrogen content in glove box;
Destruction step: put in disintegrating machine through the neodymium iron boron block that hydrogen is quick-fried by 1 kilogram, starts disintegrating machine, closes disintegrating machine, obtain neodymium-iron-boron powder after 10 minutes.
Neodymium-iron-boron powder 300 mesh standard sieves are sieved, the quality of minus sieve material accounts for 30% of neodymium-iron-boron powder gross mass, the sticky sieve of neodymium-iron-boron powder, the angle of repose of neodymium-iron-boron powder is 47 degree, neodymium-iron-boron powder temperature raises 10 degree, neodymium-iron-boron powder nitrogen content 100ppm, neodymium-iron-boron powder oxygen content 2000ppm.
Can find out, embodiment 8 is compared with the present embodiment, and the fineness of the neodymium-iron-boron powder obtained is identical, but broken time decreased 60%, and the sticky sieve of powder, angle of repose reduces by 5 degree, and purity increases substantially.
It should be noted that, although above-described embodiment only employs argon gas in scrubbing procedure, other gas do not reacted with metal hydride as: helium, argon gas or nitrogen etc. also can be used for the present invention.
As mentioned above, just the present invention can be realized preferably.
Claims (8)
1. a metal hydride preparation technique, is characterized in that, comprises the following steps:
Preparation process: add grinding aid in disintegrating apparatus;
Destruction step: metal hydride is added disintegrating apparatus, starts disintegrating apparatus and carries out fragmentation, screening to metal hydride, obtain metal hydride powder.
2. a kind of metal hydride preparation technique according to claim 1, is characterized in that:
In described preparation process, described grinding aid is gaseous state.
3. a kind of metal hydride preparation technique according to claim 2, is characterized in that:
The concentration of grinding aid in protective atmosphere of described gaseous state is 0.1-10g/m
3.
4. a kind of metal hydride preparation technique according to claim 2, is characterized in that:
In described preparation process, grinding aid and the inert protective gas of described gaseous state together add disintegrating apparatus.
5. a kind of metal hydride preparation technique according to claim 1, is characterized in that:
Before described preparation process, also comprise scrubbing procedure: in disintegrating apparatus, repeatedly pass into inert gas, discharge the foreign gas in disintegrating apparatus.
6. want a kind of metal hydride preparation technique in 1 ~ 5 described in any one according to right, it is characterized in that: described grinding aid is boiling point lower than at least one in the ketone of 150 DEG C and alcohols.
7. a kind of metal hydride preparation technique according to claim 6, is characterized in that: described grinding aid is methyl alcohol, ethanol or acetone.
8. want a kind of metal hydride preparation technique in 1 ~ 5 described in any one according to right, it is characterized in that: described metal hydride is the neodymium iron boron after hydrogenated niobium, zircoium hydride or hydrogenation.
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Application publication date: 20150204 |