CN106956009A - A kind of alloy powder and preparation method thereof - Google Patents
A kind of alloy powder and preparation method thereof Download PDFInfo
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- CN106956009A CN106956009A CN201710120351.XA CN201710120351A CN106956009A CN 106956009 A CN106956009 A CN 106956009A CN 201710120351 A CN201710120351 A CN 201710120351A CN 106956009 A CN106956009 A CN 106956009A
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Abstract
The present invention provides a kind of alloy powder and preparation method thereof；The alloy powder preparation method of the present invention, comprises the following steps：Complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；Generate gel step：Polyethylene glycol is added to described complex solution, gel is formed；Drying steps：Processing is dried in described gel, xerogel is obtained；Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.Alloy powder of the present invention and preparation method thereof has technique simple, and the characteristics of can accurately matching has greater advantage in uniformity and economy；Secondly, short time ball milling is carried out to gained powder on the basis of sol-gal process, alloying element preferably solid solution can be made, and make powder granule more tiny, traditional MA methods are compared closer to spherical, comparing general sol-gal process and preparing on the method that prealloy powder carries out ball milling again, particle diameter also has some superiority.
Description
Technical field
The invention belongs to field of alloy preparation technology, and in particular to a kind of alloy powder and preparation method thereof.
Background technology
Oxide dispersion intensifying (ODS) steel alloy has good anti-radiation performance, mechanical behavior under high temperature, corrosion resistance
The advantages such as energy, workability energy, therefore the active material as forth generation fission-type reactor and following fusion reactor structural member.Yittrium oxide is made
It is its excellent high performance and the key of anti-radiation performance for its main dispersion-strengtherning phase, the degree of scatter of yittrium oxide turns into ODS
The key factor of alloy Steel Properties.
Mechanical Alloying (Mechanical Alloying, MA) is the main flow and crucial work for preparing ODS steel at present
Skill, is the main method of oxide particle Dispersed precipitate, is also the method for unique industrialized production ODS steel now, commercial at present
ODS alloys such as MA956, MA957, PM2000 are mechanical alloying preparation.But as what ODS Steel Properties were required constantly carries
Height, mechanical alloying preparation technology gradually faces some bottleneck problems：
It is the oxidation and pollution problem of powder first.It is canned and take powder mistake in ball milling because the oxygen content of starting powder is high
Easy oxygen uptake in journey, and during this fine powder is taken out, because its specific surface area is big, surface-active is more difficult to greatly
Avoid oxidation.In mechanical milling process, interaction strength between abrading-ball powder and ball grinder, abrading-ball is big, this cause abrading-ball and
Material in ball grinder easily enters powder and polluted；
Secondly, the last preparatory phase of mechanical alloying need to generally use hot rolling or hot extrusion technique, and this can cause material
The problem of microstructure and mechanical property have anisotropy.
To overcome above mentioned problem, improved mechanical alloying technique and the brand-new technique for preparing ODS steel turn into ODS steels
The focus of standby research, but generally existing enhancing oxide particle size is excessive, strengthen the drawbacks of effect is limited.
The content of the invention
The used technical scheme that solves the above problems is a kind of alloy powder and preparation method thereof.
A kind of alloy powder preparation method that the present invention is provided, comprises the following steps：
Complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Generate gel step：Polyethylene glycol is added to described complex solution, gel is formed；
Drying steps：Processing is dried in described gel, xerogel is obtained；
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
It is preferred that, in the complexation approach, metallic element and citric acid are mol ratio 1 in alloying component:2.
There are hydroxyl and carboxyl on citric acid, can occur esterification and aggregate into high polymer, as gelation process；Add
Solubility increases and forms single-phase association colloid solution alloying element compound in a solvent afterwards；Meanwhile, the hydrolysis of colloidal sol formation
In balance, the addition of citric acid to hydrolyze further progress, so as to accelerate the formation of colloidal sol, is risen in the reaction for forming colloidal sol
To the effect of solubilising and hydrotropy.Added citric acid will be excessively because the metal ion having complexing power under strong acid compares
Weak, excessively favourable complexing, the excessive citric acid of another aspect is conducive to disperseing to keep apart metal ion, after baking sometimes
Particle diameter can be reduced.
It is preferred that, in the complexation approach, the condition of the complexation approach is heating stirring 3-5 hours at 50-60 DEG C.
It is preferred that, in the complexation approach, the pH value of the solution is 7-10.
Citric acid can form complex compound with metallic element, and some metal ions complexing power under strong acid is weaker, has
Metal ion can be precipitated under intermediate acidity, regulation pH to neutral or alkalescence is conducive to more equably forming complex compound, has
It is also possible that metal ion does not adjust pH.
It is preferred that, in the generation gel step, concentration of the polyethylene glycol in complete solution is complexed is
0.005-0.01g/ml；
Described generation gel step is at 70 DEG C, stirring progress.
Wherein, polyethylene glycol is used as surfactant, it is possible to increase esterifying efficiency and the degree of cross linking.
It is preferred that, the condition of the drying steps is at 120-160 DEG C, is more than or equal to 8 hours the heat time.
It is preferred that, described calcination processing includes：Heated 2-3 hours at 200-300 DEG C, then, at 500-600 DEG C
Heating 4-6 hours.
It is preferred that, described reduction treatment includes：Reduced 3-4 hours under 1150-1200 DEG C, reducing atmosphere；
Described reducing atmosphere includes hydrogen, helium, and both mol ratios are 1:1.
It is preferred that, described pulverization process includes：It is 15 in ball material mass ratio：Under 1, ball milling 5-10 hours.
The present invention also provides a kind of alloy powder, and described alloy powder is to use above-mentioned alloy powder preparation method system
Standby.
The present invention is the sol-gel process based on molecule Yu colloid particle size rank, and the preparation for alloy powder is provided
New thinking.The technique mainly uses metallorganic or mineral solution, at low temperature, passes through the hydrolysis of solution, polymerization
Deng chemical reaction, colloidal sol is firstly generated, and then generates the gel with certain space structure, it is then dry by being heat-treated or depressurizing
It is dry, prepare the oxide powder of metal.Then at a certain temperature, part of the metal oxide reduced gas is reduced.Not
The metal oxide of reduction can be uniformly distributed in the metal-powder reduced by disperse.All steps of the technique with point
Son or colloidal particle rank are carried out, thus in final alloy powder product, particle mixing and dispersed oxide yardstick are all expected to protect
Hold in molecule or colloid particle size rank, so as to increase substantially alloy powder performance.
The present invention is by the way that to gel, solution environmental (pH value), drying temperature, lapping mode problem is studied, shape
Into a kind of preparation method of the sol-gel process of more perfect alloy powder.It is gel by selecting polyethylene glycol, and
Sol pH is adjusted to neutral or alkalescent, gel needed for being made then obtains corresponding xerogel using oil bath pan drying.Then
Calcining, reduction, are finally ground using ball milling method, obtain particle uniformly, particle diameter is much smaller than the particle of other preparation methods.
Advantages and advantages of the invention are：A kind of method for preparing alloy powder as sol-gel process first, tool
There is technique simple, the characteristics of can accurately matching has greater advantage in uniformity and economy；Secondly, in sol-gel process
On the basis of short time ball milling is carried out to gained powder, alloying element preferably solid solution can be made, and make powder granule more tiny,
Traditional MA methods are compared closer to spherical, general sol-gal process is compared and prepares the method that prealloy powder carries out ball milling again, particle diameter
On also have some superiority.
Brief description of the drawings
Fig. 1 is obtained particle diameter micro Distribution of the alloy powder under ESEM in embodiment 1；
Fig. 2 is the particle diameter distribution statistics of obtained alloy powder in embodiment 1；
Fig. 3 is obtained particle diameter micro Distribution of the alloy powder under ESEM in embodiment 2；
Fig. 4 is the particle diameter distribution statistics of obtained alloy powder in embodiment 2；
Fig. 5 is obtained particle diameter micro Distribution of the alloy powder under ESEM in embodiment 3；
Fig. 6 is the particle diameter distribution statistics of obtained alloy powder in embodiment 3；
Fig. 7 is obtained particle diameter micro Distribution of the alloy powder under ESEM in embodiment 4；
Fig. 8 is the particle diameter distribution statistics of obtained alloy powder in embodiment 4；
Fig. 9 is obtained particle diameter micro Distribution of the alloy powder under ESEM in embodiment 5；
Figure 10 is the particle diameter distribution statistics of obtained alloy powder in embodiment 5.
Embodiment
To make those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and specific embodiment party
Formula is described in further detail to the present invention.
Embodiment 1
The present embodiment provides a kind of alloy powder and preparation method thereof, and alloying component is as follows：Fe-13Cr-3W-0.4Ti-
0.35Y2O3；Comprise the following steps：
1) complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Metallic element and citric acid are mol ratio 1 in alloying component:2；The element of alloying component it is general with the element can
The form of soluble is provided, for example, ferric nitrate, chromic nitrate etc..Corresponding salt is weighed according to ratio between alloying element to be prepared
.
It is added to the water specifically, the soluble-salt containing subject alloy element is weighed up in alloying component ratio, and adds
The citric acid of corresponding proportion；Wherein, the mass ratio of water and other materials is 3:1；
Above-mentioned complexing is carried out under heating and stirring, and actual temp and time are shown in Table 1；
In above-mentioned complexation approach, in order to which the progress for accelerating complexing can be neutral or alkaline by the pH value modulability of solution, tool
Body pH value is shown in Table 1.
2) gel step is generated：Polyethylene glycol is added to described complex solution, gel is formed；
Concentration of the polyethylene glycol in complete solution is complexed is shown in Table 1；
Described generation gel step is at 70 DEG C, stirring is carried out, and untill magneton can not be stirred, product is black
Or brown gel.
3) drying steps：Processing is dried in described gel, xerogel is obtained；
Gel is heated in oil bath pan, the xerogel of expansion is finally given, the heat time using obtain completely xerogel as
It is accurate.Specific heating-up temperature and heat time are shown in Table 1.
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
4) calcination processing：Xerogel is ground, is put into porcelain boat, is calcined twice in heat-treatment furnace, is calcined twice
Temperature and time be shown in Table 1.
5) reduction treatment：By the product after calcining in reduction furnace, reduced under reducing atmosphere, the temperature restored
Degree and time are shown in Table 1, hydrogen, helium wherein in reducing atmosphere, and both mol ratios are 1:1.
6) pulverization process：Powder carries out ball milling after reducing, wherein, ball material mass ratio is 15：Under 1, Ball-milling Time is shown in Table
1.Thus obtain that particle diameter is smaller, the more uniform alloy powder of particle diameter distribution, by above-mentioned obtained alloy powder under ESEM
Its particle diameter micro Distribution is observed as shown in figure 1, the particle diameter distribution statistics of above-mentioned alloy powder is shown in Fig. 2.
Embodiment 2
The present embodiment provides a kind of alloy powder and preparation method thereof, and alloying component is as follows：Fe-14Cr-3W-0.2Ti-
0.3Y；Comprise the following steps：
1) complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Metallic element and citric acid are mol ratio 1 in alloying component:2；The element of alloying component it is general with the element can
The form of soluble is provided, for example, nitrate etc..Corresponding salt is weighed according to ratio between alloying element to be prepared.
It is added to the water specifically, the soluble-salt containing subject alloy element is weighed up in proportion, and adds corresponding proportion
Citric acid；Wherein, the mass ratio ratio of water and other materials is 15:1；
Above-mentioned complexing is carried out under heating and stirring, and actual temp and time are shown in Table 1；
In above-mentioned complexation approach, in order to which the progress for accelerating complexing can be neutral or alkaline by the pH value modulability of solution, tool
Body pH value is shown in Table 1.
2) gel step is generated：Polyethylene glycol is added to described complex solution, gel is formed；
Concentration of the polyethylene glycol in complete solution is complexed is shown in Table 1；
Described generation gel step is at 70 DEG C, stirring is carried out, and untill magneton can not be stirred, product is black
Or brown gel.
3) drying steps：Processing is dried in described gel, xerogel is obtained；
Gel is heated in oil bath pan, the xerogel of expansion is finally given, the heat time using obtain completely xerogel as
It is accurate.Specific heating-up temperature and heat time are shown in Table 1.
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
4) calcination processing：Xerogel is ground, is put into porcelain boat, is calcined twice in heat-treatment furnace, is calcined twice
Temperature and time be shown in Table 1.
5) reduction treatment：By the product after calcining in reduction furnace, reduced under reducing atmosphere, the temperature restored
Degree and time are shown in Table 1, hydrogen, helium wherein in reducing atmosphere, and both mol ratios are 1:1.
6) pulverization process：Powder carries out ball milling after reducing, wherein, ball material mass ratio is 15：Under 1, Ball-milling Time is shown in Table
1.Thus obtain that particle diameter is smaller, the more uniform alloy powder of particle diameter distribution, by above-mentioned obtained alloy powder under ESEM
Its particle diameter micro Distribution is observed as shown in figure 3, the particle diameter distribution statistics of above-mentioned alloy powder is shown in Fig. 4.
Embodiment 3
The present embodiment provides a kind of alloy powder and preparation method thereof, and alloying component is as follows：Fe-9Cr-3W-0.4Ti-
0.4Y2O3；Comprise the following steps：
1) complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Metallic element and citric acid are mol ratio 1 in alloying component:2；The element of alloying component it is general with the element can
The form of soluble is provided, for example, nitrate etc..Corresponding salt is weighed according to ratio between alloying element to be prepared.
It is added to the water specifically, the soluble-salt containing subject alloy element is weighed up in proportion, and adds corresponding proportion
Citric acid；Wherein, the mass ratio ratio of water and other materials is 4:1；
Above-mentioned complexing is carried out under heating and stirring, and actual temp and time are shown in Table 1；
In above-mentioned complexation approach, in order to which the progress for accelerating complexing can be neutral or alkaline by the pH value modulability of solution, tool
Body pH value is shown in Table 1.
2) gel step is generated：Polyethylene glycol is added to described complex solution, gel is formed；
Concentration of the polyethylene glycol in complete solution is complexed is shown in Table 1；
Described generation gel step is at 70 DEG C, stirring is carried out, and untill magneton can not be stirred, product is black
Or brown gel.
3) drying steps：Processing is dried in described gel, xerogel is obtained；
Gel is heated in oil bath pan, the xerogel of expansion is finally given, the heat time using obtain completely xerogel as
It is accurate.Specific heating-up temperature and heat time are shown in Table 1.
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
4) calcination processing：Xerogel is ground, is put into porcelain boat, is calcined twice in heat-treatment furnace, is calcined twice
Temperature and time be shown in Table 1.
5) reduction treatment：By the product after calcining in reduction furnace, reduced under reducing atmosphere, the temperature restored
Degree and time are shown in Table 1, hydrogen, helium wherein in reducing atmosphere, and both mol ratios are 1:1.
6) pulverization process：Powder carries out ball milling after reducing, wherein, ball material mass ratio is 15：Under 1, Ball-milling Time is shown in Table
1.Thus obtain that particle diameter is smaller, the more uniform alloy powder of particle diameter distribution, by above-mentioned obtained alloy powder under ESEM
Its particle diameter micro Distribution is observed as shown in figure 5, the particle diameter distribution statistics of above-mentioned alloy powder is shown in Fig. 6.
Embodiment 4
The present embodiment provides a kind of alloy powder and preparation method thereof, and alloying component is as follows：Fe-1.5Y2O3；Including following
Step：
1) complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Metallic element and citric acid are mol ratio 1 in alloying component:2；The element of alloying component it is general with the element can
The form of soluble is provided, for example, nitrate etc..Corresponding salt is weighed according to ratio between alloying element to be prepared.
It is added to the water specifically, the soluble-salt containing subject alloy element is weighed up in proportion, and adds corresponding proportion
Citric acid；Wherein, the mass ratio of water and other materials is 3:1；
Above-mentioned complexing is carried out under heating and stirring, and actual temp and time are shown in Table 1；
In above-mentioned complexation approach, in order to which the progress for accelerating complexing can be neutral or alkaline by the pH value modulability of solution, tool
Body pH value is shown in Table 1.
2) gel step is generated：Polyethylene glycol is added to described complex solution, gel is formed；
Concentration of the polyethylene glycol in complete solution is complexed is shown in Table 1；
Described generation gel step is at 70 DEG C, stirring is carried out, and untill magneton can not be stirred, product is black
Or brown gel.
3) drying steps：Processing is dried in described gel, xerogel is obtained；
Gel is heated in oil bath pan, the xerogel of expansion is finally given, the heat time using obtain completely xerogel as
It is accurate.Specific heating-up temperature and heat time are shown in Table 1.
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
4) calcination processing：Xerogel is ground, is put into porcelain boat, is calcined twice in heat-treatment furnace, is calcined twice
Temperature and time be shown in Table 1.
5) reduction treatment：By the product after calcining in reduction furnace, reduced under reducing atmosphere, the temperature restored
Degree and time are shown in Table 1, hydrogen, helium wherein in reducing atmosphere, and both mol ratios are 1:1.
6) pulverization process：Powder carries out ball milling after reducing, wherein, ball material mass ratio is 15：Under 1, Ball-milling Time is shown in Table
1.Thus obtain that particle diameter is smaller, the more uniform alloy powder of particle diameter distribution, by above-mentioned obtained alloy powder under ESEM
Its particle diameter micro Distribution is observed as shown in fig. 7, the particle diameter distribution statistics of above-mentioned alloy powder is shown in Fig. 8.
Embodiment 5
The present embodiment provides a kind of alloy powder and preparation method thereof, and alloying component is as follows：Fe-14Cr-Ti-0.4Y2O3；
Comprise the following steps：
1) complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Metallic element and citric acid are mol ratio 1 in alloying component:2；The element of alloying component it is general with the element can
The form of soluble is provided, for example, nitrate etc..Corresponding salt is weighed according to ratio between alloying element to be prepared.
It is added to the water specifically, the soluble-salt containing subject alloy element is weighed up in proportion, and adds corresponding proportion
Citric acid；Wherein, the mass ratio ratio of water and other materials is 12:1；
Above-mentioned complexing is carried out under heating and stirring, and actual temp and time are shown in Table 1；
In above-mentioned complexation approach, in order to which the progress for accelerating complexing can be neutral or alkaline by the pH value modulability of solution, tool
Body pH value is shown in Table 1.
2) gel step is generated：Polyethylene glycol is added to described complex solution, gel is formed；
Concentration of the polyethylene glycol in complete solution is complexed is shown in Table 1；
Described generation gel step is at 70 DEG C, stirring is carried out, and untill magneton can not be stirred, product is black
Or brown gel.
3) drying steps：Processing is dried in described gel, xerogel is obtained；
Gel is heated in oil bath pan, the xerogel of expansion is finally given, the heat time using obtain completely xerogel as
It is accurate.Specific heating-up temperature and heat time are shown in Table 1.
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
4) calcination processing：Xerogel is ground, is put into porcelain boat, is calcined twice in heat-treatment furnace, is calcined twice
Temperature and time be shown in Table 1.
5) reduction treatment：By the product after calcining in reduction furnace, reduced under reducing atmosphere, the temperature restored
Degree and time are shown in Table 1, hydrogen, helium wherein in reducing atmosphere, and both mol ratios are 1:1.
6) pulverization process：Powder carries out ball milling after reducing, wherein, ball material mass ratio is 15：Under 1, Ball-milling Time is shown in Table
1.Thus obtain that particle diameter is smaller, the more uniform alloy powder of particle diameter distribution, by above-mentioned obtained alloy powder under ESEM
Its particle diameter micro Distribution is observed as shown in figure 9, the particle diameter distribution statistics of above-mentioned alloy powder is shown in Figure 10.
The embodiment 1-5 alloy powder preparation process relevant parameters of table 1
| Item controlled | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Complexation temperature (DEG C) | 60 | 60 | 60 | 50 | 55 |
| Complexation time (h) | 5 | 5 | 4 | 3 | 4 |
| Complex solution pH | 9 | 8 | 8 | 8 | 10 |
| Drying temperature (DEG C) | 120 | 160 | 140 | 135 | 150 |
| Polyethylene glycol (g/ml) | 0.005 | 0.009 | 0.01 | 0.007 | 0.006 |
| First time calcining heat (DEG C) | 300 | 250 | 250 | 270 | 270 |
| First time calcination time (h) | 3 | 3 | 3 | 2 | 2.5 |
| Second of calcining heat (DEG C) | 550 | 550 | 550 | 500 | 500 |
| Second of calcination time (h) | 5 | 5 | 6 | 4 | 4.5 |
| Reduction temperature (DEG C) | 1200 | 1170 | 1150 | 1150 | 1190 |
| Recovery time (h) | 3 | 3.5 | 4 | 3 | 3 |
| Ball-milling Time (h) | 10 | 6 | 8 | 5 | 5 |
By caning be found that the powder granule after ball-milling treatment is more thin in above-described embodiment 1-5 figure and statistical analysis
It is small, and alloying element can be preferably solid-solution among Fe, Cr alloy substrate.
Compared with the powder obtained by the powder and conventional sol gel method obtained by traditional MA methods, particle diameter is more thin
Small, most of particle diameter distribution is between 0.4-1.2 μm, and size is more uniformly distributed, soilless sticking phenomenon, compared to MA methods and typically molten
Sol-gel more connects after preparing small an order of magnitude of particle diameter of the made particle of method that prealloy powder carries out ball milling again, ball milling
It is subsphaeroidal.And the alloy powder composition controllable precise of this method.
In addition, powder granule produced by the present invention has smaller particle, composition evenly and profile so that it is follow-up
By with the advantage become apparent in sintering and heat treatment process, agglutinating property also will be more excellent with mouldability.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, but the invention is not limited in this.For those skilled in the art, the essence of the present invention is not being departed from
In the case of refreshing and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of alloy powder preparation method, it is characterised in that comprise the following steps：
Complexation approach：Alloying component is complexed in the solution with citric acid, complex solution is formed；
Generate gel step：Polyethylene glycol is added to described complex solution, gel is formed；
Drying steps：Processing is dried in described gel, xerogel is obtained；
Described xerogel is subjected to calcination processing, reduction treatment, pulverization process, alloy powder is obtained.
2. alloy powder preparation method as claimed in claim 1, it is characterised in that in the complexation approach, in alloying component
Metallic element is mol ratio 1 with citric acid:2.
3. alloy powder preparation method as claimed in claim 1, it is characterised in that in the complexation approach, the complexing step
Rapid condition be 50-60 DEG C at, heating stirring 3-5 hours.
4. alloy powder preparation method as claimed in claim 1, it is characterised in that in the complexation approach, the solution
PH value is 7-10.
5. alloy powder preparation method as claimed in claim 1, it is characterised in that in the generation gel step, described poly-
Concentration of the ethylene glycol in complete solution is complexed is 0.005-0.01g/ml；
Described generation gel step is at 70 DEG C, stirring progress.
6. alloy powder preparation method as claimed in claim 1, it is characterised in that the condition of the drying steps is 120-
At 160 DEG C, the heat time is more than or equal to 8 hours.
7. alloy powder preparation method as claimed in claim 1, it is characterised in that described calcination processing includes：In 200-
Heat 2-3 hours, then, heated 4-6 hours at 500-600 DEG C at 300 DEG C.
8. alloy powder preparation method as claimed in claim 1, it is characterised in that described reduction treatment includes：In 1150-
1200 DEG C, reduced 3-4 hours under reducing atmosphere；
Described reducing atmosphere includes hydrogen, helium, and both mol ratios are 1:1.
9. alloy powder preparation method as claimed in claim 1, it is characterised in that described pulverization process includes：In ball material
Mass ratio is 15：Under 1, ball milling 5-10 hours.
10. a kind of alloy powder, it is characterised in that described alloy powder is using as described in claim any one of 1-9
Prepared by alloy powder preparation method.
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