CN107671304B - A kind of method of carbothermic method synthesis of aluminium alloy powder - Google Patents
A kind of method of carbothermic method synthesis of aluminium alloy powder Download PDFInfo
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- CN107671304B CN107671304B CN201710720059.1A CN201710720059A CN107671304B CN 107671304 B CN107671304 B CN 107671304B CN 201710720059 A CN201710720059 A CN 201710720059A CN 107671304 B CN107671304 B CN 107671304B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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Abstract
A kind of method of carbothermic method synthesis of aluminium alloy powder; industrial aluminium ore of the metal oxide with partial size less than 100 μm by partial size less than 50 μm mixes; obtain mixed-powder; after mixed-powder is mixed with carbon dust under inert gas shielding; 1.5~3h is kept the temperature at 1000~1100 DEG C, then heats to 1300~1450 DEG C, and keep the temperature 1.5~3h; it is cooling, obtain soluble aluminum alloy powder.The step of The present invention reduces commercial synthesis aluminium alloys, make full use of raw mineral materials, synthesis cost is reduced, and regard industrial aluminium ore as raw material, it is alkaline that the part of compounds in industrial aluminium ore can make lysate present in dissolution, improve the uniformity of dissolution, part technical oxide can be used as reinforced phase, can moderately improve the compression strength of degradable acieral, and the present invention improves the utilization rate of aluminium ore, technique simplifies, and saves industrial production cost.
Description
Technical field
The invention belongs to metal material fields, and in particular to a kind of method of carbothermic method synthesis of aluminium alloy powder.
Background technique
The advanced technology of world unconventional oil and gas field exploitation is multilayer multistage hydraulic fracturing technology, in the technology recovery process
A large amount of downhole tools can be used.High-strength soluble material can be used for manufacturing such downhole tool, be able to satisfy base in use
This application performance requirement, especially under complicated external condition, can interior receiving high temperature and pressure at work, and can be in pressure break
Original place is dissolved after the completion of work, without being ground or the row of returning, keeps oil-gas pipeline recovery unimpeded, human and material resources and wealth are greatly saved
Power greatly improves engineering progress speed.
Currently, most common degradation material has organic polymer material and metal degradation material, due to organic polymer
The mutability of object, the features such as intensity low and high temperature performance is poor, are easy to cause card plug during pressure break.It therefore can using metal
Degradable material is a kind of current optimal selection, and metal material degradable at present has aluminium alloy and magnesium alloy.Patent
201410819770.9 propose a kind of high-strength dissolvable aluminum alloy materials, the material not only intensity with higher, Er Qie
It is not necessarily to grinding or the row of returning after playing its effect, substantially increases the working efficiency of oil-gas mining, is produced involved in the patent
Method has powder metallurgy and casting and forming.
Using activating aluminum alloys such as low-melting-point metals such as gallium, indium, tin, zinc, lithium in patent CN104480354A, make its surface
Passivating film be destroyed, so that aluminium be made quickly to dissolve in water.The intensity and chemical uniformity of material can be improved in powder metallurgy,
To improve the performance and application performance of material.
And the selection of required powder material is then the important link of powder metallurgy in powder metallurgy.Studies have shown that using not
The slag of refinement is as raw material, and by carbon thermal reduction means, available different alloy powder is greatly lowered and is produced into
This.
Patent 201410084910.2 prepares alfer using carbothermic method, and this method can be directly red from aluminium metallurgy
Alloy is synthesized in mud.Use high titanium richness niobium slag production niobium titanium alloy etc. as raw material in patent 201310449481.X, using carbon heat
Reduction method synthesizes titanium alloy, and the utilization rate of the raw material of industry can be improved.But these alloys cannot dissolve in oilfield exploitation environment, no
It can apply in the pressure break in process for petroleum recovery, it is therefore necessary to provide a kind of soluble acieral.
Summary of the invention
Present invention aims at the solubility properties for improving existing dissolvable aluminum alloy materials, provide a kind of carbothermic method conjunction
At the method for aluminium alloy powder.
To achieve the above object, the present invention can be achieved through the following technical solutions:
Metal oxide is mixed with industrial aluminium ore, is obtained by a kind of method of carbothermic method synthesis of aluminium alloy powder
To mixed-powder, after mixed-powder is mixed with carbon dust under inert gas shielding, at 1000~1100 DEG C keep the temperature 1.5~
3h then heats to 1300~1450 DEG C, and keeps the temperature 1.5~3h, cooling, obtains soluble aluminum alloy powder.
A further improvement of the present invention lies in that industrial aluminium ore is made by the following method: quality of alumina content is greater than
45% industrial aluminum is mining pulverizer carries out being milled to partial size after crushing to be made less than 100 μm.
A further improvement of the present invention lies in that metal oxide is the mixture of oxide A or oxide A and oxide B；
Wherein, oxide A is one or more of tin oxide, gallium oxide, indium oxide, zinc oxide；Oxide B is manganese oxide, oxidation
One or both of magnesium.
A further improvement of the present invention lies in that when metal oxide is the mixture of manganese oxide and oxide A, it is obtained
In soluble aluminum alloy powder, the mass percentage of manganese is 0.5~0.5%；
When metal oxide is the mixture of magnesia and oxide A, in soluble aluminum alloy powder obtained, magnesium
Mass percentage is 1~5%；
When metal oxide is the mixture of manganese oxide, magnesia and oxide A, soluble aluminum alloy powder obtained
In, the mass percentage of manganese is 0.5~0.5%, and the mass percentage of magnesium is 1~5%；
When oxide A is one or more of tin oxide, indium oxide, gallium oxide, zinc oxide, when containing tin oxide
When, in soluble aluminum alloy powder obtained, the mass percentage of tin is 2~4%；When contain indium oxide when, it is obtained can
In dissolubility aluminium alloy powder, the mass percentage of indium is 0.4~1%；When containing zinc oxide, soluble aluminum alloy obtained
In powder, the mass percentage of zinc is 0.5~2%；When containing gallium oxide, in soluble aluminum alloy powder obtained, gallium
Mass percentage be 1~3%.
A further improvement of the present invention lies in that with the heating rate of 3~5 DEG C/min from room temperature to 1000~1100
℃。
A further improvement of the present invention lies in that it is warming up to from 1000~1100 DEG C 1300 with the speed of 2~4 DEG C/min~
1450℃。
A further improvement of the present invention lies in that the mass ratio of mixed-powder and carbon dust is (5~8): 1.
A further improvement of the present invention lies in that the partial size of metal oxide is less than 50 μm.
A further improvement of the present invention lies in that cooling is to cool to room temperature with the furnace, and carry out ball milling after being cooled to room temperature.
Compared with prior art, the invention has the benefit that the present invention by by industrial aluminium ore and partial size metal
Oxide is mixed, and mixed-powder is obtained, after mixed-powder is mixed with carbon dust under inert gas shielding, to alumina ore
Carbonization and metal oxide carbonization obtain soluble aluminum alloy powder using heating stage by stage.Carbon heat provided by the present invention is also
Former method prepares the step of can dissolve aluminium alloy powder, reducing commercial synthesis aluminium alloy, makes full use of raw mineral materials, reduces synthesis
Cost, and using industrial aluminium ore as raw material, the part of compounds in industrial aluminium ore can make lysate that alkali be presented in dissolution
Property, the uniformity of dissolution is improved, part technical oxide can be used as reinforced phase, can moderately improve the anti-of degradable acieral
Compressive Strength, the present invention improve the utilization rate of aluminium ore, and technique simplifies, and save industrial production cost.
Further, metal oxide is the mixture of oxide A or oxide A and oxide B；Wherein, oxide A is
One or more of tin oxide, gallium oxide, indium oxide, zinc oxide；Oxide B is one of manganese oxide, magnesia or two
Kind.Reduction is formed by the alloying elements such as gallium, the indium of low melting point, and the presence of tin element and Zn-ef ficiency can make aluminium alloy
Corrosion potential reduce so that solubility property of the alloy in aqueous solvent increases.
Further, when oxide A is zinc oxide, industrial aluminium ore uses the block of powder metallurgical technique preparation with zinc oxide
Body material, in the KCl solution of the mass concentration 3% at 90 DEG C, degradation rate can reach 4mm/day, and compression strength is reachable
450MPa, and uniformity of degrading is good, compared to using metal, as raw material, can reduce cost is about 32%.
Further, the present invention is using semi-processed mineral aggregates such as industrial aluminium ore, zinc oxide, indium oxides, in conjunction with carbon thermal reduction
Technology, the techniques such as combining powder metallurgy, can synthesize a kind of high intensity, the degradable bulk material of the aluminium base being uniformly dissolved.Directly adopt
It is not only at high cost with gallium, indium, zinc, tin etc., but also reunion is easy to happen due to generating low temperature eutectic in synthesis process.Using this
The oxide of a little metals can not only reduce cost, but also improve the performance of powder in conjunction with carbon thermal reduction technology, to be powder
Last metallurgy etc. improves good powder material.
Specific embodiment
Below by specific embodiment, the present invention is described in detail.
Metal oxide is the mixture of oxide A or oxide A and oxide B in the present invention；Wherein, oxide A is
One or more of tin oxide, gallium oxide, indium oxide, zinc oxide；Oxide B is one of manganese oxide, magnesia or two
Kind.
Specifically, when metal oxide is oxide A, when oxide A is tin oxide, soluble aluminum alloy powder obtained
In, the mass percentage of tin is 2~4%；When oxide A is indium oxide, in soluble aluminum alloy powder obtained, the matter of indium
Measuring percentage composition is 0.4~1%；When oxide A is zinc oxide, in soluble aluminum alloy powder obtained, the quality percentage of zinc
Content is 0.5~2%；When oxide A is gallium oxide, in soluble aluminum alloy powder obtained, the mass percentage of gallium is 1
~3%；
When metal oxide is the mixture of manganese oxide and oxide A, in soluble aluminum alloy powder obtained, manganese
Mass percentage is 0.5~0.5%；
When metal oxide is the mixture of magnesia and oxide A, in soluble aluminum alloy powder obtained, magnesium
Mass percentage is 1~5%；
When metal oxide is the mixture of manganese oxide, magnesia and oxide A, soluble aluminum alloy powder obtained
In, the mass percentage of manganese is 0.5~0.5%, and the mass percentage of magnesium is 1~5%；
When oxide A is one or more of tin oxide, indium oxide, gallium oxide, zinc oxide, when containing tin oxide
When, in soluble aluminum alloy powder obtained, the mass percentage of tin is 2~4%；When contain indium oxide when, it is obtained can
In dissolubility aluminium alloy powder, the mass percentage of indium is 0.4~1%；When containing zinc oxide, soluble aluminum alloy obtained
In powder, the mass percentage of zinc is 0.5~2%；When containing gallium oxide, in soluble aluminum alloy powder obtained, gallium
Mass percentage be 1~3%.
When the mixture that metal oxide is manganese oxide and oxide A, and oxide A is tin oxide, gallium oxide, oxidation
When one of indium, zinc oxide, obtained at this time is aluminium manganese tin, aluminium manganese gallium, aluminium manganese indium or aluminium MnZn ternary alloy three-partalloy.
When the mixture that metal oxide is manganese oxide and oxide A, and oxide A is tin oxide, gallium oxide, oxidation
It is obtained at this time for corresponding quaternary alloys such as aluminium manganese tin gallium, aluminium manganese tin indium, aluminium manganese tin zinc when two kinds in indium, zinc oxide.
When the mixture that metal oxide is manganese oxide and oxide A, and oxide A is tin oxide, gallium oxide, oxidation
When three kinds in indium, zinc oxide, obtained at this time is aluminium manganese tin gallium indium, indium manganese gallium indium zinc, indium manganese tin indium zinc or aluminium manganese tin gallium zinc
Quinary alloy.
When the mixture that metal oxide is manganese oxide and oxide A, and oxide A is tin oxide, gallium oxide, oxidation
When four kinds in indium, zinc oxide, obtained at this time is the hexa-atomic alloy of aluminium manganese tin gallium indium zinc.
When metal oxide be magnesia and oxide A mixture, oxide A be tin oxide, gallium oxide, indium oxide,
When one of zinc oxide, two kinds, three kinds or four kinds, corresponding ternary alloy three-partalloy, quaternary alloy, quinary alloy or hexa-atomic conjunction are obtained
Gold.
When metal oxide is the mixture of manganese oxide, magnesia and oxide A, oxide A is tin oxide, oxidation
When one of gallium, indium oxide, zinc oxide, two kinds, three kinds or four kinds, corresponding quaternary alloy, quinary alloy, hexa-atomic conjunction are obtained
Gold or seven yuan of alloys.
It can be seen that manganese oxide, magnesia cannot be separately added in industrial aluminium ore in the present invention, need and oxide A
One or more of be added in industrial aluminium ore together.
High-strength dissolvable aluminum alloy materials powder produced by the present invention, is made of, matrix matrix phase and second phase two parts
Mutually mainly it is made of the alloy powder of the element solid solutions such as Al and Mg, Ga, Sn, Mn, In, Zn.
Embodiment 1
Carbothermic method synthesis of aluminium alloy powder processing step proposed by the invention are as follows:
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after zinc oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1100 DEG C, and 1.5h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is continuously heating to 1450 DEG C from 1100 DEG C with the speed of 2 DEG C/min, and keeps the temperature 1.5h, cool to room temperature with the furnace later；
Wherein, the mass ratio of mixed-powder and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body, the aluminium alloy powder are that aluminium zinc can dissolve alloy powder.The mass content of zinc is 0.5% in the powder.
Aluminium alloy powder made from embodiment 1 is prepared into block materials using powder metallurgical technique, the matter at 90 DEG C
In the KCl solution for measuring concentration 3%, degradation rate can reach 4mm/day, compression strength up to 450MPa, and degrade uniformity compared with
It is good, compared to using metal, as raw material, can reduce cost is about 32%.
Embodiment 2
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is tin oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 4 DEG C/min from room temperature to 1030 DEG C, and 2.5h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is continuously heating to 1300 DEG C with the speed of 3 DEG C/min, and keeps the temperature 3h, cool to room temperature with the furnace later；Wherein, it mixes
The mass ratio of powder and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body.The mass content of tin is 4% in the powder.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 2.4mm/day, and compression strength is up to 410MPa, and uniformity of degrading is preferable, compares
Using metal as raw material, can reduce cost is about 34%.
Embodiment 3
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of gallium oxide and tin oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 5 DEG C/min from room temperature to 1000 DEG C, and 3h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is continuously heating to 1400 DEG C with the speed of 4 DEG C/min, and keeps the temperature 2h, cool to room temperature with the furnace later；Wherein, it mixes
The mass ratio of powder and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body.The mass content of gallium is 1% in the powder, and the mass content of tin is 2%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 0.6mm/day, and compression strength is up to 425MPa.
Embodiment 4
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of manganese oxide, tin oxide, indium oxide and gallium oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1050 DEG C, and 2h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is warming up to 1350 DEG C with the speed of 2 DEG C/min, and keeps the temperature 2.5h, cool to room temperature with the furnace later；Wherein, mixed powder
The mass ratio of end and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body, the mass content of manganese is 0.2% in the powder, and the mass content of tin is 3%, and the mass content of indium is 1%, and the quality of gallium contains
Amount is 3%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 8.2mm/day, and compression strength is up to 320MPa, and uniformity of degrading is good, compared to adopting
Use metal as raw material, can reduce cost is about 41%.
Embodiment 5
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of indium oxide and zinc oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 5 DEG C/min from room temperature to 1080 DEG C, and 1.5h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is continuously heating to 1420 DEG C with the speed of 3 DEG C/min, and keeps the temperature 2h, cool to room temperature with the furnace later；Wherein, it mixes
The mass ratio of powder and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body.The mass content of indium is 0.4% in gained powder, and the mass content of zinc is 1%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 5.4mm/day, and compression strength is up to 410MPa, and uniformity of degrading is good, compared to adopting
Use metal as raw material, can reduce cost is about 34%.
Embodiment 6
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of magnesia, zinc oxide, tin oxide, manganese oxide, gallium oxide and indium oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1100 DEG C, and 1.5h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is continuously heating to 1450 DEG C with the speed of 2 DEG C/min, and keeps the temperature 1.5h, cool to room temperature with the furnace later；Wherein, it mixes
The mass ratio for closing powder and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body.The mass content of magnesium is 1% in the powder, and the mass content of zinc is 2%, and the mass content of tin is 2.5%, and the quality of manganese contains
Amount is 0.5%, and the mass content of gallium is 2%, and the mass content of indium is 0.7%.
Aluminium alloy powder made from the embodiment is prepared into block materials using powder metallurgical technique, the quality at 90 DEG C
In the KCl solution of concentration 3%, degradation rate can reach 6.8mm/day, and compression strength is up to 378MPa.And degradation uniformity is good,
Compared to using metal, as raw material, can reduce cost is about 38%.
Embodiment 7
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of manganese oxide, magnesia, indium oxide and gallium oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1050 DEG C, and 2h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is warming up to 1350 DEG C with the speed of 2 DEG C/min, and keeps the temperature 2.5h, cool to room temperature with the furnace later；Wherein, mixed powder
The mass ratio of end and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body, the mass content of manganese is 0.3% in the powder, and the mass content of magnesium is 5%, and the mass content of indium is 0.8%, the quality of gallium
Content is 1.5%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 5.4mm/day, and compression strength is up to 394MPa, and uniformity of degrading is good, compared to adopting
Use metal as raw material, can reduce cost is about 36%.
Embodiment 8
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of magnesia and zinc oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1050 DEG C, and 2h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is warming up to 1350 DEG C with the speed of 2 DEG C/min, and keeps the temperature 2.5h, cool to room temperature with the furnace later；Wherein, mixed powder
The mass ratio of end and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body, the mass content of magnesium is 3% in the powder, and the mass content of zinc is 1.5%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 1.8mm/day, and compression strength is up to 470MPa, and uniformity of degrading is preferable, compares
Using metal as raw material, can reduce cost is about 22%.
Embodiment 9
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of manganese oxide, magnesia and gallium oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1050 DEG C, and 2h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is warming up to 1350 DEG C with the speed of 2 DEG C/min, and keeps the temperature 2.5h, cool to room temperature with the furnace later；Wherein, mixed powder
The mass ratio of end and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body, the mass content of manganese is 0.4% in the powder, and the mass content of magnesium is 4%, and the mass content of gallium is 2.5%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 3.6mm/day, and compression strength is up to 396MPa, and uniformity of degrading is preferable, compares
Using metal as raw material, can reduce cost is about 37%.
Embodiment 10
(1) aluminium ore crushes: industrial aluminium ore (aluminium oxide > 45%wt) being crushed with pulverizer, and carries out being milled to average grain
Diameter is lower than 100 μm.
(2) the industrial aluminium ore after metal oxide and ball milling of the partial size less than 50 μm is uniformly mixed, obtains mixed-powder,
Wherein, metal oxide is the mixture of tin oxide, gallium oxide, indium oxide, zinc oxide and manganese oxide.
(3) mixed-powder that step (2) is prepared is mixed with carbon dust, is then reacted under protection of argon gas,
With the heating rate of 3 DEG C/min from room temperature to 1050 DEG C, and 2h is kept the temperature, reacts fully and generate carbide or oxidation of coal
Then object is warming up to 1350 DEG C with the speed of 2 DEG C/min, and keeps the temperature 2.5h, cool to room temperature with the furnace later；Wherein, mixed powder
The mass ratio of end and carbon dust is 5:1；
(4) the reaction synthetic product ball milling for obtaining step (3), and impurity therein is removed, Al alloy powder can be obtained
Body, the mass content of tin is 0.5% in the powder, and the mass content of gallium is 3.5%, and the mass content of indium is 0.5%, the matter of zinc
Amount is 0.8%, and the mass content of manganese is 1%.
Aluminium alloy powder obtained is prepared into block materials using powder metallurgical technique, the mass concentration 3% at 90 DEG C
KCl solution in, degradation rate can reach 6.6mm/day, and compression strength is up to 348MPa, and uniformity of degrading is good, compared to adopting
Use metal as raw material, can reduce cost is about 39%.
Claims (4)
1. a kind of method of carbothermic method synthesis of aluminium alloy powder, which is characterized in that by metal oxide and industrial aluminium ore into
Row mixing, obtains mixed-powder, after mixed-powder is mixed with carbon dust under inert gas shielding, protects at 1000~1100 DEG C
1.5~3h of temperature then heats to 1300~1450 DEG C, and keeps the temperature 1.5~3h, cooling, obtains soluble aluminum alloy powder；
Wherein, industrial aluminium ore is made by the following method: quality of alumina content is greater than to the 45% mining pulverizer of industrial aluminum
It carries out being milled to partial size after crushing and is made less than 100 μm；
Metal oxide is the mixture of oxide A or oxide A and oxide B；Wherein, oxide A is tin oxide, oxidation
One or more of gallium, indium oxide, zinc oxide；Oxide B is one or both of manganese oxide, magnesia；
When metal oxide is the mixture of manganese oxide and oxide A, in soluble aluminum alloy powder obtained, the quality of manganese
Percentage composition is 0.5~0.5%；
When metal oxide is the mixture of magnesia and oxide A, in soluble aluminum alloy powder obtained, the quality of magnesium
Percentage composition is 1~5%；
When metal oxide is the mixture of manganese oxide, magnesia and oxide A, in soluble aluminum alloy powder obtained,
The mass percentage of manganese is 0.5~0.5%, and the mass percentage of magnesium is 1~5%；
When oxide A is one or more of tin oxide, indium oxide, gallium oxide, zinc oxide, when containing tin oxide, system
In the soluble aluminum alloy powder obtained, the mass percentage of tin is 2~4%；When containing indium oxide, soluble aluminum obtained
In alloy powder, the mass percentage of indium is 0.4~1%；When containing zinc oxide, soluble aluminum alloy powder obtained
In, the mass percentage of zinc is 0.5~2%；When containing gallium oxide, in soluble aluminum alloy powder obtained, the matter of gallium
Measuring percentage composition is 1~3%；
The partial size of metal oxide is less than 50 μm；
The mass ratio of mixed-powder and carbon dust is (5~8): 1.
2. a kind of method of carbothermic method synthesis of aluminium alloy powder according to claim 1, which is characterized in that with 3~5
DEG C/heating rate of min is from room temperature to 1000~1100 DEG C.
3. a kind of method of carbothermic method synthesis of aluminium alloy powder according to claim 1, which is characterized in that with 2~4
DEG C/speed of min is warming up to 1300~1450 DEG C from 1000~1100 DEG C.
4. a kind of method of carbothermic method synthesis of aluminium alloy powder according to claim 1, which is characterized in that cooling is
It cools to room temperature with the furnace, and carries out ball milling after being cooled to room temperature.
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| CN101560619A (en) * | 2008-03-04 | 2009-10-21 | 普拉德研究及开发股份有限公司 | Methods of manufacturing degradable alloys and products made from degradable alloys |
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