CN107604186A - A kind of composite rare-earth oxide strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof - Google Patents
A kind of composite rare-earth oxide strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of composite rare-earth oxide to strengthen tungsten base high-specific-gravity alloy composite and preparation method thereof, and the composite is made up of tungsten alloy basis powder and 0.1~1.0 wt% composite rare-earth oxide particle, and wherein composite rare-earth oxide is CeO2、DyO2、Y2O3And Nd2O3In two or more, mainly include the steps such as raw material premix conjunction, a ball milling, secondary ball milling and activated sintering.The present invention can both make additive refinement and homogenization before activated sintering step using composite rare-earth oxide addition and the united mode of secondary ball milling, can improve again Binder Phase be uniformly distributed and volume fraction, alloy is set to have the more tiny W crystallite dimensions and more than 98% consistency of excellent microstructure concurrently, composite material combination property is improved, significant to high tough, superfine crystal tungsten alloy development and application.
Description
Technical field
The present invention relates to technical field of metal material, more particularly to a kind of composite rare-earth oxide to strengthen tungsten base-height ratio and overlap
Metal/composite material and preparation method thereof.
Background technology
Tungsten base high-specific-gravity alloy because with high density, high intensity, high tenacity, absorb ray ability it is strong, electrical and thermal conductivity is good,
The comprehensive excellent properties such as strong and good ductility of corrosion resistance and be widely used in national defense industry, Aero-Space and civilian
Industry, it is a kind of very important dual-use material.In recent years, with the fast development of science and technology, to tungsten base-height ratio weight
The combination property of alloy proposes the requirement of more Gao Gengxin, and the performance of traditional tungsten base high-specific-gravity alloy far can not meet to make
With requiring.Therefore, performance, high tough, the superfine crystal tungsten-based gravity alloy of research and development of tungsten base high-specific-gravity alloy how further to be improved
It is current important topic direction, and general means are mainly reflected in composition design and technological design aspect.
Rare earth is applied to tungsten alloy field due to its unique atomic structure feature and activity as grain growth inhibitor
Existing related research report.However, the reinforcing to tungsten base high-specific-gravity alloy mainly adds single rare earth oxide at present,
Patent CN101880808A discloses a kind of preparation method of nano oxide dispersion reinforced superfine crystal tungsten-based composite, with micro-
Meter level tungsten powder, yttria nanopowders or metal yttrium powder, metallic titanium powder or molybdenum powder or tantalum powder are raw material, through dispensing, mechanical alloying
Ultra-fine grain composite tungsten material is prepared with steps such as discharge plasma sintering, there is good mechanical property.But into
Divide upper addition single rare earth oxide, do not changed in process aspect, the reinforcing effect to composite is limited, its Binder Phase
The indexs such as distribution, the microstructure of composite and mechanical property are still reached to less than promising result.Therefore, there is an urgent need to grind
Study carefully a kind of composite and its preparation technology of higher performance tungsten base high-specific-gravity alloy.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy is compound
Material and preparation method thereof, improve and bond distributed mutually, refining grain size and the mechanical property for improving material.
The present invention is achieved through the following technical solutions：
First aspect, there is provided a kind of composite rare-earth oxide strengthens the preparation method of tungsten base high-specific-gravity alloy composite, including
Following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and at least two RE oxide powders are pre-mixed uniformly,
Mixed material is obtained, then mixed material is put into high energy ball mill and carries out a ball milling.
Between two or more rare earth oxide can because size, shape difference and produce steric hindrance effect
Should, the presence of the effect can make the distribution of composite rare-earth oxide in the base more uniform, and it is more obvious to strengthen effect.
S02：The obtained composite powders of the step S01 are placed in tube type high temperature sintering furnace, in 600~900 DEG C of conditions
Lower annealing 1h.
S03：The obtained composite powders of the step S02 are put into high energy ball mill and carry out secondary ball milling.
The composite rare-earth oxide that carrying out secondary ball milling herein can make to add in above-mentioned steps S01 more refines, and improves
Complex phase rare earth oxide agglomerate, make its distribution more uniform, lift its reinforcing effect to matrix, and can increase compound dilute
Space steric effect between native oxide, make the distribution of rare earth oxide in the base more uniform.Also, secondary ball milling can
To increase the amount of Binder Phase, improve the distribution of Binder Phase, improve the plastic property of alloy material, finally realize the mesh of high Strengthening and Toughening
, improve the combination property of alloy.In addition, composite rare-earth oxide nanosizing can be made using secondary ball milling herein, performance is more
It is good.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
Activated sintering, furnace cooling are carried out in daughter sintering furnace.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
The present invention uses mechanical alloying powder, is aided with discharge plasma activated sintering technology to prepare compound rare-earth oxygen
Compound strengthens tungsten base high-specific-gravity alloy, and composite rare-earth oxide can reduce impurity content and cyrystal boundary segregation in alloy, improves
Elemental redistribution in alloy, the main Dispersed precipitate in the form of second phase particles particle of the rare earth oxide particles of submicron-scale
In in crystal boundary and particle, and coupled by space steric effect and to suppress growing up for W crystal grain during sintering, fine grain is played to alloy
Strengthen the dual invigoration effect with dispersion-strengtherning, make W crystallite dimensions smaller.
The present invention optimizes flouring technology while composite rare-earth oxide is added, on ball milling flouring technology basis
Upper carry out secondary ball milling, secondary ball milling can ensure Binder Phase in alloy be uniformly distributed and volume fraction, have alloy concurrently excellent
Good microstructure more tiny W crystallite dimensions and more than 98% consistency, prepared composite material combination property are able to
Improve, it is significant to high tough, superfine crystal tungsten alloy development and application.
Preferably, the RE oxide powder is submicron order CeO2Powder, DyO2Powder, Y2O3Powder and Nd2O3
Two or more combination in powder, the addition of the RE oxide powder is the base alloy powder
0.1~1.0wt%.
The addition of rare earth oxide can reduce W crystallite dimensions, and coupling suppresses growing up for crystal grain.But when rare earth oxide adds
When dosage is larger, it is easy to segregation phenomenon occur, weakens the bond strength between interface, while sintering densification process is risen certain
Inhibition, deteriorate alloy property.Therefore, be to ensure alloy property, to the control of the addition of rare earth oxide 0.1~
Between 1.0wt%.
Preferably, tungsten base high-specific-gravity alloy basis powder include micron order 93wt% tungsten powders, 4.9wt% nickel powders,
2.1wt% iron powders.
Preferably, in the step S01, the ratio of grinding media to material of a ball milling is 3:1~10:1, Ball-milling Time is 2~48h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed is 300~400r/min, and ball milling starts preceding ball grinder
Vacuumize in advance, then pass to argon gas as protective atmosphere.
Preferably, after a ball milling composite powder be placed in vacuum drying chamber under the conditions of 70~100 DEG C carry out vacuum do
It is dry, it is incubated 1~6h.
Preferably, in the step S02, annealing atmosphere is hydrogen.
Preferably, in the step S03, the ratio of grinding media to material of secondary ball milling is 3:1~10:1, Ball-milling Time is 2~48h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed is 300~400r/min, and ball milling starts preceding ball grinder
Vacuumize in advance, then pass to argon gas as protective atmosphere.
Preferably, the composite powder after secondary ball milling, which is placed in vacuum drying chamber, carries out vacuum under the conditions of 70~100 DEG C
Dry, be incubated 1~6h.
Preferably, in the step S04, graphite jig is put into discharge plasma sintering furnace and carries out activated sintering
During：1150~1350 DEG C of sintering temperature, 3~10min being incubated, 35~50MPa of sintering pressure, sintering atmosphere is vacuum,
And vacuum is less than 10Pa.
Second aspect, the present invention also provide a kind of composite being prepared using the above method.
Technical scheme provided in an embodiment of the present invention can include following beneficial effect：
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method includes：It is pre- that the basic powder of tungsten base high-specific-gravity alloy and 0.1~1.0 wt% composite rare-earth oxide particle are subjected to raw material
The step such as mixing, a ball milling, secondary ball milling and activated sintering.Composite rare-earth oxide is added in tungsten base high-specific-gravity alloy, can
To reduce the impurity content and cyrystal boundary segregation in alloy, improve the Elemental redistribution in alloy, coupling suppresses W crystal grain during sintering
Grow up, the dual invigoration effect of refined crystalline strengthening and dispersion-strengtherning is played to alloy.Present invention addition composite rare-earth oxide
Simultaneously before activated sintering step using secondary ball milling by the way of, guarantee alloy in Binder Phase be uniformly distributed and volume integral
Number, alloy is set to have excellent microstructure, more tiny W crystallite dimensions and consistency concurrently up to more than 98% nearly full cause
Dense body, composite material combination property are improved, significant to high tough, superfine crystal tungsten alloy development and application.
Brief description of the drawings
, below will be to embodiment or existing for the clearer explanation embodiment of the present invention or technical scheme of the prior art
There is the required accompanying drawing used in technology description to be briefly described, it is clear that, to those skilled in the art, not
On the premise of paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the micro-organization chart for the product that the embodiment of the present invention 1 obtains.
Fig. 2 is the micro-organization chart for the product that the embodiment of the present invention 2 obtains.
Fig. 3 is the micro-organization chart for the product that the embodiment of the present invention 3 obtains.
Fig. 4 is the micro-organization chart for the product that the embodiment of the present invention 4 obtains.
Fig. 5 is the micro-organization chart for the product that the embodiment of the present invention 5 obtains.
Fig. 6 is the micro-organization chart for the product that the embodiment of the present invention 6 obtains.
Fig. 7 is the micro-organization chart for the product that the embodiment of the present invention 7 obtains.
Fig. 8 is the micro-organization chart for the product that comparative example 1 of the present invention obtains.
Fig. 9 is the micro-organization chart for the product that comparative example 2 of the present invention obtains.
Figure 10 is the micro-organization chart for the product that comparative example 4 of the present invention obtains.
Embodiment
In order that those skilled in the art more fully understand the technical scheme in the present invention, the present invention will be implemented below
Technical scheme in example is clearly and completely described, it is clear that described embodiment is only that a present invention part is implemented
Example, rather than whole embodiments.Based on the embodiment in the present invention, those skilled in the art are not making creative work
Under the premise of the every other embodiment that is obtained, should all belong to protection scope of the present invention.
Embodiment 1
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, composite rare-earth oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and it is described dilute
The addition of native oxide powder is the 0.1wt% of the base alloy powder（Y2O3、Dy2O3Each 0.05wt%）.After ball milling
Composite powder be dried in vacuo in vacuum drying chamber under the conditions of 70 DEG C, be incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Embodiment 2
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and the rare earth oxygen
The addition of compound powder is the 0.4wt% of the base alloy powder（Y2O3、Dy2O3Each 0.2wt%）.Answering after ball milling
Close powder to be dried in vacuo under the conditions of 70 DEG C in vacuum drying chamber, be incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Embodiment 3
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and the rare earth oxygen
The addition of compound powder is the 0.7wt% of the base alloy powder（Y2O3、Dy2O3Each 0.35wt%）.Answering after ball milling
Close powder to be dried in vacuo under the conditions of 70 DEG C in vacuum drying chamber, be incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Embodiment 4
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and the rare earth oxygen
The addition of compound powder is the 1.0wt% of the base alloy powder（Y2O3、Dy2O3Each 0.5wt%）.Answering after ball milling
Close powder to be dried in vacuo under the conditions of 70 DEG C in vacuum drying chamber, be incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Embodiment 5
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 3 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 48h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 400r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order CeO2Powder and Dy2O3Powder, and the rare earth oxygen
The addition of compound powder is the 0.4wt% of the base alloy powder（CeO2、Dy2O3Each 0.2wt%）.Answering after ball milling
Close powder to be dried in vacuo under the conditions of 100 DEG C in vacuum drying chamber, be incubated 6h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 600 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 3:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 48h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 400r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 100 DEG C, is incubated 6h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1150 DEG C of sintering temperature, is incubated 10min, sintering pressure 35MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Embodiment 6
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 10 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, and Ball-milling Time is
24h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min, and ball milling starts preceding ball grinder
Vacuumize in advance, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt%
Tungsten powder, 4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order CeO2Powder, Y2O3Powder and Dy2O3Powder
End, and the addition of the RE oxide powder is the 0.6wt% of the base alloy powder（CeO2、Y2O3、Dy2O3Respectively
0.2wt%）.Composite powder after ball milling is dried in vacuo in vacuum drying chamber under the conditions of 85 DEG C, is incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 900 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 10:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 20h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 85 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1350 DEG C of sintering temperature, is incubated 3min, sintering pressure 40MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Embodiment 7
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 7 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 5h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Nd2O3Powder and Dy2O3Powder, and the rare earth
The addition of oxide powder is the 1.0wt% of the base alloy powder（Nd2O3、Dy2O3Each 0.5wt%）.After ball milling
Composite powder is dried in vacuo in vacuum drying chamber under the conditions of 70 DEG C, is incubated 6h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 700 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 7:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 5h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 6h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Comparative example 1
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder is pre-mixed uniformly, obtains mixed material, then will mixing
Raw material is 5 according to ratio of grinding media to material:1 is put into high energy ball mill and carries out a ball milling, and Ball-milling Time 2h, ball-milling medium is anhydrous second
Alcohol, ball milling tank material are 304 stainless steels, and rotating speed 300r/min, ball grinder vacuumizes in advance before ball milling starts, and then passes to argon
Gas is as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten powders, 4.9wt% nickel powders, 2.1wt%
Iron powder.Composite powder after ball milling is dried in vacuo in vacuum drying chamber under the conditions of 70 DEG C, is incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, tungsten base-height ratio weight is obtained after the demoulding
Alloy.
Comparative example 2
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Y2O3Powder, and the RE oxide powder
Addition is the 0.4wt% of the base alloy powder.Composite powder after ball milling is in vacuum drying chamber under the conditions of 70 DEG C
It is dried in vacuo, is incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Comparative example 3
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Dy2O3Powder, and the RE oxide powder
Addition is the 0.4wt% of the base alloy powder.Composite powder after ball milling is in vacuum drying chamber under the conditions of 70 DEG C
It is dried in vacuo, is incubated 1h.
S02：The composite powder that the step S01 is obtained is in tube type high temperature sintering furnace, under the conditions of 800 DEG C at annealing
1h is managed, annealing atmosphere is hydrogen.
S03：By the composite powder that the step S02 is obtained according to ratio of grinding media to material be 5:1 is put into high energy ball mill and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, rotating speed 300r/min,
Ball grinder vacuumizes in advance before ball milling starts, and then passes to argon gas as protective atmosphere.Composite powder after secondary ball milling is in true
It is dried in vacuo in empty drying box under the conditions of 70 DEG C, is incubated 1h.
S04：The composite powder that the step S03 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
Comparative example 4
The present invention provides a kind of composite rare-earth oxide and strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof, the side
Method is carried out in accordance with the following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and RE oxide powder are pre-mixed uniformly, mixed
Raw material, it is then 5 according to ratio of grinding media to material by mixed material:1 is put into high energy ball mill and carries out a ball milling, Ball-milling Time 2h,
Ball-milling medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed 300r/min, ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powders,
4.9wt% nickel powders, 2.1wt% iron powders, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and the rare earth oxygen
The addition of compound powder is the 0.4wt% of the base alloy powder（Y2O3、Dy2O3Each 0.2wt%）.Answering after ball milling
Close powder to be dried in vacuo under the conditions of 70 DEG C in vacuum drying chamber, be incubated 4h.
S02：The composite powder that the step S01 is obtained loads in graphite jig, by graphite jig be put into electric discharge etc. from
It is sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, is incubated 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum is less than 10Pa, furnace cooling after the completion of sintering.
S03：Take out the graphite jig in the step S02 to continue to cool down at room temperature, compound rare-earth oxygen is obtained after the demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite.
The product that above-described embodiment 1 to embodiment 7 obtains is observed into its microstructure under a scanning electron microscope,
Obtain result as shown in Figures 1 to 7.From Fig. 1 to Fig. 4, embodiment 1 is close with the crystallite dimension of embodiment 2, embodiment
2 Binder Phase is more and uniformity coefficient is higher, i.e. W-W Connected degrees are low, and the crystallite dimension of embodiment 3 and embodiment 4 is all big
In embodiment 1 and the crystallite dimension of embodiment 2, instead the composite rare-earth oxide powder for illustrating to add excessive content is unfavorable for crystalline substance
The reduction of particle size, with the rising of rare earth oxide content, crystal grain refinement is in reducing tendency, when composite rare-earth oxide content
Based on alloy powder 0.4wt% when, the W crystallite dimensions in obtained product are tiny, and Binder Phase can wrap up W crystal grain well,
Its W- γ (Ni, Fe) Connected degree is low, and Binder Phase, which is divided equally, to be distributed.Being understood with reference to Fig. 5 and Fig. 7, the compound species of rare earth oxide is different,
Its grain refinement effect and reinforcing effect differ, and when three kinds of rare earth oxide compound tenses, it couples suppression crystal grain and grows up effect more
It is good（Shown in Fig. 6）.
Comparison diagram 2 and Fig. 8 understand, embodiment 2 adds composite rare-earth oxide relative to not adding relative to comparative example 1
For adding rare earth oxide, obtained product tungsten grain size more fine uniform.Comparison diagram 2 and Fig. 9 understand, the phase of embodiment 2
For comparative example 2, that is, composite rare-earth oxide is added for single rare earth oxide is added, due to rare earth oxide
Particle size shape is different, easily forms space steric effect, makes its distribution in the base more preferably uniform, coupling suppresses crystal grain
Grow up better, the volume fraction and uniformity of Binder Phase are also guaranteed.Comparison diagram 2 and Figure 10 understand, the phase of embodiment 2
For comparative example 4, i.e. for secondary ball milling for a ball milling, obtained product bonds phase volume fraction and distributing homogeneity
More preferably.
The product that the product and comparative example 1 to comparative example 4 that above-described embodiment 1 is obtained to embodiment 7 obtain enters respectively
Row performance test, test condition is identical, and testing result is as shown in table 1 below：
Table 1：Each embodiment product property testing result
Certainly, described above is also not limited to the example above, the technical characteristic of the invention without description can by or use
Prior art is realized, will not be repeated here；It is to the present invention that above example, which is merely to illustrate technical scheme not being,
Limitation, the present invention is described in detail with reference to preferred embodiment, it will be understood by those within the art that,
The variations, modifications, additions or substitutions that those skilled in the art are made in the essential scope of the present invention are not
Depart from spirit of the invention, should also belong to the claims of the present invention.
Claims (10)
1. a kind of composite rare-earth oxide strengthens the preparation method of tungsten base high-specific-gravity alloy composite, it is characterised in that including
Following steps：
S01：Ready tungsten base high-specific-gravity alloy basis powder and at least two RE oxide powders are pre-mixed uniformly,
Mixed material is obtained, then mixed material is put into high energy ball mill and carries out a ball milling；
S02：The obtained composite powders of the step S01 are placed in tube type high temperature sintering furnace, moved back under the conditions of 600~900 DEG C
Fire processing 1h；
S03：The obtained composite powders of the step S02 are put into high energy ball mill and carry out secondary ball milling；
S04：The composite powder that the step S03 is obtained loads in graphite jig, and graphite jig is put into discharge plasma
Activated sintering, furnace cooling are carried out in sintering furnace；
S05：Take out the graphite jig in the step S04 to continue to cool down at room temperature, composite rare-earth oxide is obtained after the demoulding
Strengthen tungsten base high-specific-gravity alloy composite.
2. a kind of composite rare-earth oxide according to claim 1 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that the RE oxide powder is submicron order CeO2Powder, DyO2Powder, Y2O3Powder and Nd2O3Powder
In two or more combination, the addition of the RE oxide powder for the base alloy powder 0.1~
1.0wt%。
3. a kind of composite rare-earth oxide according to claim 1 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that tungsten base high-specific-gravity alloy basis powder includes micron order 93wt% tungsten powders, 4.9wt% nickel powders, 2.1wt%
Iron powder.
4. a kind of composite rare-earth oxide according to claim 1 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that in the step S01, the ratio of grinding media to material of a ball milling is 3:1~10:1, Ball-milling Time is 2~48h, ball milling
Medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed is 300~400r/min, and ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.
5. a kind of composite rare-earth oxide according to claim 4 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that composite powder is dried in vacuo in vacuum drying chamber under the conditions of 70~100 DEG C after a ball milling, is protected
1~6h of temperature.
6. a kind of composite rare-earth oxide according to claim 1 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that in the step S02, annealing atmosphere is hydrogen.
7. a kind of composite rare-earth oxide according to claim 1 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that in the step S03, the ratio of grinding media to material of secondary ball milling is 3:1~10:1, Ball-milling Time is 2~48h, ball milling
Medium is absolute ethyl alcohol, and ball milling tank material is 304 stainless steels, and rotating speed is 300~400r/min, and ball grinder is advance before ball milling starts
Vacuumize, then pass to argon gas as protective atmosphere.
8. a kind of composite rare-earth oxide according to claim 7 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that the composite powder after secondary ball milling is dried in vacuo in vacuum drying chamber under the conditions of 70~100 DEG C,
It is incubated 1~6h.
9. a kind of composite rare-earth oxide according to claim 1 strengthens the preparation side of tungsten base high-specific-gravity alloy composite
Method, it is characterised in that in the step S04, graphite jig is put into the process being sintered in discharge plasma sintering furnace
In：1150~1350 DEG C of sintering temperature, 3~10min is incubated, 35~50MPa of sintering pressure, sintering atmosphere is vacuum, and vacuum
Degree is less than 10Pa.
10. a kind of composite rare-earth oxide strengthens tungsten base high-specific-gravity alloy composite, it is characterised in that using claim 1
Method described in~9 any one is prepared.
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