CN107604186B - A kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method - Google Patents
A kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method Download PDFInfo
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Abstract
The present invention provides a kind of composite rare-earth oxides to strengthen tungsten base high-specific-gravity alloy composite material and preparation method, which is made of the composite rare-earth oxide particle of tungsten alloy basis powder and 0.1~1.0 wt%, and wherein composite rare-earth oxide is CeO2、DyO2、Y2O3And Nd2O3In two or more, mainly include raw material premix conjunction, a ball milling, secondary ball milling and activated sintering.The present invention can both make additive refine and homogenize 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 both the consistency of more tiny W crystallite dimension and 98% of excellent microstructure or more, composite material combination property is improved, and is of great significance to high tough, superfine crystal tungsten alloy development and application.
Description
Technical field
Strengthen tungsten base-height ratio the present invention relates to technical field of metal material more particularly to a kind of composite rare-earth oxide to be overlapped
Metal/composite material and preparation method thereof.
Background technique
Tungsten base high-specific-gravity alloy because have high density, high intensity, high tenacity, absorb ray ability it is strong, electrical and thermal conductivity is good,
Corrosion resistance is strong and the comprehensive excellent properties such as good ductility and is widely used in national defense industry, aerospace and civilian
Industry 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 comprehensive performance of alloy proposes the requirement of more Gao Gengxin, and the performance of traditional tungsten base high-specific-gravity alloy, which has been far from satisfying, to be made
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 to be further increased
It is current important topic direction, and general means are mainly reflected in ingredient design and craft design aspect.
Rare earth is applied to tungsten alloy field due to its unique atomic structure feature and activity, as grain growth inhibitor
Has relevant research report.However, single rare earth oxide mainly is added to the reinforcing of tungsten base high-specific-gravity alloy at present,
Patent CN101880808A discloses a kind of preparation method of nano oxide dispersion reinforced superfine crystal tungsten-based composite material, 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 ingredient, mechanical alloying
Ultra-fine grain composite tungsten material is prepared with discharge plasma sintering, there is good mechanical property.But at
Divide upper addition single rare earth oxide, is not changed in process aspect, it is limited to the strengthening effect of composite material, Binder Phase
The indexs such as distribution, the microstructure of composite material and mechanical property are still reached to less than promising result.Therefore, there is an urgent need to grind
Study carefully the composite material and its preparation process of a kind of higher performance tungsten base high-specific-gravity alloy.
Summary 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 improves Binder Phase distribution, refining grain size and the mechanical property for improving material.
The present invention is achieved through the following technical solutions:
In a first aspect, a kind of preparation method of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material is provided,
Include the following steps:
S01: ready tungsten base high-specific-gravity alloy basis powder and at least two RE oxide powders are pre-mixed
Uniformly, mixed raw material is obtained, then mixed raw material is put into high energy ball mill and carries out a ball milling.
Between two or more rare earth oxide can because size, the difference of shape and generate steric hindrance effect
It answers, the presence of the effect can make the distribution of composite rare-earth oxide in the base more uniform, and strengthening effect is more obvious.
S02: the obtained composite powder of the step S01 is placed in tube type high temperature sintering furnace, in 600~900 DEG C of conditions
Lower annealing 1h.
S03: the obtained composite powder of the step S02 is put into high energy ball mill and carries out secondary ball milling.
Carrying out secondary ball milling herein can be such that the composite rare-earth oxide being added in above-mentioned steps S01 more refines, and improve
Complex phase rare earth oxide agglomerate keeps its distribution more uniform, promotes its strengthening effect to matrix, and is capable of increasing compound dilute
Space steric effect between native oxide keeps 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 realizes the mesh of high Strengthening and Toughening
, improve the comprehensive performance 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 is packed into graphite jig, by graphite jig be put into electric discharge etc. from
Activated sintering, furnace cooling are carried out in daughter sintering furnace.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
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 inhibit sintering during W crystal grain grow up, fine grain is played to alloy
Strengthen the dual invigoration effect with dispersion-strengtherning, keeps W crystallite dimension smaller.
The present invention optimizes flouring technology while adding composite rare-earth oxide, on ball milling flouring technology basis
Upper carry out secondary ball milling, secondary ball milling can guarantee Binder Phase in alloy be uniformly distributed and volume fraction, have both alloy excellent
The consistency of the more tiny W crystallite dimension and 98% of good microstructure or more, prepared composite material combination property are able to
It improves, is of great significance 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 additive amount of the RE oxide powder are the base alloy powder
0.1~1.0wt%.
The addition of rare earth oxide can reduce W crystallite dimension, and coupling inhibits 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 guarantee alloy property, to the control of the additive amount of rare earth oxide 0.1~
Between 1.0wt%.
Preferably, tungsten base high-specific-gravity alloy basis powder include micron order 93wt% tungsten powder, 4.9wt% nickel powder,
2.1wt% iron powder.
Preferably, the ratio of grinding media to material of a ball milling is 3:1~10:1 in the step S01, Ball-milling Time is 2~48h,
Ball-milling medium is dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed is 300~400r/min, and ball milling starts preceding ball grinder
It vacuumizes in advance, then passes to argon gas as protective atmosphere.
Preferably, it is dry to carry out vacuum under the conditions of composite powder is placed in a vacuum drying oven 70~100 DEG C after a ball milling
It is dry, keep the temperature 1~6h.
Preferably, annealing atmosphere is hydrogen in the step S02.
Preferably, the ratio of grinding media to material of secondary ball milling is 3:1~10:1 in the step S03, Ball-milling Time is 2~48h,
Ball-milling medium is dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed is 300~400r/min, and ball milling starts preceding ball grinder
It vacuumizes in advance, then passes to argon gas as protective atmosphere.
Preferably, the composite powder after secondary ball milling carries out vacuum under the conditions of being placed in a vacuum drying oven 70~100 DEG C
It is dry, keep the temperature 1~6h.
Preferably, graphite jig is put into discharge plasma sintering furnace and carries out activated sintering in the step S04
During: 1150~1350 DEG C of sintering temperature, 3~10min is kept the temperature, 35~50MPa of sintering pressure, sintering atmosphere is vacuum,
And vacuum degree is less than 10Pa.
Second aspect, the present invention also provides a kind of composite materials being prepared using the above method.
Technical solution provided in an embodiment of the present invention may include it is following the utility model has the advantages that
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
The method of stating includes: that the composite rare-earth oxide particle of the basic powder of tungsten base high-specific-gravity alloy and 0.1~1.0 wt% are carried out original
Expect premixing, a ball milling, secondary ball milling and activated sintering.Compound rare-earth oxidation is added in tungsten base high-specific-gravity alloy
Object can reduce impurity content and cyrystal boundary segregation in alloy, improve the Elemental redistribution in alloy, and coupling inhibits during sintering
W crystal grain is grown up, and the dual invigoration effect of refined crystalline strengthening and dispersion-strengtherning is played to alloy.The present invention adds compound rare-earth oxidation
While object before activated sintering step by the way of secondary ball milling, guarantee alloy in Binder Phase be uniformly distributed and volume
Score, make alloy have both excellent microstructure, more tiny W crystallite dimension and consistency up to 98% or more it is close complete
Dense body, composite material combination property are improved, and are of great significance to high tough, superfine crystal tungsten alloy development and application.
Detailed description of the invention
Illustrate the embodiment of the present invention or technical solution in the prior art in order to clearer, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it is clear that, to those skilled in the art, not
Under the premise of making the creative labor, it is also possible to obtain other drawings based on these 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.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention below will be implemented the present invention
Technical solution in example is clearly and completely described, it is clear that described embodiment is only that present invention a part is implemented
Example, instead of all the embodiments.Based on the embodiments of the present invention, those skilled in the art are not making creative work
Under the premise of every other embodiment obtained, protection scope of the present invention all should belong to.
Embodiment 1
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, composite rare-earth oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and institute
The additive amount for stating RE oxide powder is the 0.1wt%(Y of the base alloy powder2O3、Dy2O3Each 0.05wt%).Ball
Composite powder after mill is dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keeps the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Embodiment 2
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and it is described dilute
The additive amount of native oxide powder is the 0.4wt%(Y of the base alloy powder2O3、Dy2O3Each 0.2wt%).After ball milling
Composite powder be dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keep the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Embodiment 3
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and it is described dilute
The additive amount of native oxide powder is the 0.7wt%(Y of the base alloy powder2O3、Dy2O3Each 0.35wt%).After ball milling
Composite powder be dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keep the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Embodiment 4
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and it is described dilute
The additive amount of native oxide powder is the 1.0wt%(Y of the base alloy powder2O3、Dy2O3Each 0.5wt%).After ball milling
Composite powder be dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keep the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Embodiment 5
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 3:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
48h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving speed 400r/min, and ball milling starts preceding ball grinder
It vacuumizes in advance, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt%
Tungsten powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order CeO2Powder and Dy2O3Powder, and it is described
The additive amount of RE oxide powder is the 0.4wt%(CeO of the base alloy powder2、Dy2O3Each 0.2wt%).Ball milling
Composite powder afterwards is dried in vacuo under the conditions of 100 DEG C in a vacuum drying oven, keeps the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 3:1 and carries out two
Secondary ball milling, Ball-milling Time 48h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 100 DEG C in empty drying box, keeps the temperature 6h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1150 DEG C of sintering temperature, keeps the temperature 10min, sintering pressure 35MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Embodiment 6
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 10:1 and carries out a ball milling by mixed raw material, Ball-milling Time
For for 24 hours, ball-milling medium is dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving speed 300r/min, and ball milling starts preceding ball milling
Tank vacuumizes in advance, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order
93wt% tungsten powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order CeO2Powder, Y2O3Powder and
Dy2O3Powder, and the additive amount of the RE oxide powder is the 0.6wt%(CeO of the base alloy powder2、Y2O3、
Dy2O3Each 0.2wt%).Composite powder after ball milling is dried in vacuo under the conditions of 85 DEG C in a vacuum drying oven, is kept the temperature
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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 10:1 and carries out two
Secondary ball milling, Ball-milling Time 20h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 85 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1350 DEG C of sintering temperature, keeps the temperature 3min, sintering pressure 40MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Embodiment 7
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 7:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
5h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Nd2O3Powder and Dy2O3Powder, and it is described dilute
The additive amount of native oxide powder is the 1.0wt%(Nd of the base alloy powder2O3、Dy2O3Each 0.5wt%).After ball milling
Composite powder be dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keep the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 7:1 and carries out two
Secondary ball milling, Ball-milling Time 5h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 6h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Comparative example 1
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry out in accordance with the following steps:
S01: ready tungsten base high-specific-gravity alloy basis powder being pre-mixed uniformly, mixed raw material is obtained, and then will
Mixed raw material is put into high energy ball mill for 5:1 according to ratio of grinding media to material and carries out a ball milling, and Ball-milling Time 2h, ball-milling medium is nothing
Water-ethanol, ball milling tank material are 304 stainless steels, and revolving speed 300r/min, ball grinder vacuumizes in advance before ball milling starts, and then leads to
Enter argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder be micron order 93wt% tungsten powder, 4.9wt% nickel powder,
2.1wt% iron powder.Composite powder after ball milling is dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keeps the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and tungsten base-height ratio weight is obtained after demoulding
Alloy.
Comparative example 2
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Y2O3Powder, and the RE oxide powder
Additive amount be the base alloy powder 0.4wt%.Composite powder after ball milling 70 DEG C of conditions in a vacuum drying oven
Under be dried in vacuo, keep the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Comparative example 3
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Dy2O3Powder, and the rareearth oxidate powder
The additive amount at end is the 0.4wt% of the base alloy powder.Composite powder after ball milling 70 DEG C of items in a vacuum drying oven
It is dried in vacuo under part, keeps the temperature 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: the composite powder that the step S02 is obtained is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out two
Secondary ball milling, Ball-milling Time 2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, revolving 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 under the conditions of 70 DEG C in empty drying box, keeps the temperature 1h.
S04: the composite powder that the step S03 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
Comparative example 4
The present invention provides a kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method, institute
Method is stated to carry 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, obtained
Then mixed raw material is put into high energy ball mill according to ratio of grinding media to material for 5:1 and carries out a ball milling by mixed raw material, Ball-milling Time is
2h, ball-milling medium are dehydrated alcohol, and ball milling tank material is 304 stainless steels, and revolving speed 300r/min, ball grinder is pre- before ball milling starts
It first vacuumizes, then passes to argon gas as protective atmosphere.Wherein, tungsten base high-specific-gravity alloy basis powder is micron order 93wt% tungsten
Powder, 4.9wt% nickel powder, 2.1wt% iron powder, RE oxide powder are submicron order Y2O3Powder and Dy2O3Powder, and it is described dilute
The additive amount of native oxide powder is the 0.4wt%(Y of the base alloy powder2O3、Dy2O3Each 0.2wt%).After ball milling
Composite powder be dried in vacuo under the conditions of 70 DEG C in a vacuum drying oven, keep the temperature 4h.
S02: the composite powder that the step S01 is obtained is packed into graphite jig, by graphite jig be put into electric discharge etc. from
It being sintered in daughter sintering furnace, 1250 DEG C of sintering temperature, keeps the temperature 5min, sintering pressure 50MPa, sintering atmosphere is vacuum, and
Vacuum degree is less than 10Pa, furnace cooling after the completion of sintering.
S03: the graphite jig taken out in the step S02 continues to cool down at room temperature, and compound rare-earth oxygen is obtained after demoulding
Compound strengthens tungsten base high-specific-gravity alloy composite material.
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.By Fig. 1 to Fig. 4 it is found that 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 degree is low, and the crystallite dimension of embodiment 3 and embodiment 4 is all big
In the crystallite dimension of embodiment 1 and embodiment 2, illustrate instead the composite rare-earth oxide powder for adding 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
For basic alloy powder 0.4wt% when, the obtained W crystallite dimension in product is 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.In conjunction with Fig. 5 and Fig. 7 it is found that the compound type of rare earth oxide is different,
Its grain refinement effect and strengthening effect are different, and when three kinds of rare earth oxide compound tenses, coupling inhibits crystal grain to grow up effect more
Good (shown in Fig. 6).
Comparison diagram 2 and Fig. 8 are it is found that embodiment 2 is relative to comparative example 1, i.e. addition composite rare-earth oxide is not relative to adding
For adding rare earth oxide, obtained product tungsten grain size more fine uniform.Comparison diagram 2 and Fig. 9 are it is found that 2 phase of embodiment
For comparative example 2, i.e. addition composite rare-earth oxide is for adding single rare earth oxide, due to rare earth oxide
Particle size shape is different, space steric effect easy to form, keeps its distribution in the base more preferably uniform, and coupling inhibits crystal grain
It grows up better effect, the volume fraction and uniformity of Binder Phase are also guaranteed.Comparison diagram 2 and Figure 10 are it is found that 2 phase of embodiment
For comparative example 4, i.e. secondary ball milling is for a ball milling, obtained product bonding phase volume fraction and distributing homogeneity
More preferably.
By the product that above-described embodiment 1 to embodiment 7 obtains and the product that comparative example 1 to comparative example 4 obtains respectively into
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, above description is also not limited to the example above, technical characteristic of the present invention without description can by or
It is realized using the prior art, details are not described herein；It is not to this that the above examples are only used to illustrate the technical scheme of the present invention
The limitation of invention, describes the invention in detail referring to preferred embodiment, and those skilled in the art should
Understand, the variations, modifications, additions or substitutions that those skilled in the art are made within the essential scope of the present invention
Without departure from spirit of the invention, it also should belong to claims of the invention.
Claims (3)
1. the preparation method that a kind of composite rare-earth oxide strengthens tungsten base high-specific-gravity alloy composite material, which is characterized 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 raw material is obtained, then mixed raw material is put into high energy ball mill and carries out a ball milling；
S02: the obtained composite powder of the step S01 is placed in tube type high temperature sintering furnace, is moved back under the conditions of 600~900 DEG C
Fire processing 1h；
S03: the obtained composite powder of the step S02 is put into high energy ball mill and carries out secondary ball milling；After secondary ball milling
Composite powder is dried in vacuo under the conditions of 70~100 DEG C in a vacuum drying oven, keeps the temperature 1~6h；
S04: the composite powder that the step S03 is obtained is packed into graphite jig, and graphite jig is put into discharge plasma
Activated sintering, furnace cooling are carried out in sintering furnace；
S05: the graphite jig taken out in the step S04 continues to cool down at room temperature, and composite rare-earth oxide is obtained after demoulding
Strengthen tungsten base high-specific-gravity alloy composite material；
Tungsten base high-specific-gravity alloy basis powder includes micron order 93wt% tungsten powder, 4.9wt% nickel powder, 2.1wt% iron powder；
The RE oxide powder is submicron order CeO2Powder, DyO2Powder, Y2O3Powder and Nd2O3Two kinds in powder or
Two or more combinations, the additive amount of the RE oxide powder are 0.1~1.0wt% of the base alloy powder；
In the step S01, the ratio of grinding media to material of a ball milling is 3:1~10:1, and Ball-milling Time is 2~48h, and ball-milling medium is anhydrous
Ethyl alcohol, ball milling tank material are 304 stainless steels, and revolving speed is 300~400r/min, and ball grinder vacuumizes in advance before ball milling starts, so
After be passed through argon gas as protective atmosphere；
Composite powder is dried in vacuo under the conditions of 70~100 DEG C in a vacuum drying oven after ball milling, keeps the temperature 1~6h；
In the step S03, the ratio of grinding media to material of secondary ball milling is 3:1~10:1, and Ball-milling Time is 2~48h, and ball-milling medium is anhydrous
Ethyl alcohol, ball milling tank material are 304 stainless steels, and revolving speed is 300~400r/min, and ball grinder vacuumizes in advance before ball milling starts, so
After be passed through argon gas as protective atmosphere；
In the step S04, graphite jig is put into during being sintered in discharge plasma sintering furnace: sintering temperature
1150~1350 DEG C, 3~10min, 35~50MPa of sintering pressure are kept the temperature, sintering atmosphere is vacuum, and vacuum degree is less than 10Pa.
2. the preparation side that a kind of composite rare-earth oxide according to claim 1 strengthens tungsten base high-specific-gravity alloy composite material
Method, which is characterized in that in the step S02, annealing atmosphere is hydrogen.
3. a kind of composite rare-earth oxide strengthens tungsten base high-specific-gravity alloy composite material, which is characterized in that using claim 1 or
Method described in 2 is prepared.
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| CN109518023B (en) * | 2018-12-28 | 2020-09-29 | 有研工程技术研究院有限公司 | Method for improving use tolerance temperature of tungsten-aluminum composite material |
| CN110358941B (en) * | 2019-08-12 | 2021-04-16 | 河南科技大学 | Tungsten-based alloy material and preparation method thereof |
| CN111005025B (en) * | 2020-01-08 | 2020-11-03 | 江苏久祥汽车电器集团有限公司 | Preparation method of high-temperature wear-resistant coating for automobile valve mold |
| CN112030026B (en) * | 2020-08-31 | 2021-10-15 | 合肥工业大学 | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material |
| CN112170854B (en) * | 2020-10-14 | 2021-06-15 | 中南大学 | Method for preparing nano spherical oxide dispersion strengthening phase |
| CN112442610A (en) * | 2020-11-24 | 2021-03-05 | 深圳市注成科技股份有限公司 | Preparation method of nano tungsten alloy |
| CN113136514B (en) * | 2021-04-10 | 2022-04-08 | 广州市华司特合金制品有限公司 | High-strength high-specific gravity alloy material and preparation method thereof |
| CN115673327B (en) * | 2022-10-18 | 2024-04-30 | 北京工业大学 | High-strength and high-toughness tungsten alloy and preparation method thereof |
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