CN101525714B - Tungsten alloy material containing yttria and preparation method thereof - Google Patents
Tungsten alloy material containing yttria and preparation method thereof Download PDFInfo
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- CN101525714B CN101525714B CN2009100387403A CN200910038740A CN101525714B CN 101525714 B CN101525714 B CN 101525714B CN 2009100387403 A CN2009100387403 A CN 2009100387403A CN 200910038740 A CN200910038740 A CN 200910038740A CN 101525714 B CN101525714 B CN 101525714B
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- tungsten alloy
- yttrium oxide
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Abstract
The invention provides a tungsten alloy material containing yttria and a preparation method thereof by optimizing and selecting of a tungsten alloy composition formulation and a sintering process. The method concretely includes the steps of matching raw material powder according to the following mass percentage: 92.50- 93 .50 of W, 4.50-5.50 of Ni, 1.00-2.00 of Fe and 0.05-0.60 of Y2O3; then uniformly mixing the powder by a roller type flour mixing machine; and then performing charge plasma rapid sintering to the powder with the sintering pressure of 30-50MPa, sintering with the heating rate of 50-300 DEG C/min, sintering at the temperature of 1170-1300 DEG C, sintering and holding for 2-10 minutes and sintering with the vacuum of not more than 4Pa, thereby obtaining a high-proportion tungsten alloy block material which has the characteristics of nearly full-density, high hardness, good bending strength resistance under room temperature, excellent high-temperature mechanical performance, and the like and has good price-performance advantage and broad application prospect.
Description
Technical field
The present invention relates to powder metallurgy technology, specifically be meant a kind of tungsten alloy material that contains yttrium oxide and preparation method thereof.
Background technology
The W-Ni-Fe high-density alloy has obtained widespread use in fields such as aerospace device, radiation shielding, military project weapons for a long time because of having excellent mechanical property such as high-density, high strength and good corrosion resistance.W-Ni-Fe high-density alloy of the prior art; mainly nickel, iron etc. are formed mutually with bonding by matrix tungsten; and adopt traditional compacting and liquid-phase sintering process to reach near complete fine and close; yet adopt the liquid phase sintering tungsten grain to grow up rapidly; usually can reach 30～50 μ m; thereby weakened the mechanical property under the mechanical property of alloy, particularly high temperature.
At present, investigation of materials person generally believe that the thin brilliant microtexture of acquisition will help improving the over-all properties of block tungstenalloy both at home and abroad.Add grain growth inhibitor, be considered to obtain a kind of comparatively feasible method of thin brilliant tungstenalloy.Wherein adding a spot of rare earth oxide not only can crystal grain thinning, can also play the effect of dispersion-strengthened.Ryu Ho J equals 2003 363 volume 1-2 phase " Materials Science ﹠amp; Engineering A " on studied to trial property yttrium oxide (Y in the paper " Fabricationand properties of mechanical alloyed oxide-dispersed tungsten heavy alloy " delivered
2O
3) to the influence of 93W-5.6Ni-1.4Fe microstructure and mechanical property.Studies show that Y
2O
3Disperse is distributed in around the W crystal grain, can play the effect of dispersion-strengthened and refinement W crystal grain, and Y
2O
3Content is high more, and the W grain refining in the sintered alloy is remarkable more, and the high temperature compression strength of sintered alloy is high more, and can produce " from sharpening " effect under the condition that does not form the Adiabatic Shear band.But this paper fails the component prescription of the W in the material, Ni and Fe is optimized; And at research Y
2O
3When the quality percentage composition changes in 0.1～5% scope the time, improve Y noticing
2O
3When content can improve the hot strength of sintered alloy, do not consider high Y
2O
3Content will weaken the room temperature strength of sintered alloy, thereby to Y
2O
3Content is optimized; In addition, owing to adopt traditional heating means to carry out sintering, sintering time reached more than 1 hour, so that W crystal grain still exists more significantly and grows up in the sintered alloy, thereby had influenced the further raising of sintered alloy over-all properties.In recent ten years, fast development a kind of discharge plasma sintering method of getting up, the essence of this method is exactly the strong pulse electric current sintering.Because the strong pulse electric current can reduce sintering temperature and shorten sintering time the activation of powder, so this method is considered to prepare a kind of very effective, the low-cost approach of thin crystalline substance, ultra-fine crystal block body material, and, also can effectively control the dimensional precision of sintered alloy or part because this sintering method is applied with certain external force in sintering process.In the paper " the SPS sintering behavior of W-Ni-Fe high-density alloy " that Mei Xuezhen equals to deliver on volume the 5th phase " University of Science ﹠ Technology, Beijing's journal " in 2007 the 29th, adopt discharge plasma sintering method to prepare the 93W-5.6Ni-1.4Fe high-density alloy, confirm that discharge plasma sintering can suppress tungsten grain really and grow up, and obtained grain-size microtexture comparatively uniformly, but owing to do not add Y
2O
3With tungstenalloy composition prescription and sintering process are fully optimized, still fail to obtain to organize tiny block sintered alloy, thereby significantly improve the over-all properties of sintered alloy.
Summary of the invention
The objective of the invention is at preparation block high specific gravity tungsten alloy material weak point of the prior art, by optimized choice to tungstenalloy composition prescription and sintering process, a kind of tungsten alloy material that contains yttrium oxide and preparation method thereof is provided, realizes the preparation of the thin crystal block body material of high-specific gravity tungsten alloy of even and tiny, near full densification of microtexture and excellent combination property.
Realize the present invention by following measure.
A kind of tungsten alloy material that contains yttrium oxide contains tungsten, nickel and iron, it is characterized in that: it also contains the small amounts yttrium, specifically is that by mass percentage component and content thereof is: W92.50～93.50%, Ni4.50～5.50%, Fe1.00～2.00%, Y
2O
30.05～0.60%, all the other are inevitable trace impurity.
A kind of preparation method who contains the tungsten alloy material of yttrium oxide comprises the steps:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Raw material tungsten, nickel, iron and yttrium oxide powder are carried out proportioning: W92.50～93.50% by following mass percent consumption, Ni4.50～5.50%, Fe1.00～2.00%, Y
2O
30.05～0.60%, all the other are inevitable trace impurity;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places the powder machine that mixes with powder stock set by step, mixes and is no less than 5 hours;
Step 3: plasma discharging Fast Sintering
Mixed powder after step 2 mixed is packed in the graphite sintering mold, adopts the plasma discharging Fast Sintering again, and the sintering process condition is as follows:
Sintering current type: dc pulse current
Sintering pressure: 30～50MPa
Sintering heating rate: 50～300 ℃/min
Sintering temperature: 1170～1300 ℃
The sintered heat insulating time: 2～10min
Sintering vacuum tightness :≤4Pa
Obtain to organize tiny, uniform a kind of high-specific gravity tungsten alloy block materials that contains yttrium oxide through Fast Sintering.
For realizing the present invention better, described plasma discharging Fast Sintering, its selection process is: heating rate is 250～300 ℃/min, sintering temperature is 1200～1250 ℃, and the sintered heat insulating time is 2～4min.
The present invention compared with prior art has the following advantages:
1, passes through W, Ni, Fe and Y
2O
3The optimization of quality percentage composition, the tungsten alloy material prescription that contains yttrium oxide of the present invention is reasonable, both can utilize Y
2O
3In the restraining effect of sintering process to the W grain growing, obtain to organize tiny, uniform sintered state material, can reduce price comparatively expensive Ni and Y again
2O
3Usage quantity in W alloy is avoided because of Y
2O
3Too high levels and weaken the alloy at room temperature comprehensive mechanical property.In addition, the test by to the block materials comprehensive mechanical property of embodiment preparation has confirmed to adopt optimization of C of the present invention can effectively improve the comprehensive mechanical property of sintered state material under room temperature and high temperature.
2, the present invention adopts the discharge plasma sintering technique sintering to contain an amount of Y
2O
3The W-Ni-Fe alloy, can make full use of Y
2O
3To the inhibiting while of W grain growing in the sintering process, series of advantages such as the low and sintering time of discharge effect, sintering temperature of performance discharge plasma sintering technique is short, thereby the further tissue of refinement sintered alloy, and obtain homogeneous microstructure, tiny block sintered state tungstenalloy.
3, the present invention has optimized and has contained a small amount of Y
2O
3The discharge plasma sintering process of W-Ni-Fe alloy, when heating rate, sintering temperature and soaking time are preferably 250～300 ℃/min, 1200～1250 ℃ and 2～4min respectively, more can give full play to the advantage of discharge plasma sintering W alloy, thereby when obtaining high dense sintering W alloy, fully suppress the growth of W crystal grain.
4, because of in W alloy, having reduced comparatively expensive Ni and the Y of price
2O
3Usage quantity, reduced material cost, because of adopting discharge plasma sintering technique, lowered preparation cost again; So prepared a kind of tungsten alloy material that contains yttrium oxide of the present invention, not only reduced cost effectively, and have near complete fine and close, hardness is high, room temperature bending strength good and characteristics such as mechanical behavior under high temperature excellence, has good superiority of effectiveness, have a extensive future.
Embodiment
The invention will be further described by following embodiment, but embodiments of the present invention are not limited only to this.
Embodiment 1:
A kind of preparation method who contains the tungsten alloy material of yttrium oxide comprises the steps:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Component by mass percentage and content thereof are: W92.50%, Ni5.50%, Fe1.50%, Y
2O
30.50%, all the other are inevitable trace impurity;
Above-mentioned raw materials tungsten, nickel and iron all add with simple substance form, wherein, and about 2.3～2.7 μ m of tungsten powder average particulate diameter, purity 〉=99.0%; About 1～3 μ m of nickel powder average particulate diameter, purity 〉=99.8%; About 1～3 μ m of iron powder average particulate diameter, purity 〉=99.5%; About 1～2 μ m of yttrium oxide powder average particulate diameter, purity 〉=99.9%;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places drum-type to mix the powder machine powder stock and mixed 5 hours set by step;
Step 3: discharge plasma sintering
With the 30g mixed powder diameter of packing into is in the graphite sintering mold of Φ 20mm, Fast Sintering in discharging plasma sintering equipment, and wherein sintering pressure is 50MPa, sintering temperature is 1170 ℃, heating rate is 100 ℃/min, and soaking time is 10 minutes, and vacuum tightness is 4Pa.Obtain the tungstenalloy block materials that contains yttrium oxide of 92.50W-5.50Ni-1.50Fe-0.50Y2O3 behind the sintering, this high-density alloy block materials is organized tiny and even, the tungsten grain distribution of sizes is in 2～3 mu m ranges, mean sizes is 2.5 μ m, density is 17.2g/cm3, room temperature hardness and compressive strength at room temperature are respectively 42HRC and 2010MPa, and the ultimate compression strength under 800 ℃ is 750MPa.
Embodiment 2:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Component by mass percentage and content thereof are: W93.50%, Ni4.50%, Fe1.50%, Y
2O
30.50%, all the other are inevitable trace impurity;
Above-mentioned raw materials tungsten, nickel and iron all add with simple substance form, wherein, and about 2.3～2.7 μ m of tungsten powder average particulate diameter, purity 〉=99.0%; About 1～3 μ m of nickel powder average particulate diameter, purity 〉=99.8%; About 1～3 μ m of iron powder average particulate diameter, purity 〉=99.5%; About 1～2 μ m of yttrium oxide powder average particulate diameter, purity 〉=99.99%;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places drum-type to mix the powder machine powder stock and mixed 6 hours set by step;
Step 3: discharge plasma sintering
With the 30g mixed powder diameter of packing into is in the graphite sintering mold of Φ 20mm, Fast Sintering in discharging plasma sintering equipment, and wherein sintering pressure is 30MPa, sintering temperature is 1250 ℃, heating rate is 250 ℃/min, and soaking time is 4 minutes, and vacuum tightness is 3Pa.Obtain 93.50W-4.50Ni-1.50Fe-0.50Y behind the sintering
2O
3The tungstenalloy block materials that contains yttrium oxide, this high-density alloy block materials is organized tiny and even, the tungsten grain distribution of sizes is in 2～3 mu m ranges, mean sizes is 2.6 μ m, density is 17.5g/cm
3, room temperature hardness and room temperature press ultimate compression strength to be respectively 46HRC and 2500MPa, and the ultimate compression strength under 800 ℃ is 900MPa.
Embodiment 3:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Component by mass percentage and content thereof are: W93.00%, Ni5.40%, Fe1.00%, Y
2O
30.60%, all the other are inevitable trace impurity;
Above-mentioned raw materials tungsten, nickel and iron all add with simple substance form, wherein, and about 2.3～2.7 μ m of tungsten powder average particulate diameter, purity 〉=99.0%; About 1～3 μ m of nickel powder average particulate diameter, purity 〉=99.8%; About 1～3 μ m of iron powder average particulate diameter, purity 〉=99.5%; About 1～2 μ m of yttrium oxide powder average particulate diameter, purity 〉=99.99%;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places drum-type to mix the powder machine powder stock and mixes, mixed 5 hours set by step;
Step 3: discharge plasma sintering
With the 30g mixed powder diameter of packing into is in the graphite sintering mold of Φ 20mm, carries out Fast Sintering in discharging plasma sintering equipment, and wherein sintering pressure is 50MPa, sintering temperature is 1250 ℃, heating rate is 50 ℃/min, and soaking time is 5 minutes, and vacuum tightness is 3Pa.Obtain 93.00W-5.40Ni-1.00Fe-0.60Y behind the sintering
2O
3The tungstenalloy block materials that contains yttrium oxide, this high-density alloy block materials is organized tiny and even, the tungsten grain distribution of sizes is in 2～3 mu m ranges, mean sizes is 2.7 μ m, density is 17.3g/cm
3, room temperature hardness and room temperature press ultimate compression strength to be respectively 44HRC and 2330MPa, and the ultimate compression strength under 800 ℃ is 810MPa.
Embodiment 4:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Component by mass percentage and content thereof are: W93.00%, Ni5.50%, Fe1.45%, Y
2O
30.05%, all the other are inevitable trace impurity;
Above-mentioned raw materials tungsten, nickel and iron all add with simple substance form, wherein, and about 2.3～2.7 μ m of tungsten powder average particulate diameter, purity 〉=99.0%; About 1～3 μ m of nickel powder average particulate diameter, purity 〉=99.8%; About 1～3 μ m of iron powder average particulate diameter, purity 〉=99.5%; About 1～2 μ m of yttrium oxide powder average particulate diameter, purity 〉=99.99%;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places drum-type to mix the powder machine powder stock and mixed 10 hours set by step;
Step 3: discharge plasma sintering
With the 30g mixed powder diameter of packing into is in the graphite sintering mold of Φ 20mm, carries out Fast Sintering in discharging plasma sintering equipment, and wherein sintering pressure is 30MPa, sintering temperature is 1300 ℃, heating rate is 100 ℃/min, and soaking time is 2 minutes, and vacuum tightness is 1Pa.Obtain 93.00W-5.50Ni-1.45Fe-0.05Y behind the sintering
2O
3The tungstenalloy block materials that contains yttrium oxide, this high-density alloy block materials is organized tiny and even, the tungsten grain distribution of sizes is in 2～3 mu m ranges, mean sizes is 2.7 μ m, density is 17.2g/cm
3, room temperature hardness and room temperature press ultimate compression strength to be respectively 42HRC and 2100MPa, and the ultimate compression strength under 800 ℃ is 740MPa.
Embodiment 5:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Component by mass percentage and content thereof are: W93.00%, Ni5.50%, Fe1.45%, Y
2O
30.05%, all the other are inevitable trace impurity;
Above-mentioned raw materials tungsten, nickel and iron all add with simple substance form, wherein, and about 2.3～2.7 μ m of tungsten powder average particulate diameter, purity 〉=99.0%; About 1～3 μ m of nickel powder average particulate diameter, purity 〉=99.8%; About 1～3 μ m of iron powder average particulate diameter, purity 〉=99.5%; About 1～2 μ m of yttrium oxide powder average particulate diameter, purity 〉=99.99%;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places drum-type to mix the powder machine powder stock and mixed 10 hours set by step;
Step 3: discharge plasma sintering
With the 30g mixed powder diameter of packing into is in the graphite sintering mold of Φ 20mm, carries out Fast Sintering in discharging plasma sintering equipment, and wherein sintering pressure is 50MPa, sintering temperature is 1200 ℃, heating rate is 300 ℃/min, and soaking time is 2 minutes, and vacuum tightness is 1Pa.Obtain 93.00W-5.50Ni-1.45Fe-0.05Y behind the sintering
2O
3The tungstenalloy block materials that contains yttrium oxide, this high-density alloy block materials is organized tiny and even, the tungsten grain distribution of sizes is in 2～3 mu m ranges, mean sizes is 2.5 μ m, density is 17.4g/cm
3, room temperature hardness and room temperature press ultimate compression strength to be respectively 46HRC and 2430MPa, and the ultimate compression strength under 800 ℃ is 860MPa.
Claims (5)
1. preparation method who contains the tungsten alloy material of yttrium oxide, it is characterized in that: this method comprises the steps:
Step 1: the prescription that contains the tungsten alloy material of yttrium oxide
Raw material tungsten, nickel, iron and yttrium oxide powder are carried out proportioning: W92.50～93.50% by following mass percent consumption, Ni4.50～5.50%, Fe1.00～2.00%, Y
2O
30.05～0.60%, all the other are inevitable trace impurity;
Step 2: mix powder
The consumption of a described tungsten alloy material prescription places the powder machine that mixes with powder stock set by step, mixes and is no less than 5 hours;
Step 3: plasma discharging Fast Sintering
Mixed powder after step 2 mixed is packed in the graphite sintering mold, adopts the plasma discharging Fast Sintering again, and the sintering process condition is as follows:
Sintering current type: dc pulse current
Sintering pressure: 30～50MPa
Sintering heating rate: 50～300 ℃/min
Sintering temperature: 1170～1300 ℃
The sintered heat insulating time: 2～10min
Sintering vacuum tightness :≤4Pa
Obtain to organize tiny, uniform a kind of high-specific gravity tungsten alloy block materials that contains yttrium oxide through Fast Sintering.
2. a kind of preparation method who contains the tungsten alloy material of yttrium oxide according to claim 1 is characterized in that: the heating rate of described plasma discharging Fast Sintering is 250～300 ℃/min.
3. a kind of preparation method who contains the tungsten alloy material of yttrium oxide according to claim 1 is characterized in that: the temperature of described plasma discharging Fast Sintering is 1200～1250 ℃.
4. a kind of preparation method who contains the tungsten alloy material of yttrium oxide according to claim 1 is characterized in that: the soaking time of described plasma discharging Fast Sintering is 2～4min.
5. the described a kind of prepared quality percentage composition of preparation method that contains the tungsten alloy material of yttrium oxide of one of claim 1～4 is: W92.50～93.50%, Ni4.50～5.50%, Fe1.00～2.00%, Y
2O
30.05～0.60%, all the other are for the tungsten alloy material that contains yttrium oxide of inevitable trace impurity.
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| CN101525714B true CN101525714B (en) | 2011-04-06 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268563B (en) * | 2010-06-02 | 2013-06-26 | 中国科学院金属研究所 | Casting high temperature alloy refiner and high temperature alloy casting method using the same |
| CN103182506B (en) * | 2013-03-29 | 2014-11-12 | 华南理工大学 | TiCp/M2 high-speed steel composite material and SPS (spark plasma sintering) preparation method thereof |
| CN103173670A (en) * | 2013-04-09 | 2013-06-26 | 北京科技大学 | Preparation method for in-situ synthesis of carbide enhanced tungsten-based composite material |
| CN105108131A (en) * | 2015-09-30 | 2015-12-02 | 东北大学 | Preparation method for metal-tungsten-based yttria ceramic nozzles |
| CN106756379B (en) * | 2017-01-10 | 2019-01-25 | 广州市华司特合金制品有限公司 | Tungsten alloy barricade and the electronic information card for being provided with tungsten alloy barricade |
| CN108913973B (en) * | 2018-08-01 | 2020-06-26 | 西安华山钨制品有限公司 | Preparation method of tungsten-nickel-copper alloy foil |
| CN110560700B (en) * | 2019-09-30 | 2021-09-14 | 北京科技大学 | Method for preparing high-density ultrafine-grained rare earth oxide doped tungsten alloy |
| CN113737043B (en) * | 2020-05-29 | 2022-07-26 | 核工业西南物理研究院 | Preparation method of in-situ yttrium oxide particle reinforced tungsten-based composite material |
| CN112501465B (en) * | 2020-11-30 | 2022-04-26 | 深圳市注成科技股份有限公司 | Preparation method of high-thermal-stability nano tungsten alloy |
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