CN105177332B - A kind of preparation method of high W content tungsten zirconium alloy - Google Patents
A kind of preparation method of high W content tungsten zirconium alloy Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high W content tungsten zirconium alloy, comprise the following steps：(1) with powder, mixed powder：Tungsten powder and zirconium titanium valve are mixed into powder, are granulated after mixed powder, tungsten powder addition weight proportion is 50%~70%；(2) suppress, sinter：Suppressed using the quiet moulding press such as cold, be classified release；High vacuum resistance furnace is degreasing sintered, smart car peeling, consutrode is made；(3) consumable arc-melting：The uniform high W content tungsten zirconium alloy of composition is obtained by consumable smelting at least once.The present invention prepares consutrode using powder metallurgical technique, pole strength is higher, it is not in " scaling-off " phenomenon in melting, and powder sintered the distribution of tungsten and other elements in electrode is improved well, be advantageous to the composition structural homogenity of ingot casting, and then obtain the melting state tungsten zirconium alloy that W content is up to 70%.In addition, by consumable smelting technique, alloy can be purified, elimination is mingled with, and the consistency and obdurability for making material have further raising than powder metallurgy state alloy.
Description
Technical field
The present invention relates to alloy preparation field, more particularly to a kind of preparation method of high W content tungsten zirconium alloy.
Background technology
Tungsten is a kind of very important non-ferrous metal, and it has the series of characteristics such as density is high, intensity is big, is normally used for
Weight material, shielding material and military warhead material, in fields such as medical treatment, engineering machinery, hardware ＆ tools, military affairs, space flight
Application is wide.Tungsten zirconium alloy be it is a kind of typically containing can structural material, such material quite stable at ambient temperature, and
With higher intensity, and zirconium base member procatarxis is hit and induced chemical reaction under impact loading, in tungsten zirconium alloy, releases
Release substantial amounts of heat.Utilize tungsten zirconium alloy fragmentation made of the characteristic, you can run through target come penetration using its intensity, again may be used
Injured using its release characteristics is additional to target generation, finally significantly improve damage effectiveness of the fragmentation to target, led in military affairs
There is wide application prospect in domain.
Prepared by tungsten zirconium alloy mainly have two methods：(1) it is powder metallurgical technique：Powder metallurgy can prepare W content
Very high alloy material, this technique belong to solid-phase sintering in sintering process, spread less between element, and alloying level is not
Height, it is extremely difficult to absolute densification.Tungsten very harsh to alloy performance requirement for some special dimensions, prepared by powder metallurgy
Zircaloy is unable to reach design requirement from consistency and obdurability angle.(2) vacuum smelting method：Vacuum melting can prepare
The higher alloy of material property, melting state alloy material is obtained, but due to the limitation of non-consumable electric arc melting temperature, to high tungsten
The tungsten zirconium alloy melting of content adds difficulty, and wolfram element density is high, tungsten constituent element sedimentation phenomenon easily occurs in electric arc melting,
It is difficult to prepare the high-tungsten alloy of even tissue.
Although Patent No. ZL 201110440556.9 (it is CN102492863B to authorize public number) Chinese invention patent
《A kind of electric arc melting method of high W content tungsten zirconium alloy》Disclose and W content is prepared by non-consumable electric arc melting reached
40% tungsten zirconium alloy, report is yet there are no for the method for smelting of the higher tungsten zirconium alloy of W content.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of system of high W content tungsten zirconium alloy for prior art
Preparation Method, W content can reach more than 50%, reach as high as 70%.
Technical scheme is used by the present invention solves above-mentioned technical problem：A kind of preparation side of high W content tungsten zirconium alloy
Method, it is characterised in that comprise the following steps：
(1) with powder, mixed powder
Tungsten powder and zirconium titanium valve are mixed into powder, are granulated after mixed powder, tungsten powder addition weight proportion is 50%~70%；
(2) suppress, sinter
Suppressed using the quiet moulding press such as cold, be classified release, pressed compact is made；Then high vacuum resistance furnace is degreasing sintered, essence
Car is removed the peel, and consutrode is made；
(3) consumable arc-melting
The uniform high W content tungsten zirconium alloy of composition is obtained by consumable arc-melting at least once.
For once, melting electric current be 1~1.25KA for consumable arc-melting in above-mentioned steps (3), stabilising arc electric current for 1.8~
2.5A, smelting time are 2~3min.Preferably, the consumable arc-melting is selectedWater jacketed copper crucible.
For consumable arc-melting in above-mentioned steps (3) for twice, wherein melting once electric current is 1~1.25KA, stabilising arc is electric
It is 2~3min to flow for 1.8~2.5A, smelting time；Secondary smelting is using melting once ingot casting made from melting once as melting electricity
Pole, electric current are 1.25~1.5KA of electric current, and stabilising arc electric current is 1.8~2.5A, and smelting time is 3~6min.It is preferably, described
Melting once is selectedWater jacketed copper crucible, secondary smelting are selectedWater jacketed copper crucible.
Preferably, tungsten powder particle-size is 3~5um in the step (1), zirconium titanium valve granularity is 100~150um so that powder
Shunk when end shapes, sintered and the final performance of product obtains preferable effect.
Preferably, it is 2~2.5h that the powder time is mixed in the step (1), the granulation of 5%SBP glue is mixed after mixing powder.
Preferably, briquetting pressure is 200~220MPa in the step (2), the dwell time is 2~3min.
Further, the vacuum of the consumable arc-melting in the step (3) is 10-1More than Pa, melting voltage 24~
30V, ingot casting requirement are come out of the stove when being cooled to no more than 150 DEG C.
Compared with prior art, the advantage of the invention is that：The present invention passes through powder metallurgical technique and consumable smelting technique
With reference to preparing high W content tungsten zirconium alloy, on the one hand, prepare consutrode using powder metallurgical technique, pole strength is higher, melts
Be not in " scaling-off " phenomenon in refining, and it is powder sintered can improve the distribution of tungsten and other elements in electrode well,
Be advantageous to the composition structural homogenity of ingot casting, and then the melting state tungsten zirconium alloy that W content is up to 70% can be obtained.The opposing party
Face, by consumable smelting technique, alloy can be purified, elimination is mingled with, and makes the consistency of material with obdurability than powder metallurgy state
Alloy has further raising.
Brief description of the drawings
Fig. 1 is ZrTi-50W alloy melting once metallographic microstructure photos in the embodiment of the present invention 1；
Fig. 2 is ZrTi-50W alloy secondary smelting metallographic microstructure photos in the embodiment of the present invention 1；
Fig. 3 is ZrTi-60W alloy melting once metallographic microstructure photos in the embodiment of the present invention 2；
Fig. 4 is ZrTi-70W alloy melting once metallographic microstructure photos in the embodiment of the present invention 3.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1：The preparation of ZrTi-50W alloys
(1) with powder, mixed powder
Powder is matched somebody with somebody with ZrTi powder (zirconium titanium valve) and W powder (tungsten powder) each 50% (mass percent), is well mixed with mixing tank, is mixed
The powder time is 2h, and 5%SBP glue is mixed after mixed powder and is granulated.
ZrTi powder is made by zirtan rod aerosolization in the present embodiment, and zirconium content is 40~60% in zirtan,
The granularity of ZrTi powder is 100~150 μm, and the granularity of W powder is 3~5 μm, and embodiment 2 and embodiment 3 are same with this, repeat no more.
(2) suppress, sinter
Suppressed using cold isostatic press 220MPa, pressurize 2min, be classified release, pressed compact is made；By 600 DEG C of degreasings of pressed compact,
Time is 2h, 1300 DEG C of sintering, is incubated 1.5h；Smart car scale removal, is madeCylindrical electrode, by electrode
Consutrode as consumable arc-melting.
(3) consumable arc-melting
The vacuum of consumable arc-melting is 10-1More than Pa, melting voltage is in 30V, by consumable arc-melting twice：
A, melting once
Melting 1~1.25KA of electric current, stabilising arc electric current are 1.8~2.5A, and smelting time is 2~3min, be cooled to 150 DEG C with
Under come out of the stove, high W content tungsten zirconium alloy produced by the present invention (i.e. ingot of ZrTi-50W) is can obtain after coming out of the stove, selectWater jacketed copper crucible.
Product produced above is cut into epidermis with lathe, takes block sample to enter respectively in casting head, middle part and bottom
Row constituent analysis, analysis result show the composition of tungsten in the alloy uniformly (as shown in Figure 1).
B, secondary smelting
Ingot of ZrTi-50W obtained above is used as secondary smelting electrode, melting 1.25~1.5KA of electric current, stabilising arc electricity
It is 3~6min to flow for 1.8~2.5A, smelting time, and less than 150 DEG C are cooled to after the completion of melting and is come out of the stove, i.e. available after coming out of the stove
High W content tungsten zirconium alloy (i.e. bis- ingots of ZrTi-50W) produced by the present invention, selectWater jacketed copper crucible.
Product made from above-mentioned secondary smelting is cut into epidermis with lathe, block is taken respectively in casting head, middle part and bottom
Shape sample carries out constituent analysis, and analysis result shows the composition of tungsten in the alloy uniformly (as shown in Figure 2).
Embodiment 2：The preparation of ZrTi-60W alloys
(1) with powder, mixed powder
Powder is matched somebody with somebody with 40%ZrTi powder and 60%W powder (mass percent), is well mixed with mixing tank, it is 2h to mix the powder time,
5%SBP glue is mixed after mixed powder and is granulated.
(2) suppress, sinter
Suppressed using cold isostatic press 220MPa, pressurize 2min, be classified pressure release, pressed compact is made；By 600 DEG C of degreasings of pressed compact,
Time is 2h, 1300 DEG C of sintering, is incubated 1.5h；Smart car scale removal, is madeCylindrical electrode, by electrode
Consutrode as consumable arc-melting.
(3) consumable arc-melting
The vacuum of consumable arc-melting is 10-1More than Pa, melting voltage is in 26V, by a consumable arc-melting：It is molten
1~1.25KA of electric current is refined, stabilising arc electric current is 1.8~2.5A, and smelting time is 2~3min, is cooled to less than 150 DEG C and comes out of the stove, goes out
High W content tungsten zirconium alloy produced by the present invention (i.e. ingot of ZrTi-60W) is can obtain after stove, is selectedWater-cooled copper
Crucible.
Product produced above is cut into epidermis with lathe, takes block sample to enter respectively in casting head, middle part and bottom
Row constituent analysis, analysis result show the composition of tungsten in the alloy uniformly (as shown in Figure 3).
Embodiment 3：The preparation of ZrTi-70W alloys
(1) with powder, mixed powder
Powder match somebody with somebody with 30%ZrTi powder and 70%W powder (mass percent), is well mixed with mixing tank, mixing the powder time is
2.5h, mix 5%SBP glue and be granulated.
(2) suppress, sinter
Suppressed using cold isostatic press 200MPa, pressurize 3min, be classified pressure release, pressed compact is made；By 600 DEG C of degreasings of pressed compact,
Time is 2h, 1300 DEG C of sintering, is incubated 1.5h；Smart car scale removal, is madeCylindrical electrode, by electrode
Consutrode as consumable arc-melting.
(3) consumable arc-melting
The vacuum of consumable arc-melting is 10-1More than Pa, melting voltage is in 24V, by a consumable arc-melting：It is molten
1~1.25KA of electric current is refined, stabilising arc electric current is 1.8~2.5A, and smelting time is 2~3min, is cooled to less than 150 DEG C and comes out of the stove, goes out
High W content tungsten zirconium alloy produced by the present invention (i.e. ingot of ZrTi-70W) is can obtain after stove, is selectedWater-cooled copper
Crucible.
Product produced above is cut into epidermis with lathe, takes block sample to enter respectively in casting head, middle part and bottom
Row constituent analysis, analysis result show the composition of tungsten in the alloy uniformly (as shown in Figure 4).
Claims (6)
1. a kind of preparation method of high W content tungsten zirconium alloy, it is characterised in that comprise the following steps：
(1) with powder, mixed powder
Tungsten powder and zirconium titanium valve are mixed into powder, are granulated after mixed powder, tungsten powder addition weight proportion is 60%~70%, and wherein tungsten powder particle-size is
3~5 μm, zirconium titanium valve granularity is 100~150 μm；
(2) suppress, sinter
Suppressed using the quiet moulding press such as cold, be classified release, pressed compact is made；Then high vacuum resistance furnace is degreasing sintered, and smart car is gone
Skin, consutrode is made；
(3) consumable arc-melting
The uniform high W content tungsten zirconium alloy of composition is obtained at least through a consumable arc-melting；
When consumable arc-melting is one time, melting electric current is 1~1.25kA, and stabilising arc electric current is 1.8~2.5A, and smelting time is
2~3min；
When consumable arc-melting is twice, wherein melting once electric current is 1~1.25kA, and stabilising arc electric current is 1.8~2.5A, is melted
The refining time is 2~3min；Secondary smelting using melting once ingot casting made from melting once as smelting electrode, electric current be 1.25~
1.5kA, stabilising arc electric current are 1.8~2.5A, and smelting time is 3~6min.
2. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterised in that：The consumable arc-melting
FromWater jacketed copper crucible.
3. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterised in that：The melting once is selectedWater jacketed copper crucible, secondary smelting are selectedWater jacketed copper crucible.
4. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterised in that mixed in the step (1)
The powder time is 2~2.5h, and the granulation of 5%SBP glue is mixed after mixing powder.
5. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterised in that in the step (2) into
Type pressure is 200~220MPa, and the dwell time is 2~3min.
6. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterised in that the consumable arc-melting
Vacuum be 10-1More than Pa, melting voltage are come out of the stove in 24~30V, ingot casting requirement when being cooled to no more than 150 DEG C.
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| CN106191479B (en) * | 2016-07-04 | 2018-06-08 | 武汉理工大学 | A kind of non-consumable electric arc melting preparation method of tungsten alloy |
| CN110295301A (en) * | 2019-07-09 | 2019-10-01 | 中国兵器科学研究院宁波分院 | A kind of preparation method of tungsten-titanium alloy |
| CN111826566B (en) * | 2019-12-11 | 2021-10-29 | 中国人民解放军国防科技大学 | Tungsten/zirconium supersaturated solid solution alloy powder and preparation method thereof |
| CN112877577B (en) * | 2021-01-12 | 2022-02-08 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
| CN115287489B (en) * | 2022-06-23 | 2023-07-18 | 深圳艾利门特科技有限公司 | Preparation method of high-density high-strength tungsten copper composite material |
| CN115896507B (en) * | 2022-11-23 | 2024-04-09 | 宁夏中色金航钛业有限公司 | Niobium hafnium titanium zirconium tantalum tungsten alloy and preparation process thereof |
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| CN101181744B (en) * | 2007-12-10 | 2012-06-06 | 西北有色金属研究院 | Method for preparing titanium alloy cast ingot containing alloy component |
| CN101967569B (en) * | 2010-09-27 | 2012-10-03 | 西安西工大超晶科技发展有限责任公司 | Tungsten-containing titanium alloy smelting method |
| CN102312111B (en) * | 2011-09-07 | 2013-02-06 | 上海交通大学 | Method for preparing TiAl alloy through melting with consumable vacuum arc furnace |
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| CN102965531B (en) * | 2012-12-14 | 2014-12-10 | 西北有色金属研究院 | Preparation method of titanium alloy cast ingot containing high-melting-point elements |
| CN104278167B (en) * | 2014-09-15 | 2017-02-08 | 安泰科技股份有限公司 | Manufacturing method of high-quality titanium-aluminum alloy target |
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