CN105177332A - Method for preparing high-tungsten-content tungsten-zirconium alloy - Google Patents
Method for preparing high-tungsten-content tungsten-zirconium alloy Download PDFInfo
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Abstract
The invention relates to a method for preparing high-tungsten-content tungsten-zirconium alloy. The method comprises the following steps that (1) powder is prepared and mixed, tungsten powder and zirconium-titanium powder are mixed and then pelletized, and the proportion, by weight, of the added tungsten powder is 50%-70%; (2) pressing and sintering are carried out, pressing is carried out through a cold isostatic pressing molding press, and pressure is relieved in a graded mode; degreasing sintering is carried out through a high-vacuum resistance furnace, peeling is carried out through finish turning, and a consumable electrode is obtained; and (3) consumable electric arc melting is carried out for at least one time to obtain the high-tungsten-content tungsten-zirconium alloy with uniform ingredients. The consumable electrode is prepared through powder metallurgy, the strength of the electrode is high, and the phenomenon of slag falling is avoided in smelting; the distribution state of tungsten and other elements in the electrode is well improved through powder sintering, the uniformity of ingredients and the structure of cast ingots is facilitated, and therefore the smelted-state tungsten-zirconium alloy with the tungsten content reaching up to 70% is obtained. In addition, through the consumable smelting process, the alloy can be purified, inclusions are eliminated, and the density and the toughness of the alloy are further improved compared with powder-metallurgy-state alloy.
Description
Technical field
The present invention relates to reasonable offer field, particularly relate 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, it has the series of characteristics such as density is high, intensity is large, be normally used for weight material, shielding material and military warhead material, wide in field ranges of application such as medical treatment, engineering machinery, hardware & tools, military affairs, space flight.Tungsten zirconium alloy is a kind of typical containing can structured material, such material quite stable at ambient temperature, and has higher intensity, and under impact loading, in tungsten zirconium alloy zirconium base element because being hit induced chemical reaction, discharge a large amount of heats.Utilize the tungsten zirconium alloy fragmentation that this characteristic is made, its intensity can be utilized to carry out penetration and to run through target, its release characteristics can be utilized again to produce additional injuring to target, finally significantly improve the damage effectiveness of fragmentation to target, have more wide application prospect in military field.
Tungsten zirconium alloy preparation mainly contains two kinds of methods: (1) is powder metallurgical technique: powder metallurgy can prepare the very high alloy material of W content, this technique belongs to solid state sintering in sintering process, spread less between element, alloying level is not high, is difficult to reach absolute densification.For some special dimension, alloy performance requriements is very harsh, and tungsten zirconium alloy prepared by powder metallurgy cannot reach design requirements from density and obdurability angle.(2) vacuum smelting method: vacuum melting can prepare the higher alloy of material property, obtain melting state alloy material, but due to the restriction of non-consumable arc melting temperature, difficulty is added to the tungsten zirconium alloy melting of high W content, and W elements density is high, easily there is tungsten constituent element sedimentation phenomenon in arc melting, be difficult to the high-tungsten alloy preparing homogeneous microstructure.
Although the patent No. is the Chinese invention patent " a kind of arc melting method of high W content tungsten zirconium alloy " of ZL201110440556.9 (authorize public number for CN102492863B) to be disclosed and prepare by non-consumable arc melting the tungsten zirconium alloy that W content reaches 40%, the melting method for the higher tungsten zirconium alloy of W content yet there are no report.
Summary of the invention
Technical problem to be solved by this invention is the preparation method providing a kind of high W content tungsten zirconium alloy for prior art, and W content can reach more than 50%, reaches as high as 70%.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of high W content tungsten zirconium alloy, is characterized in that comprising the following steps:
(1) powder, mixed powder is joined
Tungsten powder and zirconium titanium valve are mixed powder, granulation after mixed powder, it is 50% ~ 70% that tungsten powder adds weight proportion;
(2) suppress, sinter
Adopt the quiet moulding press compactings such as cold, classification release, obtained pressed compact; Then high vacuum resistance furnace is degreasing sintered, and finish turning is removed the peel, obtained consumable electrode;
(3) consumable arc-melting
The high W content tungsten zirconium alloy of uniform composition is obtained through consumable arc-melting at least one times.
Consumable arc-melting in above-mentioned steps (3) is once, and melting electric current is 1 ~ 1.25KA, and stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 2 ~ 3min.As preferably, described consumable arc-melting is selected
water jacketed copper crucible.
Consumable arc-melting in above-mentioned steps (3) is twice, and wherein melting once electric current is 1 ~ 1.25KA, and stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 2 ~ 3min; Secondary smelting is with the obtained melting once ingot casting of melting once for smelting electrode, and electric current is electric current 1.25 ~ 1.5KA, and stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 3 ~ 6min.As preferably, described melting once is selected
water jacketed copper crucible, secondary smelting is selected
water jacketed copper crucible.
As preferably, in described step (1), tungsten powder particle-size is 3 ~ 5um, and zirconium titanium valve granularity is 100 ~ 150um, powder processing is shaped, sintering time to shrink and the final performance of product all obtains good effect.
As preferably, in described step (1), the mixed powder time is 2 ~ 2.5h, mixes the granulation of 5%SBP glue after mixed powder.
As preferably, in described step (2), forming pressure is 200 ~ 220MPa, and the dwell time is 2 ~ 3min.
Further, the vacuum tightness of the consumable arc-melting in described step (3) is 10
-1more than Pa, melting voltage is at 24 ~ 30V, and ingot casting requires to be cooled to come out of the stove when being no more than 150 DEG C.
Compared with prior art, the invention has the advantages that: the present invention is combined by powder metallurgical technique and consumable smelting technique and prepares high W content tungsten zirconium alloy, on the one hand, powder metallurgical technique is adopted to prepare consumable electrode, pole strength is higher, there will not be " falling slag " phenomenon in melting, and the powder sintered distribution that can improve tungsten and other elements in electrode well, be conducive to the composition homogeneity of structure of ingot casting, so can obtain W content up to 70% melting state tungsten zirconium alloy.On the other hand, by consumable smelting technique, can purify alloy, elimination is mingled with, and makes the density of material have further raising with obdurability than powder metallurgy state alloy.
Accompanying drawing explanation
Fig. 1 is ZrTi-50W alloy melting once metallographic microstructure photo in the embodiment of the present invention 1;
Fig. 2 is ZrTi-50W alloy secondary smelting metallographic microstructure photo in the embodiment of the present invention 1;
Fig. 3 is ZrTi-60W alloy melting once metallographic microstructure photo in the embodiment of the present invention 2;
Fig. 4 is ZrTi-70W alloy melting once metallographic microstructure photo in the embodiment of the present invention 3.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
The preparation of embodiment 1:ZrTi-50W alloy
(1) powder, mixed powder is joined
Join powder with ZrTi powder (zirconium titanium valve) and each 50% (mass percent) of W powder (tungsten powder), mix with mixing tank, the mixed powder time is 2h, mixes 5%SBP glue and granulation after mixed powder.
In the present embodiment, ZrTi powder is obtained by the aerosolization of zirtan rod, and in zirtan, zirconium content is the granularity of 40 ~ 60%, ZrTi powder is 100 ~ 150 μm, and the granularity of W powder is 3 ~ 5 μm, and embodiment 2 and embodiment 3 are same therewith, repeat no more.
(2) suppress, sinter
Adopt cold isostatic press 220MPa compacting, pressurize 2min, classification release, obtained pressed compact; By pressed compact 600 DEG C of degreasings, the time is 2h, 1300 DEG C of sintering, insulation 1.5h; Finish turning scale removal, makes
cylindrical electrode, using the consumable electrode of electrode as consumable arc-melting.
(3) consumable arc-melting
The vacuum tightness of consumable arc-melting is 10
-1more than Pa, melting voltage at 30V, through twice consumable arc-melting:
A, melting once
Melting electric current 1 ~ 1.25KA, stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 2 ~ 3min, is cooled to less than 150 DEG C to come out of the stove, and can obtain the high W content tungsten zirconium alloy (i.e. ZrTi-50W ingot) that the present invention obtains, select after coming out of the stove
water jacketed copper crucible.
Product lathe obtained is above cut epidermis, and get block sample respectively in ingot casting head, middle part and bottom and carry out composition analysis, analytical results shows tungsten uniform composition in the alloy (as shown in Figure 1).
B, secondary smelting
Above-mentioned obtained ZrTi-50W ingot is used as secondary smelting electrode, melting electric current 1.25 ~ 1.5KA, stabilising arc electric current is 1.8 ~ 2.5A, smelting time is 3 ~ 6min, less than 150 DEG C are cooled to come out of the stove after melting completes, the high W content tungsten zirconium alloy (i.e. ZrTi-50W bis-ingots) that the present invention obtains can be obtained after coming out of the stove, select
water jacketed copper crucible.
The product lathe that above-mentioned secondary smelting is obtained cuts epidermis, and get block sample respectively in ingot casting head, middle part and bottom and carry out composition analysis, analytical results shows tungsten uniform composition in the alloy (as shown in Figure 2).
The preparation of embodiment 2:ZrTi-60W alloy
(1) powder, mixed powder is joined
Join powder with 40%ZrTi powder and 60%W powder (mass percent), mix with mixing tank, the mixed powder time is 2h, mixes 5%SBP glue and granulation after mixed powder.
(2) suppress, sinter
Adopt cold isostatic press 220MPa compacting, pressurize 2min, classification pressure release, obtained pressed compact; By pressed compact 600 DEG C of degreasings, the time is 2h, 1300 DEG C of sintering, insulation 1.5h; Finish turning scale removal, makes
cylindrical electrode, using the consumable electrode of electrode as consumable arc-melting.
(3) consumable arc-melting
The vacuum tightness of consumable arc-melting is 10
-1more than Pa, melting voltage is at 26V, through a consumable arc-melting: melting electric current 1 ~ 1.25KA, stabilising arc electric current is 1.8 ~ 2.5A, smelting time is 2 ~ 3min, be cooled to less than 150 DEG C to come out of the stove, the high W content tungsten zirconium alloy (i.e. ZrTi-60W ingot) that the present invention obtains can be obtained after coming out of the stove, select
water jacketed copper crucible.
Product lathe obtained is above cut epidermis, and get block sample respectively in ingot casting head, middle part and bottom and carry out composition analysis, analytical results shows tungsten uniform composition in the alloy (as shown in Figure 3).
The preparation of embodiment 3:ZrTi-70W alloy
(1) powder, mixed powder is joined
Join powder with 30%ZrTi powder and 70%W powder (mass percent), mix with mixing tank, the mixed powder time is 2.5h, mixes 5%SBP glue and granulation.
(2) suppress, sinter
Adopt cold isostatic press 200MPa compacting, pressurize 3min, classification pressure release, obtained pressed compact; By pressed compact 600 DEG C of degreasings, the time is 2h, 1300 DEG C of sintering, insulation 1.5h; Finish turning scale removal, makes
cylindrical electrode, using the consumable electrode of electrode as consumable arc-melting.
(3) consumable arc-melting
The vacuum tightness of consumable arc-melting is 10
-1more than Pa, melting voltage is at 24V, through a consumable arc-melting: melting electric current 1 ~ 1.25KA, stabilising arc electric current is 1.8 ~ 2.5A, smelting time is 2 ~ 3min, be cooled to less than 150 DEG C to come out of the stove, the high W content tungsten zirconium alloy (i.e. ZrTi-70W ingot) that the present invention obtains can be obtained after coming out of the stove, select
water jacketed copper crucible.
Product lathe obtained is above cut epidermis, and get block sample respectively in ingot casting head, middle part and bottom and carry out composition analysis, analytical results shows tungsten uniform composition in the alloy (as shown in Figure 4).
Claims (9)
1. a preparation method for high W content tungsten zirconium alloy, is characterized in that comprising the following steps:
(1) powder, mixed powder is joined
Tungsten powder and zirconium titanium valve are mixed powder, granulation after mixed powder, it is 50% ~ 70% that tungsten powder adds weight proportion;
(2) suppress, sinter
Adopt the quiet moulding press compactings such as cold, classification release, obtained pressed compact; Then high vacuum resistance furnace is degreasing sintered, and finish turning is removed the peel, obtained consumable electrode;
(3) consumable arc-melting
At least through the high W content tungsten zirconium alloy of a consumable arc-melting acquisition uniform composition.
2. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterized in that: the consumable arc-melting in described step (3) is once, melting electric current is 1 ~ 1.25KA, and stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 2 ~ 3min.
3. the preparation method of high W content tungsten zirconium alloy as claimed in claim 2, is characterized in that: described consumable arc-melting is selected
water jacketed copper crucible.
4. the preparation method of high W content tungsten zirconium alloy as claimed in claim 1, it is characterized in that: the consumable arc-melting in described step (3) is twice, wherein melting once electric current is 1 ~ 1.25KA, and stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 2 ~ 3min; Secondary smelting is with the obtained melting once ingot casting of melting once for smelting electrode, and electric current is 1.25 ~ 1.5KA, and stabilising arc electric current is 1.8 ~ 2.5A, and smelting time is 3 ~ 6min.
5. the preparation method of high W content tungsten zirconium alloy as claimed in claim 4, is characterized in that: described melting once is selected
water jacketed copper crucible, secondary smelting is selected
water jacketed copper crucible.
6. as the preparation method of the high W content tungsten zirconium alloy in claim 1 or 2 or 4 as described in arbitrary claim, it is characterized in that, in described step (1), tungsten powder particle-size is 3 ~ 5um, and zirconium titanium valve granularity is 100 ~ 150um.
7. as the preparation method of the high W content tungsten zirconium alloy in claim 1 or 2 or 4 as described in arbitrary claim, it is characterized in that, in described step (1), the mixed powder time is 2 ~ 2.5h, mixes the granulation of 5%SBP glue after mixed powder.
8. as the preparation method of the high W content tungsten zirconium alloy in claim 1 or 2 or 4 as described in arbitrary claim, it is characterized in that, in described step (2), forming pressure is 200 ~ 220MPa, and the dwell time is 2 ~ 3min.
9. as the preparation method of the high W content tungsten zirconium alloy in claim 1 or 2 or 4 as described in arbitrary claim, it is characterized in that, the vacuum tightness of described consumable arc-melting is 10
-1more than Pa, melting voltage is at 24 ~ 30V, and ingot casting requires to be cooled to come out of the stove when being no more than 150 DEG C.
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| CN106191479A (en) * | 2016-07-04 | 2016-12-07 | 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 |
| CN111826566A (en) * | 2019-12-11 | 2020-10-27 | 中国人民解放军国防科技大学 | Tungsten/zirconium supersaturated solid solution alloy powder and preparation method thereof |
| CN112877577A (en) * | 2021-01-12 | 2021-06-01 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
| CN115287489A (en) * | 2022-06-23 | 2022-11-04 | 深圳艾利门特科技有限公司 | Preparation method of high-density high-strength tungsten-copper composite material |
| CN115896507A (en) * | 2022-11-23 | 2023-04-04 | 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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| 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 |
| CN115287489A (en) * | 2022-06-23 | 2022-11-04 | 深圳艾利门特科技有限公司 | Preparation method of high-density high-strength tungsten-copper composite material |
| CN115896507A (en) * | 2022-11-23 | 2023-04-04 | 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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