CN105986159A - Fast preparation method for novel W-Ni-Mn alloy - Google Patents
Fast preparation method for novel W-Ni-Mn alloy Download PDFInfo
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Abstract
The invention belongs to the technical field of a novel tungsten alloy and preparation of the novel tungsten alloy and provides a fast preparation method for a novel W-Ni-Mn alloy with excellent comprehensive performance. The method specially includes the steps that firstly, W elementary powder, Ni elementary powder and Mn elementary powder are matched according to the mass percentage of 91.0-95.0% of W, 1.0-7.2% of Ni and 1.0-7.2% of Mn; then vacuum material mixing is performed on a high-energy ball mill till the raw materials are mixed uniformly; and finally, fast forming of the powder and one-step or two-step sintering are performed on a discharging plasma sintering device. The novel W-Ni-Mn alloy prepared through the method is uniform in structure, fine in W grain, high in relative density and good in comprehensive mechanical performance. The fast preparation method has the beneficial effects that forming and sintering are integrated, the sintering temperature is low, and the sintering time is short; and the fine-W-grain W-Ni-Mn alloy can be acquired easily, and the preparation cost of the material can be reduced to a certain extent.
Description
Technical field
The invention belongs to novel tungsten alloy preparing technical field, more specifically, be the fast preparation method about novel W Ni Mn alloy.
Background technology
Tungsten alloy has the performance of a series of excellence, and such as density height, intensity is high, machining property is good, thermal coefficient of expansion is little, electrical and thermal conductivity is good, and these excellent properties make it be widely used in defence and military, Aero-Space and civilian industry.Relative to conventional tungsten alloy, novel W Ni Mn alloy has more preferable Adiabatic Shear performance, can cause the increase of Adiabatic Shear Bands, thus be readily applicable to armor-piercing bullet material.When using as bullet, because having self-sharpening without reducing its penetration depth, therefore it can be competed mutually with depleted uranium bullet.
For novel W Ni Mn alloy, material powder ball milling, molding, the conventional powder metallurgical lqiuid phase sintering method of sintering is the most still utilized to prepare.This method has open defect: first, high chemism due to Mn, sintering process easily generates on alloy boundary MnO, for at utmost reducing MnO, actual liquid phase sintering conditions is often high than Binder Phase liquidus curve minimum temperature, being easily caused tungsten grain to grow up, this is unfavorable for preparing high performance alloys；Secondly as do not apply external pressure in sintering process, the gas that conventional liquid phase sintering hydrogen reducing MnO produces cannot be got rid of from sample completely, thus adds the porosity of alloy, causes alloy density to reduce；Finally, conventional liquid phase sintering process molding is undertaken in two steps with sintering, and technological process is longer, and in sintering process, heating rate is relatively slow, and the sintered specimen time is longer, and this all can increase the probability of material powder oxidation.
At present, for meeting the increasing demand to high-performance novel W Ni Mn alloy, use new method, new technology, overcome the defect of Traditional liquid phase sintering process, reduce the residual porosity and the oxide of manganese easily occurred in alloy, the size of refinement tungsten grain, and then put forward heavy alloyed consistency, the mechanical property finally improving alloy is an important topic.As a kind of material new preparation technology, compared with conventional liquid phase sintering process, discharge plasma sintering has that heating rate is fast, sintering temperature is low, sintering time is short and the many advantages such as hot pressed sintering, Worth Expecting in terms of the preparation of novel W Ni Mn alloy.Therefore, on the basis of correlational study, the present invention is from optimizing material composition proportioning, adjusting the measure such as preprocessing method of raw materials, innovation discharge plasma sintering process, it is proposed that a kind of quick preparation has the method for excellent comprehensive performance W Ni Mn alloy.
Summary of the invention
The technical disadvantages that instant invention overcomes that the technological process that conventional liquid phase sintering W Ni Mn alloy exists is longer, sintering temperature is higher, temperature retention time is longer etc., it is provided that a kind of simple and quick prepared high fine and close and method of premium properties W Ni Mn alloy.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The fast preparation method of a kind of novel W Ni Mn alloy, it is characterised in that comprise the technical steps that:
(1) material composition proportioning: with W, Ni, Mn elemental powders as alloy raw material, and according to following mass percent dispensing: W 91.0 95.0%, Ni 1.0 7.2%, Mn 1.0 7.2%；
(2) raw material uniformly mixes: is loaded in ball grinder by the above-mentioned material powder for preparing, carries out Vacuum Mixture, it is thus achieved that mixed uniformly material powder on high energy ball mill；
(3) powder Fast Sintering: after above-mentioned uniform mixed-powder is loaded graphite jig, is placed in discharge plasma sintering system heating intracavity, carries out discharge plasma sintering after evacuation.
Described high energy ball mill is planetary ball mill, vibration type ball mill or stirring ball mill.
Described discharge plasma sintering is a step sintering process or two-step sintering technique.
A described step sintering process conditions is as follows:
Sintering vacuum < 3Pa, sintering pressure 30 90MPa, 100 400 DEG C/min of heating rate, sintering temperature 1,000 1250 DEG C, temperature retention time 3 5min.
Described two-step sintering process conditions are as follows:
The first step: sintering vacuum < 3Pa, sintering pressure 30 90MPa, 50 200 DEG C/min of heating rate, sintering temperature 900 1000 DEG C, temperature retention time 10 20min；
Second step: sintering vacuum < 3Pa, sintering pressure 30 90MPa, 200 400 DEG C/min of heating rate, sintering temperature 1,000 1200 DEG C, temperature retention time 0min.
Compared with prior art, the present invention has advantage highlighted below and a beneficial effect:
1. the present invention make use of high energy ball mill in the batch mixing of W, Ni, Mn raw material, compared with common V-type batch mixer or tumbling ball mill, can improve batch mixing efficiency and uniformity coefficient；Compared with carrying out high-energy ball milling with ball adding, introducing and the rising of powder oxygen content of impurity can be avoided.
2. the present invention is on the basis of plasma discharging one step sinters, and further with plasma discharging " two-step sintering " method, reduces W/W Connected degree as far as possible, can obtain the more preferable novel W Ni Mn alloy of comprehensive mechanical property while controlling W grain growth.
3. the present invention takes full advantage of the technical characterstic of discharge plasma sintering, there is the advantages such as molding and sintering integratedization, sintering temperature is relatively low, sintering time is shorter, thus be readily available thin W crystal grain W Ni Mn alloy, and the preparation cost of material can be reduced to a certain extent.
4. the novel W Ni Mn alloy that prepared by the present invention has that even tissue, W crystal grain is tiny, relative density high, thus compares conventional liquid phase sintering, and the comprehensive mechanical property of W Ni Mn alloy is more preferable.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The fast preparation method of the novel W 1.8Ni 7.2Mn alloy of the present embodiment, comprises the following steps and process conditions:
(1) material composition proportioning: with W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing: W 91.0%, Ni
1.8%, Mn 7.2%；The purity of W, Ni, Mn powder>99.9%, mean diameter<3 μm.
(2) raw material uniformly mixes: load in ball grinder by the above-mentioned material powder for preparing, Vacuum Mixture 12h on planetary ball mill, it is thus achieved that mixed uniformly material powder.
(3) powder Fast Sintering: after uniform for above-mentioned 60g mixed-powder is loaded Ф 30mm graphite jig, it is placed in discharge plasma sintering system heating intracavity, plasma discharging one step sintering is carried out after evacuation, sintering process conditions is: sintering vacuum is less than 1Pa, sintering pressure 80MPa, 350 DEG C/min of heating rate, sintering temperature 1110 DEG C, temperature retention time 3min.
By method made above, it is thus achieved that the novel W 1.8Ni 7.2Mn alloy of even tissue, its W crystal grain is less than 6 μm, and relative density is more than 97%, and macrohardness is 38HRC, and bending strength is 1124MPa.
Embodiment 2
The fast preparation method of the novel W 2.8Ni 4.2Mn alloy of the present embodiment, comprises the following steps and process conditions:
(1) material composition proportioning: with W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing: W 93.0%, Ni
2.8%, Mn 4.2%；The purity of W, Ni, Mn powder>99.9%, mean diameter<3 μm.
(2) raw material uniformly mixes: load in ball grinder by the above-mentioned material powder for preparing, Vacuum Mixture 8h on vibration type ball mill, it is thus achieved that mixed uniformly material powder.
(3) powder Fast Sintering: after uniform for above-mentioned 60g mixed-powder is loaded Ф 30mm graphite jig, it is placed in discharge plasma sintering system heating intracavity, plasma discharging one step sintering is carried out after evacuation, sintering process conditions is: sintering vacuum is less than 2Pa, sintering pressure 50MPa, 100 DEG C/min of heating rate, sintering temperature 1010 DEG C, temperature retention time 4min.
By method made above, it is thus achieved that the novel W 2.8Ni 4.2Mn alloy of even tissue, its W crystal grain is less than 5 μm, and relative density is more than 98%, and macrohardness is 43HRC, and bending strength is 1193MPa.
Embodiment 3
The fast preparation method of the novel W 2.8Ni 4.2Mn alloy of the present embodiment, comprises the following steps and process conditions:
(1) material composition proportioning: with W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing: W 93.0%, Ni
2.8%, Mn 4.2%；The purity of W, Ni, Mn powder>99.9%, mean diameter<3 μm.
(2) raw material uniformly mixes: load in ball grinder by the above-mentioned material powder for preparing, Vacuum Mixture 8h on vibration type ball mill, it is thus achieved that mixed uniformly material powder.
(3) powder Fast Sintering: after uniform for above-mentioned 60g mixed-powder is loaded Ф 30mm graphite jig, it is placed in discharge plasma sintering system heating intracavity, plasma discharging two-step sintering is carried out after evacuation, sintering process conditions is: the first step: sintering vacuum is less than 2Pa, sintering pressure 40MPa, 100 DEG C/min of heating rate, sintering temperature 920 DEG C, temperature retention time 13min；Second step: sintering vacuum is less than 2Pa, sintering pressure 70MPa, 300 DEG C/min of heating rate, sintering temperature 1000 DEG C, temperature retention time 0min.
By method made above, it is thus achieved that the novel W 2.8Ni 4.2Mn alloy of even tissue, its W crystal grain is less than 4.5 μm, and relative density is more than 99%, and macrohardness is 50HRC, and bending strength is 1307MPa.
Embodiment 4
The fast preparation method of the novel W 4.2Ni 2.8Mn alloy of the present embodiment, comprises the following steps and process conditions:
(1) material composition proportioning: with W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing: W 93.0%, Ni
4.2%, Mn 2.8%；The purity of W, Ni, Mn powder>99.9%, mean diameter<3 μm.
(2) raw material uniformly mixes: load in ball grinder by the above-mentioned material powder for preparing, Vacuum Mixture 10h on stirring ball mill, it is thus achieved that mixed uniformly material powder.
(3) powder Fast Sintering: after uniform for above-mentioned 60g mixed-powder is loaded Ф 30mm graphite jig, it is placed in discharge plasma sintering system heating intracavity, plasma discharging one step sintering is carried out after evacuation, sintering process conditions is: sintering vacuum is less than 2Pa, sintering pressure 60MPa, 150 DEG C/min of heating rate, sintering temperature 1060 DEG C, temperature retention time 4min.
By method made above, it is thus achieved that the novel W 4.2Ni 2.8Mn alloy of even tissue, its W crystal grain is less than 5 μm, and relative density is more than 98%, and macrohardness is 45HRC, and bending strength is 1220MPa.
Embodiment 5
The fast preparation method of the novel W 4.2Ni 2.8Mn alloy of the present embodiment, comprises the following steps and process conditions:
(1) material composition proportioning: with W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing: W 93.0%, Ni
4.2%, Mn 2.8%；The purity of W, Ni, Mn powder>99.9%, mean diameter<3 μm.
(2) raw material uniformly mixes: load in ball grinder by the above-mentioned material powder for preparing, Vacuum Mixture 10h on stirring ball mill, it is thus achieved that mixed uniformly material powder.
(3) powder Fast Sintering: after uniform for above-mentioned 60g mixed-powder is loaded Ф 30mm graphite jig, it is placed in discharge plasma sintering system heating intracavity, plasma discharging two-step sintering is carried out after evacuation, sintering process conditions is: the first step: sintering vacuum is less than 2Pa, sintering pressure 50MPa, 150 DEG C/min of heating rate, sintering temperature 950 DEG C, temperature retention time 16min；Second step: sintering vacuum is less than 2Pa, sintering pressure 80MPa, 250 DEG C/min of heating rate, sintering temperature 1040 DEG C, temperature retention time 0min.
By method made above, it is thus achieved that the novel W 4.2Ni 2.8Mn alloy of even tissue, its W crystal grain is less than 4.5 μm, and relative density is more than 99%, and macrohardness is 54HRC, and bending strength is 1357MPa.
Embodiment 6
The fast preparation method of the novel W 4Ni 1Mn alloy of the present embodiment, comprises the following steps and process conditions:
(1) material composition proportioning: with W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing: W 95.0%, Ni
4.0%, Mn 1.0%；The purity of W, Ni, Mn powder>99.9%, mean diameter<3 μm.
(2) raw material uniformly mixes: load in ball grinder by the above-mentioned material powder for preparing, Vacuum Mixture 12h on planetary ball mill, it is thus achieved that mixed uniformly material powder.
(3) powder Fast Sintering: after uniform for above-mentioned 60g mixed-powder is loaded Ф 30mm graphite jig, it is placed in discharge plasma sintering system heating intracavity, plasma discharging one step sintering is carried out after evacuation, sintering process conditions is: sintering vacuum is less than 3Pa, sintering pressure 70MPa, 200 DEG C/min of heating rate, sintering temperature 1250 DEG C, temperature retention time 3min.
By method made above, it is thus achieved that the novel W 4Ni 1Mn alloy of even tissue, its W crystal grain is less than 7 μm, and relative density is more than 98%, and macrohardness is 42HRC, and bending strength is 1165MPa.
Claims (5)
1. the fast preparation method of a novel W Ni Mn alloy, it is characterised in that comprise the technical steps that:
(1) material composition proportioning: with W, Ni, Mn elemental powders as alloy raw material, and according to following mass percent dispensing: W 91.0 95.0%, Ni 1.0 7.2%, Mn 1.0 7.2%；
(2) raw material uniformly mixes: is loaded in ball grinder by the above-mentioned material powder for preparing, carries out Vacuum Mixture, it is thus achieved that mixed uniformly material powder on high energy ball mill；
(3) powder Fast Sintering: after above-mentioned uniform mixed-powder is loaded graphite jig, is placed in discharge plasma sintering system heating intracavity, carries out discharge plasma sintering after evacuation.
The fast preparation method of a kind of novel W Ni Mn alloy, it is characterised in that described high energy ball mill is planetary ball mill, vibration type ball mill or stirring ball mill.
The fast preparation method of a kind of novel W Ni Mn alloy, it is characterised in that described discharge plasma sintering is a step sintering process or two-step sintering technique.
The fast preparation method of a kind of novel W Ni Mn alloy, it is characterised in that a described step sintering process conditions is as follows:
Sintering vacuum < 3Pa, sintering pressure 30 90MPa, 100 400 DEG C/min of heating rate, sintering temperature 1,000 1250 DEG C, temperature retention time 3 5min.
The fast preparation method of a kind of novel W Ni Mn alloy, it is characterised in that described two-step sintering process conditions are as follows:
The first step: sintering vacuum < 3Pa, sintering pressure 30 90MPa, 50 200 DEG C/min of heating rate, sintering temperature 900 1000 DEG C, temperature retention time 10 20min；
Second step: sintering vacuum < 3Pa, sintering pressure 30 90MPa, 200 400 DEG C/min of heating rate, sintering temperature 1,000 1200 DEG C, temperature retention time 0min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106480347A (en) * | 2016-12-05 | 2017-03-08 | 郑州丽福爱生物技术有限公司 | A kind of high-strength aluminum alloy material and preparation method thereof |
| CN106513683A (en) * | 2016-11-04 | 2017-03-22 | 天津大学 | Method for preparing fine-grain high-density yttrium oxide dispersion strengthening tungsten-base alloy |
| CN107099717A (en) * | 2017-05-16 | 2017-08-29 | 北京科技大学 | The technology of preparing of crystal boundary auto purification tungsten magnesium alloy |
| CN107326241A (en) * | 2017-07-10 | 2017-11-07 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN108515174A (en) * | 2018-04-27 | 2018-09-11 | 合肥工业大学 | A kind of resistance to high temperature oxidation W-Cr-Ti composite material and preparation methods |
| CN114657431A (en) * | 2022-02-18 | 2022-06-24 | 安泰天龙钨钼科技有限公司 | Energetic tungsten alloy material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106513683A (en) * | 2016-11-04 | 2017-03-22 | 天津大学 | Method for preparing fine-grain high-density yttrium oxide dispersion strengthening tungsten-base alloy |
| CN106480347A (en) * | 2016-12-05 | 2017-03-08 | 郑州丽福爱生物技术有限公司 | A kind of high-strength aluminum alloy material and preparation method thereof |
| CN107099717A (en) * | 2017-05-16 | 2017-08-29 | 北京科技大学 | The technology of preparing of crystal boundary auto purification tungsten magnesium alloy |
| CN107099717B (en) * | 2017-05-16 | 2018-11-09 | 北京科技大学 | The technology of preparing of crystal boundary auto purification tungsten magnesium alloy |
| CN107326241A (en) * | 2017-07-10 | 2017-11-07 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN107326241B (en) * | 2017-07-10 | 2019-01-15 | 四川大学 | A method of tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN108515174A (en) * | 2018-04-27 | 2018-09-11 | 合肥工业大学 | A kind of resistance to high temperature oxidation W-Cr-Ti composite material and preparation methods |
| CN114657431A (en) * | 2022-02-18 | 2022-06-24 | 安泰天龙钨钼科技有限公司 | Energetic tungsten alloy material and preparation method thereof |
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