CN105986159B - A kind of fast preparation method of W-Ni-Mn alloys - Google Patents
A kind of fast preparation method of W-Ni-Mn alloys Download PDFInfo
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- CN105986159B CN105986159B CN201510094172.4A CN201510094172A CN105986159B CN 105986159 B CN105986159 B CN 105986159B CN 201510094172 A CN201510094172 A CN 201510094172A CN 105986159 B CN105986159 B CN 105986159B
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Abstract
The invention belongs to novel tungsten alloy and its preparing technical field, it is proposed that a kind of quick method of the preparation with the new W-Ni-Mn alloys of excellent comprehensive performance, specifically include：First by W, Ni, Mn elemental powders W 91.0-95.0% by mass percentage, Ni 1.0-7.2%, the dispensings of Mn 1.0-7.2%, then Vacuum Mixture to raw material is well mixed on high energy ball mill, and the rapid shaping and a step or two-step sintering of powder are finally carried out on discharging plasma sintering equipment.New W-Ni-Mn alloy structures prepared by the present invention are uniformly, W crystal grain is tiny, relative density is high, and the comprehensive mechanical property of alloy is preferable.The present invention has the advantages that shaping and sintering integratedization, sintering temperature is relatively low, sintering time is shorter, is readily available thin W crystal grain W-Ni-Mn alloys, and can reduce the preparation cost of material to a certain extent.
Description
Technical field
The invention belongs to novel tungsten alloy preparing technical field, is on the fast of new W-Ni-Mn alloys more specifically
Fast preparation method.
Background technology
Tungsten alloy has a series of excellent performances, such as density is high, intensity is high, machining property is good, thermal coefficient of expansion is small,
Electrical and thermal conductivity is good etc., and these excellent properties make it obtain widely should in defence and military, Aero-Space and civilian industry
With.Relative to traditional tungsten alloy, new W-Ni-Mn alloys have more preferable Adiabatic Shear performance, can cause Adiabatic Shear Bands
Increase, thus be readily applicable to armor-piercing bullet material.As bullet in use, because penetrating depth without reducing it with self-sharpening
Degree, therefore it can mutually be competed with depleted uranium bullet.
It is main at present still to utilize material powder ball milling, shaping, the conventional powders sintered for new W-Ni-Mn alloys
It is prepared by metallurgical lqiuid phase sintering method.The method has open defect：Firstly, since Mn high chemism, easily in alloy in sintering process
MnO is generated on boundary, at utmost to reduce MnO, actual liquid phase sintering conditions are often than Binder Phase liquidus curve minimum temperature
It is high, easily cause tungsten grain to be grown up, this is unfavorable for preparing high performance alloys；It is secondly as outer without applying in sintering process
Portion's pressure, gas caused by conventional liquid phase sintering hydrogen reducing MnO can not exclude completely from sample, thus add alloy
Porosity, alloy density is caused to reduce；Finally, conventional liquid phase sintering process shaping is carried out in two steps with sintering, and technological process is longer,
Heating rate is slower in sintering process, and the sintered specimen time is longer, and this can all increase the probability of material powder oxidation.
At present, to meet the increasing demand to high-performance novel W-Ni-Mn alloys, using new method, new technology,
The defects of overcoming Traditional liquid phase sintering process, the oxide of the residual porosity easily occurred in alloy and manganese is reduced, refine tungsten grain
Size, and then improve the consistency of alloy, the final mechanical property for improving alloy is an important topic.As a kind of material
New preparation technology, compared with conventional liquid phase sintering process, discharge plasma sintering have heating rate is fast, sintering temperature is low, burn
Tie that the time is short and many advantages such as hot pressed sintering, the Worth Expecting in terms of the preparation of new W-Ni-Mn alloys.Therefore, in correlation
On Research foundation, the present invention matches from optimization material composition, adjustment preprocessing method of raw materials, innovation discharge plasma sintering process
Set out Deng measure, it is proposed that a kind of quick method of the preparation with excellent comprehensive performance W-Ni-Mn alloys.
The content of the invention
Instant invention overcomes technological process is longer, sintering temperature is higher, protects existing for conventional liquid phase sintering W-Ni-Mn alloys
A kind of technical disadvantages such as the warm time is longer, there is provided simple and quick obtained high fine and close and premium properties W-Ni-Mn alloys method.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions：
A kind of fast preparation method of new W-Ni-Mn alloys, it is characterised in that comprise the technical steps that：
（1）Material composition matches：Using 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：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is carried out on high energy ball mill
Batch mixing, obtain mixed uniformly material powder；
（3）Powder Fast Sintering：After above-mentioned uniformly mixed-powder loading graphite jig, discharge plasma sintering system is placed in
In heating chamber of uniting, discharge plasma sintering is carried out after vacuumizing.
The high energy ball mill is planetary ball mill, oscillatory type ball mill or stirring ball mill.
The discharge plasma sintering is a step sintering process or two-step sintering technique.
The one step sintering process conditions are as follows：
Sinter vacuum<The 3Pa ,-90MPa of sintering pressure 30,100-400 DEG C/min of heating rate, sintering temperature 1000-
1250 DEG C ,-the 5min of soaking time 3.
The two-step sintering process conditions are as follows：
The first step：Sinter vacuum<The 3Pa ,-90MPa of sintering pressure 30,50-200 DEG C/min of heating rate, sintering temperature
900-1000 DEG C ,-the 20min of soaking time 10；
Second step：Sinter vacuum<The 3Pa ,-90MPa of sintering pressure 30,200-400 DEG C/min of heating rate, sintering temperature
1000-1200 DEG C, soaking time 0min.
Compared with prior art, the present invention has advantage following prominent and beneficial effect：
1. the present invention make use of high energy ball mill in the batch mixing of W, Ni, Mn raw material, with common V-type batch mixer or roller
Formula ball mill is compared, and can improve batch mixing efficiency and uniformity coefficient；Compared with ball adding carries out high-energy ball milling, the introducing of impurity can be avoided
With the rising of powder oxygen content.
2. the present invention further utilizes plasma discharging " two-step sintering " on the basis of the step of plasma discharging one sintering
Method, W/W Connected degrees are reduced as far as possible while W grain growths are controlled, can obtain comprehensive mechanical property preferably new W-Ni-
Mn alloys.
3. the present invention takes full advantage of the technical characterstic of discharge plasma sintering, there is shaping and sintering integratedization, sintering
The advantages that temperature is relatively low, sintering time is shorter, thus thin W crystal grain W-Ni-Mn alloys are readily available, and can drop to a certain extent
The preparation cost of low material.
The spies such as 4. new W-Ni-Mn alloys prepared by the present invention have even tissue, W crystal grain is tiny, relative density is high
Point, thus sintered compared to conventional liquid phase, the comprehensive mechanical property of W-Ni-Mn alloys is more preferable.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
The fast preparation method of the new W -1.8Ni -7.2Mn alloys of the present embodiment, comprises the following steps and process conditions：
（1）Material composition matches：Using W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing：W
91.0%, Ni 1.8%, Mn 7.2%；W, the purity of Ni, Mn powder>99.9%, average grain diameter<3μm.
（2）Raw material uniformly mixes：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is mixed on planetary ball mill
Expect 12h, obtain mixed uniformly material powder.
（3）Powder Fast Sintering：After the uniform mixed-powders of above-mentioned 60g are loaded into Ф 30mm graphite jigs, electric discharge etc. is placed in
The step of plasma discharging one sintering is carried out in ion sintering system heating chamber, after vacuumizing, sintering process conditions are：Sinter vacuum
Less than 1Pa, sintering pressure 80MPa, 350 DEG C/min of heating rate, 1110 DEG C of sintering temperature, soaking time 3min.
By method made above, the new W -1.8Ni -7.2Mn alloys of even tissue are obtained, its W crystal grain is less than 6 μm,
Relative density is more than 97%, macrohardness 38HRC, bending strength 1124MPa.
Embodiment 2
The fast preparation method of the new W -2.8Ni -4.2Mn alloys of the present embodiment, comprises the following steps and process conditions：
（1）Material composition matches：Using W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing：W
93.0%, Ni 2.8%, Mn 4.2%；W, the purity of Ni, Mn powder>99.9%, average grain diameter<3μm.
（2）Raw material uniformly mixes：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is mixed on oscillatory type ball mill
Expect 8h, obtain mixed uniformly material powder.
（3）Powder Fast Sintering：After the uniform mixed-powders of above-mentioned 60g are loaded into Ф 30mm graphite jigs, electric discharge etc. is placed in
The step of plasma discharging one sintering is carried out in ion sintering system heating chamber, after vacuumizing, sintering process conditions are：Sinter vacuum
Less than 2Pa, sintering pressure 50MPa, 100 DEG C/min of heating rate, 1010 DEG C of sintering temperature, soaking time 4min.
By method made above, the new W -2.8Ni -4.2Mn alloys of even tissue are obtained, its W crystal grain is less than 5 μm,
Relative density is more than 98%, macrohardness 43HRC, bending strength 1193MPa.
Embodiment 3
The fast preparation method of the new W -2.8Ni -4.2Mn alloys of the present embodiment, comprises the following steps and process conditions：
（1）Material composition matches：Using W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing：W
93.0%, Ni 2.8%, Mn 4.2%；W, the purity of Ni, Mn powder>99.9%, average grain diameter<3μm.
（2）Raw material uniformly mixes：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is mixed on oscillatory type ball mill
Expect 8h, obtain mixed uniformly material powder.
（3）Powder Fast Sintering：After the uniform mixed-powders of above-mentioned 60g are loaded into Ф 30mm graphite jigs, electric discharge etc. is placed in
In ion sintering system heating chamber, plasma discharging two-step sintering is carried out after vacuumizing, sintering process conditions are：The first step：Burn
Knot vacuum is less than 2Pa, sintering pressure 40MPa, 100 DEG C/min of heating rate, 920 DEG C of sintering temperature, soaking time 13min；
Second step：Sintering vacuum is less than 2Pa, sintering pressure 70MPa, 300 DEG C/min of heating rate, 1000 DEG C of sintering temperature, insulation
Time 0min.
By method made above, the new W -2.8Ni -4.2Mn alloys of even tissue are obtained, its W crystal grain is less than 4.5 μ
M, relative density are more than 99%, macrohardness 50HRC, bending strength 1307MPa.
Embodiment 4
The fast preparation method of the new W -4.2Ni -2.8Mn alloys of the present embodiment, comprises the following steps and process conditions：
（1）Material composition matches：Using W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing：W
93.0%, Ni 4.2%, Mn 2.8%；W, the purity of Ni, Mn powder>99.9%, average grain diameter<3μm.
（2）Raw material uniformly mixes：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is mixed on stirring ball mill
Expect 10h, obtain mixed uniformly material powder.
（3）Powder Fast Sintering：After the uniform mixed-powders of above-mentioned 60g are loaded into Ф 30mm graphite jigs, electric discharge etc. is placed in
The step of plasma discharging one sintering is carried out in ion sintering system heating chamber, after vacuumizing, sintering process conditions are：Sinter vacuum
Less than 2Pa, sintering pressure 60MPa, 150 DEG C/min of heating rate, 1060 DEG C of sintering temperature, soaking time 4min.
By method made above, the new W -4.2Ni -2.8Mn alloys of even tissue are obtained, its W crystal grain is less than 5 μm,
Relative density is more than 98%, macrohardness 45HRC, bending strength 1220MPa.
Embodiment 5
The fast preparation method of the new W -4.2Ni -2.8Mn alloys of the present embodiment, comprises the following steps and process conditions：
（1）Material composition matches：Using W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing：W
93.0%, Ni 4.2%, Mn 2.8%；W, the purity of Ni, Mn powder>99.9%, average grain diameter<3μm.
（2）Raw material uniformly mixes：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is mixed on stirring ball mill
Expect 10h, obtain mixed uniformly material powder.
（3）Powder Fast Sintering：After the uniform mixed-powders of above-mentioned 60g are loaded into Ф 30mm graphite jigs, electric discharge etc. is placed in
In ion sintering system heating chamber, plasma discharging two-step sintering is carried out after vacuumizing, sintering process conditions are：The first step：Burn
Knot vacuum is less than 2Pa, sintering pressure 50MPa, 150 DEG C/min of heating rate, 950 DEG C of sintering temperature, soaking time 16min；
Second step：Sintering vacuum is less than 2Pa, sintering pressure 80MPa, 250 DEG C/min of heating rate, 1040 DEG C of sintering temperature, insulation
Time 0min.
By method made above, the new W -4.2Ni -2.8Mn alloys of even tissue are obtained, its W crystal grain is less than 4.5 μ
M, relative density are more than 99%, macrohardness 54HRC, bending strength 1357MPa.
Embodiment 6
The fast preparation method of the new W -4Ni -1Mn alloys of the present embodiment, comprises the following steps and process conditions：
（1）Material composition matches：Using W, Ni, Mn powder as alloy raw material, and according to following mass percent dispensing：W
95.0%, Ni 4.0%, Mn 1.0%；W, the purity of Ni, Mn powder>99.9%, average grain diameter<3μm.
（2）Raw material uniformly mixes：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is mixed on planetary ball mill
Expect 12h, obtain mixed uniformly material powder.
（3）Powder Fast Sintering：After the uniform mixed-powders of above-mentioned 60g are loaded into Ф 30mm graphite jigs, electric discharge etc. is placed in
The step of plasma discharging one sintering is carried out in ion sintering system heating chamber, after vacuumizing, sintering process conditions are：Sinter vacuum
Less than 3Pa, sintering pressure 70MPa, 200 DEG C/min of heating rate, 1250 DEG C of sintering temperature, soaking time 3min.
By method made above, the new W -4Ni -1Mn alloys of even tissue are obtained, its W crystal grain is less than 7 μm, relatively
Density is more than 98%, macrohardness 42HRC, bending strength 1165MPa.
Claims (2)
1. a kind of fast preparation method of W-Ni-Mn alloys, it is characterised in that comprise the technical steps that：
(1) material composition matches：Using 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：The above-mentioned material powder for preparing is fitted into ball grinder, vacuum is carried out on high energy ball mill and is mixed
Material, obtains mixed uniformly material powder；
(3) powder Fast Sintering：After above-mentioned uniformly mixed-powder loading graphite jig, it is placed in discharge plasma sintering system and adds
Hot intracavitary, discharge plasma sintering is carried out after vacuumizing；
The discharge plasma sintering is a step sintering process or two-step sintering technique；
The one step sintering process conditions are as follows：
Sinter vacuum<The 3Pa ,-90MPa of sintering pressure 30,100-400 DEG C/min of heating rate, sintering temperature 1000-1250
DEG C ,-the 5min of soaking time 3；
The two-step sintering process conditions are as follows：
The first step：Sinter vacuum<The 3Pa ,-90MPa of sintering pressure 30,50-200 DEG C/min of heating rate, sintering temperature 900-
1000 DEG C ,-the 20min of soaking time 10；
Second step：Sinter vacuum<The 3Pa ,-90MPa of sintering pressure 30,200-400 DEG C/min of heating rate, sintering temperature
1000-1200 DEG C, soaking time 0min.
A kind of 2. fast preparation method of W-Ni-Mn alloys according to claim 1, it is characterised in that the high-energy ball milling
Machine is planetary ball mill, oscillatory type ball mill or stirring ball mill.
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| 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 |
| 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 |
| 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 |
| CN108515174B (en) * | 2018-04-27 | 2019-12-27 | 合肥工业大学 | High-temperature oxidation resistant W-Cr-Ti composite material |
| CN114657431B (en) * | 2022-02-18 | 2023-01-17 | 安泰天龙钨钼科技有限公司 | Energetic tungsten alloy material and preparation method thereof |
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| 烧结工艺对90W-Ni-Mn合金微观结构和力学性能的影响;陈炳煌等;《粉末冶金材料科学与工程》;20141031;第19卷(第5期);第744页1.1-1.2节 * |
| 高密度钨合金烧结新工艺研究现状;孙文等;《稀有金属与硬质合金》;20140430;第42卷(第2期);第37页第2节 * |
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