CN101067191A - Pd Ni-Si-P block amorphous alloys and producing method thereof - Google Patents
Pd Ni-Si-P block amorphous alloys and producing method thereof Download PDFInfo
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Abstract
The present invention relates to amorphous metal material technology, and is especially one kind of lumpy amorphous Pd-Ni-Si-P alloy and its preparation process. The lumpy amorphous Pd-Cu-Si alloy has the chemical composition of Pd 40.5 at.%, Ni 40.5 at.%, Si 1-14 at.%, and P 5-18 at.%. Its preparation process includes glass coated purifying, air cooling, water quenching and metal mold forming. The lumpy amorphous Pd-Ni-Si-P alloy has certain plastic deformation capacity and high yield strength, and possesses excellent application foreground in different fields.
Description
Technical field
The invention belongs to the preparing technical field of amorphous metallic material.Be particularly related to the preparation of block amorphous alloy.This material is a kind ofly to have than large-amorphous forming capacity, high strength and the block amorphous alloy material of certain plastic deformation ability is arranged.
Background technology
There is not the such long-range order periodicity of crystalline material in its atomic arrangement of non-crystaline amorphous metal (comprising block amorphous alloy) but is unordered Mi Dui arranges, therefore there are not the defectives such as crystal boundary, dislocation in the crystalline material, do not have anisotropy simultaneously yet and be the isotropy feature, thereby non-crystaline amorphous metal has the mechanics and the functional performance of a lot of excellences.But non-crystaline amorphous metal need obtain under condition of fast cooling, most of alloy materials all need be about in speed of cooling～and 10
6Could obtain amorphous structure under the condition of K/s, therefore most non-crystaline amorphous metals can only be prepared into strip (20-50 μ m is thick), film and fine powder, make the application of amorphous alloy material be subjected to very big restriction.Therefore to have bigger amorphous formation ability, can prepare large-sized amorphous alloys be the target that the researchist pursues always in exploitation.
In nearest more than 10 year, the exploitation size has obtained progress at full speed greater than the research of the block amorphous alloy of 1mm, at a plurality of block amorphous alloys, as ZrTiCuNiBe system, ZrAlCuNi system, FeCoCrMoCBY system, PdNiCuP system, CuZrAlAg system or the like.Size the maximum has reached 72mm in the Pd40Cu30Ni10P20 block amorphous alloy of developing at present.In non-crystaline amorphous metal, the temperature range between amorphous transition temperature (Tg) and the initial crystallization temperature (Tx) is called sub-cooled liquid temperature interval (Δ T=Tx-Tg).This temperature range is big more, and the thermostability of non-crystaline amorphous metal is usually good more, simultaneously, can carry out superplasticity rheology processing in this temperature range, and amorphous alloy material is processed into component or device, and therefore, this temperature range is big more, and then process operation is easy more.Therefore, Δ T value to non-crystaline amorphous metal shape and use significant.Non-crystaline amorphous metal has very high strength, but amount of plastic deformation is usually less, and compress variation is general all less than 1～2%.Therefore it is very great to develop the novel block amorphous alloy or the exploration raising non-crystaline amorphous metal ductile method meaning that have than the large plastometric set ability.This will increase the deformation processing forming ability of this alloy material and the security of application greatly.Because the development of new block amorphous alloy is significant, carries out correlative study and explore necessary.According to document and patent retrieval, so far, Shang Weijian openly reports the block amorphous alloy that has the Pd-Ni-Si-P alloy system.
Summary of the invention
The objective of the invention is to, proposed a kind of Pd-Ni-Si-P block amorphous alloys with higher amorphous formation ability, high strength and certain plastic deformation ability.This non-crystaline amorphous metal is characterised in that: chemical ingredients consists of: Pd:40.5at%; Ni:40.5at%; Si:1-14at%; P:5-18at%.
The preparation method of Pd-Ni-Si-P block amorphous alloys is characterized in that, according to following alloy proportion: Pd:40.5at%; Ni:40.5at%; Si:1-14at%; P:5-18at% carries out following steps:
1) mother alloy melting: adopt vacuum alloy melting method to be smelted into master alloy ingot by high-purity Pd, Ni, Si and P raw material or the alloy material of alloying constituent proportioning;
2) glass is coated medium and be fused into liquid being higher than under the condition of melting temperature;
3) under vacuum condition, glass coated medium and be higher than under the above condition of its fusing point 200 degree and purify more than 2 hours, and molten glass coating medium liquid to reach state pure, that do not have bubble;
4) under vacuum condition alloy pig being added melten glass coats in the medium, temperature is increased to the temperature condition insulation purification down that is higher than more than alloy melting point 200 degree, in purification process, repeatedly alloy melt is cooled off until solidifying, and be warming up to the purification temperature once more, if alloy heats up when melting after solidifying once more, do not produce bubble, then finish purification process;
5) the alloy melt cooling that is in molten state after will purifying obtains the PdNiSiP block amorphous alloy.
The described the 2nd) step coats medium with glass and is fused into liquid under the condition of melting temperature and carries out in crucible at silica tube or alloy melting being higher than.
The described the 5th) described method of cooling of step be be in after purifying the alloy melt of molten state and coating medium on every side together slow cooling to room temperature.
The described the 5th) described method of cooling of step be be in after purifying the alloy melt of molten state and coating medium on every side together shrend to room temperature.
The described the 5th) described method of cooling of step is that the alloy melt that will be in molten state after will purifying solidifies earlier, then the alloy of purifying is melted the back rapid solidification once more or is cast into metal pattern under vacuum condition.
It is that dry glass coats medium that described glass coats medium.
The described the 4th) in the step, when alloy heats up fusing, do not produce bubble, and then purified 1～3 hour, finish purification process.
Evidence, non-crystaline amorphous metal proposed by the invention have higher yield strength, certain plastic deformation ability, have a good application prospect in various fields.
Description of drawings
Fig. 1 is the preparation product figure of embodiment 2.
Embodiment
The chemical ingredients of this alloy system consists of: Pd
40.5Ni
40.5Si
xP
19-xThat is: Pd:40.5at%; Ni:40.5at%; Si:1-14at%; P:5-18at%.This alloy organizing constitutional features is an amorphous structure.
Its preparation technology is: adopt glass to coat medium (as B
2O
3The glass coating) purifying technique purification alloy adopts methods such as air cooling, shrend, die cast to be prepared into the block amorphous alloy material then, and its size can be greater than 5mm.Pd
40.5Ni
40.5Si
xP
19-xThe preparation process of block amorphous alloy is that embodiment is as follows:
1) mother alloy melting: adopt vacuum alloy melting method to be smelted into master alloy ingot by high-purity Pd, Ni, Si and the P raw material (greater than 99.5%) of alloying constituent proportioning.
2) adopting silica tube or alloy melting crucible is the alloy melting container, dry glass is coated medium be fused into liquid being higher than under the condition of melting temperature.
3) under vacuum condition, glass coated medium and be higher than under the above condition of about 200 degree of its fusing point and purify more than 2 hours, and molten glass coating medium liquid to reach state pure, that do not have bubble.
4) under vacuum condition, alloy pig is added melten glass and coat in the medium, then temperature is increased to the temperature condition insulation purification down that is approximately higher than alloy melting point 200 degree.And in purification process, for several times with the alloy melt cooling until solidifying, and then be warming up to the purification temperature, after purifying about 1-10 hour, during fusing, do not produce bubble, the end purification process after solidifying if alloy heats up once more.In order to make refining effect better, after can after not producing bubble, continuing to purify about 1 hour, and then finish purification process.
5) can adopt the PdNiSiP block amorphous alloy of following three kinds of method preparation sizes greater than 5mm:
1〉be in after will purifying the alloy melt of molten state and coating medium on every side together slow cooling to room temperature.
2〉be in after will purifying the alloy melt of molten state and coating medium on every side together shrend to room temperature.
3〉alloy melt that is in molten state after will purifying solidifies earlier, then with the alloy of purifying fusing back rapid solidification or be cast into the metal pattern solidification forming once more under vacuum condition.
Embodiment 1:Pd
40.5Ni
40.5Si
1P
18The block amorphous alloy preparation
(1) alloying constituent: 40.5at%Pd-40.5at%Ni-1.0at%Si-18.0at%P.Adopting silica tube is the alloy melting container, and proportionately mother alloy is prepared in the alloy raw material fusing of assignment system under the argon shield condition.
(2) with anhydrous B
2O
3Coat the medium silica tube of packing into, under 700 degree conditions, be fused into liquid.Under vacuum state, will coat medium then and under about 900 degree conditions, purify more than 2 hours, and make the coating medium reach pure, no bubble state.
(3) under vacuum condition alloy pig is added fusion and coat in the medium, about 1050 degree were purified about 1-2 hour again.In purification process, lower the temperature and solidify about 5 times.
(4) will be in the alloy melt of molten state and coating medium on every side together slow cooling prepare the Pd-Ni-Si-P block amorphous alloy of size to room temperature greater than 5mm;
To be in the alloy melt of molten state and coating medium on every side together shrend to room temperature, but preparation size is greater than the Pd-Ni-Si-P block amorphous alloy of 5mm or the amorphous pole more than the φ 3mm;
Alloy after purifying melted under the vacuum condition once more and be cast into the amorphous pole that obtains in the copper mold more than about φ 4～5mm.The Pd-Ni-Si-P block amorphous alloy of preparation has the small amount of compression plastic deformation ability, can reach about 0.2% compressive plastic deformation amount.The engineering yield strength greater than 1500MPa. supercooled liquid phase temperature range Δ T greater than 100K.
Embodiment 2:Pd
40.5Ni
40.5Si
2.5P
16.5The block amorphous alloy preparation
(1) alloying constituent: 40.5at%Pd-40.5at%Ni-2.5at%Si-16.5at%P.Adopting silica tube is the alloy melting container, and proportionately mother alloy is prepared in the alloy raw material fusing of assignment system under the argon shield condition.
(2) with anhydrous B
2O
3Coat the medium silica tube of packing into, under 800 degree conditions, be fused into liquid.Under vacuum state, will coat medium then and under about 950 degree conditions, purify more than 2 hours, and make the coating medium reach pure, no bubble state.
(3) under vacuum condition alloy pig is added fusion and coat in the medium, about 1050 degree were purified about 1-2 hour again.In purification process, lower the temperature and solidify about 5 times.
(4) will be in the alloy melt of molten state and coating medium on every side together slow cooling prepare the Pd-Ni-Si-P block amorphous alloy of size to room temperature greater than 5mm;
To be in the alloy melt of molten state and coating medium on every side together shrend to room temperature, but preparation size is greater than the Pd-Ni-Si-P block amorphous alloy of 5mm or the amorphous pole more than the φ 3mm.As shown in Figure 1.
Alloy after purifying melted under the vacuum condition once more and be cast into the amorphous pole that obtains in the copper mold more than about φ 4～5mm.
The Pd-Ni-Si-P block amorphous alloy of preparation has the small amount of compression plastic deformation ability, and the best can reach about 0.5% compressive plastic deformation amount.The engineering yield strength is higher than 1600MPa. supercooled liquid phase temperature range Δ T greater than 100K.
Embodiment 3:Pd
40.5Ni
40.5Si
5P
14The block amorphous alloy preparation
(1) alloying constituent: 40.5at%Pd-40.5at%Ni-5at%Si-14at%P.Adopting silica tube is the alloy melting container, and proportionately mother alloy is prepared in the alloy raw material fusing of assignment system under the argon shield condition.
(2) with anhydrous B
2O
3Coat the medium silica tube of packing into, under 900 degree conditions, be fused into liquid.Under vacuum state, will coat medium then and under about 1000 degree conditions, purify more than 2 hours, and make the coating medium reach pure, no bubble state.
(3) under vacuum condition alloy pig is added fusion and coat in the medium, about 1150 degree were purified about 2-4 hour again.Cooling is solidified about 5 times in purification process, and does not have bubble to occur when melting once more.
(4) will be in the alloy melt of molten state and coating medium on every side together slow cooling to room temperature, but preparation size is greater than the Pd-Ni-Si-P block amorphous alloy of 5mm;
To be in the alloy melt of molten state and coating medium on every side together shrend to room temperature, but preparation size is greater than the Pd-Ni-Si-P block amorphous alloy of 5mm or the amorphous pole more than the φ 3mm;
Alloy after purifying melted under the vacuum condition once more and be cast into the amorphous pole that obtains in the copper mold more than about φ 4～5mm.The Pd-Ni-Si-P block amorphous alloy of preparation has the compressive plastic deformation ability, and the best can reach about 23% compressive plastic deformation amount.The engineering yield strength is higher than 1600MPa. supercooled liquid phase temperature range Δ T greater than 110K.
Embodiment 4:Pd
40.5Ni
40.5Si
9.5P
9.5The block amorphous alloy preparation.
(1) alloying constituent: 40.5at%Pd-40.5at%Ni-9.5at%Si-9.5at%P.Adopting silica tube is the alloy melting container, and proportionately mother alloy is prepared in the alloy raw material fusing of assignment system under the argon shield condition.
(2) with anhydrous B
2O
3Coat the medium silica tube of packing into, under 900 degree conditions, be fused into liquid.Under vacuum state, will coat medium then and under about 1000 degree conditions, purify more than 2 hours, and make the coating medium reach pure, no bubble state.
(3) under vacuum condition alloy pig is added fusion and coat in the medium, 1150 degree were purified about 3-6 hour again.Cooling is solidified about 5 times in purification process, and does not have bubble to occur when melting once more.
(4) will be in the alloy melt of molten state and coating medium on every side together slow cooling to room temperature, but preparation size is greater than the Pd-Ni-Si-P block amorphous alloy of 5mm;
To be in the alloy melt of molten state and coating medium on every side together shrend to room temperature, but preparation size is greater than Pd-Ni-Si-P block amorphous alloy or the φ 3mm amorphous pole of 5mm;
Alloy after purifying melted under the vacuum condition once more and be cast into the amorphous pole that obtains about φ 4mm in the copper mold.
The Pd-Ni-Si-P block amorphous alloy of preparation is built has about 5% compression ductility, and yield strength is higher than 1700MPa. supercooled liquid phase temperature range Δ T greater than 70K.
Embodiment 5:Pd
40.5Ni
40.5Si
14P
5Block amorphous alloy.
(1) alloying constituent: 40.5at%Pd-40.5at%Ni-14at%Si-5at%P.Adopting silica tube is the alloy melting container, and proportionately mother alloy is prepared in the alloy raw material fusing of assignment system under the argon shield condition.
(2) with anhydrous B
2O
3Coat the medium silica tube of packing into, under 900 degree conditions, be fused into liquid.Under vacuum condition, will coat medium then and under about 1000 degree conditions, purify more than 2 hours, and make the coating medium reach pure, no bubble state.
(3) under vacuum condition alloy pig is added fusion and coat in the medium, 1100 degree were purified about 6-12 hour again.Cooling is solidified about 5 times in purification process, and does not have bubble to occur when melting once more, then purifies 1 hour, finishes purification process.
(4) will be in the alloy melt of molten state and coating medium on every side together slow cooling to room temperature, but preparation size is greater than the Pd-Ni-Si-P block amorphous alloy of 5mm;
To be in the alloy melt of molten state and coating medium on every side together shrend to room temperature, but preparation size is greater than Pd-Ni-Si-P block amorphous alloy or the φ 3mm amorphous pole of 5mm;
Alloy after purifying melted under the vacuum condition once more and be cast into the amorphous pole that obtains about φ 4mm in the copper mold.
(5) Zhi Bei Pd-Ni-Si-P block amorphous alloy is built and is had about 2.5% compression ductility, and yield strength is higher than 1800MPa. supercooled liquid phase temperature range Δ T greater than 40K.
Claims (8)
1, a kind of Pd-Ni-Si-P block amorphous alloys is characterized in that chemical ingredients consists of: Pd:40.5at%; Ni:40.5at%; Si:1-14at%; P:5-18at%.
2, a kind of preparation method of Pd-Ni-Si-P block amorphous alloys is characterized in that, according to following alloy proportion: Pd:40.5at%; Ni:40.5at%; Si:1-14at%; P:5-18at% carries out following steps:
1) mother alloy melting: adopt vacuum alloy melting method to be smelted into master alloy ingot by high-purity Pd, Ni, Si and P raw material or the alloy material of alloying constituent proportioning;
2) glass is coated medium and be fused into liquid being higher than under the condition of melting temperature;
3) under vacuum condition, glass coated medium and be higher than under the above condition of its fusing point 200 degree and purify more than 2 hours, and molten glass coating medium liquid to reach state pure, that do not have bubble;
4) under vacuum condition alloy pig being added melten glass coats in the medium, temperature is increased to the temperature condition insulation purification down that is higher than more than alloy melting point 200 degree, in purification process, repeatedly alloy melt is cooled off until solidifying, and be warming up to the purification temperature once more, if alloy heats up when melting after solidifying once more, do not produce bubble, then finish purification process;
5) the alloy melt cooling that is in molten state after will purifying obtains the PdNiSiP block amorphous alloy.
3, the preparation method of Pd-Ni-Si-P block amorphous alloys as claimed in claim 2 is characterized in that, the described the 2nd) step coats medium with glass and is fused into liquid under the condition of melting temperature and carries out in crucible at silica tube or alloy melting being higher than.
4, the preparation method of Pd-Ni-Si-P block amorphous alloys as claimed in claim 2 is characterized in that, the described the 5th) described method of cooling of step be be in after purifying the alloy melt of molten state and coating medium on every side together slow cooling to room temperature.
5, the preparation method of Pd-Ni-Si-P block amorphous alloys as claimed in claim 2 is characterized in that, the described the 5th) described method of cooling of step be be in after purifying the alloy melt of molten state and coating medium on every side together shrend to room temperature.
6, the preparation method of Pd-Ni-Si-P block amorphous alloys as claimed in claim 2, it is characterized in that, the described the 5th) described method of cooling of step is that the alloy melt that will be in molten state after will purifying solidifies earlier, then the alloy of purifying is melted the back rapid solidification once more or is cast into metal pattern under vacuum condition.
7, the preparation method of Pd-Ni-Si-P block amorphous alloys as claimed in claim 2 is characterized in that, it is that dry glass coats medium that described glass coats medium.
8, the preparation method of Pd-Ni-Si-P block amorphous alloys as claimed in claim 2 is characterized in that, the described the 4th) in the step, when alloy heats up fusing, do not produce bubble, and then purified 1～3 hour, finish purification process.
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|---|---|---|---|
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| CN100507064C CN100507064C (en) | 2009-07-01 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320723A (en) * | 2013-05-28 | 2013-09-25 | 江苏迈盛新材料有限公司 | Repeated fusion-solidification treating method for raising alloy amorphous forming ability |
| CN105970125A (en) * | 2016-02-23 | 2016-09-28 | 合肥工业大学 | Molding method for improving room-temperature plasticity of metal glass component |
| CN106584012A (en) * | 2016-12-30 | 2017-04-26 | 常州世竟液态金属有限公司 | Shaping method for amorphous alloy |
| CN106609346A (en) * | 2016-03-15 | 2017-05-03 | 北京纳米能源与系统研究所 | Amorphous alloy and preparation method and application thereof |
| CN109680224A (en) * | 2019-01-16 | 2019-04-26 | 南京理工大学 | A kind of preparation method of nano porous palladium base noncrystal alloy |
-
2007
- 2007-06-15 CN CNB200710118935XA patent/CN100507064C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320723A (en) * | 2013-05-28 | 2013-09-25 | 江苏迈盛新材料有限公司 | Repeated fusion-solidification treating method for raising alloy amorphous forming ability |
| CN105970125A (en) * | 2016-02-23 | 2016-09-28 | 合肥工业大学 | Molding method for improving room-temperature plasticity of metal glass component |
| CN106609346A (en) * | 2016-03-15 | 2017-05-03 | 北京纳米能源与系统研究所 | Amorphous alloy and preparation method and application thereof |
| CN106584012A (en) * | 2016-12-30 | 2017-04-26 | 常州世竟液态金属有限公司 | Shaping method for amorphous alloy |
| CN106584012B (en) * | 2016-12-30 | 2019-07-12 | 常州世竟液态金属有限公司 | A kind of amorphous alloy shaping methods |
| CN109680224A (en) * | 2019-01-16 | 2019-04-26 | 南京理工大学 | A kind of preparation method of nano porous palladium base noncrystal alloy |
| CN109680224B (en) * | 2019-01-16 | 2021-05-04 | 南京理工大学 | Preparation method of nano porous palladium-based amorphous alloy |
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