CN107630150B - A kind of preparation method of the enhanced CuNiSi alloy of timeliness - Google Patents
A kind of preparation method of the enhanced CuNiSi alloy of timeliness Download PDFInfo
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- CN107630150B CN107630150B CN201710797709.2A CN201710797709A CN107630150B CN 107630150 B CN107630150 B CN 107630150B CN 201710797709 A CN201710797709 A CN 201710797709A CN 107630150 B CN107630150 B CN 107630150B
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Abstract
The invention discloses a kind of preparation methods of the enhanced CuNiSi alloy of timeliness; nitrogen is used to carry out vacuum induction melting alloy as protection gas point; then powder by atomization is carried out using confined type nozzle, the alloy powder of certain partial size carries out the processing of atmosphere protection hot pressed sintering after selection atomization and low temperature aging handles to obtain CuNiSi alloy.The CuNiSi material preparation method of the invention small advantage of tiny, even tissue, gross segregation with crystal grain compared with conventional casting methods, more alloying elements are uniformly distributed in matrix by way of rapid cooling, the size obtained by subsequent hot pressed sintering and ageing treatment is small, nanometer precipitated phase more than quantity, the netted precipitation phase amount of crystal boundary is reduced, effectively improve the electric conductivity of alloy, it can be used for aerospace high-performance conductive elastic element, such as lead frame and power spring gasket etc..
Description
Technical field
The invention belongs to metal-base composites technical field, it is related to a kind of enhanced CuNiSi alloy of timeliness and its preparation
Method.
Background technique
Corson alloy belongs to precipitation strength type alloy, is widely used as blaster fuse frame material.With IC chip to
High concentration, high-density packages direction are developed, and to blaster fuse frame material, more stringent requirements are proposed.Tradition preparation cupro-nickel silicon closes
The method of gold is casting, and detailed process includes the processes such as melting-solid gas coupling-cold deformation-secondary ageing, and process is complicated, and
The gross segregation of fusion process alloying element is serious, coarse grains, since the solid solution of alloying element is so that alloy conductive rate declines
Seriously.Though preparing the method for CuNiSi alloy at present and performance study achieving many progress, mainly pass through deformation process
Crystal grain is refined, alloy entirety plasticity and toughness are poor.
Summary of the invention
The purpose of the present invention is to provide the preparation methods that a kind of Precipitation strengthens Type C uNiSi alloy, solve alloy
The problem that crystallite dimension is big, component segregation is serious guarantees that alloy has uniform tissue, has preferable plasticity and toughness and conduction
Property.
To achieve the above object, the used following technical scheme of the present invention:
A kind of preparation method of the enhanced CuNiSi alloy of timeliness, includes the following steps:
Step 1, material prepare, and weigh copper billet, nickel block and the silicon grain of certain mass ratio and carry out surface preparation；
Ready copper billet, nickel block and silicon grain are placed in graphite crucible, in nitrogen protection atmosphere by step 2, alloy melting
Lower progress Medium frequency induction melting；
Atomization gas pressure is adjusted to certain value, determines nozzle diameter by step 3, powder by atomization, is then carried out aerosolization and is blown
Powder, blow-on takes powder after cooling 10-15min after the completion of atomization, and the alloy powder to guarantee preparation is not oxidized；
The screening that alloy powder after atomization carries out different-grain diameter is weighed, chooses certain partial size by step 4, hot pressed sintering
Alloy powder carry out subsequent hot pressing sintering processes；
Obtained sintered specimen is carried out atmosphere protection ageing treatment by step 5, ageing treatment in tube furnace, is obtained thin
The CuNiSi alloy of crystal grain.
As this case invention further embodiment, step 1 surface preparation be copper billet, nickel block and silicon grain are placed on it is super
9-10min is cleaned in sound wave cleaning machine.
As this case invention further embodiment, the mass ratio of Cu:Ni:Si is (94 in step 1 material preparation phase
~96): (3.3~5.0): (0.7~1.0), the scaling loss amount of nickel are 2-4%, and the scaling loss amount of silicon is 6-8%.
As this case invention further embodiment, is vacuumized in step 2 using three-level vacuum system, reached to vacuum degree
To 5-9 × 10-3It is filled with nitrogen after Pa to 0.02-0.1MPa, is heated using vacuum induction furnace, heating power supply is intermediate frequency sense
Power supply is answered, the rate of heat addition is about 1-2 DEG C/s, and the fusing degree of superheat is 150-200 DEG C, keeps the temperature 5-8min at such a temperature.
As this case invention further embodiment, pulverizing process uses confined type nozzle aerosolization, atomizing pressure in step 3
For 4-6MPa, atomizer diameter is 3-5mm, and atomization gas is nitrogen, and atomization process is about 8-15s.
As this case invention further embodiment, different-grain diameter is carried out to alloy powder before hot pressed sintering in the step 4
Screening process obtains being less than 150um alloy powder receipts powder rate in 30-50%, and 50-75um alloy powder specific gravity is maximum；Use nitrogen
Gas is sintered as protection gas point, and sintering temperature is 880-930 DEG C, sintering pressure 28-30MPa, sintering time 60-
70min。
As this case invention further embodiment, step 5 ageing treatment carries out in tube furnace, use argon gas as
Protective atmosphere, aging time 3.5-4.4h, aging temp are 440-460 DEG C.
The beneficial effects of the present invention are: CuNiSi alloy of the invention has crystalline substance compared to the alloy that routine casting method obtains
Grain is tiny, and crystal boundary is netted to be precipitated the few feature of phase amount, and the electrical and thermal conductivity of alloy is better than the alloy of casting preparation；By fast
Rapid hardening prepares CuNiSi alloy admittedly, can guarantee that enough alloying elements are dissolved into Copper substrate, reduce the inclined of alloying element
Analysis, obtained alloy grain is tiny, and even tissue, precipitated phase is evenly distributed；It can be used for the high property electrically conductive elastic device of aerospace,
Such as lead frame and power spring gasket etc..
Detailed description of the invention
Fig. 1 is the process flow chart that the present invention prepares alloy；
Fig. 2 is that the present invention prepares alloy powder interior tissue pattern；
Fig. 3 is the final aging state micro-organization chart of the embodiment of the present invention.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
As shown in Figure 1, a kind of preparation method of the enhanced CuNiSi alloy of timeliness, includes the following steps:
Step 1, material prepare, and weigh copper billet, nickel block and the silicon grain of certain mass ratio and carry out surface preparation；
Ready copper billet, nickel block and silicon grain are placed in graphite crucible, in nitrogen protection atmosphere by step 2, alloy melting
Lower progress Medium frequency induction melting；
Atomization gas pressure is adjusted to certain value, determines nozzle diameter by step 3, powder by atomization, is then carried out aerosolization and is blown
Powder, blow-on takes powder after cooling 10-15min after the completion of atomization, and the alloy powder to guarantee preparation is not oxidized；
Alloy powder after atomization is carried out different-grain diameter screening weighing, chooses certain partial size by step 4, hot pressed sintering
Alloy powder carry out subsequent hot pressing sintering processes；
Obtained sintered specimen is carried out atmosphere protection ageing treatment by step 5, ageing treatment in tube furnace, is obtained thin
The CuNiSi alloy of crystal grain.
Embodiment 1
Make the material for weighing certain mass score in the balance, nickel block 4wt%, silicon grain 1wt%, surplus is copper.It will be with graphite
The crucible of paper is put into vacuum chamber, and using confined type nozzle, atomizer diameter is 4mm, and vacuum degree has reached 7 × 10-3Pa, nitrogen
Then protective atmosphere+0.05MPa carries out induction melting, heating rate is 2 DEG C/s, and smelting temperature is 1500 DEG C, keeps the temperature 5min,
Atomizing pressure is adjusted to 6MPa, and molten metal is atomized into many tiny drops, molten metal flight course under the action of nitrogen stream
It neutralizes atomization gas and carries out heat exchange, solidified before reaching side wall and form spherical powder, this atomized alloy powder is received
Rate is 50%, carries out different-grain diameter screening process to alloy powder obtained, partial size is selected to be less than the alloy powder 30g of 75um,
Alloy powder is poured into progress hot pressed sintering processing in 21 graphite jig of Φ, sintering temperature is 910 DEG C, pressure 30MPa, is protected
The pressure time be 1h, after the sample after hot pressing is surface-treated to sample carry out 450 DEG C of ageing treatments, aging time 4h,
Obtained alloy sample consistency is 98.16%, and conductivity 32.76%IACS, hardness 107HBS, crystallite dimension is in 10-
Between 20um, precipitated phase disperse is uniformly distributed.
Fig. 2 is alloyed spherical powder interior tissue pattern made from the present embodiment, and spherical powder size is about 80um or so,
Crystallite dimension is in 5-10um or so in powder.
Fig. 3 is that the SEM for the CuNiSi material that the present embodiment is prepared using aerosol alloy powder schemes, and crystallite dimension is tiny,
There are tiny precipitation strength is strong, the netted precipitation phase amount of crystal boundary significantly reduces intra-die.
Embodiment 2
Make the material for weighing certain mass score in the balance, nickel block 4.17wt%, silicon grain 0.83wt%, surplus is copper.It will
Graphite crucible with graphite paper is put into vacuum melting room, and atomizer diameter selects 3.5mm, and vacuum degree has reached 7 × 10-3Pa,
Then nitrogen protection atmosphere+0.1MPa carries out induction melting, atomizing pressure 5MPa, smelting temperature is 1450 DEG C, heat preservation
6min, molten metal are atomized into many tiny drops under the action of nitrogen stream, in molten metal flight course and atomization gas into
The exchange of row heat solidifies before reaching side wall and forms spherical powder, this atomization is less than 150um alloy powder recovery rate and is
43%, different-grain diameter screening is carried out to the alloy powder of preparation, alloy powder 29g machine of the partial size less than 74um is selected to carry out hot pressing
Alloy powder is poured into 21 graphite jig of Φ by sintering processes, and sintering temperature is 900 DEG C, pressure 31MPa, the dwell time
For 65min, 440 DEG C, 4.2h ageing treatment then are carried out to alloy sample, obtained alloy sample consistency is 98.54%, is led
Electric rate is 30.17%IACS, hardness 114HB.
Embodiment 3
Make the material for weighing certain mass score in the balance, nickel block 4.28wt% (scaling loss amount 4%), silicon grain 0.72wt%
(scaling loss amount 8%), material gross mass 746.4g.Crucible with graphite paper is put into vacuum melting room, atomizer selects diameter
For 4.5mm, atomizing pressure selects 4MPa, and for nitrogen as protective atmosphere, the amount for being filled with nitrogen is+0.07MPa, is carried out after charging true
Empty induction melting, smelting temperature are 1450 DEG C, carry out powder by atomization after keeping the temperature 7min, molten metal is impacted by nitrogen stream at many thin
Small drop then passes through heat exchange solidification forming in flight course, this atomization obtains being less than 150um alloyed powder recovery rate
It is 38.26%, different-grain diameter screening process is carried out to the alloy powder of preparation, weighs the alloy powder 28g that partial size is less than 75um
Left and right, alloy powder is poured into 21 graphite jig of Φ, and sintering temperature is 1000 DEG C, pressure 28MPa, and the dwell time is
1h, then carries out 460 DEG C of ageing treatment aging temp, time 3.9h to alloy sample again, and obtained alloy sample consistency is
98.2%, conductivity 30.69%IACS, hardness 104HB.
The above is present pre-ferred embodiments, for the ordinary skill in the art, according to the present invention
Introduction, in the case where not departing from the principle of the present invention and spirit, changes, modifications, replacement and change that embodiment is carried out
Shape is still fallen within protection scope of the present invention.
Claims (3)
1. a kind of preparation method of the enhanced CuNiSi alloy of timeliness, which comprises the steps of:
Step 1, material prepare, and weigh copper billet, nickel block and the silicon grain of certain mass ratio and carry out surface preparation；
Ready copper billet, nickel block and silicon grain are placed in graphite crucible by the melting of step 2, alloy, under nitrogen protection atmosphere
Carry out Medium frequency induction melting；
Atomization gas pressure is adjusted to certain value, determines nozzle diameter by step 3, powder by atomization, is then carried out aerosolization and is blown powder,
Blow-on takes powder after cooling 10-15min after the completion of atomization, and the alloy powder to guarantee preparation is not oxidized；
The screening that alloy powder after atomization carries out different-grain diameter is weighed, chooses certain partial size by step 4, hot pressed sintering
Alloy powder carries out subsequent hot pressing sintering processes；
Obtained sintered specimen is carried out in tube furnace atmosphere protection ageing treatment, obtains fine grain by step 5, ageing treatment
CuNiSi alloy；
The mass ratio of Cu:Ni:Si is (94~96): (3.3~5.0): (0.7~1.0) in step 1 material preparation phase,
The scaling loss amount of nickel is 2-4%, and the scaling loss amount of silicon is 6-8%；
It is vacuumized in step 2 using three-level vacuum system, reaches 5 × 10 to vacuum degree-3-9×10-3Nitrogen is filled with after Pa extremely
0.02-0.1MPa is heated using vacuum induction furnace, and heating power supply is medium frequency induction power supply, and the rate of heat addition is about 1-2
DEG C/s, the fusing degree of superheat is 150-200 DEG C, keeps the temperature 5-8min at such a temperature；
Pulverizing process uses confined type nozzle aerosolization, atomizing pressure 4-6MPa in step 3, and atomizer diameter is 3-5mm,
Atomization gas is nitrogen, and atomization process is about 8-15s.
Different-grain diameter screening process is carried out to alloy powder before hot pressed sintering in the step 4, obtains being less than 150um alloy powder
Powder rate is received in 30-50%, 50-75um alloy powder specific gravity is maximum；Nitrogen is used to be sintered as protection gas point, sintering temperature
It is 880-930 DEG C, sintering pressure 28-30MPa, sintering time 60-70min.
2. the preparation method of the enhanced CuNiSi alloy of timeliness as described in claim 1, which is characterized in that step 1 table
Face pretreatment is that copper billet, nickel block and silicon grain are placed in supersonic wave cleaning machine to clean 9-10min.
3. the preparation method of the enhanced CuNiSi alloy of timeliness as described in claim 1, which is characterized in that when the step 5
Effect processing carries out in tube furnace, uses argon gas as protective atmosphere, aging time 3.5-4.4h, aging temp 440-
460℃。
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| CN111151764A (en) * | 2019-12-25 | 2020-05-15 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuNiSi spherical powder based on VIGA process |
| CN111074092B (en) * | 2019-12-26 | 2021-08-17 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-nickel-silicon alloy material and preparation method thereof |
| CN116005020B (en) * | 2022-12-26 | 2024-03-26 | 陕西斯瑞新材料股份有限公司 | Preparation method of CuTe contact material for high-voltage direct-current contactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2014173167A (en) * | 2013-03-12 | 2014-09-22 | Jx Nippon Mining & Metals Corp | Cu-Ni-Si BASED COPPER ALLOY |
| TW201706419A (en) * | 2015-08-10 | 2017-02-16 | 中國鋼鐵股份有限公司 | Copper-nickel-silicon-chromium quench substrate and method of producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014173167A (en) * | 2013-03-12 | 2014-09-22 | Jx Nippon Mining & Metals Corp | Cu-Ni-Si BASED COPPER ALLOY |
| TW201706419A (en) * | 2015-08-10 | 2017-02-16 | 中國鋼鐵股份有限公司 | Copper-nickel-silicon-chromium quench substrate and method of producing the same |
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Effective date of registration: 20200521 Address after: 315194 lihuaqiao village, Shounan street, Yinzhou District, Ningbo City, Zhejiang Province (Xinxing Industrial Development Park) Patentee after: NINGBO DEZHOU PRECISION ELECTRONIC Co.,Ltd. Address before: 710048 Shaanxi city of Xi'an Province Jinhua Road No. 5 Patentee before: XI'AN UNIVERSITY OF TECHNOLOGY |
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