CN107630150A - A kind of preparation method of the enhanced CuNiSi alloys of timeliness - Google Patents
A kind of preparation method of the enhanced CuNiSi alloys of timeliness Download PDFInfo
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- CN107630150A CN107630150A CN201710797709.2A CN201710797709A CN107630150A CN 107630150 A CN107630150 A CN 107630150A CN 201710797709 A CN201710797709 A CN 201710797709A CN 107630150 A CN107630150 A CN 107630150A
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Abstract
The invention discloses a kind of preparation method of the enhanced CuNiSi alloys of timeliness; vacuum induction melting alloy is carried out using nitrogen as protection qi leel; then powder by atomization is carried out using confined type nozzle, the alloy powder of certain particle diameter carries out the processing of atmosphere protection hot pressed sintering after selection atomization and low temperature aging handles to obtain CuNiSi alloys.The CuNiSi material preparation methods of the present invention have the small advantage of tiny crystal grain, even tissue, gross segregation compared with conventional casting methods, more alloying elements are uniformly distributed in matrix by way of rapid cooling, the size obtained by follow-up hot pressed sintering and Ageing Treatment is small, nanometer precipitated phase more than quantity, the netted phase amount that separates out of crystal boundary is reduced, the electric conductivity of alloy is effectively improved, available for Aero-Space high-performance conductive elastic element, such as lead frame and power spring pad etc..
Description
Technical field
The invention belongs to metal-base composites technical field, is related to a kind of enhanced CuNiSi alloys of timeliness and its preparation
Method.
Background technology
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 higher requirement is proposed to blaster fuse frame material.Tradition prepares cupro-nickel silicon and closed
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, because the solid solution of alloying element causes alloy conductive rate to decline
Seriously.Though preparing the method for CuNiSi alloys at present and performance study achieving many progress, mainly pass through deformation process
Carry out crystal grain thinning, alloy entirety plasticity and toughness are poor.
The content of the invention
It is an object of the invention to provide the preparation method that a kind of Precipitation strengthens Type C uNiSi alloys, solves alloy
The problem of crystallite dimension is big, component segregation is serious, ensures that alloy has uniform tissue, there is preferable plasticity and toughness and conduction
Property.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of the enhanced CuNiSi alloys of timeliness, comprises 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；
Step 2, alloy melting, ready copper billet, nickel block and silicon grain are placed in graphite crucible, in nitrogen protection atmosphere
Lower progress Medium frequency induction melting；
Step 3, powder by atomization, atomization gas pressure is adjusted to certain value, determines nozzle diameter, then carried out aerosolization and blow
Powder, blow-on takes powder after cooling 10-15min after the completion of atomization, to ensure that the alloy powder of preparation is not oxidized；
Step 4, hot pressed sintering, the screening that the alloy powder after atomization is carried out to different-grain diameter are weighed, and choose certain particle diameter
Alloy powder carry out follow-up hot pressing sintering processes；
Step 5, Ageing Treatment, obtained sintered specimen is subjected to atmosphere protection Ageing Treatment in tube furnace, obtained thin
The CuNiSi alloys of crystal grain.
Invent further scheme as this case, 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.
Further scheme is invented as this case, Cu in step 1 material preparation phase:Ni:Si mass ratio is (94
~96)：(3.3~5.0)：(0.7~1.0), the scaling loss amount of nickel is 2-4%, and the scaling loss amount of silicon is 6-8%.
Further scheme is invented as this case, is vacuumized in step 2 using three-level vacuum system, treats that vacuum reaches
To 5-9 × 10-3Nitrogen is filled with 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, is incubated 5-8min at such a temperature.
Further scheme is invented as this case, pulverizing process uses confined type nozzle aerosolization, atomizing pressure in step 3
For 4-6MPa, a diameter of 3-5mm of atomizer, atomization gas is nitrogen, and atomization process is about 8-15s.
As the further scheme of this case invention, different-grain diameter is carried out to alloy powder before hot pressed sintering in the step 4
Screening process, yield less than 150um alloy powders and receive powder rate in 30-50%, 50-75um alloy powders proportion maximum；Use nitrogen
Gas is sintered as protection qi leel, and sintering temperature is 880-930 DEG C, sintering pressure 28-30MPa, sintering time 60-
70min。
Invent further scheme as this case, step 5 Ageing Treatment is carried out in tube furnace, using argon gas as
Protective atmosphere, aging time 3.5-4.4h, aging temp are 440-460 DEG C.
The beneficial effects of the invention are as follows：The CuNiSi alloys of the present invention have crystalline substance compared to the alloy that routine casting method obtains
Grain is tiny, and crystal boundary is netted to separate out the few feature of phase amount, and the electrical and thermal conductivity of alloy is better than alloy prepared by casting；By fast
Rapid hardening prepares CuNiSi alloys admittedly, can ensure 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；Available for the high property electrically conductive elastic device of Aero-Space,
Such as lead frame and power spring pad etc..
Brief description of the drawings
Fig. 1 is the process 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.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
As shown in figure 1, a kind of preparation method of the enhanced CuNiSi alloys of timeliness, comprises 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；
Step 2, alloy melting, ready copper billet, nickel block and silicon grain are placed in graphite crucible, in nitrogen protection atmosphere
Lower progress Medium frequency induction melting；
Step 3, powder by atomization, atomization gas pressure is adjusted to certain value, determines nozzle diameter, then carried out aerosolization and blow
Powder, blow-on takes powder after cooling 10-15min after the completion of atomization, to ensure that the alloy powder of preparation is not oxidized；
Step 4, hot pressed sintering, the alloy powder after atomization is subjected to different-grain diameter screening and weighed, chooses certain particle diameter
Alloy powder carry out follow-up hot pressing sintering processes；
Step 5, Ageing Treatment, obtained sintered specimen is subjected to atmosphere protection Ageing Treatment in tube furnace, obtained thin
The CuNiSi alloys of crystal grain.
Embodiment 1
The material of certain mass fraction is weighed using balance, nickel block 4wt%, silicon grain 1wt%, surplus is copper.Will be with graphite
The crucible of paper is put into vacuum chamber, and using confined type nozzle, a diameter of 4mm of atomizer, vacuum has reached 7 × 10-3Pa, nitrogen
Protective atmosphere+0.05MPa, induction melting then being carried out, heating rate is 2 DEG C/s, and smelting temperature is 1500 DEG C, is incubated 5min,
Atomizing pressure is adjusted to 6MPa, and molten metal is atomized into many tiny drops, molten metal flight course in the presence of nitrogen stream
Neutralize atomization gas and carry out heat exchange, solidified before reaching side wall and form spherical powder, this atomized alloy powder is received
Rate is 50%, and different-grain diameter screening process is carried out to obtained alloy powder, the alloy powder 30g for selecting particle diameter to be less than 75um,
Alloy powder is poured into progress hot pressed sintering processing in the graphite jigs of Φ 21, sintering temperature is 910 DEG C, pressure 30MPa, is protected
The pressure time is 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 conductance 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 the SEM figures for the CuNiSi materials that the present embodiment is prepared using aerosol alloy powder, and crystallite dimension is tiny,
It is strong tiny precipitation strength to be present in intra-die, and the netted phase amount that separates out of crystal boundary significantly reduces.
Embodiment 2
The material of certain mass fraction is weighed using balance, nickel block 4.17wt%, silicon grain 0.83wt%, surplus is copper.Will
Graphite crucible with graphite paper is put into vacuum melting room, atomizer diameter selection 3.5mm, and vacuum has reached 7 × 10-3Pa,
Nitrogen protection atmosphere+0.1MPa, induction melting, atomizing pressure 5MPa are then carried out, smelting temperature is 1450 DEG C, insulation
6min, molten metal are atomized into many tiny drops in the presence of nitrogen stream, entered in molten metal flight course with atomization gas
Row heat exchange, solidified before reaching side wall and form spherical powder, this atomization is less than 150um alloy powder recovery rates
43%, different-grain diameter screening is carried out to the alloy powder of preparation, selects alloy powder 29g machine of the particle diameter less than 74um to carry out hot pressing
Sintering processes, alloy powder is poured into the graphite jigs of Φ 21, sintering temperature is 900 DEG C, pressure 31MPa, the dwell time
For 65min, 440 DEG C, 4.2h Ageing Treatments are then carried out to alloy sample, obtained alloy sample consistency is 98.54%, is led
Electric rate is 30.17%IACS, hardness 114HB.
Embodiment 3
The material of certain mass fraction, nickel block 4.28wt% (scaling loss amount 4%), silicon grain 0.72wt% are weighed using balance
(scaling loss amount 8%), material gross mass 746.4g.Crucible with graphite paper is put into vacuum melting room, atomizer selection diameter
For 4.5mm, atomizing pressure selection 4MPa, 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 being incubated 7min, molten metal is impacted into many thin by nitrogen stream
Small drop, then by heat exchange, solidification forming, this atomization yield less than 150um alloyed powder recovery rates in flight course
For 38.26%, different-grain diameter screening process is carried out to the alloy powder of preparation, weighs the alloy powder 28g that particle diameter is less than 75um
Left and right, alloy powder is poured into the graphite jigs of Φ 21, sintering temperature is 1000 DEG C, pressure 28MPa, and the dwell time is
1h, then carries out 460 DEG C, time 3.9h of Ageing Treatment aging temp to alloy sample again, and obtained alloy sample consistency is
98.2%, conductance 30.69%IACS, hardness 104HB.
Described above is present pre-ferred embodiments, for the ordinary skill in the art, according to the present invention's
Teaching, in the case where not departing from the principle of the present invention and spirit, the changes, modifications, replacement and the change that are carried out to embodiment
Shape is still fallen within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the enhanced CuNiSi alloys of timeliness, it is characterised in that comprise 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；
The melting of step 2, alloy, ready copper billet, nickel block and silicon grain are placed in graphite crucible, under nitrogen protection atmosphere
Carry out Medium frequency induction melting；
Step 3, powder by atomization, atomization gas pressure is adjusted to certain value, determines nozzle diameter, then carried out aerosolization and blow powder,
Blow-on takes powder after cooling down 10-15min after the completion of atomization, to ensure that the alloy powder of preparation is not oxidized；
Step 4, hot pressed sintering, the screening that the alloy powder after atomization is carried out to different-grain diameter are weighed, and choose certain particle diameter
Alloy powder carries out follow-up hot pressing sintering processes；
Step 5, Ageing Treatment, obtained sintered specimen is subjected to atmosphere protection Ageing Treatment in tube furnace, obtains fine grain
CuNiSi alloys.
2. the preparation method of the enhanced CuNiSi alloys of timeliness as claimed in claim 1, it is characterised 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 alloys of timeliness as claimed in claim 1, it is characterised in that step 1 material
Expect Cu in the preparatory stage:Ni:Si mass ratio is (94~96)：(3.3~5.0)：(0.7~1.0), the scaling loss amount of nickel is 2-
4%, the scaling loss amount of silicon is 6-8%.
4. the preparation method of the enhanced CuNiSi alloys of timeliness as claimed in claim 1, it is characterised in that used in step 2
Three-level vacuum system is vacuumized, and treats that vacuum reaches 5 × 10-3-9×10-3Nitrogen is filled with after Pa to 0.02-0.1MPa, is made
Heated with vacuum induction furnace, heating power supply is medium frequency induction power supply, and the rate of heat addition is about 1-2 DEG C/s, melts the degree of superheat
For 150-200 DEG C, 5-8min is incubated at such a temperature.
5. the preparation method of the enhanced CuNiSi alloys of timeliness as claimed in claim 1, it is characterised in that powder processed in step 3
Process uses confined type nozzle aerosolization, and atomizing pressure 4-6MPa, a diameter of 3-5mm of atomizer, atomization gas is nitrogen,
Atomization process is about 8-15s.
6. the preparation method of the enhanced CuNiSi alloys of timeliness as claimed in claim 1, it is characterised in that in the step 4
Different-grain diameter screening process is carried out to alloy powder before hot pressed sintering, 150um alloy powders is yielded less than and receives powder rate in 30-
50%, 50-75um alloy powder proportion are maximum；It is sintered using nitrogen as protection qi leel, sintering temperature 880-930
DEG C, sintering pressure 28-30MPa, sintering time 60-70min.
7. the preparation method of the enhanced CuNiSi alloys of timeliness as claimed in claim 1, it is characterised in that during the step 5
Effect processing is carried out in tube furnace, using argon gas as protective atmosphere, aging time 3.5-4.4h, aging temp 440-
460℃。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074092A (en) * | 2019-12-26 | 2020-04-28 | 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 |
| 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 |
| 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 |
Citations (2)
| 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 |
-
2017
- 2017-09-06 CN CN201710797709.2A patent/CN107630150B/en active Active
Patent Citations (2)
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111074092A (en) * | 2019-12-26 | 2020-04-28 | 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 |
| 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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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 |