CN109746455A - A kind of cupric kovar alloy and preparation method thereof - Google Patents
A kind of cupric kovar alloy and preparation method thereof Download PDFInfo
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Abstract
A kind of cupric kovar alloy and preparation method thereof.The invention discloses a kind of high density cupric kovar alloy, the molecular formula of cupric kovar alloy is (Fe54Ni29Co17)1‑xCux, wherein the value of x is 0.03-0.07.The present invention also provides a kind of preparation methods of above-specified high density cupric kovar alloy, comprising the following steps: (1) fusing obtains alloy liquid stream after mixing the source Fe, the source Ni, the source Co and the source Cu；(2) aluminium alloy stream progress powder by atomization is obtained into kovar prealloyed powder, sieving processing；It (3) will sieving treated kovar prealloyed powder be kneaded by dry-mixed, feeding, granulation, injection molding, sintering obtain the cupric kovar alloy.Due to the incorporation of copper, the consistency of final alloy product is high, reaches as high as 99% for high density cupric kovar alloy in the present invention, and it is big to determine expansion temperature range, can reach 20-500 DEG C.
Description
Technical field
The invention belongs to field of alloy material more particularly to a kind of kovar alloy and preparation method thereof.
Background technique
Most of metal and alloy are all heated volume expansion, cooling volume contraction, the expansion of most of pure metal
Coefficient is inversely proportional with its fusing point.But alloy composed by the transition elements such as Fe, Ni, Co, due to their ferromagnetism, in Curie
Or less temperature within the scope of there is unusual thermal expansion, some anti-ferromagnetism alloys, within the scope of the temperature below Néel point
Also there is unusual thermal expansion.Our these alloys with special hot expansibility are referred to as expansion alloy, the heat of this abnormality
Expansion characteristics are commonly referred to as kovar effect.
Kovar alloy within the scope of 20-450 DEG C have with linear expansion coefficient similar in Bohemian glass, higher curie point with
And good cryo tissue stability, effective sealing-in matching can be carried out with corresponding Bohemian glass.The oxidation film of kovar alloy causes
It is close, it is easy welding and welding, there is good plasticity, machinable is widely used in production electrovacuum element, transmitting tube, imaging
Pipe, switching tube, transistor, sealing plug and relay1 case etc..For kovar alloy because of cobalt containing ingredients, product is more wear-resisting, adopts
Have with traditional pressure processing craft when preparing complex-shaped kovar alloy Package boxes the production cycle is long, expense material is big,
The problems such as high production cost, can reduce production cost, improve by MIM technical application in preparation kovar alloy Package boxes
Production efficiency solves the problems, such as that conventional pressure processing technology faces, and promotes the popularization and application of kovar alloy.
But under current MIM process conditions, kovar alloy sintering performance is poor, finished product consistency is low, for example,
The pre-alloyed powder that Kumihito Tokui is 10 μm using median prepares kovar alloy by MIM technique, after sintering
The relative density for obtaining sample is only 92%, this will lead to generates gas leakage when packaged, can not seal, and leads to product failure, together
When kovar alloy to determine expansion coefficient smaller, be easy to generate disengaging with packaging body at high temperature, also resulting in can not be close
Envelope.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided
High density cupric kovar alloy and preparation method thereof, the kovar alloy have high-compactness, it is wide to determine expansion temperature range.For solution
Certainly above-mentioned technical problem, technical solution proposed by the present invention are as follows:
A kind of high density cupric kovar alloy, the cupric kovar alloy are passed through by kovar alloy raw material powder and copper powder
MIM technique is prepared, and the molecular formula of cupric kovar alloy is (Fe54Ni29Co17)1-xCux, wherein the value of x is
0.03-0.07 (that is, the mass ratio that copper powder accounts for total raw material powder is 3-7%).Cupric kovar alloy in the present invention is
Controlled expansion alloy, by adding a certain amount of copper in kovar alloy, the consistency of the alloy reaches as high as 99%, fixed swollen
Swollen temperature range is 20-500 DEG C.In the present invention, the additional amount of copper is too small, and modified effect is bad, but since copper is without magnetism
, so magnetostrictive effect reduces, and determining expansion effect can be deteriorated instead after increasing.We are studies have shown that pass through control copper
Additional amount be 3-7%, the cupric kovar alloy of available best performance.It is furthermore preferred that the value of control x is 0.06-
0.07。
In above-mentioned cupric kovar alloy, it is preferred that the consistency of the cupric kovar alloy is not less than 97%.
As a general technical idea, the present invention also provides a kind of preparation sides of above-specified high density cupric kovar alloy
Method, comprising the following steps:
It (1) is (Fe by molecular formula54Ni29Co17)1-xCuxTake the source Fe, the source Ni, the source Co and the source Cu, wherein the value of x is
0.03-0.07 (more preferably 0.06-0.07), and melted after the source Fe, the source Ni, the source Co and the source Cu are mixed and obtain aluminium alloy
Stream；
(2) the aluminium alloy stream in step (1) is subjected to powder by atomization and obtains kovar prealloyed powder, sieving processing；
It (3) will treated that kovar prealloyed powder is kneaded by dry-mixed, feeding, granulation, note for sieving in step (2)
Modeling, sintering obtain the cupric kovar alloy.
In above-mentioned preparation method, it is preferred that the source Fe, the source Ni, the source Co and the source Cu be purity be 99.9% Fe bar, Ni stick
Material, Co bar and Cu bar.
In above-mentioned preparation method, it is preferred that controlling fusion temperature when fusing is 1570-1590 DEG C.
In above-mentioned preparation method, it is preferred that powder by atomization concrete operations are as follows: the flow velocity of control alloy liquid stream is 15-
Then 26kg/min selects inert gas, carrying out impacting with high pressure using the gas flow rate of 90-120m/s makes the atomization point of alloy liquid stream
Droplet is dissipated into, then solidifies droplet and obtains kovar prealloyed powder.
In above-mentioned preparation method, it is preferred that the concrete operations for processing of being sieved are as follows: by 90 mesh screens, 150 mesh screens with
270 mesh screens arrange from high to low, then kovar prealloyed powder is loaded in top mesh, by the vibration of 30min,
Filter out the satisfactory powder of particle size range.
In above-mentioned preparation method, it is preferred that the granularity of sieving treated kovar prealloyed powder is 20-50 μm.It grinds
It is more excellent to study carefully the kovar alloy comprehensive performance for showing to be prepared using the kovar prealloyed powder of above-mentioned granularity.
The present invention is based on following principles: inventor is the study found that the property of kovar alloy and other Conventional alloys has very greatly
Difference, the mode that Conventional alloys promote consistency is not obvious suitable for kovar alloy, and inventor has tested a variety of doping originals
Material, the results showed that, the copper powders (also only incorporation copper effect is better) of a certain amount are mixed in kovar alloy raw material powder,
Using influencing each other, cooperate between the copper and kovar alloy raw material powder of specific quantity, and it is prepared by MIM technique
Kovar alloy, available high-compactness and the wide kovar alloy for determining expansion temperature range.Dominant mechanism is as follows:
1, the present invention effectively raises the densification of the alloy by way of mixing a certain amount of copper in kovar alloy
Degree.By the study found that copper powders addition, liquid phase can be generated in the base in sintering process, make traditional solid-solid sintering machine
System is changed into solid-liquid sintering, and then improves the consistency of alloy, reduces the porosity of alloy.
2, for the present invention by way of mixing a certain amount of copper in kovar alloy, alloy is greatly improved determines expansion
Temperature range is measured discovery by the expansion temperature of determining to above-mentioned sintered products, and first, the thermal conductivity of copper powder itself is good
It is good, the heat dissipation of copper powders being added with conducive to alloy substrate.Second, the thermal expansion coefficient of copper is smaller, is 1.7*10-5M/ DEG C, energy
Effectively restrain the trend of kovar alloy product expansion.Third, under room temperature, alloy magnetism behavior will lead to lattice lattice constant
Become larger.At high temperature, copper is mixed with conducive to the recovery of lattice lattice constant, thus with because temperature increases when normal thermal expansion
It cancels out each other.Above 3 points are jointly maintained its expansion character of determining in higher temperature, and then increase material
Surely the temperature range expanded.
Compared with the prior art, the advantages of the present invention are as follows:
1, the high density cupric kovar alloy in the present invention is due to the incorporation of copper, and the consistency of final alloy product is high, most
High it is big to determine expansion temperature range up to 99% (being not less than 97%), can reach 20-500 DEG C.
2, the high density cupric kovar alloy in the present invention is without significantly alterring raw material powder ingredient, without using valuableness
Rare earth element, low in cost, preparation process is simple, helps to prepare highdensity kovar alloyed components.
Specific embodiment
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of high density cupric kovar alloy is prepared by kovar alloy raw material powder and copper powder by MIM technique, point
Minor is (Fe54Ni29Co17)0.97Cu0.03.The preparation method of cupric kovar alloy the following steps are included:
(1) iron staff material, cobalt bar, nickel bar, copper bar material are matched by above-mentioned molecular formula, is melted at 1580 DEG C
To alloy liquid stream；
(2) flow velocity for controlling alloy liquid stream is 20kg/min, inert gas is then selected, using the gas flow rate of 100m/s
Carrying out high pressure (2MPa) impact makes alloy liquid stream aerosol dispersion at droplet, then solidifies droplet and obtains kovar prealloy powder
End；
(3) 90 mesh screens, 150 mesh screens and 270 mesh screens are arranged from high to low, then by kovar prealloyed powder
It is loaded in top mesh, by the vibration of 30min, filters out the satisfactory powder of particle size range；
(4) the satisfactory powder of particle size range will be filtered out in step (3) to be kneaded, granulation, infuse by dry-mixed, feeding
Modeling, sintering obtain the cupric kovar alloy of cylindrical shape.
The concrete operations of above-mentioned steps (4) are as follows: dry-mixed to be uniformly mixed it with the method for mechanical mixture, mixing apparatus
For the dry-mixed device of four tanks, the dry-mixed time is 2h.Appropriate oil based binder is added by the 55% of powder loading, makes it by the way that 1h is dry-mixed
It is uniformly mixed.Be added to binder mixed powder it is dry blended uniformly after, be fitted into mixing facilities and be kneaded, so that metal powder
It is uniformly mixed between binder, obtains the feeding of good fluidity.Sample is completed to inject with injection machine, is infused by adjusting
Temperature, mold temperature, injection pressure, injection speed are penetrated, flawless part injection base is obtained.After obtaining injection base, it will inject
Base, which is placed in normal heptane, carries out solvent degreasing.Base is injected after solvent degreasing, remaining binder is removed using thermal debinding side.Heat
Sample carries out high temperature sintering in vacuum sintering furnace after degreasing.Maximum temperature is 1350 DEG C when sample is sintered, soaking time 3h.
Sample furnace cooling after heat preservation.
Performance detection is carried out to the cupric kovar alloy for the cylindrical shape being prepared in embodiment.Measure final products
Consistency be 97%, determine expansion temperature range is 20-460 DEG C, and the opposite raising of consistency determines expansion temperature range and broadens.Tool
Volume data see the table below 1.
The performance of the kovar alloy of difference Cu content compares at 1:1350 DEG C of table
Embodiment 2:
A kind of high density cupric kovar alloy is prepared by kovar alloy raw material powder and copper powder by MIM technique, point
Minor is (Fe54Ni29Co17)0.95Cu0.05.The preparation method of cupric kovar alloy the following steps are included:
(1) iron staff material, cobalt bar, nickel bar, copper bar material are matched by above-mentioned molecular formula, is melted at 1580 DEG C
To alloy liquid stream；
(2) flow velocity for controlling alloy liquid stream is 20kg/min, inert gas is then selected, using the gas flow rate of 100m/s
Carrying out high pressure (2MPa) impact makes alloy liquid stream aerosol dispersion at droplet, then solidifies droplet and obtains kovar prealloy powder
End；
(3) 90 mesh screens, 150 mesh screens and 270 mesh screens are arranged from high to low, then by kovar prealloyed powder
It is loaded in top mesh, by the vibration of 30min, filters out the satisfactory powder of particle size range；
(4) the satisfactory powder of particle size range will be filtered out in step (3) to be kneaded, granulation, infuse by dry-mixed, feeding
Modeling, sintering obtain the cupric kovar alloy of cylindrical shape.
The concrete operations of above-mentioned steps (4) are as follows: dry-mixed to be uniformly mixed it with the method for mechanical mixture, mixing apparatus
For the dry-mixed device of four tanks, the dry-mixed time is 2h.Appropriate oil based binder is added by the 55% of powder loading, makes it by the way that 1h is dry-mixed
It is uniformly mixed.Be added to binder mixed powder it is dry blended uniformly after, be fitted into mixing facilities and be kneaded, so that metal powder
It is uniformly mixed between binder, obtains the feeding of good fluidity.Sample is completed to inject with injection machine, is infused by adjusting
Temperature, mold temperature, injection pressure, injection speed are penetrated, flawless part injection base is obtained.After obtaining injection base, it will inject
Base, which is placed in normal heptane, carries out solvent degreasing.Base is injected after solvent degreasing, remaining binder is removed using thermal debinding side.Heat
Sample carries out high temperature sintering in vacuum sintering furnace after degreasing.Maximum temperature is 1350 DEG C when sample is sintered, soaking time 3h.
Sample furnace cooling after heat preservation.
Performance detection is carried out to the cupric kovar alloy being prepared in embodiment.The consistency for measuring final products is
98%, determining expansion temperature range is 20-475 DEG C, and consistency is opposite to be improved, and determines expansion temperature range and broadens.Specific data are seen below
Table 2.
The performance of the kovar alloy of difference Cu content compares at 2:1350 DEG C of table
Embodiment 3:
A kind of high density cupric kovar alloy is prepared by kovar alloy raw material powder and copper powder by MIM technique, point
Minor is (Fe54Ni29Co17)0.93Cu0.07.The preparation method of cupric kovar alloy the following steps are included:
(1) iron staff material, cobalt bar, nickel bar, copper bar material are matched by above-mentioned molecular formula, is melted at 1580 DEG C
To alloy liquid stream；
(2) flow velocity for controlling alloy liquid stream is 20kg/min, inert gas is then selected, using the gas flow rate of 100m/s
Carrying out high pressure (2MPa) impact makes alloy liquid stream aerosol dispersion at droplet, then solidifies droplet and obtains kovar prealloy powder
End；
(3) 90 mesh screens, 150 mesh screens and 270 mesh screens are arranged from high to low, then by kovar prealloyed powder
It is loaded in top mesh, by the vibration of 30min, filters out the satisfactory powder of particle size range；
(4) the satisfactory powder of particle size range will be filtered out in step (3) to be kneaded, granulation, infuse by dry-mixed, feeding
Modeling, sintering obtain the cupric kovar alloy of cylindrical shape.
The concrete operations of above-mentioned steps (4) are as follows: dry-mixed to be uniformly mixed it with the method for mechanical mixture, mixing apparatus
For the dry-mixed device of four tanks, the dry-mixed time is 2h.Appropriate oil based binder is added by the 55% of powder loading, makes it by the way that 1h is dry-mixed
It is uniformly mixed.Be added to binder mixed powder it is dry blended uniformly after, be fitted into mixing facilities and be kneaded, so that metal powder
It is uniformly mixed between binder, obtains the feeding of good fluidity.Sample is completed to inject with injection machine, is infused by adjusting
Temperature, mold temperature, injection pressure, injection speed are penetrated, flawless part injection base is obtained.After obtaining injection base, it will inject
Base, which is placed in normal heptane, carries out solvent degreasing.Base is injected after solvent degreasing, remaining binder is removed using thermal debinding side.Heat
Sample carries out high temperature sintering in vacuum sintering furnace after degreasing.Maximum temperature is 1350 DEG C when sample is sintered, soaking time 3h.
Sample furnace cooling after heat preservation.
Performance detection is carried out to the cupric kovar alloy being prepared in embodiment.The consistency for measuring final products is
99%, determining expansion temperature range is 20-500 DEG C, and consistency is opposite to be improved, and determines expansion temperature range and broadens.Specific data are seen below
Table 3.
The performance of the kovar alloy of difference Cu content compares at 3:1350 DEG C of table
Comparative example 1:
This comparative example compared with Example 1, the difference is that the value of x be 0.01.
Performance detection is carried out to the cupric kovar alloy being prepared in this comparative example.Measure the consistency of final products
It is 94%, determining expansion temperature range is 20-450 DEG C.
Comparative example 2:
This comparative example compared with Example 1, the difference is that the value of x be 0.08.
Performance detection is carried out to the cupric kovar alloy being prepared in this comparative example.Measure the consistency of final products
It is 99%, determining expansion temperature range is 20-480 DEG C.
Claims (9)
1. a kind of high density cupric kovar alloy, which is characterized in that the cupric kovar alloy by kovar alloy raw material powder and
Copper powder is prepared by MIM technique, and the molecular formula of cupric kovar alloy is (Fe54Ni29Co17)1-xCux, wherein x's takes
Value is 0.03-0.07.
2. cupric kovar alloy according to claim 1, which is characterized in that the value of x is 0.06-0.07.
3. cupric kovar alloy according to claim 1 or 2, which is characterized in that the densification of the cupric kovar alloy
Degree is not less than 97%.
4. a kind of preparation method of high density cupric kovar alloy, which is characterized in that be prepared by MIM technique, including following
Step:
It (1) is (Fe by molecular formula54Ni29Co17)1-xCuxTake the source Fe, the source Ni, the source Co and the source Cu, wherein the value of x is 0.03-
0.07, and melted after the source Fe, the source Ni, the source Co and the source Cu are mixed and obtain alloy liquid stream；
(2) the aluminium alloy stream in step (1) is subjected to powder by atomization and obtains kovar prealloyed powder, sieving processing；
It (3) will treated that kovar prealloyed powder is kneaded by dry-mixed, feeding, granulation, injection molding, is burnt for sieving in step (2)
Knot obtains the cupric kovar alloy.
5. the preparation method according to claim 4, which is characterized in that the source Fe, the source Ni, the source Co and the source Cu are that purity is
99.9% Fe bar, Ni bar, Co bar and Cu bar.
6. the preparation method according to claim 4, which is characterized in that controlling fusion temperature when fusing is 1570-1590 DEG C.
7. the preparation method according to claim 4, which is characterized in that powder by atomization concrete operations are as follows: control aluminium alloy
The flow velocity of stream is 15-26kg/min, then selects inert gas, and carrying out impacting with high pressure using the gas flow rate of 90-120m/s makes
Then alloy liquid stream aerosol dispersion solidifies droplet and obtains kovar prealloyed powder at droplet.
8. the preparation method according to claim 4, which is characterized in that the concrete operations for processing of being sieved are as follows: by 90 meshes
Net, 150 mesh screens and 270 mesh screens arrange from high to low, then kovar prealloyed powder is loaded in top mesh, lead to
The vibration for crossing 30min filters out the satisfactory powder of particle size range.
9. the preparation method according to any one of claim 4-8, which is characterized in that treated that kovar is prefabricated for sieving
The granularity of alloy powder is 20-50 μm.
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