CN110434341A - A kind of preparation method of full-mesh high porosity nickel-bass alloy material - Google Patents
A kind of preparation method of full-mesh high porosity nickel-bass alloy material Download PDFInfo
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- CN110434341A CN110434341A CN201910814672.9A CN201910814672A CN110434341A CN 110434341 A CN110434341 A CN 110434341A CN 201910814672 A CN201910814672 A CN 201910814672A CN 110434341 A CN110434341 A CN 110434341A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
- B22F3/1025—Removal of binder or filler not by heating only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
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Abstract
The present invention provides a kind of preparation methods of full-mesh high porosity nickel-bass alloy material, comprising the following steps: one, prepare using 3D printing the porous resin presoma of full-mesh；Two, Co-based alloy powder and the tert-butyl alcohol are configured to slurry；Three, by the porous resin presoma of slurry cast to full-mesh, idiosome is obtained；Four, green body is freeze-dried；Five, the green body after freeze-drying is subjected to high temperature sintering, obtains full-mesh high porosity nickel-bass alloy material.The present invention accurately controls the pore structure and pore-size distribution of the porous resin presoma of full-mesh by 3D printing, the control to nickel-bass alloy material porosity, pore structure and pore-size distribution is realized in turn, the nickel-bass alloy material of preparation has full-mesh structure, porosity is up to 65%~80%, specific surface area is high, ventilation resistance is small, mechanical property is good, meets each field to the application demand of porous Ni-base alloy material.
Description
Technical field
The invention belongs to metal polyporous material and nickel-bass alloy material preparation technical fields, and in particular to a kind of full-mesh is high
The preparation method of porosity nickel-bass alloy material.
Background technique
Porous Ni-base alloy material has low-density, high specific strength, good creep rupture strength, excellent oxygen resistant to high temperatures
Change performance and be a kind of important structure-function integration material the features such as corrosion resistance, can be widely applied to aerospace,
The fields such as energy conservation and environmental protection and petrochemical industry.The preparation method of porous Ni-base alloy material is mainly by the U.S., Britain, Russia sieve at present
This, solid powder pack cementation method, electrodeposition process, infusion process and the gas alloying method etc. of Holland and Japan and other countries exploitation, so
And above-mentioned technique has certain disadvantage: in the preparation process of solid powder pack cementation method, powder easy-sintering is in porous Ni-base
The skeleton surface of alloy, reduces the strainability of material, while infiltration layer is uneven, so that the mechanical property of alloy is lower；Electricity
The thickness of the porous Ni-base alloy material of sedimentation preparation is mostly 1mm~5mm, it is difficult to which preparation structure is uniform, thickness is more than 20mm
Alloy material, and the chromium in plating solution brings biggish industrial pollution；The skeleton of porous Ni-base alloy material prepared by infusion process
Unevenly, and there is blind hole in regional area；Gas alloying method is also difficult to prepare the uniform porous Ni-base alloy material of skeleton.
3D printing is one kind based on digital model file, with adhesive materials such as powdery metal or plastics, is led to
After the mode successively printed come the method for constructing object, the every aspect of society is had been applied at present, but 3D printing is direct
Limitation of the metal material by current technology is prepared, the metal powders of many series not can be carried out 3D printing, can only be at present
It is selected in some metal systems, and metal material is directly prepared using 3D printing and is still in the development phase, technique is unstable, cost
Height, and low output.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of high hole of full-mesh
The preparation method of gap rate nickel-bass alloy material, the present invention accurately control the hole of the porous resin presoma of full-mesh by 3D printing
Structure and pore-size distribution, and then the control to nickel-bass alloy material porosity, pore structure and pore-size distribution is realized, obtained nickel
Base alloy material has full-mesh structure, and porosity is up to 65%~80%, and specific surface area is high, ventilation resistance is small, mechanical property
Well, phenomena such as avoiding uneven pore structure existing for existing porous Ni-base alloy material, blind hole, poor mechanical property.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of full-mesh high porosity nickel-base alloy
The preparation method of material, which is characterized in that method includes the following steps:
Step 1:, using resin as raw material, being prepared using 3D printing and being connected entirely according to target product nickel-bass alloy material
Logical porous resin presoma；
Step 2: Co-based alloy powder and the tert-butyl alcohol are carried out mixed processing, slurry is obtained；
Step 3: by the porous resin presoma of full-mesh obtained in slurry cast to step 1 obtained in step 2
It is interior, so that slurry is filled up completely the hole in resin precursor, obtains green body；
Step 4: green body obtained in step 3 is carried out freeze-drying process；
Step 5: treated green body freeze-dried in step 4 is carried out high temperature sintering processing, full-mesh height is obtained
Porosity nickel-bass alloy material；The porosity of the nickel-bass alloy material is 65%~80%.
The present invention prepares the porous resin presoma of full-mesh using 3D printing first using resin as raw material, by Ni-based conjunction
The slurry cast that bronze end and the tert-butyl alcohol are prepared obtains green body into the hole of the porous resin presoma of full-mesh, then passes through
Freeze-drying removes the part tert-butyl alcohol in green body, make Co-based alloy powder in the porous resin presoma hole of full-mesh at
Type, then handled using high temperature sintering, the porous resin presoma and the remaining tert-butyl alcohol of the full-mesh in green body are removed, is made in green body
Co-based alloy powder be sintered to form metallurgical bonding, obtain full-mesh high porosity nickel-bass alloy material.The present invention is by 3D printing
With freeze-drying, high temperature sintering combine, accurately controlled by 3D printing the porous resin presoma of full-mesh pore structure and
Pore-size distribution, and then the control to nickel-bass alloy material porosity, pore structure and pore-size distribution is realized, it effectively increases Ni-based
The porosity of alloy material, phenomena such as avoiding pore structure existing for existing porous Ni-base alloy material uneven, blind hole, this hair
Bright obtained nickel-bass alloy material has full-mesh structure, and porosity is up to 65%~80%, and specific surface area is high, ventilation resistance
Small, mechanical property is good, meets each field to the application demand of porous Ni-base alloy material.
The present invention prepares the porous resin presoma of full-mesh, the porous tree for the full-mesh that ensure that by 3D printing
The hole and grain of rouge presoma uniformly, without plug-hole and disconnected muscle phenomenon, thus in porous resin forerunner's internal casting of full-mesh
Be not in clogging when slurry, be conducive to the intracorporal hole of porous resin forerunner that slurry is filled up completely full-mesh, and
The surface of the even porous resin presoma inner pore for being attached to full-mesh, is not in smoothers phenomenon, while using resin conduct
The raw material of the presoma of full-mesh completely removes during Post isothermal treatment, the shadow to nickel-bass alloy material without aspect of performance
It rings.
The present invention uses freeze-drying process, realizes the complete molding of slurry in idiosome, effectively increases the intensity of slurry,
So that slurry is become the solid with some strength, then handled by high temperature sintering, obtains having the full-mesh of complete structure high
Porosity nickel-bass alloy material, the freezing medium by using the tert-butyl alcohol as freeze-drying process, in freezing dry process
Can fully charge and volume change is small, surface vapor pressure is high, and then the volume for realizing slurry in freezing dry process will not
It changes, ensure that the pore structure of nickel-bass alloy material will not change, shorten the time of freeze-drying process.
A kind of preparation method of above-mentioned full-mesh high porosity nickel-bass alloy material, which is characterized in that institute in step 1
The aperture for stating the porous resin presoma of full-mesh is 40 μm~60 μm.The aperture of the porous resin presoma of full-mesh of the present invention
It is 40 μm~60 μm, making slurry cast is not in the process clogging, is conducive to slurry and is filled up completely the porous of full-mesh
Hole in resin precursor.
A kind of preparation method of above-mentioned full-mesh high porosity nickel-bass alloy material, which is characterized in that institute in step 2
The mass percent for stating Co-based alloy powder in slurry is 75%~85%.The quality hundred of Co-based alloy powder in slurry of the present invention
Score is 75%~85%, so that slurry is had good mobility, slurry is made to be filled up completely the porous resin presoma of full-mesh
Interior hole improves the integrality of nickel-bass alloy material, avoids that slurry is excessively dilute to be caused after freeze-drying process because of the tert-butyl alcohol
It distils and generates non-uniform hole.
A kind of preparation method of above-mentioned full-mesh high porosity nickel-bass alloy material, which is characterized in that institute in step 4
The temperature for stating freeze-drying process is -30 DEG C~-40 DEG C, and the time is 0.3h~2h.The temperature of freeze-drying process of the present invention be-
30 DEG C~-40 DEG C, make the slurry fully charge in idiosome, be conducive to the molding of slurry, the time of freeze-drying process is 0.3h
~2h, forms slurry in idiosome completely, and the nickel-bass alloy material with complete structure is obtained after high temperature sintering, will not be because cold
Freeze and be dried time deficiency and generate slurry unshaped, and causes the nickel-based alloy material surface after high temperature sintering to be recessed, office
Portion hole breaking of muscle and tendon opens the problems such as uneven with pore-size distribution.
A kind of preparation method of above-mentioned full-mesh high porosity nickel-bass alloy material, which is characterized in that institute in step 5
State high temperature sintering processing process are as follows: vacuum degree be 1 × 10-2In the vacuum drying oven of Pa, 500 are warming up to the rate of 3 DEG C/min
1h is kept the temperature after DEG C, and 1.5h~3h is kept the temperature after being then warming up to 1200 DEG C~1300 DEG C with the rate of 10 DEG C/min.High temperature of the present invention
Sintering processes are 1 × 10 in vacuum degree-2It is carried out in the vacuum drying oven of Pa, protection idiosome is not oxidized, using the heating speed of 3 DEG C/min
Rate, it is not in produce because of uneven heating that making idiosome, which is not in be deformed in temperature-rise period because heating rate is too fast,
Raw cracking, using being heated to keeping the temperature 1h after 500 DEG C, the porous resin presoma of full-mesh is decomposed at 500 DEG C, keeps the temperature 1h
Be conducive to completely remove the porous resin presoma of full-mesh and the remaining tert-butyl alcohol, to nickel-bass alloy material without aspect of performance
It influences, using the heating rate of 10 DEG C/min, the slow thermal sintering of Co-based alloy powder ensure that the performance of nickel-bass alloy material
And shape does not change, and using 1.5h~3h is kept the temperature after being heated to 1200 DEG C~1300 DEG C, makes the burning between Co-based alloy powder
Knot neck physically well develops, and reaches metallurgical bonding, improves the plasticity, draftability and compressibility of nickel-bass alloy material.
Compared with the prior art, the present invention has the following advantages:
1, the present invention combines freeze-drying and high temperature sintering by 3D printing, obtains with the Ni-based conjunction of full-mesh high porosity
Golden material, the porosity of nickel-bass alloy material are 65%~80%, have low-density, high specific strength, high-specific surface area, low pass wind
The advantages that resistance and excellent mechanical property, at the same there is pore structure controllable, even aperture distribution, there is no blind hole and hole shape and
The advantages that shape designability is strong meets each field to the application demand of porous Ni-base alloy material.
2, the present invention using resin as raw material, by 3D printing prepare full-mesh porous resin presoma, full-mesh
The hole and grain of porous resin presoma are uniform, and no plug-hole and disconnected muscle phenomenon, are not in smoothers phenomenon, and in sintering processes
In the process, readily removed, residual is not had.
3, the mass percent of Co-based alloy powder is 75%~85% in the slurry that uses of the present invention, makes slurry with good
Good mobility, is conducive to the intracorporal hole of porous resin forerunner that slurry is filled up completely full-mesh, and slurry will not be excessively dilute, no
Hole can be generated after freeze-drying process.
4, the present invention uses freeze-drying process, forms slurry in idiosome completely, is transformed into consolidating with some strength
Body is conducive to carry out high temperature sintering processing；The present invention uses freezing medium of the tert-butyl alcohol as freeze-drying process, dry in freezing
It is dry during fully charge, green structure will not be impacted, be conducive to distillation progress, save freeze-drying when
Between.
5, the present invention is realized by technological parameters such as pressure, heating rate, temperature and the soaking times of control high temperature sintering
The porous resin presoma of full-mesh and the remaining tert-butyl alcohol completely remove, Co-based alloy powder slow thermal sintering, sintering
Neck physically well develops, and reaches metallurgical bonding, improves the plasticity, draftability and compressibility of nickel-bass alloy material structure.
6, preparation process of the present invention is simple, and strong operability has a wide range of application, it is easy to accomplish industrialized production.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is the pictorial diagram of full-mesh high porosity nickel-bass alloy material prepared by the embodiment of the present invention 1.
Specific embodiment
Embodiment 1
The present embodiment the following steps are included:
Step 1: use 3D printing preparation aperture for 55 μm, having a size of 50mm × 30mm × 10mm's (length × width × height)
The porous resin presoma of cuboid full-mesh；
Step 2: the 0.5kg tert-butyl alcohol and 2kg Co-based alloy powder are mixed, then it is stirred, is made Ni-based with glass bar
Alloy powder is uniformly dispersed, and obtains slurry；
Step 3: by the porous resin presoma of full-mesh obtained in slurry cast to step 1 obtained in step 2
It is interior, so that slurry is filled up completely the hole in resin precursor, obtains green body；
Step 4: green body obtained in step 3 is put into freeze drying plant, it is dry that freezing is then carried out at -35 DEG C
Dry processing 1h；
Step 5: treated that green body is put into that vacuum degree is 1 × 10 by freeze-dried in step 4-2The vacuum drying oven of Pa
It is interior, it is heated to keeping the temperature 1h after 500 DEG C with the heating rate of 3 DEG C/min, is then heated to 1250 with the heating rate of 10 DEG C/min
DEG C heat preservation 2h, then furnace cooling obtain full-mesh, the nickel-bass alloy material that porosity is 75%.
Fig. 1 is the pictorial diagram of full-mesh high porosity nickel-bass alloy material manufactured in the present embodiment, can from Fig. 1
Out, full-mesh high porosity nickel-bass alloy material manufactured in the present embodiment does not have plug-hole and closed pore phenomenon, and nickel-bass alloy material
In even aperture distribution.
Embodiment 2
The present embodiment the following steps are included:
Step 1: use 3D printing preparation aperture for 60 μm, the cylindrical body having a size of 70mm × 100mm (diameter × height) it is complete
The porous resin presoma of connection；
Step 2: the 1.5kg tert-butyl alcohol and 4.5kg Co-based alloy powder are mixed, then it is stirred with glass bar, makes nickel
Base alloy powder is uniformly dispersed, and obtains slurry；
Step 3: by the porous resin presoma of full-mesh obtained in slurry cast to step 1 obtained in step 2
It is interior, so that slurry is filled up completely the hole in resin precursor, obtains green body；
Step 4: green body obtained in step 3 is put into freeze drying plant, it is dry that freezing is then carried out at -30 DEG C
Dry processing 2h；
Step 5: treated that green body is put into that vacuum degree is 1 × 10 by freeze-dried in step 4-2The vacuum drying oven of Pa
It is interior, it is heated to keeping the temperature 1h after 500 DEG C with the heating rate of 3 DEG C/min, then heats 1300 DEG C with the heating rate of 10 DEG C/min
3h, then furnace cooling are kept the temperature, obtains full-mesh, the nickel-bass alloy material that porosity is 80%.
Embodiment 3
The present embodiment the following steps are included:
Step 1: use 3D printing preparation aperture for 40 μm, having a size of 80mm × 50mm × 20mm (outer diameter × internal diameter ×
It is high) three-dimensional annulus full-mesh porous resin presoma；
Step 2: the 0.1kg tert-butyl alcohol and 0.567kg Co-based alloy powder are mixed, then it is stirred, is made with glass bar
Co-based alloy powder is uniformly dispersed, and obtains slurry；
Step 3: by the porous resin presoma of full-mesh obtained in slurry cast to step 1 obtained in step 2
It is interior, so that slurry is filled up completely the hole in resin precursor, obtains green body；
Step 4: green body obtained in step 3 is put into freeze drying plant, it is dry that freezing is then carried out at -37 DEG C
Dry processing 0.5h；
Step 5: treated that green body is put into that vacuum degree is 1 × 10 by freeze-dried in step 4-2The vacuum drying oven of Pa
It is interior, it is heated to keeping the temperature 1h after 500 DEG C with the heating rate of 3 DEG C/min, is then heated to 1200 with the heating rate of 10 DEG C/min
DEG C heat preservation 2h, then furnace cooling obtain full-mesh, the nickel-bass alloy material that porosity is 65%.
Embodiment 4
The present embodiment the following steps are included:
Step 1: using 3D printing preparation aperture for 48 μm, the positive rectangular pyramid having a size of (bottom edge × height) 35mm × 30mm
The porous resin presoma of full-mesh；
Step 2: the 0.1kg tert-butyl alcohol and 0.4kg Co-based alloy powder are mixed, then it is stirred with glass bar, makes nickel
Base alloy powder is uniformly dispersed, and obtains slurry；
Step 3: by the porous resin presoma of full-mesh obtained in slurry cast to step 1 obtained in step 2
It is interior, so that slurry is filled up completely the hole in resin precursor, obtains green body；
Step 4: green body obtained in step 3 is put into freeze drying plant, it is dry that freezing is then carried out at -40 DEG C
Dry processing 0.3h；
Step 5: treated that green body is put into that vacuum degree is 1 × 10 by freeze-dried in step 4-2The vacuum drying oven of Pa
It is interior, it is heated to keeping the temperature 1h after 500 DEG C with the heating rate of 3 DEG C/min, is then heated to 1250 with the heating rate of 10 DEG C/min
DEG C heat preservation 1.5h, then furnace cooling obtain full-mesh, the nickel-bass alloy material that porosity is 70%.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (5)
1. a kind of preparation method of full-mesh high porosity nickel-bass alloy material, which is characterized in that method includes the following steps:
Step 1:, using resin as raw material, full-mesh is prepared using 3D printing according to target product nickel-bass alloy material
Porous resin presoma；
Step 2: Co-based alloy powder and the tert-butyl alcohol are carried out mixed processing, slurry is obtained；
Step 3: by the porous resin presoma of full-mesh obtained in slurry cast to step 1 obtained in step 2,
So that slurry is filled up completely the hole in resin precursor, obtains green body；
Step 4: green body obtained in step 3 is carried out freeze-drying process；
Step 5: treated green body freeze-dried in step 4 is carried out high temperature sintering processing, the high hole of full-mesh is obtained
Rate nickel-bass alloy material；The porosity of the nickel-bass alloy material is 65%~80%.
2. a kind of preparation method of full-mesh high porosity nickel-bass alloy material according to claim 1, which is characterized in that
The aperture of the porous resin presoma of full-mesh described in step 1 is 40 μm~60 μm.
3. a kind of preparation method of full-mesh high porosity nickel-bass alloy material according to claim 1, which is characterized in that
The mass percent of Co-based alloy powder is 75%~85% in slurry described in step 2.
4. a kind of preparation method of full-mesh high porosity nickel-bass alloy material according to claim 1, which is characterized in that
The temperature of freeze-drying process described in step 4 is -30 DEG C~-40 DEG C, and the time is 0.3h~2h.
5. a kind of preparation method of full-mesh high porosity nickel-bass alloy material according to claim 1, which is characterized in that
High temperature sintering described in step 5 processing process are as follows: vacuum degree be 1 × 10-2In the vacuum drying oven of Pa, with the rate of 3 DEG C/min
1h is kept the temperature after being warming up to 500 DEG C, and 1.5h~3h is kept the temperature after being then warming up to 1200 DEG C~1300 DEG C with the rate of 10 DEG C/min.
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| WO2021192698A1 (en) * | 2020-03-27 | 2021-09-30 | 富山住友電工株式会社 | Porous metal body and method for manufacturing porous metal body |
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Application publication date: 20191112 |