CN110760710A - Preparation method of nickel-based alloy porous material - Google Patents
Preparation method of nickel-based alloy porous material Download PDFInfo
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- CN110760710A CN110760710A CN201910940375.9A CN201910940375A CN110760710A CN 110760710 A CN110760710 A CN 110760710A CN 201910940375 A CN201910940375 A CN 201910940375A CN 110760710 A CN110760710 A CN 110760710A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
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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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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Abstract
The invention discloses a preparation method of a nickel-based alloy porous material, which comprises the following steps: step 1, weighing nickel-based alloy powder and pore-forming agent K according to proportion2CO3Powder for standby; step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing to obtain mixed powder; step 3, pouring the mixed powder into a mold for prepressing, and putting the prepressed mixed powder and the mold into a spark plasma sintering furnace for spark plasma sintering to obtain a blank; step 4, the green body obtained in the step 3 is processedAnd cooling by water to obtain the alloy porous material. The invention mixes the alloy powder with K2CO3Sintering after the pore-forming agent is fully mixed, K2CO3It decomposes at high temperature, initially taking up space with K2CO3Volatilization and disappearance, increase of pores in the blank, K2CO3The melting point is higher, the material can not be decomposed prematurely when the sintering is not fully finished, the pores are easier to control, the stability is good, and no toxicity is generated.
Description
Technical Field
The invention belongs to the technical field of porous materials, and relates to a preparation method of a nickel-based alloy porous material.
Background
Sintered metal porous materials are generally prepared by pressing, high-temperature sintering and other processes on the basis of metal powder, metal wire mesh or metal fibers, often have good pore permeability characteristics and good mechanical properties, and are favored as excellent filtering functional materials, biological functional materials and energy-absorbing functional materials in various industries such as aerospace, petrochemical industry, biomedical treatment, papermaking, fishing, environmental protection and the like. At present, the research and application of metal porous materials are relatively concentrated on stainless steel, nickel-copper alloy, titanium alloy and the like, for example, porous stainless steel elements are commonly used in the corrosive environments of nitric acid, sulfuric acid, seawater, chemical fertilizers, industrial alkali and the like, and the service temperature can reach 500 ℃; the porous nickel-copper alloy is used in the environments of alkaline solution, hydrogen fluoride, seawater, salt and the like, and the service temperature can reach 400 ℃; the porous titanium is applied to the atmosphere of low-concentration hydrochloric acid, sulfuric acid, alkali, metal chloride and the like, but the using temperature of the porous titanium can only reach 150 ℃ generally. However, at present, with the increasing demand for porous elements in the fields of petrochemical industry, nuclear power, aerospace and the like, the porous elements are increasingly applied in various service environments, and traditional metals such as titanium, stainless steel and the like cannot completely meet the harsh service working condition requirements of high temperature resistance, corrosion resistance, oxidation resistance, long service time and the like, so that a metal porous material with heat resistance, corrosion resistance and excellent mechanical properties is urgently needed.
The sintered nickel-based superalloy porous material has good thermodynamic characteristics and controllable pore characteristics, the service temperature of the sintered nickel-based superalloy porous material can reach 650-1000 ℃, and the sintered nickel-based superalloy porous material is often used as a heat dissipation and heat transfer element of an aerospace engine. The nickel-based alloy has excellent mechanical property, oxidation resistance, high temperature resistance and corrosion resistance, and also has good hot workability and welding property, and is the most used high-temperature alloy in the world so far. The addition of the alloy elements makes the alloy have excellent high-temperature performance.
The traditional sintering process for preparing the metal porous material has the following defects: the preparation is mostly carried out by adopting non-spherical powder, the treatment process is various, the process is complicated, and the period is long; the shape, the size and the like of pores are difficult to control, stress concentration is easy to occur under the stress action when the porous piece is in service to form cracks to cause failure, spherical and approximately spherical pores are ideal porous structures, but are difficult to control in actual preparation; in order to improve the porosity, adding pore-forming agents is a common means for preparing porous materials, but the conventional pore-forming agents such as ammonium bicarbonate, urea and the like are difficult to completely remove at the later stage, and the cleanliness of products is difficult to ensure.
Disclosure of Invention
The invention aims to provide a preparation method of a nickel-based alloy porous material, which solves the problem of uneven pore distribution in an alloy material in the prior art.
The technical scheme adopted by the invention is that the preparation method of the nickel-based alloy porous material specifically comprises the following steps:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to proportion2CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, and putting the prepressed mixed powder and the mold into a spark plasma sintering furnace for spark plasma sintering to obtain a blank;
and 4, performing water cooling on the blank obtained in the step 3 to obtain the alloy porous material.
In step 1, a pore-forming agent K2CO3The mass ratio of the powder to the nickel-based alloy powder is 1: 6-9.
In the step 1, the granularity of the nickel-based alloy powder is 53-150 mu m.
In the step 2, the mixing time of the mixer is 2-3 h.
And step 3, specifically, placing the pre-pressed mixed powder and the die into a discharge plasma sintering furnace for sintering, wherein the sintering temperature is 1100-1500 ℃, the sintering time is 1-2 hours, the heating pressure is 20-50 MPa, the unloading pressure is normal pressure after the mixed powder and the die are heated to the sintering temperature, and then the temperature is kept for 5-30 min.
In the step 3, the mold is a graphite mold, zinc stearate is uniformly coated in the mold, and the size of the mold is phi 40 multiplied by 60 mm.
And 4, cooling the alloy to 120-140 ℃ by water, and then opening the furnace to obtain the alloy porous material.
The invention has the beneficial effects that the alloy powder and the K are mixed2CO3Sintering after the pore-forming agent is fully mixed, K2CO3It decomposes at high temperature, initially taking up space with K2CO3Volatilization and disappearance, increase of pores in the blank, K2CO3Higher melting point, no premature decomposition when the sintering is not fully finished, easier pore control, good stability, no toxicity, lower price, no conventional pore-forming agent such as urea and ammonium bicarbonate which can be decomposed at low temperature when volatilized, toxic gas such as ammonia gas and the like, and residual K in the blank2CO3Easily dissolved in boiling water, can be removed by boiling at high temperature, has no pollution, and can be used for treating K2CO3The powder is fully ball-milled, and the pore size of the green body is easier to control when the powder is sintered.
Drawings
FIG. 1 is an electron microscope image of the nickel-based alloy porous material prepared by the invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
A preparation method of a nickel-based alloy porous material specifically comprises the following steps:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to proportion2CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, and putting the prepressed mixed powder and the mold into a spark plasma sintering furnace for spark plasma sintering to obtain a blank;
and 4, performing water cooling on the blank obtained in the step 3 to obtain the alloy porous material.
In step 1, a pore-forming agent K2CO3The mass ratio of the powder to the nickel-based alloy powder is 1: 6-9.
In the step 1, the granularity of the nickel-based alloy powder is 53-150 mu m.
In the step 2, the mixing time of the mixer is 2-3 h.
And step 3, specifically, placing the pre-pressed mixed powder and the die into a discharge plasma sintering furnace for sintering, wherein the sintering temperature is 1100-1500 ℃, the sintering time is 1-2 hours, the heating pressure is 20-50 MPa, the unloading pressure is normal pressure after the mixed powder and the die are heated to the sintering temperature, and then the temperature is kept for 5-30 min.
In the step 3, the mold is a graphite mold, zinc stearate is uniformly coated in the mold, and the size of the mold is phi 40 multiplied by 60 mm.
And 4, cooling the alloy to 120-140 ℃ by water, and then opening the furnace to obtain the alloy porous material.
As can be seen from FIG. 1, in the process of preparing the porous material of the nickel-base alloy, when the temperature is 1200 ℃, good sintering necks are formed among the alloy powder particles, and a large number of initial irregular holes in the blank are gradually reduced and spheroidized to be smooth and exist in a regular sphere shape and a nearly sphere shape.
The nickel-based alloy powder used by the alloy comprises the following components in percentage by mass:
c: 0.012% -0.014%, O: 0.009% -0.011%, N: 0.0065% -0.0072%, H: 0.0025% -0.0032%, Al: 0.45% -0.53%, B: 0.001-0.005%, Nb: 5.06% -5.16%, Mo: 3.11% -3.25%, P: 0.0012% -0.014%, Si: 0.012% -0.15%, Mn: 0.02% -0.04%, Cu: 0.025-0.031%, Ti: 0.85% -0.93%, Cr: 18.25% -19.36%, Ni: 52.86-54.36 percent and the balance of Fe.
The nickel-based alloy powder used in the invention is SS-PREP spherical powder, compared with non-spherical powder sintering, the SS-PREP powder has higher sphericity, the shape of pores among the powder is more regular compared with the non-spherical powder, the pore distribution is more uniform, the stress concentration is not easy to generate cracks, and the mechanical property of a porous product is more excellent when the porous product is used;
the sintering mode is spark plasma sintering, the blank is sintered under the combined action of direct current pulse current, joule heat and pressure, the highest heating rate exceeds 200 ℃/min, and the sintering rate is greatly improved. During sintering, impulse discharge can generate shock waves, meanwhile, electrons and ions flow at high speed, gas adsorbed on the surface of the powder is promoted to escape, an oxide film on the surface of the powder is broken down to a certain degree, and the powder is purified and activated and is suitable for the requirement of high cleanliness on working conditions. The heating is carried out in a graded heating mode, the heating rate of 0-800 ℃ is 100 ℃/min, the heating rate of 800-000 ℃ is 50 ℃/min, the heating rate of 1000-1500 ℃ is 20 ℃/min, the shortest sintering time can be less than 1h, the sintering efficiency can be effectively improved by adopting high heating rate at low temperature, the coarsening of crystal grains caused by overhigh temperature can be prevented by adopting low heating rate at high temperature, the performance of a sample can be ensured, the porosity of the prepared nickel-based alloy porous material is 10-40%, the pore size is 1-30 mu m, the porosity is high, the pores are uniform and distributed, the mechanical property is excellent, the cleanliness is high, the heating speed is high, the sintering time is short, the product is clean, compared with other sintering processes, the preparation time and the production period of the product can be greatly reduced, the cleanliness of the product is higher, and the method is particularly suitable for mass production of the product.
Example 1
A preparation method of a nickel-based alloy porous material specifically comprises the following steps:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to the mass ratio of 1:62CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing for 2 hours to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, putting the prepressed mixed powder and the mold into a discharge plasma sintering furnace for discharge plasma sintering, wherein the sintering temperature is 1100 ℃, the sintering time is 2 hours, the pressure is kept at 30MPa during heating, the pressure is unloaded to normal pressure after the mixed powder is heated to the sintering temperature, and then the temperature is kept for 30min to obtain a green body;
and 4, performing water cooling on the blank obtained in the step 3, and opening the furnace after the temperature is reduced to 140 ℃ to obtain the alloy porous material.
Example 2
A preparation method of a nickel-based alloy porous material specifically comprises the following steps:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to the mass ratio of 1:82CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing for 2.5 hours to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, putting the prepressed mixed powder and the mold into a discharge plasma sintering furnace for discharge plasma sintering, wherein the sintering temperature is 1500 ℃, the sintering time is 1h, the pressure is kept at 20MPa during heating, the pressure is unloaded to normal pressure after the mixed powder is heated to the sintering temperature, and then the temperature is kept for 30min to obtain a green body;
and 4, performing water cooling on the blank obtained in the step 3, and opening the furnace after cooling to 120 ℃ to obtain the alloy porous material.
Example 3
A preparation method of a nickel-based alloy porous material specifically comprises the following steps:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to the mass ratio of 1:72CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing, and mixing for 3 hours to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, putting the prepressed mixed powder and the mold into a discharge plasma sintering furnace for discharge plasma sintering, wherein the sintering temperature is 1200 ℃, the sintering time is 1.5h, the pressure is kept at 50MPa during heating, the pressure is unloaded to normal pressure after the heating is carried out to the sintering temperature, and then the temperature is kept for 5min to obtain a green body;
and 4, performing water cooling on the blank obtained in the step 3, and opening the furnace after cooling to 120 ℃ to obtain the alloy porous material.
Example 4
A preparation method of a nickel-based alloy porous material specifically comprises the following steps:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to the mass ratio of 1:92CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing, and mixing for 3 hours to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, putting the prepressed mixed powder and the mold into a discharge plasma sintering furnace for discharge plasma sintering, wherein the sintering temperature is 1400 ℃, the sintering time is 2 hours, the pressure is kept at 40MPa during heating, the pressure is unloaded to normal pressure after the mixed powder is heated to the sintering temperature, and then the temperature is kept for 20min to obtain a green body;
and 4, performing water cooling on the blank obtained in the step 3, cooling to 130 ℃, and then opening the furnace to obtain the alloy porous material.
TABLE 1 Properties of porous materials prepared according to the invention
| Porosity (%) | Average pore size (. mu.m) | |
| Example 1 | 38.41 | 30 |
| Example 2 | 22.74 | 8 |
| Example 3 | 24.57 | 17 |
| Example 4 | 34.20 | 12 |
As can be seen from the table, the porous material prepared by the invention is gradually densified with the increase of sintering temperature and pressure, the porosity is reduced, the pore size tends to be reduced, and the pore generation is facilitated by adding a certain proportion of pore-forming agent.
Claims (7)
1. The preparation method of the nickel-based alloy porous material is characterized by comprising the following steps of:
step 1, weighing nickel-based alloy powder and pore-forming agent K according to proportion2CO3Powder for standby;
step 2, the nickel-based alloy powder obtained in the step 1 and a pore-forming agent K2CO3Putting the powder into a mixer for fully mixing to obtain mixed powder;
step 3, pouring the mixed powder into a mold for prepressing, and putting the prepressed mixed powder and the mold into a spark plasma sintering furnace for spark plasma sintering to obtain a blank;
and 4, performing water cooling on the blank obtained in the step 3 to obtain the alloy porous material.
2. The method for preparing the nickel-based alloy porous material as claimed in claim 1, wherein in the step 1, a pore-forming agent K is used2CO3The mass ratio of the powder to the nickel-based alloy powder is 1: 6-9.
3. The method for preparing the nickel-based alloy porous material according to the claim 1, wherein in the step 1, the particle size of the nickel-based alloy powder is 53-150 μm.
4. The preparation method of the nickel-based alloy porous material according to claim 1, wherein in the step 2, the mixing time of a mixer is 2-3 h.
5. The preparation method of the nickel-based alloy porous material according to claim 1, wherein the step 3 is specifically that the pre-pressed mixed powder and the die are placed into a spark plasma sintering furnace for sintering, the sintering temperature is 1100-1500 ℃, the sintering time is 1-2 hours, the heating pressure is 20-50 MPa, the sintering temperature is reached, the unloading pressure is reached to the normal pressure, and then the temperature is kept for 5-30 min.
6. The method for preparing a nickel-based alloy porous material according to claim 1, wherein in the step 3, the mold is a graphite mold, zinc stearate is uniformly coated in the mold, and the size of the mold is phi 40 x 60 mm.
7. The preparation method of the nickel-based alloy porous material as claimed in claim 1, wherein in the step 4, the furnace is opened after the temperature is cooled to 120-140 ℃ by water, so as to obtain the alloy porous material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112609108A (en) * | 2020-12-07 | 2021-04-06 | 武汉银海焊接科技有限公司 | Preparation method of nickel-based material |
| CN115383114A (en) * | 2022-09-19 | 2022-11-25 | 西北有色金属研究院 | Preparation method of high-porosity Al-rich phase porous Ni-Al intermetallic compound |
| CN115747603A (en) * | 2022-11-21 | 2023-03-07 | 北京航空材料研究院股份有限公司 | Porous high-temperature alloy material and preparation method thereof |
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