CN101914707A - Nickel-copper-iron-silicon (Ni-Cu-Fe-Si) porous alloy and preparation method thereof - Google Patents
Nickel-copper-iron-silicon (Ni-Cu-Fe-Si) porous alloy and preparation method thereof Download PDFInfo
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- CN101914707A CN101914707A CN 201010283559 CN201010283559A CN101914707A CN 101914707 A CN101914707 A CN 101914707A CN 201010283559 CN201010283559 CN 201010283559 CN 201010283559 A CN201010283559 A CN 201010283559A CN 101914707 A CN101914707 A CN 101914707A
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Abstract
The invention discloses a nickel-copper-iron-silicon (Ni-Cu-Fe-Si) porous alloy and a preparation method thereof, which relate to a porous material. The preparation method is simple and practical, and the prepared product has the porosity of 45 to 80 percent and the compression strength of 80 to 100MPa. The porous alloy comprises the following raw materials in the atomic percent: 65 percent of Ni, 30 percent of Cu, 3 percent of Fe and 2 percent of Si. The preparation method comprises the following steps of: mixing Ni powder, Cu powder, Fe powder and Si powder and performing ball milling to obtain alloy powder; mixing the alloy powder after the ball milling and a material to be built on stilts to obtain mixed powder; placing the mixed powder into a ball milling tank and uniformly mixing in vacuum; tabletting the mixed powder to obtain a green body; soaking the green body into water, heating the water, cleaning the green body, and dissolving residual sodium chloride (NaCl); and soaking the cleaned sample into the water, heating the water, detecting whether the NaCl in the sample is cleaned or not, and drying the cleaned sample to obtain the Ni-Cu-Fe-Si porous alloy.
Description
Technical field
The present invention relates to a kind of porous material, especially relate to a kind of employing NaCl as built on stilts material, volume fraction, holding temperature and soaking time by control NaCl reach Ni-Cu-Fe-Si porous alloy of control material porosity and mechanical property and preparation method thereof.
Background technology
Monel metal (1.Kyung-Ho Park, Debasish Mohapatra, B.Ramachandra Reddy, etal.Hydrometallurgy.86 (2007) 164-171) be to be the Ni-Cu alloy of base with metal Ni, it is a most widely used alloy in the abros.By in ambrose alloy binary alloy system, adding a small amount of other metals or non-metallic element, can obtain the Monel metal of different systems.This alloy has superior corrosion resistance, rub resistance, high intensity and hardness and good processing properties, therefore is specially adapted to corrosive atmosphere and rubs serious occasion.
The performance (yield strength etc.) that its macrostructure (size in hole and whole porosity) and alloy itself are had is depended in the application of porous material usually.Select suitable alloy system, rationally the hole of control material adopts suitable preparation method can make the porous material of desired properties.At present, porous material preparation method commonly used has eutectic solidification method, substitution method, pore to form the agent decomposition method, spread sintering process and salt certainly duplicates the method for forming (2.J.Banhart, Prog.Mater.Sci.46 (2001) 559-632) (3.J.T.Clemow, A.M.Weinstein, J.J.Klawitter, J.Koeneman, J.Anderson, J.Biomed.Material.Res.15 (1981) 73).Wherein, salt duplicates the method for forming and is most widely used, production cost is also lower, conventional metal polyporous material can be prepared (4.J.F.Despois by this simple and practical relatively method, A.Marmottant, L.Salvo, A.Mortensen, Mater.Sci.Eng.A 54 (2006) 2069-2073; 5.K.Kitazono, Y.Takiguchi, Scripta Mater.55 (2006) 501-504; 6.B.Y.Li, L.J.Rong, Y.Y.Li, V.E.Gjunter, Acta Mater.48 (2000) 3895-3904).But the problem that salt duplicates method of forming maximum is that the material perviousness for preparing is relatively poor, mainly is because the fused alloy is common and reactant salt, and salt is wrapped up, and stops up hole, reduces the material porosity.
More existing patent reports relevant with the Ni-Cu-Fe-Si porous alloy, as:
Publication number is that the Korean Patent of KR20070010829 (A) has been introduced a kind of method for preparing the ambrose alloy porous alloy, at first uses amino acid methyl ester as precursor, and copper powder is coated in the precursor surface, reaches preset thickness, forms the copper matrix of three-dimensional structure; Nickel powder is coated in the copper matrix surface for preparing in advance, at last the green compact that prepare sintering in reductibility, the amino acid methyl ester decomposes forms the nickel porous copper alloy again.The advantage of this method is that the porous alloy porosity of preparation can reach very high; Its shortcoming is that the nickel porous copper alloy mechanical property of preparation can be very not high, and the composition of ambrose alloy is not easy to control.
Publication number is that the Japanese Patent of JP10046268 (A) is introduced a kind of method for preparing the nickel chromium triangle porous alloy, and this method utilizes the foam Gum Rosin as matrix, and nickel powder, chromium powder are coated in resin surface.Be heated to 700～900 ℃ then, Gum Rosin is decomposed, Alloying Treatment is carried out in reheat to 1100～1300 ℃, prepares the nickel chromium triangle porous alloy.This method is similar to patent KR20070010829 (A), and shortcoming also is that composition is not easy accurate control, and mechanical property is not high.
Publication number is that the English Patent of GB 1013375 has been introduced a kind of employing organic adhesive metal mixture and prepared multi-porous alloy material, the weak point of this invention is that the particle scale of matrix metal requires below 10nm, when mixing, form cluster easily, and mixing and the easy oxidation of sintering process with body material.The product porosity of preparation is lower, and mostly the hole that forms be sealing, and filter effect is bad.
At present, the research of Ni-Cu-Fe-Si porous alloy also is in the primary stage, and is also less at the report of its preparation method and application.
Summary of the invention
The objective of the invention is to the problems referred to above at existing Ni-Cu-Fe-Si porous alloy existence, provide a kind of method simple, the porosity of the product of preparation can reach 45%～80%, and ultimate compression strength reaches Ni-Cu-Fe-Si porous alloy of 80～100MPa and preparation method thereof.
The raw material of Ni-Cu-Fe-Si porous alloy of the present invention is formed and by atom percentage content is: nickel (Ni): copper (Cu): iron (Fe): silicon (Si)=65: 30: 3: 2.
The preparation method of Ni-Cu-Fe-Si porous alloy of the present invention may further comprise the steps:
1) nickel, copper, iron, Si powder are mixed, ball milling gets alloy powder;
2) with alloy powder behind the ball milling and built on stilts material mixing, mixed powder is placed in the ball grinder, vacuum is mixed to evenly;
3), get green compact with the mixed powder compressing tablet;
4) will be immersed in behind the green sintering in the water, heating is cleaned, and dissolves residual NaCl;
5) sample after cleaning is immersed in the water, heating, whether the NaCl in the test sample cleans up, and the sample after cleaning drying gets the Ni-Cu-Fe-Si porous alloy.
In step 1), described ball milling, after nickel, copper, iron, Si powder can being mixed, ball milling 8～12h in planetary ball mill, to the powder particle size be 400 orders; Described ball milling, can be in mechanical milling process the adition process control agent, in mechanical milling process, reunite or be bonded on the ball milling tank skin to prevent powder; Described process control agent can adopt stearic acid or alcohol etc.
In step 2) in, described built on stilts material can adopt NaCl etc.; The volume fraction of described built on stilts material can be 45%～80%.
In step 3), described compressing tablet can adopt unidirectional tabletting machine compressing tablet, and the pressure of described unidirectional tabletting machine compressing tablet can be 200～250MPa.
In step 4), described agglomerating temperature can be 900～1100 ℃, and the time of corresponding insulation can be 4～24h, can feed argon gas in the sintering process as shielding gas; The temperature of described heating can be 50 ℃, insulation 12h.
In step 5), the temperature of described heating can be 50 ℃, and whether the NaCl in the described test sample cleans up, and can adopt AgNO
3Solution.
The present invention is by regulating the volume ratio of powdered alloy and built on stilts material (NaCl), the porous material of preparation different porosities; Also can be by size and the distribution of controlling holding temperature and soaking time adjustment apertures rate, hole.The porosity difference, mechanical properties such as corresponding porous material ultimate compression strength are also different.
In the present invention, in the Ni-Cu alloy, add a spot of Fe and Si, can obtain the Ni-Cu-Fe-Si alloy.Porous Ni-Cu-Fe-Si alloy has corrosion-resistant, the wear-resisting wiping of block Ni-Cu-Fe-Si alloy, higher mechanical property and the over-all properties of porous material concurrently.
The present invention adopts NaCl to prepare the Ni-Cu-Fe-Si porous alloy as built on stilts material.The controllability of the structural parameter (porosity, pore size etc.) that adopt this method to prepare the porous material biggest advantage to be porous material, and the changeable parameters scope is bigger.Select the required porous alloy system of suitable built on stilts material preparation, can reduce the blocked degree of hole.
Description of drawings
Fig. 1 is the ball milling SEM image of Ni-Cu-Fe-Si alloy powder afterwards.In Fig. 1, a adopts stearic acid as process control agent, the pattern after the ball milling, presentation layer sheet; B is for adopting alcohol as process control agent, and the pattern after the ball milling presents particulate state; After the moulding of particulate state powder the performance of sample than the moulding of synusia shape powder after the performance of sample good, therefore in follow-up experiment, all adopt alcohol as process control agent; Scale is 10 μ m.
Fig. 2 is 65% sample for the NaCl volume fraction, the SEM image of prepared sample under the insulation different time.In Fig. 2, a is the sample of insulation 4h; B is the sample of insulation 8h; C is the sample of insulation 12h; D is the sample of insulation 24h, and temperature is 1100 ℃; When soaking time was 8h, hole was comparatively even, and the porosity maximum is about 52%; Long when soaking time, when surpassing 12h, hole begins to shrink, and porosity descends; Scale is 100 μ m.
Fig. 3 is 65% for the NaCl volume fraction, in the final ultimate compression strength of 1100 ℃ of insulation different time gained samples.In Fig. 3, X-coordinate is soaking time/h, and ordinate zou is final ultimate compression strength/MPa; Point a is that intensity level is 78MPa in the final ultimate compression strength of 1100 ℃ of insulation 4h samples; Point b is that intensity level is 98MPa in the final ultimate compression strength of 1100 ℃ of insulation 8h samples; Point c is that intensity level is 93MPa in the final ultimate compression strength of 1100 ℃ of insulation 12h samples; Point d is that intensity level is 96MPa in the final ultimate compression strength of 1100 ℃ of insulation 24h samples.
Embodiment
Embodiment 1: with nickel powder, and copper powder, iron powder, silica flour were pressed atomic percent 65: 30: 3: 2 uniform mixing place planetary ball mill ball milling 8h-12h.Add stearic acid or alcohol in the mechanical milling process as process control agent, prevent to take place to reunite or be bonded on the ball milling tank skin at mechanical milling process interalloy powder.After treating that ball mill cools off fully, take out ball milling powdered alloy afterwards.Powdered alloy after the ball milling is observed under SEM, and granule-morphology as shown in Figure 1.Adopt alcohol as process control agent, the performance of powder is comparatively excellent after the ball milling.Therefore, in subsequent experimental, all adopt alcohol as process control agent.With powdered alloy behind the ball milling and built on stilts material (NaCl) uniform mixing, the NaCl volume fraction is 45%.The powder that mixes adopts unidirectional tabletting machine compression moulding.The green compact of compression moulding are placed on sintering in the tube furnace, feed argon gas in the sintering process all the time as shielding gas.In the tube furnace temperature-rise period, at first, be warming up to 900 ℃ then, be incubated 4h once more, furnace cooling at 810 ℃ of insulation 4h.Sample behind the sintering is immersed in the distilled water, and water bath with thermostatic control is heated to 50 ℃, insulation 12h.Repeatedly clean, dissolve residual NaCl.The distilled water sample after cleaning is immersed in the deionized water, and water bath with thermostatic control is heated to 50 ℃.Use AgNO
3Whether NaCl residual in the solution test sample cleans up.Sample after the washed with de-ionized water is placed in the vacuum drying oven, and is complete to the sample oven dry.The sample for preparing is observed down in scanning electron microscope (SEM), and the porosity of utilizing mercury injection apparatus to record sample is about 35.6%, and final ultimate compression strength can reach 90Mpa.
Identical with embodiment 1 step, just the volume fraction of NaCl is respectively 65%, 80%, records porosity for being respectively 52.7%, 69.3%, and final ultimate compression strength is respectively 48MPa, 90MPa.
Embodiment 4,5
Identical with embodiment 2 steps, be that final sintering temperature is respectively 1000 ℃, 1100 ℃, record porosity 55.6%, 51.3%, final ultimate compression strength is 83MPa, 88MPa.
Embodiment 6～8
Identical with embodiment 5 steps, just be respectively 8h, 12h, 24h 1100 ℃ of soaking times, recording porosity is 49.6%, 32%, 21%, final resistance to compression is 98MPa, 93MPa, 91.6MPa.
Claims (10)
1. Ni-Cu-Fe-Si porous alloy is characterized in that its raw material forms and by atom percentage content be: nickel: copper: iron: silicon=65: 30: 3: 2.
2. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1 is characterized in that may further comprise the steps:
1) nickel, copper, iron, Si powder are mixed, ball milling gets alloy powder;
2) with alloy powder behind the ball milling and built on stilts material mixing, mixed powder is placed in the ball grinder, vacuum is mixed to evenly;
3), get green compact with the mixed powder compressing tablet;
4) will be immersed in behind the green sintering in the water, heating is cleaned, and dissolves residual NaCl;
5) sample after cleaning is immersed in the water, heating, whether the NaCl in the test sample cleans up, and the sample after cleaning drying gets the Ni-Cu-Fe-Si porous alloy.
3. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1, it is characterized in that in step 1) described ball milling is after nickel, copper, iron, Si powder are mixed, ball milling 8～12h in planetary ball mill, to the powder particle size be 400 orders.
4. as the preparation method of claim 1 or 3 described a kind of Ni-Cu-Fe-Si porous alloys, it is characterized in that in step 1) that described ball milling is an adition process control agent in mechanical milling process; Described process control agent is stearic acid or alcohol.
5. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1 is characterized in that in step 2) in, described built on stilts material is NaCl.
6. as the preparation method of claim 1 or 5 described a kind of Ni-Cu-Fe-Si porous alloys, it is characterized in that in step 2) in, the volume fraction of described built on stilts material is 45%～80%.
7. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1 is characterized in that in step 3), and described compressing tablet is to adopt unidirectional tabletting machine compressing tablet, and the pressure of described unidirectional tabletting machine compressing tablet is 200～250MPa.
8. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1 is characterized in that in step 4), and described agglomerating temperature is 900～1100 ℃, and the time of corresponding insulation is 4～24h; Feed argon gas in the sintering process as shielding gas; The temperature of described heating is 50 ℃, insulation 12h.
9. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1 is characterized in that in step 5), and the temperature of described heating is 50 ℃.
10. the preparation method of a kind of Ni-Cu-Fe-Si porous alloy as claimed in claim 1 is characterized in that in step 5) whether the NaCl in the described test sample cleans up, and is to adopt AgNO
3Solution.
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| CN104190918A (en) * | 2014-08-31 | 2014-12-10 | 成都易态科技有限公司 | Powder sintering porous filter alloy, preparation method thereof and pre-pressing molding body for preparing powder sintering porous filter alloy |
| CN104353826A (en) * | 2014-10-29 | 2015-02-18 | 苏州莱特复合材料有限公司 | Wear-resistant and corrosion-resistant nickel-base composite material and powder metallurgy preparation method thereof |
| WO2015027746A1 (en) * | 2013-08-30 | 2015-03-05 | 成都易态科技有限公司 | Powder sintered metallic porous body, filter element and method for improving permeability thereof |
| CN110468303A (en) * | 2019-07-30 | 2019-11-19 | 华南理工大学 | A kind of medical magnetic thermotherapy corronil and preparation method thereof |
| CN114453587A (en) * | 2021-12-31 | 2022-05-10 | 西安理工大学 | Preparation method of nano porous copper-nickel alloy |
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| CN104419848A (en) * | 2013-08-30 | 2015-03-18 | 成都易态科技有限公司 | Powdery sintered metal porous body, filter element and method for improving permeability thereof |
| CN104419848B (en) * | 2013-08-30 | 2016-09-28 | 成都易态科技有限公司 | Powder sintered metal porous body, filter element and improve its infiltrative method |
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| CN110468303A (en) * | 2019-07-30 | 2019-11-19 | 华南理工大学 | A kind of medical magnetic thermotherapy corronil and preparation method thereof |
| CN110468303B (en) * | 2019-07-30 | 2020-05-22 | 华南理工大学 | Medical magnetic heat treatment copper-nickel alloy and preparation method thereof |
| CN114453587A (en) * | 2021-12-31 | 2022-05-10 | 西安理工大学 | Preparation method of nano porous copper-nickel alloy |
| CN114453587B (en) * | 2021-12-31 | 2024-02-27 | 西安理工大学 | Preparation method of nano porous copper-nickel alloy |
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