CN101717873A - Powder forging and molding method for preparing porous amorphous alloy block material - Google Patents
Powder forging and molding method for preparing porous amorphous alloy block material Download PDFInfo
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Abstract
The invention discloses a powder forging and molding method for preparing a porous amorphous alloy block material. The method comprises the following steps of: after respectively sieving amorphous powder and a powdered NaCl pore-forming agent, proportionally weighing the two components according to a porosity requirement; after uniformly mixing the components by a material mixer, carrying out sheathing, degassing and enveloping; carrying out heating and heat preservation on the sheathed and enveloped powder in a cold liquid phase area (Tg-Tx) for 5-15 minutes; forging and molding according to a set forging ratio, maintaining pressure for 30-90s and then forging; removing sheaths by adopting a machining method; and removing the pore forming agent by a water dissolving method to obtain the porous amorphous alloy block material. The method is simple and easy to apply, the prepared porous amorphous alloy material has the characteristics of controlled porosity, opening structure, uniform pore size distribution, and the like; meanwhile, the structural behavior of the powder can also be maintained. The dissolution of the pore forming agent is environmentally friendly, and the pore forming agent can be repeatedly used after treated.
Description
Technical field
The present invention relates to a kind of powder forging and molding method for preparing porous amorphous alloy block material, this method can prepare pore dimension, porosity is controlled, the open-celled structure block body stephanoporate amorphous alloy material of even aperture distribution.
Background technology
Amorphous alloy makes its dual nature that has common metal and glass concurrently because its atomic arrangement does not have the long-range atomic ordered, has excellent performances such as physics, chemistry and mechanics, has obtained in recent years paying close attention to widely.The porous amorphous alloy material is as a kind of novel porous material; have excellent mechanical property, corrosion resistance nature and energy absorption; the high strength that had both had metal polyporous material; the highly corrosion resistant performance that has stupalith again; be ideal filtration and chemical separation, catalysis and energy material, have the important application prospect in the contour performance structure of aerospace, nuclear power, oil, chemical industry, medicine and environment protection, function and structure-function integration field.
In order to prepare the porous amorphous alloy material, people have carried out many exploration work.At present, the method for preparing the porous amorphous alloy material both at home and abroad mainly comprises foaming, melt permeating casting etc.Apfel proposed to adopt whipping agent volatile, do not dissolve, do not take place chemical reaction in melt and glass to form melt-mixing in 1993, the pressurization fusing, fast decompression in the melt quenching process, dispersive foaming liquid gasification rapidly causes producing the required quick cooling of inhibition melt crystallization, melt is evenly cooled off, prepare foam porous material.Because the decompression rate height can form effective rate of cooling, the large block amorphous solid through-hole foam of batch preparations material [R.E.Apfel, Foam metallic glass.United States Patent, No.5384203,1995].Up to 2003, Schroers etc. just utilized hydration B
2O
3(Hydrated B
2O
3) foam in melt as whipping agent, the melt that will foam then carries out shrend, prepares Pd
43Ni
10Cu
27P
20Amorphous closed-cell foam material [JSchroers, C Veazey, W L Johnson, Appl.Phys.Lett., 82 (2003) 370-372].Because after the whipping agent foaming, can influence heat passage in the melt quenching process, thereby influence the formation of amorphous and the size of prepared block materials, they improve this method, at first melt is carried out shrend and obtain bulk amorphous alloy, then bulk amorphous alloy is heated to supercooling liquid phase region and makes the whipping agent foaming and intumescing, obtain porosity up to 85% Pd
43Ni
10Cu
27P
20Amorphous closed-cell foam material [J Schroers, C Veazey, M D Demetriou, W L Johnson, Phys., 96 (2004) 7723-7730].2004, it was Pd that the foaming of employing 1.5MPa hydrogen such as Wada has prepared composition
42.5Cu
30Ni
7.5P
20The amorphous porous material, prepared material is closed-cell materials [T Wada, A Inoue, Mater.Trans., 45 (2004) 2761-2765].2007, Demetriou etc. as whipping agent, prepared Fe with ZrH2
48Cr
15Mo
14Y
2C
15B
6Block body stephanoporate amorphous [M D Demetriou, GDuan, C Veazey, K DBlauwe, W L Johnson, Scripta Mater., 57 (2007) 9? 2].
2004, use hollow carbon spheres such as Brothers prepared Vit106 (Zr as placeholder
57Nb
5Cu
15.4Ni
12.6Al
10) porous material [A H Brothers, D C Dunand, Appl.Phys.Lett., 84 (2004) 1108-1110]; 2007, Brothers etc. used hollow iron ball as placeholder, and adopting uses the same method has prepared Mg
60Cu
21Ag
7Gd
12Amorphous porous material [A H Brothers, D C Dunand, Q Zheng, J Xu, J.Appl.Phys., 102 (2007) 023508].2008, employing porous Mo particles such as Jang were equipped with Mg as the erect-position system
58Cu
28.5Ag
2.5Gd
11Porous material [J.S.C.Jang, J Y Ciou, T H Hung, J C Huang, X H Du, Appl.Phys.Lett., 92 (2008) 011930].2005, Brothers etc. used sintering BaF2 stephanoporate framework as mould bases, adopted the method for seepage flow casting to prepare Zr
57Nb
5Cu
15.4Ni
12.6Al
10(Vit106) amorphous porous material [A H Brothers, D C Dunand, Adv.Mater., 17 (2005) 484-486; A H Brothers, D C Dunand, Acta Mater., 53 (2005) 4427-4440].
These methods all are the methods of liquid foam or prepare the amorphous porous material by adding placeholder to the mother alloy melt.Recently, people begin to explore powder metallurgy process and prepare the block body stephanoporate amorphous alloy material.2007, Demetriou etc. utilized MgCO
3.nH
2O is as whipping agent, with 95%Pd
43Ni
10Cu
27P
20Powder and 5%MgCO
3.nH
2After the O powder mixes, foaming then through hot isostatic pressing has earlier prepared Pd43Ni10Cu27P20 porous material [M D Demetriou, J P Schramm, CVeazey, W L Johnson, J C Hanan, N B Phelps, Appl.Phys.Lett., 91 (2007) 161903].2006, trials such as Xie adopted the electrical spark plasma agglomeration to prepare Zr
55Cu
30Al
10Ni
5Amorphous porous material [G Xie, WZhang, D V Louzguine-Luzgin, H Kimura, A Inoue, Scripta Mater., 55 (2006) 687-690].2007, trials such as Yoshikawa adopted microwave sintering to prepare Ni
52.5Zr
15Nb
10Ti
15Pt
7.5Porous material is but the amorphous porous material bonding strength height of preparation has much room for improvement [N Yoshikawa, D V Louzguin-Luzgin, K Mashiko, GXie, M Sato, A Inoue, S Taniguchi, Mater.Trans., 48 (2007) 632-634].
More or less there are some problems in above-mentioned these block body stephanoporate amorphous alloys preparation method:
(1) foaming requires to have low reactive behavior between whipping agent and the amorphous formation alloy, otherwise can reduce the amorphous formation ability of alloy, influences the size of prepared block materials.In the melt stage foaming, because the introducing of hole has reduced thermal conductivity, the size of prepared porous amorphous alloy material is littler than the size of compact block amorphous alloy material under the same terms.In the supercooling liquid phase region foaming, then because blowing temperature is lower, and the porous nickel of prepared porous material is relatively poor, percentage of open area is low.
(2) prepare amorphous alloy material with hollow ball as placeholder, because the introducing of placeholder can reduce thermal conductivity equally, and the placeholder of introducing can become heterogeneous nucleus, can reduce the amorphous formation ability of alloy, reduce the size of prepared porous material, the hole that obtains is a unicellular structure.Hollow ball as placeholder generally can be retained in the material, removes difficulty, occupies the volume and weight of material, influences its performance and application.
(3) melt permeating casting process complexity, sintered porous mould bases can restrict porosity, pore dimension and the shape of prepared block body stephanoporate non-crystalline material, influences the formation of amorphous.Melt is filled when incomplete, can form defective.The dissolving of mould bases may cause corrosion to prepared amorphous alloy.The preparation process complexity of sintered porous mould bases, the cost height.
(4) pore-forming material that adds in the melt, all can influence setting rate as the hollow ball of placeholder, porous mould bases etc., influence the formation of amorphous, thereby reduce the size of prepared porous amorphous alloy material.
(5) be subjected to the restriction of alloy system amorphous formation ability, the size of the block body stephanoporate amorphous alloy material of foaming and the preparation of melt permeating casting is limited, and its industrial application is restricted.
(6) powder hot isostatic pressing+foaming method prepares porous material, because foaming process can destroy the bonding strength at powder particle interface, therefore reduces the mechanical property of block body stephanoporate material.
(7) porous material of electrical spark plasma agglomeration, microwave sintering method preparation, porosity, aperture etc. are uncontrollable, are difficult to obtain the porous material of macroporsity.
Summary of the invention
The porous amorphous alloy material that technical problem to be solved by this invention provides a kind of preparation has controlled, the even aperture distribution of porosity, characteristics such as open-celled structure, the structural state that can keep powder simultaneously, the stripping environmental friendliness of pore-forming material, pore-forming material is reusable after treatment and technology is simple, cost is low, the powder forging and molding method of the preparation porous amorphous alloy block material that efficient is high.
In order to solve the problems of the technologies described above, the powder forging and molding method of preparation porous amorphous alloy block material provided by the invention is got amorphous powder, add Powdered pore-forming material in proportion, use the mixer uniform mixing, then mixed powder is carried out jacket, degasification, big envelope, the powder that jacket is encapsulated carries out heat tracing, excellent suitability for press forming, remove jacket, remove pore-forming material, drying, obtain the block body stephanoporate amorphous alloy material, comprise following steps:
1, selects the amorphous powder of atomizing, mechanical alloying (MA) or additive method preparation for use, pore dimension and porosity requirement according to prepared porous non-crystalline material, with screening or additive method powder is carried out classification, the present invention uses-200 orders and the accurate Tyler mesh mesh screen of-400 targets to be divided into 3 kinds of powder: 1. particle diameter is greater than 74 μ m powder; 2. particle diameter is 74 μ m～38 μ m powder; 3. particle diameter is less than 38 μ m powder; Utilize the glass transformation temperature Tg and the crystallization temperature Tx of dsc measurement amorphous powder.
2, select pore-forming material, require selected pore-forming material not react, easily remove behind the excellent suitability for press forming with amorphous powder, nontoxic, pore-forming material and chemical dissolution substance environment close friend thereof, choice of powder shape sodium-chlor of the present invention; The size of selected pore-forming material determines according to the aperture size and the porosity of the particle diameter of amorphous powder and prepared porous material, the present invention select for use particle diameter less than 65 μ m or less than the NaCl powder of 38 μ m (with sieving or additive method carries out classification to powder) as pore-forming material; The pore-forming material dehydration can be selected the appropriate means dehydration by the characteristic of pore-forming material, NaCl powder loft drier, 100 ℃～200 ℃ heating 5h～10h, air seasoning dehydration.
3, according to the porosity requirement of design, calculate amorphous powder and pore-forming material proportion of powder, volume calculated and quality take by weighing powder by quality by volume, use the mixer batch mixing, and mixing time is 1h～3h.
4, the amorphous powder, the pore-forming material powder mixes powder that mix are packed into jacket, with steel wire one little absorbent cotton is filled in below the tube sealing position of extraction pipe or the bottom, block the jacket extraction pipe bottom mouth of pipe (powder is taken away when preventing to vacuumize degasification), with the vacuum unit jacket that installs mixed powder is vacuumized degasification then, simultaneously the jacket that installs powder is carried out the oil bath heating, Heating temperature is 80 ℃～150 ℃, and the vacuum tightness that the jacket of mixed powder is housed is extracted into 10
-2After the above 1h～3h of Pa, carry out local fast heating at above 20mm～80mm position, jacket extraction pipe bottom with alcohol blast burner, kerosene blastburne or other rapid heating method, the hammering tube sealing is cut off unnecessary extraction pipe then.Employed sheath material is a copper, or soft steel.
5, after the temperature that (between Tg～Tx) sets in furnace temperature being heated between the amorphous powder supercooling liquid phase region, the jacket of 4 package hybrid powder is put into furnace chamber heat tracing 5min～15min set by step again.
6, the jacket powder behind the heat tracing is forged and pressed with press, and pressurize 30s～90s; According to the rheological characteristics of amorphous powder and the requirement of strength of prepared amorphous porous material, ratio of forging reduction is generally selected greater than 3: 1; In order to prevent jacket powder fast cooling in the forging and pressing process, it is heat insulation generally can to place a glass wool on the forging and pressing platform, on glass wool, place a steel briquetting (being called lower lock block) again, the jacket powder is placed on the steel briquetting, then on the jacket powder, place a steel briquetting (being called upper holder block) under the press pressure head again, between upper holder block and press pressure head, put a heat insulation glass wool of using again; Before the forging and pressing, heat lower lock block and upper holder block, Heating temperature is identical with the jacket powder, or 300 ℃～400 ℃, but heat-up time should be more longer heat-up time than the jacket powder.
7, adopt the mechanical cutting method to remove the jacket of the block materials of 6 excellent suitability for press forming set by step.
8, adopt water-soluble solution to remove pore-forming material NaCl, the block materials that is about to remove jacket is put into room temperature water, makes pore-forming material NaCl dissolving remove pore-forming material.
9, will dissolve the block body stephanoporate material of removing pore-forming material and put into loft drier and dehydrate, can dehydrate at air seasoning 2h～10h below 150 ℃.
Porous amorphous alloy material by the above-mentioned steps preparation, pore size is controlled, porosity is 10%～50%, even aperture distribution, open-celled structure, the prepared amorphous porous material that goes out be hole axially penetrating, be evenly distributed, radially fine and close relatively porous material, kept the structural state of powder simultaneously.
The present invention has following advantage and positively effect:
(1) can prepare large-sized porous material; Adopt liquid metal forging, can also prepare the goods of various different shapeies and size.
(2) porosity of prepared material has good designability, even aperture distribution, and the material hole is axially penetrating, be evenly distributed, axial fine and close relatively porous material, can keep the structural state of powder simultaneously.
(3) stripping of pore-forming material is simple, complete, and environmental friendliness is reusable after treatment;
(4) preparation equipment, technology are simple, and cost is low, and the efficient height is fit to large-scale production.
In sum, the invention provides a kind of method for preparing the block body stephanoporate amorphous alloy material.This method is simple.
Description of drawings
Fig. 1 is Zr of the present invention
50Cu
40Al
10The thermal stability analysis of atomized powder (DSC) curve, adopting inert atmosphere, temperature rise rate is 20k/min;
Fig. 2 is a powder jacket used in the present invention.
Embodiment
The present invention adopts homemade atomizing amorphous powder, has prepared a series of Zirconium-based block porous amorphous alloy materials.Below in conjunction with example and accompanying drawing the specific embodiment of the invention is described further.
Embodiment 1: prepare a kind of aperture size and less than 65 μ m, porosity be 30%～40% Zr
50Cu
40Al
10The block body stephanoporate amorphous alloy material
With the argon gas Zr that atomizes
50Cu
40Al
10Powder, particle diameter is the Zr of 74 μ m～38 μ m after sieving
50Cu
40Al
10Amorphous powder utilizes dsc measurement to obtain Zr
50Cu
40Al
10The Tg=438 of amorphous powder ℃ and crystallization temperature Tx=497 ℃ (adopting inert atmosphere, temperature rise rate is 20k/min, sees Fig. 1).Select for use particle diameter less than the NaCl powder of 65 μ m (powder being carried out classification) with screening or additive method as pore-forming material, with loft drier in 100 ℃～200 ℃ heating 5h～10h, air seasoning dehydration.With particle diameter is the Zr of 74 μ m～38 μ m
50Cu
40Al
10Amorphous powder with less than the NaCl powder of 65 μ m, 7: 3 by volume volume calculated and quality, take by weighing powder by quality, mix machine batch mixing 90min with V-type.With the amorphous, the pore-forming material mixed powder that the mix jacket of packing into, with steel wire one little absorbent cotton is filled in below the tube sealing position of extraction pipe or the bottom, block the jacket extraction pipe bottom mouth of pipe (powder is taken away when preventing to vacuumize degasification), with the vacuum unit jacket that installs powder is vacuumized degasification then, simultaneously the jacket that installs powder is carried out the oil bath heating, Heating temperature is 80 ℃～150 ℃, and the vacuum tightness that the jacket of mixed powder is housed is extracted into 10
-2After the above 1h～3h of Pa, use alcohol blast burner, kerosene blastburne or other rapid heating method to carry out local fast heating at the above 20mm in jacket extraction pipe bottom～80mm position, the hammering tube sealing is cut off unnecessary extraction pipe then.Employed sheath material is the copper material (see figure 2).After 460 ℃ of the temperature that (between Tg～Tx) sets in being heated to furnace temperature between the amorphous powder supercooling liquid phase region, again the jacket of package hybrid powder is put into furnace chamber heat tracing 10min～15min.Jacket powder behind the heat tracing is forged and pressed with 500 tons of press, and pressurize 30s～90s; Ratio of forging reduction is selected 5: 1; In order to prevent jacket powder fast cooling in the forging and pressing process, it is heat insulation to place a glass wool on the forging and pressing platform, on glass wool, place a steel briquetting (being called lower lock block) again, the jacket powder is placed on the steel briquetting, then on the jacket powder, place a steel briquetting (being called upper holder block) under the press pressure head again, between upper holder block and press pressure head, put a heat insulation glass wool of using again; Before the forging and pressing, lower lock block and upper holder block are heated, Heating temperature is 300 ℃～400 ℃, heat-up time 30min.After the excellent suitability for press forming, remove jacket with the mechanical cutting method.The block materials of removing jacket is put into room temperature water, and pore-forming material NaCl is removed in dissolving.Dissolving is removed the block body stephanoporate material of pore-forming material and put into loft drier, dehydrate, obtain porosity and be 30%～40% perforate porous material at air seasoning 5h～10h below 150 ℃.Because preparation temperature is between Tg～Tx, the porous blocks material of preparation has kept the structural state of powder.
Embodiment 2: prepare a kind of aperture size and be 40%～50% Zr less than 38 μ m, porosity
50Cu
40Al
10The block body stephanoporate amorphous alloy material
With the argon gas Zr that atomizes
50Cu
40Al
10Powder obtains the Zr of particle diameter less than 38 μ m after screening
50Cu
40Al
10Amorphous powder utilizes dsc measurement to obtain Zr
50Cu
40Al
10The Tg=438 of amorphous powder ℃ and crystallization temperature Tx=497 ℃ (adopting inert atmosphere, temperature rise rate is 20k/min).Select for use particle diameter less than the NaCl powder of 38 μ m (powder being carried out classification) with screening or additive method as pore-forming material, with loft drier in 100 ℃～200 ℃ heating 5h～10h, air seasoning dehydration.6: 4 by volume calculated weights, take by weighing powder, mix machine batch mixing 90min in V-type.Prepare according to the method for example 1 and step then that to obtain porosity be 40%～50% Zr
50Cu
40Al
10The perforate porous material.
Claims (4)
1. powder forging and molding method for preparing porous amorphous alloy block material, get amorphous powder, add Powdered pore-forming material in proportion, use the mixer uniform mixing, then mixed powder is carried out jacket, degasification, big envelope, powder to the jacket encapsulation carries out heat tracing, and excellent suitability for press forming is removed jacket, remove pore-forming material, drying obtains the block body stephanoporate amorphous alloy material, it is characterized in that:
(1) select amorphous powder for use, according to the pore dimension and the porosity requirement of prepared porous non-crystalline material, use-200 orders and the accurate Tyler mesh mesh screen of-400 targets to be divided into 3 kinds of powder: 1. particle diameter is greater than 74 μ m powder; 2. particle diameter is 74 μ m～38 μ m powder; 3. particle diameter is less than 38 μ m powder; Utilize the glass transformation temperature Tg and the crystallization temperature Tx of dsc measurement amorphous powder;
(2) select for use particle diameter less than 65 μ m or less than the NaCl powder of 38 μ m as pore-forming material, NaCl powder loft drier, 100 ℃～200 ℃ heating 5h～10h, air seasoning dehydration;
(3) according to the porosity requirement of design, calculate amorphous powder and pore-forming material proportion of powder, volume calculated and quality take by weighing powder by quality by volume, use the mixer batch mixing, and mixing time is 1h～3h;
(4) amorphous powder, the pore-forming material powder mixes powder that mix are packed into jacket, with the vacuum unit jacket that installs mixed powder is vacuumized degasification then, simultaneously the jacket that installs powder is carried out the oil bath heating, Heating temperature is 80 ℃～150 ℃, the vacuum tightness that the jacket of mixed powder is housed is extracted into after the above 1h～3h of 102Pa, carry out local fast heating at above 20mm～80mm position, jacket extraction pipe bottom with the rapid heating method, hammering tube sealing then, cut off unnecessary extraction pipe, employed sheath material is copper or soft steel;
(5) after being the temperature of setting between Tg～Tx in furnace temperature being heated between the amorphous powder supercooling liquid phase region, again will be set by step the jacket of (4) package hybrid powder put into furnace chamber heat tracing 5min～15min;
(6) the jacket powder behind the heat tracing is forged and pressed with press, according to the rheological characteristics of amorphous powder and the requirement of strength of prepared amorphous porous material, ratio of forging reduction is selected greater than 3: 1, and pressurize 30s～90s; In order to prevent jacket powder fast cooling in the forging and pressing process, it is heat insulation to place a glass wool on the forging and pressing platform, on glass wool, place a steel briquetting again, be called lower lock block, the jacket powder is placed on the steel briquetting, then on the jacket powder, place a steel briquetting under the press pressure head again, be called upper holder block, between upper holder block and press pressure head, put a heat insulation glass wool of using again; Before the forging and pressing, heat lower lock block and upper holder block, Heating temperature is identical with the jacket powder, or 300 ℃～400 ℃, but heat-up time is more longer heat-up time than the jacket powder;
(7) adopt the mechanical cutting method to remove the jacket of the block materials of (6) excellent suitability for press forming set by step;
(8) adopt water-soluble solution to remove pore-forming material NaCl, the block materials that is about to remove jacket is put into room temperature water, makes pore-forming material NaCl dissolving remove pore-forming material;
(9) will dissolve the block body stephanoporate material of removing pore-forming material and put into loft drier and dehydrate, can dehydrate at air seasoning 2h～10h below 150 ℃.
2. the powder forging and molding method of preparation porous amorphous alloy block material according to claim 1 is characterized in that: described amorphous powder is selected atomizing or the preparation of mechanical alloying method for use.
3. the powder forging and molding method of preparation porous amorphous alloy block material according to claim 1, it is characterized in that: before with the vacuum unit jacket that installs mixed powder being vacuumized degasification in the described step (4), with steel wire one little absorbent cotton is filled in below the tube sealing position of extraction pipe or the bottom, powder is taken away when blocking the jacket extraction pipe bottom mouth of pipe and preventing to vacuumize degasification.
4. the powder forging and molding method of preparation porous amorphous alloy block material according to claim 1 is characterized in that: the rapid heating method described in the above-mentioned steps (4) is for using alcohol blast burner or kerosene blastburne rapid heating.
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| CN101942580A (en) * | 2010-09-30 | 2011-01-12 | 中南大学 | Powder thermo-forming method for preparing porous amorphous alloy block material |
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| CN100376710C (en) * | 2006-04-21 | 2008-03-26 | 江苏大学 | Method for preparing porous bulk amorphous alloy |
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| CN101942580A (en) * | 2010-09-30 | 2011-01-12 | 中南大学 | Powder thermo-forming method for preparing porous amorphous alloy block material |
| CN101942580B (en) * | 2010-09-30 | 2011-12-21 | 中南大学 | Powder thermo-forming method for preparing porous amorphous alloy block material |
| CN101984104A (en) * | 2010-12-08 | 2011-03-09 | 沈阳工业大学 | Preparation method of biomedical bulk porous amorphous alloy |
| CN103853909A (en) * | 2012-12-06 | 2014-06-11 | 北京华成经纬软件科技有限公司 | Void elimination analysis method in automobile connecting rod powder forging process |
| US20150023827A1 (en) * | 2013-07-22 | 2015-01-22 | National Central University | Porous Amorphous Alloy Artificial Joint and Manufacturing Method Thereof |
| CN103643180A (en) * | 2013-12-02 | 2014-03-19 | 北京理工大学 | Aluminum-based amorphous alloy foam material and forming method thereof |
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| CN109465442B (en) * | 2018-11-12 | 2019-10-25 | 华中科技大学 | A kind of forging of amorphous alloy part/increasing material composite manufacturing method |
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