CN112941384A - Method for preparing carbon nano material reinforced AZ91 alloy semi-solid slurry - Google Patents
Method for preparing carbon nano material reinforced AZ91 alloy semi-solid slurry Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000000956 alloy Substances 0.000 title claims abstract description 72
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- 238000000034 method Methods 0.000 title claims abstract description 61
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- 239000002002 slurry Substances 0.000 title claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 22
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 17
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 100
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 84
- 230000008569 process Effects 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 18
- 238000010791 quenching Methods 0.000 claims abstract description 16
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 11
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 65
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 23
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 22
- 238000002604 ultrasonography Methods 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 19
- 239000011777 magnesium Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000155 melt Substances 0.000 claims description 15
- 238000003760 magnetic stirring Methods 0.000 claims description 14
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- 238000005520 cutting process Methods 0.000 claims description 10
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- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- 239000011701 zinc Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000011888 foil Substances 0.000 claims description 5
- -1 magnesium-aluminum-zinc-carbon Chemical compound 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- 235000011837 pasties Nutrition 0.000 claims description 5
- 239000000523 sample Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
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- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000010099 solid forming Methods 0.000 description 4
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
-
- B22F1/0003—
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
- C22B9/026—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves by acoustic waves, e.g. supersonic waves
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for preparing carbon nano material reinforced AZ91 alloy semi-solid slurry, belonging to the technical field of metal material manufacturing. A method for preparing a carbon nanomaterial reinforced AZ91 alloy semi-solid slurry, comprising: the AZ91 alloy is subjected to grain refinement by utilizing the excellent performance of the carbon nano tube, and the damage to the self structure of the carbon nano tube is avoided and the wettability of the carbon nano tube is improved by pre-dispersing the carbon nano tube and preparing the intermediate precast block of Mg-Al-Zn-CNTs. Refining the AZ91 alloy under the protection of argon, pressing the intermediate precast block into the alloy melt by using a bell jar, applying mechanical stirring and high-energy ultrasonic, rapidly cooling to 520-580 ℃, preserving heat, performing secondary high-energy ultrasonic for 60-90s, rapidly quenching with water, and finally preparing the spheroidized uniform semi-solid structure under the preferred process. The method has safe operation and stable process, the structure of the prepared carbon nano tube-AZ 91 alloy semi-solid slurry is obviously refined compared with the original matrix structure, and the carbon nano tube and the matrix interface are well combined.
Description
Technical Field
The invention belongs to the technical field of metal material manufacturing, and particularly relates to a method for preparing carbon nano material reinforced AZ91 alloy semi-solid slurry.
Background
The magnesium alloy has a plurality of excellent material properties, such as high specific strength, high specific rigidity, good thermal conductivity, good electromagnetic shielding property and the like, and is known as a green engineering material in the 21 st century. Due to the special properties of magnesium alloy, especially with the attention on carbon emission at home and abroad, the requirements of light weight and environmental protection are gradually highlighted, and the application of magnesium alloy is more and more extensive, especially the application in the industrial fields of automobiles, aerospace and the like, and even considered to be the light structural metal material with the application prospect in the two industries. The AZ91 magnesium alloy has excellent casting performance, can be used for producing various thin-wall parts and parts with complex structures, and is one of the most widely used cast magnesium alloys. However, the magnesium alloy has some limitations in industrial application due to its disadvantages of low strength, poor heat resistance, poor plasticity, small modulus, and easy corrosion. Therefore, the research on the high-performance magnesium-based composite material and the improvement on the short plate of the material have great practical significance for providing an effective solution for industrial application.
Carbon Nanotubes (CNTs), a tubular article formed by crimping hexagonal graphite meshes, have excellent properties such as high temperature resistance, corrosion resistance, high strength, high elastic modulus, thermal conductivity, and electrical conductivity. The tensile strength of the carbon nano tube can reach 10-250GPa, which is about 100 times of that of steel, and the density of the carbon nano tube is less than 1/7 of the steel, and is at least one order of magnitude higher than that of the conventional graphite fiber. Its elastic modulus can reach 1000GPa, is equivalent to that of diamond, is about 5 times that of steel, is a material with highest specific strength which can be prepared at present, and is known as "super fiber". Researches show that the carbon nano tube can be used as a heterogeneous nucleation core during magnesium crystallization, can block the movement of a primary phase interface, can refine an alpha-Mg phase in the AZ91 alloy, can play a role in lapping and strengthening crystal grains and crystal boundaries, and further improves the performance of the AZ91 alloy material. Therefore, carbon nanotubes are considered to be a nano reinforcing phase with great application value in metal matrix composites, and the carbon nanotubes are utilized to improve mechanical properties such as strength and elasticity of magnesium alloys, so that the carbon nanotubes are widely focused in the field of research of magnesium matrix composites.
However, the agglomeration, the uneven distribution of the reinforcing phase and the effective combination of the carbon nanotube and the magnesium alloy grain boundary in the magnesium alloy melt are the main difficulties in preparing the carbon nanotube reinforced magnesium-based composite material. In the publication No. CN109554569A entitled "a preparation method for compounding and integrating carbon material and magnesium alloy", graphene and carbon nanotubes are used as reinforcement to improve the mechanical property of an AZ91D alloy matrix. Although the composite material with good compactness can be obtained by the method, the carbon nano tube is not coated, the wettability of the carbon nano tube and the alloy melt is insufficient due to the structural characteristics of the carbon nano tube, and the process flow is complex and the cost is high. In the publication No. CN107904430A entitled "preparation of magnesium alloy structural member doped with single-walled carbon nanotube", single-walled carbon nanotube powder and AZ91 series magnesium alloy scrap raw materials are mechanically mixed, and then the AZ91 magnesium alloy structural member is prepared by a semi-solid extrusion forming method. The process is simple and environment-friendly, but the dispersion state of the carbon nano tube is difficult to control in the melting process, and the excellent mechanical property of the carbon nano tube is damaged by crushing the carbon nano tube to a certain extent, so that the improvement of the performance of the composite material is not facilitated. In the publication No. CN108085549A entitled "method for preparing novel magnesium-based composite material by ultrasonic-assisted mechanical stirring", carbon nano tubes are pre-dispersed, stirred in a semisolid-state interval of an alloy melt, and added with the carbon nano tubes, and then the melt is heated, kept warm, cooled and ultrasonically dispersed. Aiming at the problems, the research on novel casting preparation technology is developed, the homogenization composite process of the carbon nano tube and the magnesium alloy is explored, the cycle time of the preparation process is shortened, and the complicated molding component is very important.
The metal semi-solid forming process was originally proposed and developed by professor Flemings, etc. in the 70 th 20 th century, and semi-solid forming is forming by utilizing the characteristic of non-dendritic state of metal material in the process of converting from solid state to liquid state or from liquid state to solid state. Compared with the traditional casting and forging process, the metal semi-solid forming process has many advantages, such as stable mold filling, no turbulence and splashing, and less gas entrapment; the deformation resistance is small, the equipment investment is reduced, and the energy is saved; the forming temperature is low, and the service life of the die is long; the solidification shrinkage is small, the precision of a workpiece is high, the workpiece is almost formed in a near-net shape, and raw materials are saved; the internal structure of the formed part is compact, the hole defects are few, and the mechanical property is high; the solidification time is shortened, the production efficiency is high, and the like. Semi-solid slurry making is one of the keys of semi-solid forming technology, and the core of the semi-solid slurry making is the thinning and spheroidizing of metal grains.
The existing method for preparing the semi-solid slurry mainly comprises a mechanical stirring method, an electromagnetic stirring method, a strain induced melt activation method, a near liquid phase line method, a high-energy ultrasonic method and the like. The mechanical stirring method has the following disadvantages: the molten metal is easily polluted and corroded by the stirrer, a stirring blind area exists, the uniformity of the slurry is insufficient, gas and impurities are easily involved in the stirring process, and the quality of the semi-solid blank is further influenced. The electromagnetic stirring method has the following disadvantages: stirring equipment is expensive, the electromagnetic gap of the device is large, magnetic leakage is serious, and part of energy cannot be used for stirring the metal melt, so that the production cost is greatly increased. The strain-induced melt activation method has the following disadvantages: an additional pre-deformation process is required, the cost is increased, and the size of the prepared semi-solid blank is smaller. The near liquid phase line method has the following disadvantages: the preparation period is long, and the pouring temperature of the melt is difficult to accurately control.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing carbon nano material reinforced AZ91 alloy semi-solid slurry. The method realizes the purpose of reinforcing the AZ91 alloy matrix by the carbon nano tube through the methods of preparing an intermediate precast block, hot-pressing and sintering in vacuum and casting by high-energy ultrasound. The method has the advantages that: the solution dispersion not only keeps the inherent structure of the carbon nano tube, but also can play a pre-dispersion role in the magnesium powder-aluminum powder-zinc powder-carbon nano tube powder; the carbon nano tube is added in the form of a magnesium-aluminum-zinc carbon nano tube (Mg-Al-Zn-CNTs) intermediate precast block, the density of the carbon nano tube is larger than that of an alloy melt, the carbon nano tube is prevented from floating on a liquid surface, and the wetting of the carbon nano tube and a matrix is facilitated; high-energy ultrasound is applied to the AZ91 alloy melt, the generated transient high temperature and high pressure change the local balance, the surface tension of the liquid surface is reduced, strong local impact is generated, and the uniform dispersion of the carbon nano tube in the AZ91 melt is further promoted; the secondary high-energy ultrasound can prevent the aggregation of the carbon nano tubes in the cooling process of the melt and is helpful for spheroidizing crystal grains; the addition of carbon nanotubes enables the grain size of the AZ91 alloy to be refined.
The invention is realized by the following technical scheme:
a method for preparing a carbon nano-material reinforced AZ91 alloy semi-solid slurry comprises the following steps:
1) mixing the carbon nano tube with magnesium powder, aluminum powder and zinc powder by using ultrasound to obtain a mixed solution;
2) magnetically stirring the mixed solution under the action of a constant-temperature heating magnetic stirrer, drying the mixed solution in a vacuum drying oven after stirring, sintering the dried powder in a vacuum hot-pressing sintering furnace to obtain an Mg-Al-Zn-CNTs intermediate precast block, cutting the precast block into small particles, and coating the small particles with aluminum foil paper for later use;
3) cutting AZ91 matrix alloy into small pieces, placing the small pieces into a graphite crucible, placing the graphite crucible into a resistance furnace, heating to 620-680 ℃, preserving heat for 25-30min to completely melt the matrix alloy, then pressing the Mg-Al-Zn-CNTs intermediate precast block into an alloy melt by using a bell jar, and applying high-energy ultrasound while adding the precast block;
4) and 3) after the high-energy ultrasonic treatment is finished, quickly reducing the temperature of the melt to 520-580 ℃, preserving the temperature, applying secondary ultrasonic treatment for 60-90s, and immediately quenching the slurry obtained by the secondary ultrasonic treatment to obtain a semi-solid structure with fine grains.
Further, the specific step of mixing in the step 1) is to mix the carbon nano tube with absolute ethyl alcohol according to 2.5-3.5g of the carbon nano tube mixed with each 100ml of ethyl alcohol, and then put the mixture into an ultrasonic instrument for ultrasonic dispersion treatment for 2-3h, wherein the ultrasonic power is 400-480W, and the frequency is 35-45 kHz; mixing magnesium powder, aluminum powder, zinc powder and absolute ethyl alcohol according to the proportion that each 100ml of ethyl alcohol is mixed with 17-19g of magnesium powder, 1.7-1.9g of aluminum powder and 0.18-0.20g of zinc powder for 2-3h by mechanical stirring, wherein the stirring speed is 120-160 r/min; and then uniformly adding the mixed and dispersed magnesium powder, aluminum powder and zinc powder ethanol mixed solution into the carbon nano tube ethanol dispersion liquid after ultrasonic treatment, continuously performing ultrasonic dispersion, wherein the power is 800-1200W, the frequency is 35-45kHz, and simultaneously performing mechanical stirring, the stirring speed is 200-250r/min, and the duration is 2-3 h.
Furthermore, the outer diameter of the carbon nano tube is 20-60nm, the length of the carbon nano tube is 10-30 mu m, and the purity of the carbon nano tube is more than or equal to 99.5 percent; the purity of the magnesium powder, the aluminum powder and the zinc powder is more than or equal to 99.9 percent, and the granularity is 100-200 meshes.
Further, the magnetic stirring heating temperature in the step 2) is 45-55 ℃, and the stirring speed is 1500-; in particular, to avoid the delamination of the mixed powder and the carbon nanotubes, the magnetic stirring is maintained until the mixture is pasty.
Further, the sintering temperature in the step 2) is 400-450 ℃, the hot-pressing pressure is 40-60MPa, and the pressure maintaining time is 2-3 h; particularly, the CNTs in the intermediate prefabricated block of Mg-Al-Zn-CNTs obtained after sintering accounts for 5-10% by mass, Al accounts for 8.5-9.5% by mass, Zn accounts for 0.9-1.0% by mass, and the balance is Mg.
Further, in the step 3), the AZ91 matrix alloy comprises the following elements in percentage by weight: 8.5 to 9.5 percent of aluminum, 0.9 to 1.0 percent of zinc and the balance of magnesium.
Further, after the base alloy in the step 3) is completely melted, hexachloroethane accounting for 0.2-0.3 wt.% of the melt mass is added for refining and slagging off.
Further, the step 3) of pressing the magnesium-aluminum-zinc carbon nanotube intermediate precast block, wherein the adding amount of the carbon nanotube accounts for 0.5-1.5 wt% of the total amount of the alloy melt.
Further, the high-energy ultrasonic operation method in the step 3) is that an ultrasonic amplitude transformer probe is immersed into the alloy melt, the ultrasonic power is applied to the alloy melt to be 2.1-3.2kW, the frequency is 18-22kHz, and the time is 10-15 min; argon is filled in the whole ultrasonic process for protection.
Compared with other methods, the high-energy ultrasonic method has fewer defects, can obtain an ideal non-dendritic crystal semi-solid structure in a short time, and really realizes low energy consumption and high efficiency. When high-energy ultrasound is applied to the melt, acoustic cavitation and acoustic flow effects can be generated, and high-temperature and high-pressure shock waves generated by the acoustic cavitation effect play an important role in the aspects of breaking crystal grains, promoting nucleation, destroying a boundary layer and the like. Meanwhile, the carbon nano tubes can be promoted to be uniformly dispersed in the melt through an ultrasonic casting method and to be better infiltrated with the alloy melt, which plays an important role in obtaining fine and round semi-solid crystal grains.
Further, the parameters of the secondary ultrasound except time in the step 4) are consistent with the ultrasound in the step 3).
Further, the water quenching temperature in the step 4) is 20-30 ℃, and the water quenching is carried out and then the drying is carried out in a temperature field of 40-50 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) the crystal grains of the AZ91 alloy are refined by utilizing the excellent characteristics of the carbon nano tube; (2) the added carbon nano tube is dispersed by ultrasonic and is mixed with the metal powder by magnetic stirring, so that the structural damage of the carbon nano tube is avoided; (3) the Mg-Al-Zn-CNTs intermediate precast block prepared by the vacuum hot pressing sintering mode can effectively improve the wetting property of the carbon nano tube and the melt; (4) the application of high-energy ultrasonic waves promotes the uniform dispersion of the carbon nanotubes in the AZ91 alloy melt; (5) and in the semi-solid temperature range, applying secondary ultrasound to further spheroidize the semi-solid slurry structure.
The preparation process is stable, the semi-solid structure of the prepared composite material is obviously refined, and the carbon nano tube and the AZ91 alloy matrix interface are well combined.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature.
Example 1
A method for preparing a carbon nanotube material reinforced AZ91 alloy semi-solid slurry comprises the following steps:
(1) mixing a proper amount of carbon nanotubes with the outer diameter of 20-60nm, the length of 10-30 mu m and the purity of more than or equal to 99.5 percent with absolute ethyl alcohol in a beaker according to the proportion that every 100ml of the ethyl alcohol is mixed with 3.0g of the carbon nanotubes, and then putting the mixture into an ultrasonic instrument for ultrasonic dispersion treatment for 2.5h, wherein the ultrasonic power is 440W and the frequency is 40 kHz; mixing magnesium powder, aluminum powder, zinc powder and absolute ethyl alcohol with the purity of more than or equal to 99.9 percent and the granularity of 100-200 meshes with 18g of magnesium powder, 1.8g of aluminum powder and 0.2g of zinc powder in a ceramic container according to 100ml of ethanol, and mechanically stirring for 2.5 hours at the stirring speed of 140 r/min; and then uniformly adding the mixed and dispersed magnesium powder, aluminum powder, zinc powder and ethanol mixed solution into the carbon nano tube ethanol dispersion solution after ultrasonic treatment, continuously performing ultrasonic dispersion with the power of 1000W and the frequency of 40kHz, and simultaneously performing mechanical stirring at the stirring speed of 230r/min for 2.5 hours to obtain the mixed solution.
(2) And (2) placing the mixed solution prepared in the step (1) on a constant-temperature heating magnetic stirrer for magnetic stirring, wherein the heating temperature is 50 ℃, the magnetic stirring speed is 1800r/min, and in order to avoid the layering phenomenon of the mixed powder and the CNTs, the magnetic stirring is kept until the mixed solution is pasty, and then the mixed solution is placed in a vacuum drying oven for drying at 80 ℃.
(3) And putting the dried powder into a vacuum hot-pressing sintering furnace for sintering, wherein the sintering temperature is 430 ℃, the hot-pressing pressure is 50MPa, and the pressure maintaining time is 2.5h, so as to obtain the Mg-Al-Zn-CNTs intermediate precast block, wherein the CNTs accounts for 8% by mass, the Al accounts for 9% by mass, the Zn accounts for 1% by mass, and the balance is Mg, and cutting the precast block into small particles and coating the small particles with aluminum foil paper for later use.
(4) Cutting AZ91 matrix alloy (Al accounts for 9.0 wt%, Zn accounts for 1.0 wt%, and Mg accounts for the rest) into small pieces, placing into a dried graphite crucible, placing the crucible into a resistance furnace, heating to 650 ℃, and keeping the temperature for 30 min; argon is required for protection in the process.
(5) After the alloy is completely melted, hexachloroethane accounting for 0.25 wt.% of the melt mass is added for refining and slagging off. Then pressing the Mg-Al-Zn-CNTs intermediate prefabricated block into the alloy melt by using a bell jar, wherein the addition amount of the CNTs accounts for 1.0 wt% of the total weight of the alloy melt. Applying high energy ultrasound while adding the pre-agglomerate particles: immersing an ultrasonic amplitude transformer probe into the alloy melt, and applying ultrasonic power of 2.8kW, frequency of 20kHz and time of 13 min; argon is filled in the whole ultrasonic process for protection.
(6) And (3) after the high-energy ultrasonic is applied, when the temperature of the melt is rapidly reduced to 550 ℃, applying secondary ultrasonic to the semi-solid slurry for 80s, wherein the rest ultrasonic parameters are the same as those in the step (5). And immediately carrying out water quenching on the slurry obtained by the secondary ultrasound after the secondary ultrasound is finished, wherein the water quenching temperature is 25 ℃, and drying in a 45 ℃ temperature field after the water quenching is finished to obtain the AZ91 alloy semi-solid structure with fine grains.
The semi-solid state grain structure of the carbon nanotube-AZ 91 material prepared under the condition of the embodiment is fine, the average grain size is reduced by 46.8% compared with that of the matrix alloy without the Mg-Al-Zn-CNTs intermediate precast block under the same condition, and the average shape coefficient is correspondingly improved by 29.4%.
Example 2
A method for preparing a carbon nanotube material reinforced AZ91 alloy semi-solid slurry comprises the following steps:
(1) mixing a proper amount of carbon nanotubes with the outer diameter of 20-60nm, the length of 10-30 mu m and the purity of more than or equal to 99.5 percent with absolute ethyl alcohol in a beaker according to the proportion that 2.5g of the carbon nanotubes are mixed in per 100ml of the ethanol, and then putting the mixture into an ultrasonic instrument for ultrasonic dispersion treatment for 2 hours, wherein the ultrasonic power is 400W, and the frequency is 35 kHz; mixing magnesium powder, aluminum powder, zinc powder and anhydrous ethanol with the purity of more than or equal to 99.9 percent and the granularity of 100-200 meshes with 18g of magnesium powder, 1.8g of aluminum powder and 0.2g of zinc powder in a ceramic container according to 100ml of ethanol, and mechanically stirring for 2 hours at the stirring speed of 120 r/min; and then uniformly adding the mixed and dispersed magnesium powder, aluminum powder, zinc powder and ethanol mixed solution into the carbon nano tube ethanol dispersion solution after ultrasonic treatment, continuously performing ultrasonic dispersion with the power of 800W and the frequency of 40kHz, and simultaneously performing mechanical stirring at the stirring speed of 200r/min for 2 hours to obtain the mixed solution.
(2) And (2) placing the mixed solution prepared in the step (1) on a constant-temperature heating magnetic stirrer for magnetic stirring, wherein the heating temperature is 45 ℃, the magnetic stirring speed is 1500r/min, and in order to avoid the layering phenomenon of the mixed powder and the CNTs, the magnetic stirring is kept until the mixed solution is pasty, and then the mixed solution is placed in a vacuum drying oven for drying at 80 ℃.
(3) And putting the dried powder into a vacuum hot-pressing sintering furnace for sintering, wherein the sintering temperature is 400 ℃, the hot-pressing pressure is 40MPa, and the pressure maintaining time is 2h, so as to obtain the Mg-Al-Zn-CNTs intermediate precast block, wherein the CNTs accounts for 5% by mass, the Al accounts for 9% by mass, the Zn accounts for 1% by mass, and the balance is Mg, and cutting the precast block into small particles and coating the small particles with aluminum foil paper for later use.
(4) Cutting AZ91 matrix alloy (Al accounts for 9.0 wt%, Zn accounts for 1.0 wt%, and Mg accounts for the rest) into small pieces, placing into a dried graphite crucible, heating the crucible to 620 deg.C in a resistance furnace, and maintaining the temperature for 25 min; argon is required for protection in the process.
(5) After the alloy is completely melted, hexachloroethane accounting for 0.2 wt.% of the melt mass is added for refining and slagging off. Then pressing the Mg-Al-Zn-CNTs intermediate prefabricated block into the alloy melt by using a bell jar, wherein the addition amount of the CNTs accounts for 0.5 wt% of the total weight of the alloy melt. Applying high energy ultrasound while adding the pre-agglomerate particles: immersing an ultrasonic amplitude transformer probe into the alloy melt, and applying ultrasonic power of 2.1kW, frequency of 20kHz and time of 10 min; argon is filled in the whole ultrasonic process for protection.
(6) And (3) after the high-energy ultrasonic is applied, when the temperature of the melt is rapidly reduced to 520 ℃, applying secondary ultrasonic to the semi-solid slurry for 60s, wherein the rest ultrasonic parameters are the same as those in the step (5). And immediately carrying out water quenching on the slurry obtained by the secondary ultrasound after the secondary ultrasound is finished, wherein the water quenching temperature is 20 ℃, and drying in a temperature field of 40 ℃ after the water quenching is finished to obtain the AZ91 alloy semi-solid structure with fine grains.
The semi-solid state grain structure of the carbon nanotube-AZ 91 material prepared under the condition of the embodiment is fine, the average grain size is reduced by 30.4% compared with that of the matrix alloy without the Mg-Al-Zn-CNTs intermediate precast block under the same condition, and the average shape coefficient is correspondingly improved by 21.3%.
Example 3
A method for preparing a carbon nanotube material reinforced AZ91 alloy semi-solid slurry comprises the following steps:
(1) mixing a proper amount of carbon nanotubes with the outer diameter of 20-60nm, the length of 10-30 mu m and the purity of more than or equal to 99.5 percent with absolute ethyl alcohol in a beaker according to the proportion that every 100ml of the ethyl alcohol is mixed with 3.5g of the carbon nanotubes, and then putting the mixture into an ultrasonic instrument for ultrasonic dispersion treatment for 3 hours, wherein the ultrasonic power is 480W, and the frequency is 45 kHz; mixing magnesium powder, aluminum powder, zinc powder and anhydrous ethanol with the purity of more than or equal to 99.9 percent and the granularity of 100-200 meshes with 18g of magnesium powder, 1.8g of aluminum powder and 0.2g of zinc powder in a ceramic container according to 100ml of ethanol, and mechanically stirring for 3 hours at the stirring speed of 160 r/min; and then uniformly adding the mixed and dispersed magnesium powder, aluminum powder, zinc powder and ethanol mixed solution into the carbon nano tube ethanol dispersion solution after ultrasonic treatment, continuously performing ultrasonic dispersion with the power of 1200W and the frequency of 40kHz, and simultaneously performing mechanical stirring at the stirring speed of 250r/min for 3 hours to obtain the mixed solution.
(2) And (2) placing the mixed solution prepared in the step (1) on a constant-temperature heating magnetic stirrer for magnetic stirring, wherein the heating temperature is 50 ℃, the magnetic stirring speed is 2000r/min, and in order to avoid the layering phenomenon of the mixed powder and the CNTs, the magnetic stirring is kept until the mixed solution is pasty, and then the mixed solution is placed in a vacuum drying oven for drying at 80 ℃.
(3) And putting the dried powder into a vacuum hot-pressing sintering furnace for sintering, wherein the sintering temperature is 450 ℃, the hot-pressing pressure is 60MPa, and the pressure maintaining time is 3h, so as to obtain the Mg-Al-Zn-CNTs intermediate precast block, wherein the CNTs accounts for 10% by mass, the Al accounts for 9% by mass, the Zn accounts for 1% by mass, and the balance is Mg, and cutting the precast block into small particles and coating the small particles with aluminum foil paper for later use.
(4) Cutting AZ91 matrix alloy (Al accounts for 9.0 wt%, Zn accounts for 1.0 wt%, and Mg accounts for the rest) into small pieces, placing into a dried graphite crucible, placing the crucible into a resistance furnace, heating to 680 deg.C, and maintaining the temperature for 30 min; argon is required for protection in the process.
(5) After the alloy is completely melted, hexachloroethane accounting for 0.3 wt.% of the melt mass is added for refining and slagging off. Then pressing the Mg-Al-Zn-CNTs intermediate prefabricated block into the alloy melt by using a bell jar, wherein the addition amount of the CNTs accounts for 1.5 wt% of the total weight of the alloy melt. Applying high energy ultrasound while adding the pre-agglomerate particles: immersing an ultrasonic amplitude transformer probe into the alloy melt, and applying ultrasonic power of 3.2kW, frequency of 20kHz and time of 15 min; argon is filled in the whole ultrasonic process for protection.
(6) And (3) after the high-energy ultrasonic is applied, when the temperature of the melt is rapidly reduced to 580 ℃, applying secondary ultrasonic to the semi-solid slurry for 90s, wherein the rest ultrasonic parameters are the same as those in the step (5). And immediately carrying out water quenching on the slurry obtained by the secondary ultrasound after the secondary ultrasound is finished, wherein the water quenching temperature is 25 ℃, and drying in a 45 ℃ temperature field after the water quenching is finished to obtain the AZ91 alloy semi-solid structure with fine grains.
The semi-solid state grain structure of the carbon nanotube-AZ 91 material prepared under the condition of the embodiment is fine, the average grain size is reduced by 41.2% compared with that of the matrix alloy without the Mg-Al-Zn-CNTs intermediate precast block under the same condition, and the average shape coefficient is correspondingly improved by 25.6%.
The above-described embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications can be made by one skilled in the art, and any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for preparing a carbon nano material reinforced AZ91 alloy semi-solid slurry is characterized by comprising the following steps:
1) mixing the carbon nano tube with magnesium powder, aluminum powder and zinc powder by using ultrasound to obtain a mixed solution;
2) magnetically stirring the mixed solution under the action of a constant-temperature heating magnetic stirrer, drying the stirred mixed solution in a vacuum drying oven, sintering the dried powder in a vacuum hot-pressing sintering furnace to obtain a magnesium-aluminum-zinc-carbon nanotube intermediate precast block, cutting the precast block into small particles, and coating the small particles with aluminum foil paper for later use;
3) cutting AZ91 matrix alloy into small pieces, placing the small pieces into a graphite crucible, placing the crucible into a resistance furnace, heating to 620-680 ℃, preserving heat for 25-30min to completely melt the matrix alloy, then pressing the magnesium-aluminum-zinc-carbon nanotube intermediate precast block into an alloy melt by using a bell jar, and applying high-energy ultrasound while adding the precast block;
4) and 3) after the high-energy ultrasonic treatment is finished, quickly reducing the temperature of the melt to 520-580 ℃, preserving the temperature, applying secondary ultrasonic treatment for 60-90s, and immediately quenching the slurry obtained by the secondary ultrasonic treatment to obtain a semi-solid structure with fine grains.
2. The method for preparing the semi-solid slurry of the AZ91 alloy reinforced by the carbon nano material as claimed in claim 1, wherein the step 1) is that the carbon nano tube and absolute ethyl alcohol are mixed according to the proportion of 2.5-3.5g carbon nano tube per 100ml ethanol, and then the mixture is put into an ultrasonic instrument for ultrasonic dispersion treatment for 2-3h, the ultrasonic power is 400-480W, and the frequency is 35-45 kHz; mixing magnesium powder, aluminum powder, zinc powder and absolute ethyl alcohol according to the proportion that each 100ml of ethyl alcohol is mixed with 17-19g of magnesium powder, 1.7-1.9g of aluminum powder and 0.18-0.20g of zinc powder for 2-3h by mechanical stirring, wherein the stirring speed is 120-160 r/min; and then uniformly adding the mixed and dispersed magnesium powder, aluminum powder and zinc powder ethanol mixed solution into the carbon nano tube ethanol dispersion liquid after ultrasonic treatment, continuously performing ultrasonic dispersion, wherein the power is 800-1200W, the frequency is 35-45kHz, and simultaneously performing mechanical stirring, the stirring speed is 200-250r/min, and the duration is 2-3 h.
3. The method for preparing the carbon nanomaterial reinforced AZ91 alloy semisolid slurry according to claim 2, characterized in that the carbon nanotube has an outer diameter of 20-60nm, a length of 10-30 μm and a purity of more than or equal to 99.5%; the purity of the magnesium powder, the aluminum powder and the zinc powder is more than or equal to 99.9 percent, and the granularity is 100-200 meshes.
4. The method for preparing the semi-solid slurry of the AZ91 alloy reinforced by the carbon nano material as claimed in claim 1, wherein the magnetic stirring heating temperature in the step 2) is 45-55 ℃, and the stirring speed is 1500-;
in particular, to avoid the delamination of the mixed powder and the carbon nanotubes, the magnetic stirring is maintained until the mixture is pasty.
5. The method for preparing the semi-solid slurry of the AZ91 alloy reinforced by the carbon nano material as claimed in claim 1, wherein the sintering temperature in the step 2) is 400-450 ℃, the hot-pressing pressure is 40-60MPa, and the pressure holding time is 2-3 h;
particularly, the mass percent of the carbon nano tube in the intermediate precast block of the magnesium-aluminum-zinc carbon nano tube obtained after sintering is 5-10%, the mass percent of the aluminum powder is 8.5-9.5%, the mass percent of the zinc powder is 0.9-1.0%, and the balance is magnesium.
6. The method for preparing the semi-solid slurry of the AZ91 alloy reinforced by the carbon nano material as claimed in claim 1, wherein the AZ91 base alloy in the step 3) comprises the following elements in percentage by weight: 8.5 to 9.5 percent of aluminum, 0.9 to 1.0 percent of zinc and the balance of magnesium.
7. The method for preparing the semi-solid slurry of the AZ91 alloy reinforced by the carbon nano material as claimed in claim 1, wherein the step 3) of pressing the intermediate precast block of the Mg-Al-Zn-C nanotubes comprises the carbon nanotubes added in an amount of 0.5-1.5 wt% of the total amount of the alloy melt.
8. The method for preparing the semi-solid slurry of the AZ91 alloy reinforced by the carbon nano material as claimed in claim 1, wherein the high-energy ultrasonic operation method in step 3) is to immerse an ultrasonic horn probe into the alloy melt, and the ultrasonic power is 2.1-3.2kW, the frequency is 18-22kHz, and the time is 10-15 min; argon is filled in the whole ultrasonic process for protection.
9. The method for preparing the carbon nanomaterial reinforced AZ91 alloy semisolid slurry according to claim 1, wherein the parameters of the secondary ultrasound except time in the step 4) are consistent with those of the ultrasound in the step 3).
10. The method for preparing the AZ91 alloy semi-solid slurry reinforced by the carbon nano material according to claim 1, wherein the water quenching temperature in the step 4) is 20-30 ℃, and the semi-solid slurry is dried in a temperature field of 40-50 ℃ after water quenching.
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