CN101829777A - Process and equipment for preparing nanoparticle-reinforced metal matrix composite material - Google Patents

Process and equipment for preparing nanoparticle-reinforced metal matrix composite material Download PDF

Info

Publication number
CN101829777A
CN101829777A CN 201010126913 CN201010126913A CN101829777A CN 101829777 A CN101829777 A CN 101829777A CN 201010126913 CN201010126913 CN 201010126913 CN 201010126913 A CN201010126913 A CN 201010126913A CN 101829777 A CN101829777 A CN 101829777A
Authority
CN
China
Prior art keywords
nano particle
metal
powder
premixed powder
casting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN 201010126913
Other languages
Chinese (zh)
Inventor
丁刚
丁家伟
耿德英
强颖怀
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN 201010126913 priority Critical patent/CN101829777A/en
Publication of CN101829777A publication Critical patent/CN101829777A/en
Pending legal-status Critical Current

Links

Images

Abstract

The invention discloses a process and equipment for preparing a nanoparticle-reinforced metal matrix composite material. The process comprises the following steps of: mixing reinforcing nanoparticles with matrix metals and a grain growth inhibitor in a stirring ball mill together, and then loading the mixture into a steel pipe; casting the mixture together with the matrix metals in a water cooling crystallizer or casting and forming the mixture together with a molten metal in a casting mould; and performing quick solidification and crystallization after electromagnetic stirring and ultrasonic vibration to ensure that the two phase materials achieve complete metallurgical bonding, wherein because of the electromagnetic stirring and the ultrasonic vibration, the two phase materials are mixed more uniformly, and all properties of the composite material can be further improved. by using the process and the equipment, a production process is simple, the cost is low, the efficiency is high, the product performance is high, the process is easy to control, the external dimensions of products are not limited by the process, and large-sized nanoparticle-reinforced metal matrix composite materials can be manufactured.

Description

Nanoparticle-reinforced metal matrix composite material preparation technology and equipment
Technical field
The invention belongs to the metal-base composites technical field, relate to a kind of nano metal composite and preparation method thereof, particularly a kind of nanoparticle-reinforced metal matrix composite material preparation technology and equipment.
Background technology
The develop rapidly of modern science and technology, promoted the technological progress of new material greatly, along with continuing to bring out of new material preparation technology, new material constantly emerges, and the development of various nonmetallic materials (macromolecular material, ceramic material etc.) has reached unprecedented speed.The appearance of engineering plastics has proposed the slogan of " to the iron and steel challenge ", and the plastic-steel of the U.S. has reached more than 25% than in recent years; Ceramic material develop over nearly two, 30 years also very fast, the new varieties level is not poor, and special cermacis has been broken through the notion and the category of traditional ceramics in many aspects, the revolution variation on the ceramic development history occurred, someone even proposition, the mankind second Stone Age that be about to enter into.The situation that various materials develop rapidly makes the principal status of public economy of metal material be subjected to strong challenge, and the proportion of nonmetallic materials in total amount of material just progressively improves.Therefore in general, metal has reached the peak as material of main part in 20th century, and 21 century will be the epoch that metal material, macromolecular material, ceramic material and composite are run neck and neck.
Even to this day, in today that various materials continue to bring out, metal material still is a main body, and iron and steel is still occupied an leading position in metal material.At present, China's output of steel surpasses 500,000,000 tons, except that the minority steel grade, has satisfied the needs of China's economic construction substantially.According to statistics, in order to reach the production scale of above-mentioned steel, in decades, country successively drops into about more than 7,000 hundred million RMB.Iron and steel production engineering great, the heaviness of equipment, energy resource consumption surprising, environmental pollution seriously be on record.Scholarly forecast, by performance, the quality of present steel, in order to satisfy the demand that Chinese national economy is built, output of steel every year should be with the speed increase more than 5%.If well imagine. only write an article from the amount of steel, the whole system of present steel production in China, from mine → smelting → processing, from the input → energy → consumption → environmental pollution, complete must being doubled, such prospect is hardly imaginable.
In the face of above-mentioned situation, the metallargist is exploring a new approach, is promptly keeping making great efforts to make the performance of steel to double under the constant substantially condition of existing output of steel scale.If one ton of steel can be worked as two tons of usefulness, keeping under the constant substantially situation of existing production scale, the imbalance between supply and demand of steel just can be resolved.
In recent years, from improving the degree of purity of steel, aspects such as the matrix of refinement steel and emblem alloying improved performance, the quality of steel to the metallargist, and this is one of measure that realizes above-mentioned target.But the degree of purity that improves steel also is a system engineering.Degree of purity and steel scrap and molten steel quality, refractory quality, smelting process is all multifactor relevant with smelting technique level etc.Therefore the degree of purity that improves steel is not only an engineering that difficulty is very big, and will pay a high price.
For improving the intensity and the performance of metal material, reduce rolled steel dosage, in the later stage nineties 20th century, Japan, Korea S, China propose the ultra-fine grain steel development plan in succession, and significant more status is brought up in the effect of grain refinement.The state-run research institution that Japan official supports has carried out the basic research of grain refinement, inquires into the limit of grain refinement; A lot of enterprises then utilize the thought of grain refinement, carry out different brackets, satisfy the exploitation of the concrete material of different performance requirement, have developed the fine-grained steel of commercial scale different performance and purposes etc.Korea S is representative with POSCO, carried out the exploitation of high strength, corrosion-resistant, welding ferrous materials of new generation, and explored the approach of commercial Application.Meanwhile, application corresponding research has also been carried out in Europe.1999, European Coal steel alliance (ECSC) established the Ultrafine Grained Steel feasibility study project in 1 year by a definite date, had started the research project of " utilizing the innovation deformation process to make ultra-fine grain steel " by name subsequently again in calendar year 2001.The purpose of this project is the deformation process of research steel, is making the ferrous materials of new generation that has good mechanics and serviceability, has good response in following process on the commercial scale.This project comprises four working cells, relates separately to several important ferrous materials such as surperficial ultra-fine crystalline substance, low-carbon superfine crystalline substance, middle carbon ultrafine crystalline substance, high carbon ultrafine crystalline substance.This project makes substantial progress at present.China will have started national great basic research planned project " the great basic research of ferrous materials of new generation " the end of the year 1998, under the thought guidance of " strive for that ferrous materials homogenizes, pureization, grain refining ", 400,800, item research such as 1500Mpa level super-steel has obtained major progress, and take the lead in having carried out in the world suitability for industrialized production and application, cause international attention, indicate that China's ferrous materials research has entered a new stage.
But at present the domestic and international ultra-fine grain steel of developing mainly adopts heavy reduction rolling distortion, high strain rate, low deformation temperature, rapid thermal cycles, complicated process combination and to the accurate control of technical process etc.These require how much to have exceeded steel mill's existing equipment ability and production capacity, and production cost is significantly increased, thereby become one of subject matter of restriction ultra-fine grain steel suitability for industrialized production, in addition, ultra-fine grain steel also exists structure stability and two stubborn problems of plastic stability, thereby present stage overwhelming majority nanometers and sub-micron steel also only limit to laboratory research.In addition, the ultra-fine grain steel material of manufacturing both at home and abroad is only applicable to sheet material, wire rod and the tubing etc. of general applications under the low temperature at present, and for instrument and die industry, the metal wear resistant material industry is still inapplicable, and its application is restricted.
Modern industry development and technological progress have proposed new requirement to traditional structural material.The ferrous materials of particularly big, applied range to use amount, people wish to utilize minimum resource, minimum cost is manufactured out and is had the very excellent advanced ferrous materials of every combination property, to satisfy production development and the scientific and technological progress special demands to new material.
Particles reiforced metal-base composition has higher specific stiffness, specific modulus, low thermal coefficient of expansion and low cost owing to it and has obtained to use widely in precision and optical instrument.Because there is size problem bigger than normal (often all tens more than the micron even of several microns) in the enhancing particle that uses in the research in the past, brings certain limitation for the amplitude that strengthens.
Nano material is the important research and development direction of in the nano science.In recent years, along with the rise of nano science, nano material has caused widely in many scientific domains to be paid attention to, and becomes the focus of material science research.So-called nano material is by the molecular solid material of the nanoparticle of nanometer scale, the size of nano particle generally is no more than 100nm, when the particle chi directly enters nanometer scale 1~100nm, because the ratio of the surface atom of nano particle and volume total atom number reduces and sharply increases with grain size, makes it demonstrate 4 basic effects: strong quantum size effect, surface and interfacial effect, bulk effect and macro quanta tunnel effect.These characteristics make nano material present many peculiar character and have some excellent performance, as high thermal expansion coefficient, high specific heat capacity, low melting point, peculiar magnetic, extremely strong absorbing property etc.Nanoparticle is small-sized, and the surface atom number of nano particle and the ratio of its total atom number reduce and sharply increase with grain size, so nano material has high density of defects, high excess energy, big specific area and interfacial excess volume.Therefore nano material also has many special performances, as high elastic modelling quantity, stronger toughness, high strength, superpower wearability, self lubricity and superplasticity etc.Because the specific performance of nano material, thereby have extensive and important application prospects.
Metal-base nanometer composite material (Metal matrix nanocom-posites, MMNC s) be to be matrix with metal and alloy, the composite that combines with one or more metals or nonmetal nanoscale wild phase.A particulate reinforced metal-based nano composite material is exactly that nano particle is fused in metallic matrix, and nano particle and metallic matrix are combined closely, and makes it to have long-term stability.And after compound, also can demonstrate bigger advantage at aspects such as optics, mechanical performances.Nano material and metallic matrix are carried out organically compound, the effect of utilizing the interaction of nano material and matrix to produce can also realize both mutual supplement with each other's advantages, the new functional material of exploitation excellent performance.Experiment shows: add nonmetal nano powder in steel, can roll up heterogeneous core external in the molten steel, make the field trash disperseization in the steel, reduce or eliminate the illeffects of field trash, so just can reduce the requirement to the steel degree of purity.Add the also matrix of possible refinement steel of nonmetal nano powder in the steel, the existence of a large amount of heterogeneous particles can play dispersion-strengtherning in steel.Therefore, in steel, add the performance that nonmetal nano powder can improve steel greatly, improve the quality of steel.Have that mechanical property is good, shear strength is high, operating temperature is higher, wear-resistant, conductive and heat-conductive good, non-hygroscopic, not air-breathing, dimensionally stable, advantage such as aging, so with its excellent performance applications in automation, space flight, aviation and high-tech sectors such as auto industry, advanced manufacturing industry.
Because above-mentioned every premium properties that metal-base nanometer composite material had and the extensive market prospects that is had, R and D are energetically all being carried out to it in countries in the world, and have developed various preparation technologies.At present, the method of being developed for preparing metal-base nanometer composite material mainly contains mechanical alloying method (Mechanical alloying both at home and abroad, MA), melt spinning (Meltspun, MS) method, powder metallurgic method (Powder metallurgy, PM), machinery brings out synthetic (the Self-propagatinghigh-temperature synthesis of self propagating high temperature, SHS) reaction method, vacuum evaporation inert gases agglomeration and vacuum add in-place platen press (Inert gas con-densation method combined with vacuum co-evaporation andin-situ compaction, but all there is following shortcoming in above-mentioned several preparation method ICVCSC) etc.:
1) mechanical alloying method technology simple, strengthen body and be evenly distributed, strengthen that body volume fraction scope is big, quality of item is better, output is high, can prepare high-melting point metal and alloy nano-material.Shortcoming is: easily introduce in preparation process that impurity, crystallite dimension are inhomogeneous, ball milling and oxidation meeting bring pollution.
2) melt spinning method technology is simple, equipment investment is few, production cost is lower.Shortcoming is: strengthen body volume fraction limited (generally being no more than 20%), have the possibility of interfacial reaction, enhancing body distribution difficulty to reach homogenising, pore is arranged, need secondary operations.
3) there is not interfacial reaction basically in powder metallurgic method, steady quality, and strengthening the body volume fraction can be higher, strengthens body and is evenly distributed.Shortcoming is: the possibility that process is many, manufacturing cycle is long, cost is high, reduce cost is little.
4) vacuum evaporation inert gases agglomeration and vacuum add in-place platen press are applied widely, the enhancing body is evenly distributed, quality of item is good.Shortcoming is: process equipment costliness, output are extremely low, the manufacturing large parts is had any problem, and is imappropriate as the refrigerating work procedure arrangement, can produce tangible interfacial reaction, and manufacturing cycle is longer.
5) machinery brings out self propagating high temperature building-up reactions method process simply, does not need complex apparatus, product purity height, can obtain complicated phase and metastable phasing.Shortcoming is: be difficult for obtaining high product density, can not strictly control course of reaction and properties of product.
6) reaction in-situ composite algorithm cost lower, strengthen that body is evenly distributed, essentially no interfacial reaction, can use traditional metal melting Casting Equipment, process cycle is shorter.Shortcoming is: technical process is strict, difficult the grasp, and the composition and the volume fraction of wild phase are wayward.
7) amorphous alloy crystallization method cost is low, output is big, interface cleanness is fine and close, pore-free crack, grain size change easy to control in the sample.Shortcoming is the alloy system that only is applicable to that amorphous formation ability is stronger.
They differ from one another above-mentioned various preparation technology, the scope of application is not quite similar, the prepared various metal-base nanometer composite materials that go out are compared all with traditional material on performance and are greatly improved, and are playing huge impetus aspect development conventional composite materials and the development of new composite.But all there is self limitation in these technologies of preparing, and wherein great majority are because apparatus expensive, complex process and be difficult to control and still concentrate on the laboratory research stage.
For realizing the manufacturing of nano particle reinforced composite, all carried out a large amount of research and developments both at home and abroad, constantly worked out new preparation technology, making on the non-ferrous metal nano particle reinforced composite technology, Chinese invention patent ZL200510011568.4 discloses a kind of nano particle and has strengthened high-toughness casting magnesium alloy and preparation moulding process thereof, the magnesium alloy substrate component of this technology manufacturing and weight percent content are 5.0~10.0%Al, 0.1~1.0%Zn, 0.05~0.5%Mn, constraint element Si≤0.05%, Fe≤0.005%, Cu≤0.01%, Ni≤0.002%, all the other are magnesium.The particle that uses is the SiC nano particle, and particle diameter is less than 100nm, and addition is 0.1~3.0% of an alloy volume content.The SiC nano particle will carry out preliminary treatment before adding, and its pretreating process is:
1, import an amount of straight alcohol of analyzing in container, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC nano particle and ethanol is 1g/10ml~1g/3ml;
2, the poly-vinyl alcohol solution that will account for said mixture volume 1/50~1/10 joins in the mixture of SiC nano particle and ethanol, fully stirs, and mixes;
3, the said mixture that will contain the SiC nano particle places baking oven dry, and baking temperature is 80~95 ℃.
The preparation moulding process that nano particle strengthens cast magnesium alloy is:
1, magnesium alloy materials is joined in the dry crucible of brushing coating,, use solvent or high-purity argon gas to be protected, dissolve the back solution temperature and remain on 680~720 ℃ for preventing magnesium alloy from oxidative combustion in the fusion process;
2, control magnesium alloy solution temperature to 650~700 ℃ (being higher than 60~80 ℃ of liquid magnesium alloy phase lines) or 5850~610 ℃ (being lower than 50~30 ℃ of liquid magnesium alloy phase lines), remove surface scum, the SiC nano particle that passes through liquor treating process that accounts for magnesium alloy volume 0.1~3.0 is added in the alloy liquid, be pressed under the liquid level and stir, mixing time 3~10 minutes, 10000~2000 rev/mins of agitator speeds;
3, after the refining degasification, the control pouring temperature is 650~700 ℃ and removes out surface scum, obtains the high-toughness casting Mg alloy castings that nano particle strengthens by gravity mold casting or die casting.This technology by adding the nano reinforcement particle, improves the obdurability of cast magnesium alloy on the basis of traditional cast magnesium alloy; By nano particle is carried out preliminary treatment, increase the wetability of particle and magnesium alloy; By controlling suitable liquid magnesium alloy temperature and mechanical agitation technology, nano particle is evenly distributed in liquid magnesium alloy.But because the employed SiC nano particle of this technology just can decompose at 800 ℃, and rising along with temperature, decompose and become more violent, and the SiC nano particle directly adds in the alloy, can't solve the reunion of nano particle, it is few to strengthen grain amount, uses mechanical agitation, therefore this technology is only applicable to non-ferrous metal, and inapplicable and high-temperature metal.Chinese invention patent ZL200510127307.9 discloses a kind of composite material with nano silicon carbide granulate strengthening aluminium base and preparation method, and this method is to adopt nano silicon carbide granulate and aluminium powder to make as raw material; Wherein the volume of nano silicon carbide granulate accounts for 0.5~20% of raw material volume, and the volume of aluminium powder accounts for 80~99.5% of raw material volume.Its preparation method is: 1, raw material mix is dropped into to vacuumize behind the sealing ball grinder and charge into argon gas again and carry out repeatedly 2~10 times; 2, high-energy ball milling; 3, hot pressed sintering; 4, hot extrusion promptly obtains composite material with nano silicon carbide granulate strengthening aluminium base.Preparation technology of the present invention is simple, and cost is low, and nano silicon carbide granulate is evenly distributed in aluminum substrate, powder process rate height, and also the mechanical property of composite is significantly increased.It has solved in the method for traditional preparation process particle enhanced aluminum-based composite material nanoscale and strengthens particle and can not be uniformly distributed in the aluminum substrate, and preparation technology is numerous and diverse, the problem that cost is high.But because this process using aluminium powder is made raw material, and hot extrusion again behind the employing powder metallurgical technique hot pressed sintering, because complex process, the cost height, equipment investment is big, and technical difficulty is big, is only applicable to low-temperature metal equally.
For realizing the production of nano alloyed steel, make it on mold materials and high-abrasive material field, realize using, in recent years, carried out a large amount of research both at home and abroad, developed some novel preparation process.Chinese invention patent ZL200610046063.6 discloses a kind of high-strength abrasion-proof thermostable nano alloyed steel material and preparation method thereof, and this invention is for to produce nano alloyed steel according to smelting process.The chemical composition of this material (by weight percentage) is: tungsten (W) 0.06~6.0%, manganese (Mn) 0.6~3.0%, vanadium (V) 0.06~6.0%, niobium (Nb) 0.22~4.0%, molybdenum (Mo) 0.0~7.0, carbon (C) 0.5~4.0, chromium (Cr) 1.0~8.0, other elements 0.1~3.0, all the other are iron (Fe).Used main equipment is a vaccum sensitive stove.Technological process mainly comprises the raw material preparation, goes into three process such as stove smelting, casting.Raw material adopts the pig iron or straight carbon steel, and alloy adopts the ferroalloy of above-mentioned institute formulated component element.Production technology is for to carry out vacuum metling with above-mentioned various raw materials in vaccum sensitive stove, when temperature reaches 1620~1750 ℃, feed stock for blast furnace all melt and composition evenly after, smelt tapping, the ingot casting moulding.The steel ingot of being produced is through checking 80% grain size less than 50nm.It is simple that this technology has production technology, low cost and other advantages.But this technology only is to utilize at present the microalloy crystal grain thinning of institute's extensive use both at home and abroad, suppress by alloying element that the grain growth principle of steel is prepared, that utilizes especially that niobium (Nb) had in the metallic crystal process can suppress crystallization again, the performance of the recrystallization temperature of raising material is made, the steel ingot of manufacturing still belongs to the fine-grained steel scope, can not be called nano alloyed steel.And this technology is the mode that combines by high cleanliness molten metal and microalloying, at the certain forming core particle of the inner formation of steel, because these particles are almost separated out in the subsolidus austenite, so the forming core to austenite itself does not have the forming core central role, promptly to the not effect of refinement as cast condition crystal grain, can only play the pinning inhibition to the grain growth in the later stage hot procedure, thereby exist degree of purity to require high to molten steel, the quality stability of the steel alloy of being produced is poor, lack the pinning of the second phase particle to crystal grain, difficult quality guarantee, process controllability is poor, defectives such as production process control is had relatively high expectations, and the control difficulty is big.
At present, the nano composite material that countries in the world are developed is confined in the polymeric material more, and the technology that adopts nano powder modified integral metal material aspect to be done is fewer, this is thereby for metal material matrix, does not still have good especially process for dispersing the nano-powder of aggregating state is disperseed.The preparation of metal-base nanometer composite material is more complicated and much more difficult than polymer based nanocomposites, and its main difficult point is: the surface that the surface that (1) is huge produced can make and have extremely strong agglomeration between the object with nano-scale and make particle size become big.How these nano unit bodies can be dispersed in and constitute composite in the metallic matrix, making it not reunite and keeping the single body of nano-scale is the matter of utmost importance that synthetic metal-base nanometer composite material must solve to give full play to its nano effect.Yet still not having highly effective process for dispersing up to now disperses in metallic matrix the nano-powder of aggregating state; (2) carry out good compoundly for guaranteeing to strengthen to be on good terms with nanometer, parent metal must have enough flowabilities, mouldability.But parent metal generally all has high melt point, and therefore, harmful chemical reaction such as serious interfacial reaction, oxidation will certainly take place when high temperature prepares metal-base nanometer composite material.The another key point how strict control interfacial reaction is a preparation high-performance metal based nano composite material; (3) metallic matrix and nanometer second mutually between wellability poor, even soak into, must manage nanoparticle is carried out suitable surface treatment to improve the wellability with matrix; (4) process of setting and interface problem.Process of setting becomes complicated more owing to the existence that strengthens body makes the process of setting of parent metal, existing metal freezing is obviously theoretical and inapplicable, strengthen the adding of body, the thermodynamics and kinetics process of temperature field in its process of setting and concentration field, crystal growth all can change.Because general process of setting all is in nonequilibrium condition.Therefore flow behavior, the reallocation rule of solute and the tissue morphology of solidifying body of fluid also have corresponding variation, and this all will produce significantly influence to the performance of metal-base composites.Because existing above-mentioned many key factors, seriously restricting the Application and Development of metal-base nanometer composite material, causing at present, the preparation technology of domestic and international some metal-base nanometer composite materials of developing still rests on the experimental stage, make present research still belong to vacancy, at least also do not form product for Metal Substrate one nano composite material.
At present, the application of nano material also is in beginning and exploratory stage, though people prepare multi-purpose nano material with various method, the preparation expense is too high, some characteristics such as yield poorly but exist, hamper its application in field in every respect, the particularly application of three-dimensional dimension nano material and wait further exploitation.Yet as a kind of new material of having very much a development prospect, nanometer technology demonstrates application prospect in the ascendant.Therefore, it is simple that research and development have preparation technology, nanoparticle-reinforced metal matrix composite material preparation technology that production cost is low and equipment are to realizing substantial nano metal composite in industrial application, and enormous function has great scientific meaning and economic implications to make metal-base nanometer composite material bring into play more with its excellent characteristic in fields such as new material, metallurgy, automation and Aero-Space.
Summary of the invention
The objective of the invention is to solve deficiency of the prior art, providing a kind of adds nano particle in steel or the non-ferrous metal matrix to, nano particle is evenly distributed in parent metal, realize the effectively compound of nano particle and metal material, the unusual characteristic of performance nano material, thereby prepare the excellent more novel high-performance nano particle of performance and strengthen ultra-fine grain steel and nonferrous materials, it is simple that acquisition has preparation technology, production cost is low, the nanoparticle-reinforced metal matrix composite material preparation technology and the equipment of good product performance.
The equipment scheme that solves its technical problem is: this equipment is synthetic by nano particle, diffusion, mixing apparatus and two systems of casting equipment form; Wherein nano particle is synthetic, diffusion, mixing apparatus adopts the high-energy stirring ball mill standard device, casting equipment is made up of fusion cast process and moulding by casting device systems, fusion cast process equipment is by the electrode holde on the column that has lowering or hoisting gear that is installed on the workbench, consutrode or non-consumable electrode are installed on electrode holde, and be connected with cathode power supply, vertical place with consutrode is equipped with water mold below electrode holde, the water mold outside is equipped with magnetic stirrer, ultrasonic vibrator is equipped with in top or bottom at water mold, both sides, top in water mold are separately installed with the high energy pulse electrode, be connected with end water tank and end water tank lowering or hoisting gear in the bottom of water mold, on end water tank, be connected with negative power supply, and form electric loop with the cathode power supply on the electrode holde, outside at the said equipment is equipped with seal box, is externally connected to inert gas jar and vavuum pump and control valve equipment at seal box; Moulding by casting equipment is by the casting mold that is installed on the bottom board, outside at casting mold is equipped with magnetic stirrer, ultrasonic vibrator is equipped with in top or bottom at casting mold, both sides, top in casting mold are separately installed with the high energy pulse electrode, next door at bottom board is equipped with feed trumpet, and there is the cast runner at the center of feed trumpet and is connected with the hole of casting mold bottom, is connected with pouring ladle on the top of feed trumpet, in pouring ladle, fill parent metal liquid, stopper equipment is installed in pouring ladle forms.
Water mold comprises water tank and is connected with the cooling water inlet in the bottom of water tank, and the top is connected with coolant outlet, and the center of water tank is a clear opening, and power supply is a low-voltage and high-current, and its voltage and current all can be adjusted on a large scale.
Mold material adopts ferrous metal or refractory material manufacturing.
Solving the process technology scheme that its technical problem adopts is:
1, the preparation of nano-crystalline granule liquid mixed powder: at first will from carbide, nitride, boride, oxide nano particles, CNT one group element, select wherein one or more elements and certain content from Cr 3C 2, VC, TaC, ZrC, NbC, HfC, TiB, TiN, NbN, AlN, VN, Ca, Al, Ba, Mg, N and rare earth oxide a group element in be placed on after selecting the parent metal powder of the grain inhibitor of one or more elements wherein and corresponding composition to mix simultaneously and carry out high-energy ball milling in the high-energy stirring ball mill machine, be prepared into the premixed powder that contains nano-crystalline granule;
But or, add Al powder, Cu powder, the Fe of synthesizing carbide, nitride, the carbon dust of boride required dosage, nitrogenous object and doses with the forming element of Ti, V, Zr, Nb, B, W, Mo strong carbide, strong nitride, boride forming element and other original position synthesizing carbide, nitride, boride 2O 3Select wherein one or more elements and the parent metal powder of corresponding composition to be placed on after mixing simultaneously and to carry out high-energy ball milling in the high-energy stirring ball mill machine in powder one group element, bring out the premixed powder of self propagating high temperature nano-crystalline granule of original position synthetic 70~90% in ball mill by machinery;
For preventing the powder oxidation, adopt inert gas shielding in the mechanical milling process, the premixed powder that contains nano particle that ball milling is good seals in the thin-wall low carbon steel steel pipe of packing into and vacuumizes after Passivation Treatment; Or the premixed powder that contains nano particle that ball milling is good carries out briquet, oven dry on forcing press; The premixed powder thin-wall low carbon steel steel pipe that nano particle maybe will be housed is rolling or be drawn into the belt carcass alloy wire that has nano particle premixed powder on milling train or drawbench;
2, the melting of parent metal: start the Metal Melting furnace, various alloying elements by required parent metal composition preparation respective numbers, and in the parent metal alloying component, add metal grain refinement and the crystallization inhibitor again of V, 0.1~2% the Ti of 0.1~3% Nb and 0.1~5%, wherein V and Ti can only add that wherein any or two kinds add simultaneously or two kinds do not add, with melted parent metal liquid pour in the metal liquid tundish on the workbench;
3, casting: will pour in the tundish on the workbench melted parent metal liquid be cast into consutrode, or directly use it for casting-up; The good consutrode of cast is installed on the electrode holde, and the thin-wall low carbon steel steel pipe that simultaneously one or more is equipped with nano particle premixed powder is welded on the consutrode;
Or one or more thin-wall low carbon steel steel pipe or one or more belt carcass alloy wire that has nano particle premixed powder that nano particle premixed powder is housed is installed on the electrode holde;
Or, be fixed on the center of casting mold, or in casting mold, fix along even distribution the in the center of casting mold according to certain spacing distance with one or more thin-wall low carbon steel steel pipe or nano particle premixed powder pressing block that nano particle premixed powder is housed;
The liquid slag of required composition poured into form slag bath in the water mold, start vavuum pump, protective cover is evacuated or opens the inert gas pump, in protective cover, charge into inert protective gas, start the consutrode power supply, the consutrode of the thin-wall low carbon steel sealed steel pipe of nano particle premixed powder is housed inserts and carry out founding in the liquid slag bath being installed in welding on the electrode holde, thin-wall low carbon steel sealed steel pipe and consutrode that nano particle premixed powder is housed are melted in slag bath simultaneously;
Or will be inserted into continuously in the slag bath with certain controlled velocity through the belt carcass alloy wire that has nano particle premixed powder rolling or that drawing is made, melt simultaneously with the parent metal consutrode;
To be installed in maybe that on the electrode holde one or more is equipped with the thin-wall low carbon steel steel pipe of nano particle premixed powder or one or more has the belt carcass alloy wire of nano particle premixed powder, insert and carry out founding in the liquid slag bath, the belt carcass alloy wire that makes the thin-wall low carbon steel steel pipe that nano particle premixed powder is housed or have a nano particle premixed powder melts in slag bath, the nanometer that contains that fusing is good strengthens the composition metal drop of particle through after the synthetic wash heat refining of slag, drop in the metal bath, start magnetic stirrer and ultrasonic vibrator, two phase materials are mixed in water mold, and under the quick cooling of water mold rapid solidification and crystalline forming, promptly obtain contain the metal-base composites that nano particle strengthen identical on the end water tank with the water mold cavity shape, start the high energy pulse power supply, carry out thinning processing by high energy pulse electrode pair metal-base composites crystalline structure, nanoparticle-reinforced metal matrix composite material as the big length of need production, start the stripping device, it is moved down, production is carried out continuously, and produced the metal-base composites that nano particle strengthens that contains of Len req;
Maybe will smelt good parent metal liquid directly is poured in the casting mold that fixes one or more thin-wall low carbon steel sealed steel pipe that nano particle premixed powder is housed or nano particle premixed powder pressing block as requested;
Or in casting process, will join in the parent metal liquid of being poured into a mould continuously with certain controlled velocity through the belt carcass alloy wire that has nano particle premixed powder rolling or that drawing is made;
Start magnetic stirrer and ultrasonic vibrator, two phase materials are mixed in casting mold, and in casting mold, solidify and crystalline forming, be cast as contain the metal-base composites that nano particle strengthen identical with the casting mold cavity shape, start the high energy pulse power supply, carry out thinning processing by high energy pulse electrode pair composite crystalline structure, both can obtain having the nanoparticle-reinforced metal matrix composite material of well-crystallized tissue.
Slag in the water mold is the slag system that urmaterie or multi-component are formed, and composition is by CaFe 2One urmaterie or by CaFe 2With Al 2O 3Or MgO, MnO, CaO, TiO 2, the slag system that is no less than binary substance formed of one or more elements of selecting among the RE, RExOy one group element;
Matrix material in the metal-base composites is ferrous metal, non-ferrous metal, an intermetallic compound any composition and that can include rare earth alloy; The mass fraction that nanometer strengthens particle is 0.1%~60% of a composite weight; The mass fraction of grain inhibitor be composite weight 0.1%~2% or for the premixed powder body weight 0.1%~5%; The thin-wall low carbon steel steel pipe sizes of loading nano particle premixed powder is φ 3mm~φ 20mm, be of a size of φ 3mm~φ 10mm through the belt carcass alloy wire that has nano particle premixed powder rolling or that drawing is made, the mass fraction of parent metal powder is 1%~60% of a premixed powder body weight.
Beneficial effect
Owing to adopted such scheme, in the present invention owing to adopt high-energy stirring ball mill mechanical alloy metallization processes, nano particle is carried out the high energy mechanical stirring ball-milling jointly with a certain amount of parent metal powder and grain inhibitor and mix, thereby nano particle and parent metal powder and grain inhibitor a large amount of collision phenomenon in stirring ball-milling and mixed process is occurred between ball powder and the abrading-ball, serious plastic deformation takes place in captive powder under the collision effect, make powder seam and fracture repeatedly.Through " miniature forging " effect, element powders is realized evenly mixing, and crystal particle scale reaches nanoscale, and specific area increases greatly.Owing to increased the contact area of reaction, shortened diffusion length, can fully spread between element powders, diffusion rate reduces the restriction of reaction power, and crystal grain produces high density of defects, laid in a large amount of distortional strain energies, reacting driving force is increased greatly, can make the lower alloy powder generation counterdiffusion of immiscible alloying element or solubility, formation has the over-saturation solid solution and the amorphous phase of certain solubility or big solubility, thereby make powder in mixed process, realize nanometer and synthesis of nano compound, realize the even distribution of nano particle in parent metal and grain inhibitor.Because in mixed process, add a certain amount of parent metal powder and grain inhibitor, thereby solved the reunion and the dispersion technology difficult problem of nano particle, and the production efficiency height, preparation cost is low.
Because the nanocrystal activity is very big, in casting process, very easily grow up, therefore, adopt and in nanometer premixed powder, add grain inhibitor, from suppressing further growing up of crystal grain to a certain extent.Simultaneously, long and the crystallization again for the crystal grain that solves parent metal, in parent metal, adopt to add grain refinement and crystallization inhibitor again, make it in the parent metal crystallization process, form certain forming core particle in metal inside, because these particles are almost separated out in the subsolidus austenite, thereby can carry out refinement to the crystal grain of parent metal and suppress crystallization again, improve the recrystallization temperature of material, grain growth in the later stage hot procedure is played the pinning inhibition, improve the serviceability temperature of metal material.Adding by nano particle, refinement the grain structure of metal, realized the pinning effect of the second phase ultrafine particle to metal grain, the structure stability and the plastic stability of metal material have been improved, can be applicable to instrument, die industry and metal wear resistant material industry, enlarged the range of application of metallic composite.
Because the poor lubricity of nano particle and metal bath and skin effect that itself has and high activity, the normal gathering of nano particle that joins in the melt is agglomerating, it is very difficult adopting traditional mechanical agitation to make its even dispersion in melt, high-energy ultrasound can produce periodic stress and acoustic pressure in the melt medium, and can cause many nonlinear effects thus, as acoustic cavitation and acoustic streaming effect etc.These effects of high-energy ultrasonic can significantly be improved the wetability of subparticle and melt in the utmost point in the short time (tens of seconds), and force its evenly dispersion in melt.When metal bath solidifies in rotating excitation field, its inner meeting produces eddy current, the interaction meeting in this eddy current and magnetic field produces a kind of moment of torsion in metal inside, formation is to the tangential shearing force of metal bath, when this shearing force arrives certain value greatly, i.e. when shear strain reaches the cataclasm value of dendrite, just can effectively suppress or cataclasm dendrite of radially growing up, also destroyed simultaneously the orderly arrangement of atomic group in the melt, suppressed the reunion of atomic group, made melt form more forming core barycenter.Because the existence of tangential velocity then produces centrifugal force to the unit melt, the existence of this centrifugal force constantly makes melt be in abducent trend simultaneously.Like this, one side is to produce " relaxation force " between each stream group, makes melt be difficult to form big elementide, and the while also breaks or cuts off established dendrite, even also have more tiny forming core barycenter in the melt.On the other hand, because being in outermost metal bath is subjected to stopping of crystallizer or casting mold when centrifugal, cause recoil, inwardly motion, the internal layer melt follows outside impact closely, extruding is constantly washed away melt so layer by layer, mixes, and thisly wash away mixing, strengthen melt " eddy currentization " simultaneously, make the viscous friction drag that produces between each stream group repeatedly, thus help suppressing and cataclasm radially and horizontal dendrite.Moreover, because turbulent flow in " relaxing " between each stream group and the whole melt has increased the melt thermal diffusivity, can play the overheated effect of quick dissipation.Particularly turbulent flow can cause temperature fluctuation, if the amplitude of fluctuation is bigger, then the average speed of growth of crystal grain reduces, and periodic remelting phenomenon can occur before solid liquid interface is moved.The rising of the thermal pulse that the liquid turbulent flow in dendrite end is caused can make dendritic arm fusing, and the arm that will break brings in the liquid state and go, and make crystal grain multiplication in the liquid, and be tending towards even distribution, thereby crystal grain thinning promotes column crystal and changes to equiax crystal.The heat radiation of melt has been quickened in the strong agitation effect of rotating excitation field, has quickened solidifying of alloy, thereby the crystallization temperature interval is obviously dwindled.Because the above-mentioned performance that high-energy ultrasonic and electromagnetic agitation are had, therefore, the present invention handles high-energy ultrasonic with electromagnetic agitation and mutually combines, thereby makes in the nano particle cast form process, has realized that the even dispersion of nano particle in melt distributes.For preventing in the casting process, the grain growth of nano particle, the present invention adopts water mold that melt is carried out quick crystallisation by cooling, can control growing up of nanocrystal and melt crystal grain effectively, make prepared composite have high density and thin crystalline structure, thus realized nanoparticle-reinforced metal matrix composite material preparation.
For improving the degree of purity of composite, in the present invention, adopt the electroslag refining technology that melt is carried out refining, thereby obtained to have the nanoparticle-reinforced metal matrix composite material of high cleanliness.
When using the present invention to produce nanoparticle-reinforced metal matrix composite material, have that production technology is simple, production efficiency is high, production cost is low, properties of product and quality be good, technology is easy to control.Through the refining of secondary high temperature, the nanometer that adds strengthens the body material surface and produces fusion, makes two phase materials reach complete metallurgical binding in high temperature sludge liquid for nanometer enhancing body that adds and parent metal mixed liquor.The appearance and size of product is not subjected to process limitation, can make large-sized nanoparticle-reinforced metal matrix composite material, and prepared composite has good heat-resistant deforming ability, in follow-up processing, can adopt various heat processing techniques to carry out.
Adopt technology of the present invention, can select the nano particle of various parent metals and various performances to carry out combination manufacturing flexibly, thereby satisfy the requirement of various applications according to different applying working conditions.The prepared nanoparticle-reinforced metal matrix composite material of the present invention can be applied to each field such as industry, agricultural, national defence and aerospace, have applied widely, serviceability is good, the cost performance height, economic benefit and social benefit, obvious environment benefit have good application and promotion prospect.
Description of drawings
Fig. 1 is the structure chart of first embodiment of the invention.
Fig. 2 is the structure chart of second embodiment of the invention.
Fig. 3 is the structure chart of third embodiment of the invention.
Fig. 4 is the structure chart of fourth embodiment of the invention.
The specific embodiment
Embodiment 1: in Fig. 1, equipment is synthetic by nano particle, diffusion, two systems of mixing apparatus and casting equipment form, wherein nano particle is synthetic, diffusion, mixing apparatus adopts high-energy stirring ball mill standard device, casting equipment cathode power supply 1, electrode holde 2, consutrode 3, the thin-wall low carbon steel sealed steel pipe 4 of premixed nano-powder 16 is housed or has the belt carcass alloy wire 4 of nano particle premixed powder, slag bath 5, outlet pipe 6, contain the metal-base composites 7 that nano particle strengthens, magnetic stirrer 8, end water tank 9, negative power supply 10, high energy pulse electrode 11, high energy pulse power supply 12, metal bath 13, water mold 14, water inlet pipe 15, nano particle premixed powder 16, ultrasonic vibrator 17, stripping device 18 is formed.
1, the preparation of nano-crystalline granule liquid mixed powder: at first will be from carbide, nitride, boride, oxide nano particles, select in CNT one group element wherein one or more elements and certain content from Cr3C2, VC, TaC, ZrC, NbC, HfC, TiB, TiN, NbN, AlN, VN, Ca, Al, Ba, Mg, be placed on after the parent metal powder of the grain inhibitor of selection one or more elements wherein and corresponding composition mixes simultaneously in one group element of N and rare earth oxide and carry out high-energy ball milling in the high-energy stirring ball mill machine, be prepared into the premixed powder 16 that contains nano-crystalline granule; Or with Ti, V, Zr, Nb, B, W, the Mo strong carbide, strong nitride, but boride forming element and other original position synthesizing carbide, nitride, the forming element of boride, add synthesizing carbide, nitride, the carbon dust of boride required dosage, the Al powder of nitrogenous object and doses, the Cu powder, select wherein one or more elements and the parent metal powder of corresponding composition to be placed on after mixing simultaneously and to carry out high-energy ball milling in the high-energy stirring ball mill machine in Fe2O3 powder one group element, bring out the premixed powder 16 of self propagating high temperature nano-crystalline granule of original position synthetic 70~90% in ball mill by machinery, for preventing the powder oxidation, adopt inert gas shielding in the mechanical milling process, the premixed powder that contains nano particle that ball milling is good seals in the thin-wall low carbon steel steel pipe 4 of packing into and vacuumizes after Passivation Treatment; Or the premixed powder that contains nano particle that ball milling is good carries out briquet 4, oven dry on forcing press; The premixed powder 16 thin-wall low carbon steel steel pipes 4 that nano particle maybe will be housed are rolling or be drawn into the belt carcass alloy wire 4 that has nano particle premixed powder on milling train or drawbench;
2, the melting of parent metal: start the Metal Melting furnace, various alloying elements by required parent metal composition preparation respective numbers, and in the parent metal alloying component, add metal grain refinement and the crystallization inhibitor again of V%, 0.1~2 the Ti% of 0.1~3% Nb and 0.1~5, wherein V and Ti can only add that wherein any or two kinds add simultaneously or two kinds do not add, with melted parent metal liquid pour in the metal liquid tundish on the workbench;
3, casting: will pour in the tundish on the workbench melted parent metal liquid be cast into consutrode 3, the good consutrode 3 of cast is installed on the electrode holde 2, and the thin-wall low carbon steel steel pipe 4 that simultaneously one or more is equipped with nano particle premixed powder 16 is welded on the consutrode 3; Or one or more thin-wall low carbon steel steel pipe 4 or one or more belt carcass alloy wire 4 that has nano particle premixed powder 16 that nano particle premixed powder 16 is housed is installed on the electrode holde 2; Pour the liquid slag of required composition in water mold formation slag bath 5, start consutrode power supply 1 and 10, the consutrode 3 of the thin-wall low carbon steel sealed steel pipe 4 of nano particle premixed powder 16 is housed inserts in the liquid slag bath 5 and carry out founding being installed in welding on the electrode holde 2, make thin-wall low carbon steel sealed steel pipe 4 and consutrode 3 fusing in slag bath 5 simultaneously that nano particle premixed powder 16 is housed, or will be inserted into continuously in the slag bath 5 with certain controlled velocity through the belt carcass alloy wire 4 that has nano particle premixed powder 16 rolling or that drawing is made, melt simultaneously with parent metal consutrode 3, to be installed in maybe that on the electrode holde 2 one or more is equipped with the thin-wall low carbon steel steel pipe 4 of nano particle premixed powder 16 or one or more has the belt carcass alloy wire 4 of nano particle premixed powder 16, insert and carry out founding in the liquid slag bath, the belt carcass alloy wire 4 that makes the thin-wall low carbon steel steel pipe 4 that nano particle premixed powder 16 is housed or have a nano particle premixed powder 16 is 5 fusings in slag bath, the nanometer that contains that fusing is good strengthens the composition metal drop of particle through after the synthetic wash heat refining of slag, drop in the metal bath 13, start magnetic stirrer 8 and ultrasonic vibrator 17, two phase materials are mixed in water mold 14, and under the quick cooling of water mold 14 rapid solidification and crystalline forming, promptly obtain contain the metal-base composites 7 that nano particle strengthen identical on the end water tank 9 with water mold 14 cavity shapes, start high energy pulse power supply 12, carry out thinning processing by 11 pairs of metal-base composites 7 crystalline structures of high energy pulse electrode, nanoparticle-reinforced metal matrix composite material 7 as the big length of need production, start stripping device 18, it is moved down, production is carried out continuously, and produced the metal-base composites 7 that nano particle strengthens that contains of Len req;
Slags 4 in the water mold 14 are the slag system that urmaterie or multi-component are formed, and composition is by CaFe2 one urmaterie or the slag system that is no less than binary substance be made up of one or more elements of selecting in CaFe2 and Al2O3 or MgO, MnO, CaO, TiO2, RE, RExOy one group element; Matrix material in the metal-base composites 7 is ferrous metal any composition and that can include rare earth alloy, coloured gold, intermetallic compound is arranged; The mass fraction that nanometer strengthens particle is 0.1%~60% of composite 7 weight; The mass fraction of grain inhibitor be composite 7 weight 0.1%~2% or for premixed powder 16 weight 0.1%~5%; The thin-wall low carbon steel steel pipe 4 that loads nano particle premixed powder 16 is of a size of φ 3mm~φ 20mm, be of a size of φ 3mm~φ 10mm through the belt carcass alloy wire 4 that has nano particle premixed powder 16 rolling or that drawing is made, the mass fraction of parent metal powder is 1%~60% of a premixed powder body weight.
Embodiment 2: in Fig. 2, casting equipment is cast moulding by casting device systems, moulding by casting equipment is by the metal mold 23 that is installed on the bottom board 24, in the outside of casting mold 23 magnetic stirrer 8 is installed, ultrasonic vibrator 17 is equipped with in top or bottom at casting mold 23, both sides, top in casting mold 23 are separately installed with high energy pulse electrode 11 and are connected power supply 12, on the next door of bottom board 24 feed trumpet 26 is installed, there is cast runner 25 at the center of feed trumpet 26 and links to each other with the hole of casting mold 23 bottoms, be connected with pouring ladle 29 on the top of feed trumpet 26, in pouring ladle 29, fill parent metal liquid 28, stopper equipment 27 is installed in pouring ladle 29 forms, mold material is the ferrous metal metal material.
During the work beginning, the pressing block 4 that one or more that has prepared is equipped with the thin-wall low carbon steel sealed steel pipe 4 of nano particle premixed powder 16 or nano particle premixed powder 16 is fixed on the center of casting mold 23, or in casting mold 23, fix along even distribution the in the center of casting mold 23 according to certain spacing distance, open the stopper 27 in the pouring ladle 29, directly be poured in the casting mold 23 smelting the hole of good parent metal liquid 28 by feed trumpet 26 cast runners 25 and casting mold 23 bottoms, or in casting process, will join in the parent metal liquid of being poured into a mould 28 continuously with certain controlled velocity through the belt carcass alloy wire 4 that has nano particle premixed powder 16 rolling or that drawing is made, start magnetic stirrer 8 and ultrasonic vibrator 17, two phase materials are mixed in casting mold 23, and in casting mold 23, solidify and crystalline forming, be cast as contain the metal-base composites 7 that nano particle strengthen identical with casting mold 23 cavity shapes, start high energy pulse power supply 12, carry out thinning processing by 11 pairs of nanoparticle-reinforced metal matrix composite material 7 crystalline structures of high energy pulse electrode, both can obtain having the metal-base composites 7 that the nano particle of well-crystallized tissue strengthens.
Other technical process and equipment and embodiment 1 omit together.
Embodiment 3: in Fig. 3, be that with embodiment 2 differences moulding by casting equipment composition is by casting mold 22, in the outside of casting mold 22 magnetic stirrer 8 is installed, on the top of casting mold 22 ultrasonic vibrator 17 is housed, ultrasonic vibrator power supply 21, both sides, middle part in casting mold 22 are separately installed with high energy pulse electrode 11 and are connected power supply 12, casting mold 22 top pouring ladle 19 is arranged, in pouring ladle 19, fill parent metal liquid 20.The material of casting mold 22 is made by refractory material or ferrous metal metal material.
During the work beginning, the pressing block 4 that one or more that has prepared is equipped with the thin-wall low carbon steel sealed steel pipe 4 of nano particle premixed powder 16 or nano particle premixed powder 16 is fixed on the center of casting mold 22, or in casting mold 22, fix along even distribution the in the center of casting mold 22 according to certain spacing distance, directly be poured in the casting mold 22 smelting good parent metal liquid 20, or in casting process, will join in the parent metal liquid of being poured into a mould 20 continuously with certain controlled velocity through the belt carcass alloy wire 4 that has nano particle premixed powder 16 rolling or that drawing is made, start magnetic stirrer 8 and ultrasonic vibrator 17, two phase materials are mixed in casting mold 22, and in casting mold 22, solidify and crystalline forming, be cast as contain the metal-base composites 7 that nano particle strengthen identical with casting mold 22 cavity shapes, start high energy pulse power supply 12, carry out thinning processing by 11 pairs of nanoparticle-reinforced metal matrix composite material 7 crystalline structures of high energy pulse electrode, both can obtain having the metal-base composites 7 that the nano particle of well-crystallized tissue strengthens.
Other technical process and equipment and embodiment 1 and 2 omit together.
Embodiment 4: in Fig. 4, be connected with seal box 31 in the casting device external, on seal box 31, be connected with inert gas jar 30 by pipeline, centre at inert gas jar 30 and seal box 31 is connected with ventilating control valve 29, it charges into the flow of inert gas in seal box 31 by control valve 29 controls, seal box 31 is connected with vavuum pump 32 by pipeline, thereby seal box 31 is vacuumized.
During work, at first start 32 pairs of equipment of vavuum pump and vacuumize, at this moment equipment is in work under the vacuum state; Perhaps after vacuumizing, opens equipment valve 29; in equipment, charge into inert gas; it is being produced under low-pressure inert gas guard mode or under the vacuum state; enter in the nanoparticle-reinforced metal matrix composite material to reduce pernicious gas; prevent metal liquid and the easily oxidation of oxide alloy material simultaneously, improve the quality of products.Other technical process and equipment and embodiment 1, slightly.

Claims (7)

1. the preparation technology of a nanoparticle-reinforced metal matrix composite material is characterized in that: the 1) preparation of nano-crystalline granule liquid mixed powder; 2) melting of parent metal; 3) casting; Concrete steps are as follows:
(1) preparation of nano-crystalline granule liquid mixed powder: at first will from carbide, nitride, boride, oxide nano particles, CNT one group element, select wherein one or more elements and certain content from Cr 3C 2, VC, TaC, ZrC, NbC, HfC, TiB, TiN, NbN, AlN, VN, Ca, Al, Ba, Mg, N and rare earth oxide a group element in be placed on after selecting the parent metal powder of the grain inhibitor of one or more elements wherein and corresponding composition to mix simultaneously and carry out high-energy ball milling in the high-energy stirring ball mill machine, be prepared into the premixed powder that contains nano-crystalline granule;
But or, add Al powder, Cu powder, the Fe of synthesizing carbide, nitride, the carbon dust of boride required dosage, nitrogenous object and doses with the forming element of Ti, V, Zr, Nb, B, W, Mo strong carbide, strong nitride, boride forming element and other original position synthesizing carbide, nitride, boride 2O 3Select wherein one or more elements and the parent metal powder of corresponding composition to be placed on after mixing simultaneously and to carry out high-energy ball milling in the high-energy stirring ball mill machine in powder one group element, bring out the premixed powder of self propagating high temperature nano-crystalline granule of original position synthetic 70~90% in ball mill by machinery;
For preventing the powder oxidation, adopt inert gas shielding in the mechanical milling process, the premixed powder that contains nano particle that ball milling is good is after Passivation Treatment, the sealing of packing in the thin-wall low carbon steel steel pipe vacuumizes or the premixed powder that contains nano particle that ball milling is good carries out briquet on forcing press, oven dry; The premixed powder thin-wall low carbon steel steel pipe that nano particle maybe will be housed is rolling or be drawn into the belt carcass alloy wire that has nano particle premixed powder on milling train or drawbench;
(2) melting of parent metal: start the Metal Melting furnace, various alloying elements by required parent metal composition preparation respective numbers, and in the parent metal alloying component, add metal grain refinement and the crystallization inhibitor again of V, 0.1~2% the Ti of 0.1~3% Nb and 0.1~5%, wherein V and Ti can only add that wherein any or two kinds add simultaneously or two kinds do not add, with melted parent metal liquid pour in the metal liquid tundish on the workbench;
(3) casting: will pour in the tundish on the workbench melted parent metal liquid be cast into consutrode, or directly use it for casting-up; The good consutrode of cast is installed on the electrode holde, and the thin-wall low carbon steel steel pipe that simultaneously one or more is equipped with nano particle premixed powder is welded on the consutrode;
Or one or more thin-wall low carbon steel steel pipe or one or more belt carcass alloy wire that has nano particle premixed powder that nano particle premixed powder is housed is installed on the electrode holde;
Or, be fixed on the center of casting mold, or in casting mold, fix along even distribution the in the center of casting mold according to certain spacing distance with one or more thin-wall low carbon steel steel pipe or nano particle premixed powder pressing block that nano particle premixed powder is housed;
The liquid slag of required composition poured into form slag bath in the water mold, start vavuum pump, protective cover is evacuated or opens the inert gas pump, in protective cover, charge into inert protective gas, start the consutrode power supply, the consutrode of the thin-wall low carbon steel sealed steel pipe of nano particle premixed powder is housed inserts and carry out founding in the liquid slag bath being installed in welding on the electrode holde, thin-wall low carbon steel sealed steel pipe and consutrode that nano particle premixed powder is housed are melted in slag bath simultaneously;
Or will be inserted into continuously in the slag bath with certain controlled velocity through the belt carcass alloy wire that has nano particle premixed powder rolling or that drawing is made, melt simultaneously with the parent metal consutrode;
To be installed in maybe that on the electrode holde one or more is equipped with the thin-wall low carbon steel steel pipe of nano particle premixed powder or one or more has the belt carcass alloy wire of nano particle premixed powder, insert and carry out founding in the liquid slag bath, the belt carcass alloy wire that makes the thin-wall low carbon steel steel pipe that nano particle premixed powder is housed or have a nano particle premixed powder melts in slag bath;
The nanometer that contains that fusing is good strengthens the composition metal drop of particle through after the synthetic wash heat refining of slag, drop in the metal bath, start magnetic stirrer and ultrasonic vibrator, two phase materials are mixed in water mold, and under the quick cooling of water mold rapid solidification and crystalline forming, promptly obtain contain the metal-base composites that nano particle strengthen identical on the end water tank with the water mold cavity shape, start the high energy pulse power supply, carry out thinning processing by high energy pulse electrode pair metal-base composites crystalline structure, nanoparticle-reinforced metal matrix composite material as the big length of need production, start the stripping device, it is moved down, production is carried out continuously, and produced the metal-base composites that nano particle strengthens that contains of Len req;
Maybe will smelt good parent metal liquid directly is poured in the casting mold that fixes one or more thin-wall low carbon steel sealed steel pipe that nano particle premixed powder is housed or nano particle premixed powder pressing block as requested;
Or in casting process, will join in the parent metal liquid of being poured into a mould continuously with certain controlled velocity through the belt carcass alloy wire that has nano particle premixed powder rolling or that drawing is made;
Start magnetic stirrer and ultrasonic vibrator, two phase materials are mixed in casting mold, and in casting mold, solidify and crystalline forming, be cast as contain the metal-base composites that nano particle strengthen identical with the casting mold cavity shape, start the high energy pulse power supply, carry out thinning processing by high energy pulse electrode pair composite crystalline structure, both can obtain having the nanoparticle-reinforced metal matrix composite material of well-crystallized tissue;
Slag in the described water mold is the slag system that urmaterie or multi-component are formed, and composition is by CaFe 2One urmaterie or by CaFe 2With Al 2O 3Or MgO, MnO, CaO, TiO 2, the slag system that is no less than binary substance formed of one or more elements of selecting among the RE, RExOy one group element;
Matrix material in the metal-base composites is ferrous metal, non-ferrous metal, an intermetallic compound any composition and that can include rare earth alloy; The mass fraction that nanometer strengthens particle is 0.1%~60% of a composite weight; The mass fraction of grain inhibitor be composite weight 0.1%~2% or for the premixed powder body weight 0.1%~5%; The thin-wall low carbon steel steel pipe sizes of loading nano particle premixed powder is φ 3mm~φ 20mm, be of a size of φ 3mm~φ 10mm through the belt carcass alloy wire that has nano particle premixed powder rolling or that drawing is made, the mass fraction of parent metal powder is 1%~60% of a premixed powder body weight.
2. equipment of realizing nanoparticle-reinforced metal matrix composite material preparation technology is characterized in that: this equipment is synthetic by nano particle, diffusion, mixing apparatus and two systems of casting equipment form; Casting equipment is made up of fusion cast process and moulding by casting device systems, fusion cast process equipment is by the electrode holde on the column that has lowering or hoisting gear that is installed on the workbench, consutrode or non-consumable electrode are installed on electrode holde, and be connected with cathode power supply, vertical place with consutrode is equipped with water mold below electrode holde, the water mold outside is equipped with magnetic stirrer, ultrasonic vibrator is equipped with in top or bottom at water mold, both sides, top in water mold are separately installed with the high energy pulse electrode, be connected with end water tank and end water tank lowering or hoisting gear in the bottom of water mold, on end water tank, be connected with negative power supply, and form electric loop with the cathode power supply on the electrode holde.
3. nanoparticle-reinforced metal matrix composite material preparation technology's according to claim 2 equipment, it is characterized in that: moulding by casting equipment is by the casting mold that is installed on the bottom board, outside at casting mold is equipped with magnetic stirrer, ultrasonic vibrator is equipped with in top or bottom at casting mold, both sides, top in casting mold are separately installed with the high energy pulse electrode, next door at bottom board is equipped with feed trumpet, there is the cast runner at the center of feed trumpet and is connected with the hole of casting mold bottom, top at feed trumpet is connected with pouring ladle, in pouring ladle, fill parent metal liquid, stopper is installed in pouring ladle.
4. nanoparticle-reinforced metal matrix composite material preparation technology's according to claim 2 equipment is characterized in that: the outside of fusion cast process equipment is equipped with seal box, is externally connected to inert gas jar and vavuum pump and control valve equipment at seal box;
5. nanoparticle-reinforced metal matrix composite material preparation technology's according to claim 2 equipment is characterized in that: nano particle is synthetic, the high-energy stirring ball mill standard device is adopted in diffusion, mixing apparatus.
6. nanoparticle-reinforced metal matrix composite material preparation technology's according to claim 2 equipment, it is characterized in that: water mold comprises water tank and is connected with the cooling water inlet in the bottom of water tank, the top is connected with coolant outlet, the center of water tank is a clear opening, power supply is a low-voltage and high-current, and its voltage and current all can be adjusted on a large scale.
7. nanoparticle-reinforced metal matrix composite material preparation technology's according to claim 3 equipment is characterized in that: mold material adopts ferrous metal or refractory material manufacturing.
CN 201010126913 2010-03-18 2010-03-18 Process and equipment for preparing nanoparticle-reinforced metal matrix composite material Pending CN101829777A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010126913 CN101829777A (en) 2010-03-18 2010-03-18 Process and equipment for preparing nanoparticle-reinforced metal matrix composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201010126913 CN101829777A (en) 2010-03-18 2010-03-18 Process and equipment for preparing nanoparticle-reinforced metal matrix composite material

Publications (1)

Publication Number Publication Date
CN101829777A true CN101829777A (en) 2010-09-15

Family

ID=42714075

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201010126913 Pending CN101829777A (en) 2010-03-18 2010-03-18 Process and equipment for preparing nanoparticle-reinforced metal matrix composite material

Country Status (1)

Country Link
CN (1) CN101829777A (en)

Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102062543A (en) * 2011-01-12 2011-05-18 西安交通大学 Electromagnetic stirring and vibration combined device for preparing semi-solid slurry of black metal
CN102296198A (en) * 2011-10-12 2011-12-28 北京科技大学 Method for preparing tungsten block material by dispersing and reinforcing nano tantalum carbide
CN102310596A (en) * 2011-07-01 2012-01-11 广州有色金属研究院 Method for producing reinforced wear resistance composite material by partially positioning of ceramic particles
CN103484706A (en) * 2013-09-16 2014-01-01 西北工业大学 Preparing device and method of directional carbon nano tube reinforced metal matrix composite material
CN104073666A (en) * 2014-07-21 2014-10-01 温州宏丰电工合金股份有限公司 Preparation method for particle dispersion strengthening metal basal composite material
CN104388733A (en) * 2014-10-13 2015-03-04 北京科技大学 Preparation method of TiAl/alpha-Al2O3 nano-composite material
WO2015191018A1 (en) * 2014-06-12 2015-12-17 Olgun Ugursoy Novel production method and use of new nano-metal and metal-ceramic composite catalysers
RU2574534C2 (en) * 2014-06-17 2016-02-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Composite material with metal matrix and nanoscale reinforcing particles and method of its manufacturing
US9327347B2 (en) 2008-03-05 2016-05-03 Southwire Company, Llc Niobium as a protective barrier in molten metals
US9382598B2 (en) 2010-04-09 2016-07-05 Southwire Company, Llc Ultrasonic device with integrated gas delivery system
US9481031B2 (en) 2015-02-09 2016-11-01 Hans Tech, Llc Ultrasonic grain refining
US9528167B2 (en) 2013-11-18 2016-12-27 Southwire Company, Llc Ultrasonic probes with gas outlets for degassing of molten metals
US9617617B2 (en) 2010-04-09 2017-04-11 Southwire Company, Llc Ultrasonic degassing of molten metals
CN107419151A (en) * 2017-08-17 2017-12-01 东北大学 Nanocrystalline gradient hard alloys of a kind of high rigidity top layer richness WC and preparation method thereof
WO2017209720A2 (en) 2016-06-01 2017-12-07 Dokuz Eylul Universitesi Rektorlugu Composite production method with continuous squeeze cast metal matrix
US10022786B2 (en) 2015-09-10 2018-07-17 Southwire Company Ultrasonic grain refining
CN109482847A (en) * 2018-12-27 2019-03-19 江苏奇纳新材料科技有限公司 Magnetic-moves the molding machine and method of combined precision complexity fine grain casting
US10233515B1 (en) 2015-08-14 2019-03-19 Southwire Company, Llc Metal treatment station for use with ultrasonic degassing system
CN109763014A (en) * 2019-01-10 2019-05-17 上海交通大学 A kind of method of micro-nano granules enhancing metal-base composites
CN109865819A (en) * 2017-12-01 2019-06-11 张志国 A method of it is heated using inductance coil transverse magnetic flux and carries out precast body casting infiltration production ceramic phase reinforcement metal-base composites
CN110093530A (en) * 2019-06-10 2019-08-06 河南科技大学 It is a kind of high to lead wear-resistant copper based composites and preparation method thereof
CN110106383A (en) * 2019-06-10 2019-08-09 河南科技大学 A kind of WC Reinforced Cu-Cr composite material and preparation method
CN110669902A (en) * 2019-09-30 2020-01-10 鞍钢股份有限公司 Aluminum-based intermediate with uniformly dispersed nano particles and preparation and application methods thereof
CN111101049A (en) * 2018-10-26 2020-05-05 青海民族大学 In-situ NbC particle and iron-based amorphous alloy synergistically reinforced manganese steel-based composite material and preparation method thereof
WO2020131874A1 (en) * 2018-12-17 2020-06-25 Jones William F Metal matrices and methods and systems of production thereof
CN113667853A (en) * 2021-08-24 2021-11-19 燕山大学 Preparation method of rare earth oxide reinforced copper-based multi-scale grain structure composite material
CN114406228A (en) * 2022-01-10 2022-04-29 营口理工学院 Copper alloy casting forming nano chromium phase in solidification process and casting method
CN115090382A (en) * 2022-07-05 2022-09-23 长沙理工大学 Asphalt production equipment capable of dispersing asphalt molecular groups and use method
CN116656996A (en) * 2023-07-28 2023-08-29 江东金具设备有限公司 Composite material preparation system and method
CN117144162A (en) * 2023-07-31 2023-12-01 光微半导体材料(宁波)有限公司 Preparation method of copper-manganese alloy material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5167271A (en) * 1988-10-20 1992-12-01 Lange Frederick F Method to produce ceramic reinforced or ceramic-metal matrix composite articles
CN1148095A (en) * 1996-04-11 1997-04-23 丁刚 Process for producing hard alloy and metallic composition material
CN1352314A (en) * 2001-11-03 2002-06-05 丁刚 Process for producing hard phase strengthened metal base composite material
CN101020973A (en) * 2006-02-14 2007-08-22 丁刚 Process and apparatus for making multicomponent phase reinforced composite metal material
CN101134237A (en) * 2007-10-11 2008-03-05 丁家伟 Reinforcing phase metallic gradient composite material manufacturing process and equipment thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5167271A (en) * 1988-10-20 1992-12-01 Lange Frederick F Method to produce ceramic reinforced or ceramic-metal matrix composite articles
CN1148095A (en) * 1996-04-11 1997-04-23 丁刚 Process for producing hard alloy and metallic composition material
CN1352314A (en) * 2001-11-03 2002-06-05 丁刚 Process for producing hard phase strengthened metal base composite material
CN101020973A (en) * 2006-02-14 2007-08-22 丁刚 Process and apparatus for making multicomponent phase reinforced composite metal material
CN101134237A (en) * 2007-10-11 2008-03-05 丁家伟 Reinforcing phase metallic gradient composite material manufacturing process and equipment thereof

Cited By (43)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9327347B2 (en) 2008-03-05 2016-05-03 Southwire Company, Llc Niobium as a protective barrier in molten metals
US10640846B2 (en) 2010-04-09 2020-05-05 Southwire Company, Llc Ultrasonic degassing of molten metals
US9382598B2 (en) 2010-04-09 2016-07-05 Southwire Company, Llc Ultrasonic device with integrated gas delivery system
US9617617B2 (en) 2010-04-09 2017-04-11 Southwire Company, Llc Ultrasonic degassing of molten metals
CN102062543A (en) * 2011-01-12 2011-05-18 西安交通大学 Electromagnetic stirring and vibration combined device for preparing semi-solid slurry of black metal
CN102062543B (en) * 2011-01-12 2012-08-15 西安交通大学 Electromagnetic stirring and vibration combined device for preparing semi-solid slurry of black metal
CN102310596B (en) * 2011-07-01 2014-07-09 广州有色金属研究院 Method for producing reinforced wear resistance composite material by partially positioning of ceramic particles
CN102310596A (en) * 2011-07-01 2012-01-11 广州有色金属研究院 Method for producing reinforced wear resistance composite material by partially positioning of ceramic particles
CN102296198A (en) * 2011-10-12 2011-12-28 北京科技大学 Method for preparing tungsten block material by dispersing and reinforcing nano tantalum carbide
CN103484706A (en) * 2013-09-16 2014-01-01 西北工业大学 Preparing device and method of directional carbon nano tube reinforced metal matrix composite material
US9528167B2 (en) 2013-11-18 2016-12-27 Southwire Company, Llc Ultrasonic probes with gas outlets for degassing of molten metals
US10316387B2 (en) 2013-11-18 2019-06-11 Southwire Company, Llc Ultrasonic probes with gas outlets for degassing of molten metals
WO2015191018A1 (en) * 2014-06-12 2015-12-17 Olgun Ugursoy Novel production method and use of new nano-metal and metal-ceramic composite catalysers
RU2574534C2 (en) * 2014-06-17 2016-02-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Composite material with metal matrix and nanoscale reinforcing particles and method of its manufacturing
CN104073666B (en) * 2014-07-21 2016-09-14 温州宏丰电工合金股份有限公司 A kind of preparation method of particle dispersion-strengthened metal based composites
CN104073666A (en) * 2014-07-21 2014-10-01 温州宏丰电工合金股份有限公司 Preparation method for particle dispersion strengthening metal basal composite material
CN104388733B (en) * 2014-10-13 2017-02-15 北京科技大学 Preparation method of TiAl/alpha-Al2O3 nano-composite material
CN104388733A (en) * 2014-10-13 2015-03-04 北京科技大学 Preparation method of TiAl/alpha-Al2O3 nano-composite material
US9481031B2 (en) 2015-02-09 2016-11-01 Hans Tech, Llc Ultrasonic grain refining
US10441999B2 (en) 2015-02-09 2019-10-15 Hans Tech, Llc Ultrasonic grain refining
US10233515B1 (en) 2015-08-14 2019-03-19 Southwire Company, Llc Metal treatment station for use with ultrasonic degassing system
US10022786B2 (en) 2015-09-10 2018-07-17 Southwire Company Ultrasonic grain refining
US10639707B2 (en) 2015-09-10 2020-05-05 Southwire Company, Llc Ultrasonic grain refining and degassing procedures and systems for metal casting
WO2017209720A2 (en) 2016-06-01 2017-12-07 Dokuz Eylul Universitesi Rektorlugu Composite production method with continuous squeeze cast metal matrix
CN107419151B (en) * 2017-08-17 2019-01-04 东北大学 Nanocrystalline gradient hard alloy of a kind of high rigidity surface layer richness WC and preparation method thereof
CN107419151A (en) * 2017-08-17 2017-12-01 东北大学 Nanocrystalline gradient hard alloys of a kind of high rigidity top layer richness WC and preparation method thereof
CN109865819A (en) * 2017-12-01 2019-06-11 张志国 A method of it is heated using inductance coil transverse magnetic flux and carries out precast body casting infiltration production ceramic phase reinforcement metal-base composites
CN111101049A (en) * 2018-10-26 2020-05-05 青海民族大学 In-situ NbC particle and iron-based amorphous alloy synergistically reinforced manganese steel-based composite material and preparation method thereof
WO2020131874A1 (en) * 2018-12-17 2020-06-25 Jones William F Metal matrices and methods and systems of production thereof
CN109482847A (en) * 2018-12-27 2019-03-19 江苏奇纳新材料科技有限公司 Magnetic-moves the molding machine and method of combined precision complexity fine grain casting
CN109763014A (en) * 2019-01-10 2019-05-17 上海交通大学 A kind of method of micro-nano granules enhancing metal-base composites
CN110093530A (en) * 2019-06-10 2019-08-06 河南科技大学 It is a kind of high to lead wear-resistant copper based composites and preparation method thereof
CN110106383A (en) * 2019-06-10 2019-08-09 河南科技大学 A kind of WC Reinforced Cu-Cr composite material and preparation method
CN110669902A (en) * 2019-09-30 2020-01-10 鞍钢股份有限公司 Aluminum-based intermediate with uniformly dispersed nano particles and preparation and application methods thereof
CN110669902B (en) * 2019-09-30 2021-10-22 鞍钢股份有限公司 Aluminum-based intermediate with uniformly dispersed nano particles and preparation and application methods thereof
CN113667853A (en) * 2021-08-24 2021-11-19 燕山大学 Preparation method of rare earth oxide reinforced copper-based multi-scale grain structure composite material
CN114406228A (en) * 2022-01-10 2022-04-29 营口理工学院 Copper alloy casting forming nano chromium phase in solidification process and casting method
CN115090382A (en) * 2022-07-05 2022-09-23 长沙理工大学 Asphalt production equipment capable of dispersing asphalt molecular groups and use method
CN115090382B (en) * 2022-07-05 2023-11-21 长沙理工大学 Asphalt production equipment capable of dispersing asphalt molecular groups and application method
CN116656996A (en) * 2023-07-28 2023-08-29 江东金具设备有限公司 Composite material preparation system and method
CN116656996B (en) * 2023-07-28 2023-11-03 江东金具设备有限公司 Composite material preparation system and method
CN117144162A (en) * 2023-07-31 2023-12-01 光微半导体材料(宁波)有限公司 Preparation method of copper-manganese alloy material
CN117144162B (en) * 2023-07-31 2024-03-01 光微半导体材料(宁波)有限公司 Preparation method of copper-manganese alloy material

Similar Documents

Publication Publication Date Title
CN101829777A (en) Process and equipment for preparing nanoparticle-reinforced metal matrix composite material
Guan et al. A review on grain refinement of aluminum alloys: progresses, challenges and prospects
CN101880746B (en) Preparation process of nano powder modified and reinforced die steels
Sharma et al. A study of fabrication methods of aluminum based composites focused on stir casting process
CN103866154B (en) In a kind of composite, micro-nano granules strengthens the Dispersed precipitate method of phase
WO2016184237A1 (en) 6x82 aluminium-based composite material for use in automobile control arm and preparation method thereof
CN102383030A (en) Preparation process for nano strengthened wear-resistant die steel
CN102732740B (en) Nano-material interalloy modifier and preparation method thereof, and alloy preparation method
CN100447274C (en) Particle reinforced steel-base composite material roller by in-situ synthesis and process for preparing same
CN101921930B (en) Multicomponent microalloyed titanium alloy and preparation method thereof
CN103789656B (en) High manganese wear-resistant steel of a kind of tungstenic-chromium-vanadium and preparation method thereof
CN106636933B (en) A kind of method for preparing multiphase reinforced ferrite alloy
CN102433475B (en) High-strength and high-hardness aluminum alloy and preparation method thereof
CN102357653A (en) Preparation process for nanoparticle reinforced die steel
CN102791893B (en) Particulate aluminium matrix nano-composites and a process for producing the same
CN109825756B (en) Preparation method of high-wear-resistance alloy steel material
CN113249547B (en) Smelting method for refining inclusions in H13 hot work die steel
CN111041297A (en) High-corrosion-resistance in-situ nanoparticle reinforced aluminum-based composite material and preparation method thereof
CN102433472B (en) High strength aluminium alloy and smelting and casting methods thereof
CN110129596A (en) Thin ribbon shaped nanometer Al3The preparation method of (Sc, Zr)/Al composite inoculant
CN102660693B (en) Aluminum alloy treated by using TiN powder and BeH2 powder, and preparation method thereof
Zhang et al. Effect of copper addition on microstructures and mechanical properties of in situ TiCp/Fe composites
CN101362198A (en) Rotary pouring manufacture method of AZ91D magnesium alloy semisolid slurry
CN114990420A (en) Aluminum-boron-chromium-nitrogen-iron alloy and preparation method and application thereof
CN101407870B (en) Multicomponent flux composition method capable of lowering metal-matrix composite synthesis temperature

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Open date: 20100915