CN102784916B - Negative pressure injection molding process for preparation of high-alloying material with tight coupling nozzle - Google Patents
Negative pressure injection molding process for preparation of high-alloying material with tight coupling nozzle Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of a high-performance metal material, and relates to a process method for preparation of a high-alloying material (high-temperature alloy and high-speed steel) with a tight coupling atomization nozzle via negative pressure injection molding. The advantages of an injection molding process and an atomization nozzle are fully combined. An alloy material is molten with a vacuum induction melting device, and a blank for atomization and deposition of the high-alloying material (high-temperature alloy and high-speed steel) with high bulk density, fine grains and uniform tissues is prepared with the supersonic tight coupling atomization nozzle through an optimized negative pressure atomization and deposition process, and a foundation is laid for promotion and application in injection molding of a high-temperature alloy turbine disc and injection molding of a workpiece mold steel and other materials.
Description
Technical field
The invention belongs to technical field of metal material preparation, relate to one and utilize close coupling atomizer to prepare the process of high-alloying material (high temperature alloy, high-speed steel) by negative pressure reaction-injection moulding.
Background technology
Reaction-injection moulding is a kind of melting, atomization that collects high-alloying metal material, be deposited on the short flow process technology of near-net forming of one, this technology has not only overcome the gross segregation that conventional cast technique causes and has organized thick problem, and avoided the loaded down with trivial details and Powder Oxidation of the powder metallurgical technique technical barrier such as seriously, be particularly suitable for preparing alloying level high (as high temperature alloy, high-speed steel etc.) and easily produce the metal material of segregation.Reaction-injection moulding metal material has the advantages such as fine microstructures, composition are even, high solid solubility.Thereby, spray forming technology has the diversity of applicability and product widely, it is not only applicable to various metals material, as high temperature alloy, high-speed steel, tool steel, mould steel, aluminium-silicon alloys etc., and be new material, as the development of intermetallic compound, composite and dual-property material provides a kind of advanced person's technological means.
Spray deposition processing process is mainly made up of with cooling, three continuous process of deposit preform growth aluminium alloy atomization, molten drop flight.Alloy melt, at mozzle end, is atomized airflow crash and becomes a large amount of tiny molten drop of size between several microns～hundreds of micron, and molten drop accelerates under action of high-speed airflow, carries out Rapid Thermal simultaneously exchange cooling with air-flow.Larger drop after the atomization thermal capacity due to as above in 100 μ m itself is high, quality is large, be subject to the effect of inertia force larger than droplet, acceleration in gas flowfield is slow, and the coefficient of heat transfer between drop and air-flow is low, and therefore large-sized drop is also in liquid phase state in the time arriving depositional plane.Tiny solid particle and larger drop be high fast direction depositional plane simultaneously, clashes into depositional plane, and the shock of solid particle, just as shot peening strengthening, is constantly out of shape impact to sedimentary deposit, makes cannot form large arborescent structure in sedimentary deposit; And the drop of larger volume under high-speed impact, be deformed into laminar be attached to sedimentary deposit surface or sputter occur form more tiny drop and carry out secondary deposition or depart from deposit preform.The molten drop high-speed impact depositor surface that this numerous coagulation grade is different, in depositor surface attachment, pile up, sprawl, fuse and form thin semi liquid state layer a consecutive solidification crystallization, is progressively deposited as the metal body of a large block compact.
Reaction-injection moulding is combined in the deposition of the atomization of liquid metal (rapid solidification) and atomized droplet (dynamically compact curing) in a step metallurgical operations and completes, not only reduce operation, there are obvious economic benefits, and even tissue, crystal grain is tiny, has improved the performance of difficult deformation processing metal material.At present, spray deposition processing is more employing free-falling type nozzle both at home and abroad, although such nozzle has reduced the risk of spray nozzle clogging, the metal drop size that atomization goes out is larger, affects the structural homogenity of high-alloying material.
Selecting suitable nozzle is the critical component that obtains desirable reaction-injection moulding high-alloying material structure.The factor that reaction-injection moulding designs of nozzles need to be considered comprises: (1) atomization gas can obtain large as far as possible outlet scattered-out beam and energy; (2) between atomizing medium and metal bath, can form rational spray angle; (3) working stability, is difficult for stopping up.The feature of close-coupled nozzle is that the outlet of atomization inert gas approaches metal liquid stream outlet, make maximum gas energy aggtegation in liquid metal, only have little part energy to be lost in gas vent to the turbulent flow between liquid stream, add that atomization gas can adopt larger angle to act on molten metal, therefore gas kinetic energy rejection is less, can obtain the drop that median particle diameter is less.But the outstanding problem that close-coupled nozzle exists is easy obstruction.Concrete reason is because the front end of mozzle is subject to the cooling of atomization gas, and molten metal may part solidify before atomization occurring, so close-coupled nozzle is generally used for the reaction-injection moulding of low-melting alloy, and less for materials with high melting point, as high temperature alloy etc.But adopt the grain size of high-alloying metal material prepared by the spray deposition processing of close-coupled nozzle thinner, organize more evenly, material mechanical performance is better.Therefore, if in preparation technology obtain break through, adopt close-coupled nozzle prepare dystectic alloy material as high temperature alloy be also feasible.For example, Beijing Research Inst. of Aeronautic Material adopts the spray deposition processing of close-coupled nozzle to prepare high-temperature alloy turbine disc.The Spray Formed Superalloys turbine disk of preparing has the following advantages: 1. without gross segregation and powder primary granule border (PPB), and structure refinement, oxygen content is low and without thick carbide; 2. hot and cold processing characteristics and mechanical property significantly improve; 3. preparation section is few, and efficiency is high, and production cost is low.The second is free fall style atomizer.In this kind of nozzle, to start interactional distance longer for atomization gas and molten metal, and because operating distance is long, air-flow decay is fast, and capacity usage ratio is low, and therefore the droplet size of jet deposition is thicker.
Domestic a kind of reciprocal jet shaper of control (patent No.: CN03230878.7) of preparing large specification, various shape, high-compactness, high performance alloys and composite thereof of person of outstanding talent's invention.This equipment adopts unrestricted formula, non-scanning atomizer, metal bath is under the fragmentation and drive of high speed inert gas, form atomized spray stream at a high speed, the reciprocal sedimentary movement under online accurately control is carried out in injection stream and substrate, the alloy that is deposited on substrate surface is cooling fast, obtains the deposit preform of dense structure and definite shape.This device adopts unrestricted formula (being free-falling type) nozzle, and under same atomizing pressure condition, the size of atomized drop is larger than close coupled type atomizer, adds that the flying speed of atomized droplet is lower, therefore causes the crystallite dimension in deposit preform larger.Make to adopt the spray deposition processing of unrestricted type nozzle poorer than the high-alloying material composition uniformity that adopts the spray deposition processing of close-coupled nozzle to prepare, and mechanical property is lower.
In order to improve the particularly degree of purity of high temperature alloy of reaction-injection moulding high-alloying material, oxidized method (patent No.: CN200710041267.5) that the propositions such as the Ren Sanbing of Baoshan Iron & Steel Co., Ltd are a kind of while preventing that reaction-injection moulding from preparing high temperature alloy, calandria and heat-resisting crucible material are set in reaction-injection moulding equipment, and calandria position is higher than depositor.And heat-resisting crucible material is positioned at calandria top, above it, add carbon material granule; In fusion process and course of injection, all the time carbon material granule is burnt thoroughly, carbon material granule is at high temperature oxidized, and when consuming oxygen, generates protective gas, prevents that high temperature alloy is oxidized in course of injection.But in concrete high temperature alloy stage of spray forming process, the generation of domestic and international seldom employing heating carbon has reproducibility but the virose carbon monoxide of while tool prevents high temperature alloy oxidation, and technique operability is not strong.
Summary of the invention
The object of the invention is to propose a kind of grain size that can improve high-alloying material, the employing close coupling atomizer that reduces segregation is prepared the negative pressure spray shaping technology of high-alloying metal material.
Technical solution of the present invention is:
(1) adopt vacuum induction melting high-alloying metal material; Melting kettle adopts high-purity electric-melting magnesium-aluminium spinel refractory material preparation of high temperature insostatic pressing (HIP) processing, wherein, and crucible volume density > 99%, and new crucible must be through high-temperature baking and the prepurging of similar alloy induction melting once before using;
(2) reaction-injection moulding nozzle adopts supersonic speed close coupling atomizer; The gas pressure of spray deposition is 50～60atm;
(3) pack alloy into melting kettle;
(4) vacuumize power transmission eddy-current heating alloy material: adopt mechanical pump, lobe pump and booster pump triplex system all vacuumize the working chamber of equipment, spray chamber, vacuum < 1 × 10
-2pa, power transmission heating alloy material is to alloy melting;
(5) vacuum induction melting: increase the power of vaccum sensitive stove, molten alloy in vacuum environment, after alloy melts completely, refining 10～15 minutes, makes the alloy material of fusing more even and purer;
(6) inflation: after the alloy refining under high vacuum environment completes, be filled with high-purity argon gas to working chamber and spray chamber, purity > 99.9%wt, O
2< 2ppm, pressure is 0.95～1atm;
(7) negative pressure is taken out by settling chamber: start the vacuum system of spray deposition chamber, settling chamber is vacuumized.Keep the pressure reduction of working chamber and spray deposition chamber between 0.25～0.5atm by vacuum unit, i.e. P
working chamber-P
spray deposition chamber=0.3～0.4atm;
(8) negative-pressure atomizing deposition: after the vacuum system of spray deposition chamber starts 3～5 seconds, the uniform molten steel of refining in induction melting crucible is slowly poured into by the speed of 20 kilograms per minute in the tundish flow guide system having heated, flow out behind mozzle lower end when observing melt, open rapidly the pressure gas valve of close coupling atomizer, spray deposition alloy melt forms deposit preform by molten drop jet deposition on the depositor of rotation; Atomization gas is high-purity argon gas, purity > 99.99%wt, O
2< 2ppm, atomizing pressure is 80～100atm, and spray deposition, after 30 seconds, keeps settling chamber in running order for the vacuum unit of bleeding, and settling chamber's internal gas pressure is-0.2～-0.3atm;
(9) after spray deposition completes, working chamber and spray deposition chamber are vacuumized, make high temperature deposition base in vacuum state, low vacuum is in 10
-2pa, alloy preform temperature is cooling lower than after 200 ℃, and vacuum breaker takes out deposit preform.
Advantage of the present invention and effect:
The present invention is fully in conjunction with the advantage of spray deposition processing and atomizer technology.Utilize vacuum induction melting equipment melting reaction-injection moulding alloy material, adopt supersonic speed close coupling atomizer, by the negative-pressure atomizing depositing operation of optimal design, prepare volume density high, high-alloying material (high temperature alloy, high-speed steel) the spray deposition base that crystal grain is tiny, for the materials such as the Spray Formed Superalloys turbine disk, reaction-injection moulding mould steel lay the first stone.
Advantage of the present invention also comprises: 1. prevent that close coupling atomizer from stopping up.The blockage problem of close coupling supersonic gas atomizer is the very scabrous difficult problem of domestic and international spray deposition processing always.Negative-pressure atomizing depositing operation prevented alloy molten steel because of transmission range long, the spray nozzle clogging that the increase of variations in temperature viscosity causes, has guaranteed that the smooth and easy nozzle place that flows to of alloy melt carries out atomization; 2. reduce the gas content in deposit preform.The gases at high pressure that spray from superonic flow nozzzle are under suction function, increase the relative velocity of atomization air flow to high temperature alloy liquid, make the power reciprocation of atomization gas and high temperature alloy melt stronger, degree of crushing while improving molten metal arrival deposit preform top, be conducive to the discharge of the atomization gas that entrains into or carry secretly, improve the density of deposit preform; 3. reduce the inner crystallite dimension of deposit preform; Because nebulization efficiency improves, the median particle diameter of atomized droplet further reduces, and in deposit preform, crystallite dimension is less.Therefore, the size of metallurgical imperfection and field trash also further reduces, and has improved the metallurgical quality of alloy deposition base.Research shows, the square root of the bending strength of high-speed steel and limit defects with diameters is inversely proportional to, and therefore eliminating large-sized inclusions becomes one of fundamental way improving high-speed steel intensity and quality.All spray forming high-speed steels are all made up of carbide (tungsten carbide, molybdenum carbide or vanadium carbide etc.) and the martensitic matrix of tempering.If skewness in the high steel matrix that carbide is lower at relative hardness, toughness is high of hardness, can directly shorten the service life of cutter and mould, and the carbide of spray forming high-speed steel inside is very even in the inner distribution of high-speed steel, therefore, material wear ability is better, longer service life; 4. equipment operating is more safe and reliable.Enter the inert gas of settling chamber by vacuum system, likely can cause the indoor pressure of spray deposition sharply to raise, cause danger.Force to discharge the security while having improved system operation by negative pressure system.
The present invention contributes to improve metallurgical quality and the performance of China's reaction-injection moulding high-alloying material (comprising high temperature alloy, high-speed steel etc.), promote the development of China's high performance jetting shaping high-alloying material, the gap of the developed countries such as shortening and America and Europe, solve the key issue that restriction reaction-injection moulding high-alloying material is applied, for the advanced aviation of China and airspace engine technology, and the innovation of processing and manufacturing instrument and progressively provide technical support.
The specific embodiment
Technical scheme of the present invention comprises the following steps:
(1) adopt vacuum induction melting high-alloying metal material; Melting kettle adopts high-purity electric-melting magnesium-aluminium spinel refractory material preparation of high temperature insostatic pressing (HIP) processing.Wherein, crucible volume density > 99%, and new crucible must be through high-temperature baking and the prepurging of similar alloy induction melting once before using;
(2) reaction-injection moulding nozzle adopts the supersonic speed close coupling atomizer of autonomous Design; The gas pressure of spray deposition is 50～60atm;
(3) select alloy charging: select a kind of high-alloying metal material, as the alloy pig of high temperature alloy or mould steel, alloy material is packed into crucible;
(4) vacuumize power transmission eddy-current heating alloy material: adopt mechanical pump, lobe pump and booster pump triplex system all vacuumize the working chamber of equipment, spray chamber, vacuum < 1 × 10
-2pa.Slowly power transmission heating alloy material;
(5) vacuum induction melting: increase intermediate frequency power supply power, molten alloy in vacuum environment.After alloy melts completely, refining 10～15 minutes, makes the alloy material of fusing more even and purer;
(6) inflation: after the alloy refining under high vacuum environment completes, be filled with high purity inert gas (> 99.9%wt, O to working chamber and spray chamber
2< 2ppm), pressure is 0.95～1atm;
(7) negative pressure is taken out by settling chamber: start the vacuum system of spray deposition chamber, settling chamber is vacuumized.Keep the pressure reduction of working chamber and spray deposition chamber between 0.25～0.5atm by vacuum unit, i.e. P
working chamber-P
spray deposition chamber=0.3～0.4atm.
(8) negative-pressure atomizing deposition: after the vacuum system of spray deposition chamber starts 3～5 seconds, the uniform molten steel of refining in induction melting crucible is slowly poured into by the speed of 20 kilograms per minute in the tundish flow guide system having heated, flow out behind mozzle lower end when observing melt, open rapidly the pressure gas valve of close coupling atomizer, spray deposition alloy melt forms deposit preform by molten drop jet deposition on the depositor of rotation; Atomization gas is high purity inert gas (> 99.99%wt, O
2< 2ppm), atomizing pressure is 80～100atm.After spray deposition 30 seconds, must remain that settling chamber is in running order for the vacuum unit of bleeding, settling chamber's internal gas pressure is-0.2～-0.3atm;
The major advantage of negative-pressure atomizing deposition comprises: 1. prevent that close-coupled nozzle from stopping up.The blockage problem of close coupling supersonic gas atomizer is the very scabrous difficult problem of domestic and international spray deposition processing always.Negative-pressure atomizing depositing operation prevented alloy molten steel because of transmission range long, the spray nozzle clogging that the increase of variations in temperature viscosity causes, has guaranteed that the smooth and easy nozzle place that flows to of alloy melt carries out atomization; 2. reduce the gas content in deposit preform.The gases at high pressure that spray from superonic flow nozzzle are under suction function, increase the relative velocity of atomization air flow to high temperature alloy liquid, make the power reciprocation of atomization gas and high temperature alloy melt stronger, degree of crushing while improving molten metal arrival deposit preform top, be conducive to the discharge of the atomization gas that entrains into or carry secretly, improve the density of deposit preform; 3. reduce inclusion size; Because nebulization efficiency improves, the median particle diameter of high temperature alloy fine powder further reduces, and therefore, the size of field trash also further reduces, and has improved the metallurgical quality of alloy deposition base; 4. equipment operating is more safe and reliable.Enter the inert gas of settling chamber by vacuum system, likely can cause the indoor pressure of spray deposition sharply to raise, cause danger.Force to discharge the security while having improved system operation by negative pressure system.
(9) after spray deposition completes, working chamber and spray deposition chamber are vacuumized, make high temperature deposition base in vacuum state, low vacuum is in 10
-2pa.Alloy preform temperature is cooling lower than after 200 ℃, and vacuum breaker takes out deposit preform.
Embodiment
Take alloy material chemical composition as (wt%): C1.5; W12.3; Co4.66; V5.2; Cr4.16; Mo0.22; The high-alloying material of remaining Fe is example, and how much weight of putting into alloy material is determined by crucible size.
The main operating process that reaction-injection moulding is prepared high-alloying material is: adopt vacuum induction melting high-alloying metal material; Melting kettle adopts high-purity electric-melting magnesium-aluminium spinel refractory material preparation of high temperature insostatic pressing (HIP) processing.Wherein, crucible volume density > 99%, and new crucible must be through high-temperature baking and the prepurging of similar alloy induction melting once before using; Reaction-injection moulding nozzle adopts the supersonic speed close coupling atomizer of autonomous Design; The gas pressure of spray deposition is 50～60atm; Alloy material is packed into crucible; Working chamber, spray chamber are vacuumized to vacuum < 1 × 10
-2pa.Slowly power transmission heating alloy material; Increase intermediate frequency power supply power, molten alloy in vacuum environment.After alloy melts completely, refining 10～15 minutes.After alloy refining completes, be filled with high purity inert gas (> 99.9%wt, O to working chamber and spray chamber
2< 2ppm), pressure is 0.95～1atm; Start the vacuum system of spray deposition chamber, keep the pressure reduction of working chamber and spray deposition chamber between 0.25～0.5atm by vacuum unit, i.e. P
working chamber-P
spray deposition chamber=0.3～0.4atm.After the vacuum system of spray deposition chamber starts 3～5 seconds, the uniform molten steel of refining in induction melting crucible is slowly poured into by the speed of 20 kilograms per minute in the tundish flow guide system having heated, flow out behind mozzle lower end when observing melt, open the high-pressure atomization gas valve of close coupling atomizer, spray deposition alloy melt forms deposit preform molten drop jet deposition on the depositor of rotation; Atomization gas is high purity inert gas (> 99.99%wt, O
2< 2ppm), gas pressure is 80～100atm.After spray deposition 30 seconds, remain that settling chamber's internal gas pressure is-0.2～-0.3atm.After spray deposition completes, working chamber and spray deposition chamber are vacuumized, make high temperature deposition base in vacuum state, low vacuum is in 10
-2pa.Alloy preform temperature is cooling lower than after 200 ℃, and vacuum breaker takes out deposit preform.
Claims (1)
1. adopt close-coupled nozzle to prepare a negative pressure spray deposition processing for high-alloying material, the steps include:
(1) adopt vacuum induction melting high-alloying metal material: melting kettle adopts high-purity electric-melting magnesium-aluminium spinel refractory material preparation of high temperature insostatic pressing (HIP) processing, wherein, crucible volume density > 99%, and new crucible must be through high-temperature baking and the prepurging of similar alloy induction melting once before using;
(2) reaction-injection moulding nozzle adopts supersonic speed close coupling atomizer: the gas pressure of spray deposition is 50～60atm;
(3) pack alloy into melting kettle;
(4) vacuumize power transmission eddy-current heating alloy material: adopt mechanical pump, lobe pump and booster pump triplex system all vacuumize the working chamber of equipment, spray chamber, vacuum < 1 × 10
-2pa, power transmission heating alloy material is to alloy melting;
(5) vacuum induction melting: increase the power of vaccum sensitive stove, molten alloy in vacuum environment, after alloy melts completely, refining 10～15 minutes, makes the alloy material of fusing more even and purer;
(6) inflation: after the alloy refining under high vacuum environment completes, be filled with high-purity argon gas to working chamber and spray chamber, purity > 99.9%wt, O
2< 2ppm, pressure is 0.95～1atm;
(7) negative pressure is taken out by settling chamber: start the vacuum system of spray deposition chamber, settling chamber is vacuumized, keep the pressure reduction of working chamber and spray deposition chamber between 0.25～0.5atm, i.e. P by vacuum unit
working chamber-P
spray deposition chamber=0.25～0.5atm;
(8) negative-pressure atomizing deposition: after the vacuum system of spray deposition chamber starts 3～5 seconds, the uniform aluminium alloy of refining in induction melting crucible is slowly poured into by the speed of 20 kilograms per minute in the tundish flow guide system having heated, flow out behind mozzle lower end when observing melt, open rapidly the pressure gas valve of close coupling atomizer, spray deposition alloy melt forms deposit preform by molten drop jet deposition on the depositor of rotation; Atomization gas is high-purity argon gas, purity > 99.99%wt, O
2< 2ppm, atomizing pressure is 80～100atm, and spray deposition, after 30 seconds, keeps settling chamber in running order for the vacuum unit of bleeding, and settling chamber's internal gas pressure is-0.2～-0.3atm;
(9) after spray deposition completes, working chamber and spray deposition chamber are vacuumized, make high temperature deposition base in vacuum state, low vacuum is in 10
-2pa, alloy preform temperature is cooling lower than after 200 ℃, and equipment vacuum breaker takes out deposit preform.
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| CN111390174B (en) * | 2020-04-16 | 2022-05-03 | 广东明路电力电子有限公司 | 3D printing metal spraying equipment, 3D printing device and control method thereof |
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