CN102784916A - 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 a kind of process of utilizing the close coupling atomizer to prepare high-alloying material (high temperature alloy, high-speed steel) through the negative pressure reaction-injection moulding.
Background technology
Reaction-injection moulding is a kind of melting that collects the high-alloying metal material, atomize, 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 technology causes and has organized thick problem; And avoided the loaded down with trivial details and powder oxidation of powder metallurgical technique seriously to wait technical barrier, be particularly suitable for preparing the metal material that alloying level height (like high temperature alloy, high-speed steel etc.) is easy to generate segregation.The reaction-injection moulding metal material has organizes tiny, advantages such as composition is even, high solid solubility.Thereby; Spray forming technology has the diversity of extensive applicability and product; It is not only applicable to multiple metal material; Like high temperature alloy, high-speed steel, tool steel, mould steel, aluminium-silicon alloys etc., and be new material, a kind of advanced person's technological means is provided like the development of intermetallic compound, composite and dual-property material.
The spray deposition processing process mainly is made up of the atomizing of alloy liquid, molten drop flight and cooling, three continuous process of deposit preform growth.Alloy melt is terminal at mozzle, is atomized airflow crash and becomes a large amount of tiny molten drop of size between several microns～hundreds of micron, and molten drop quickens under action of high-speed airflow, carries out Rapid Thermal exchange cooling with air-flow simultaneously.big drop after the atomizing is as the thermal capacity owing to itself is high more than the 100 μ m, quality is big; Receive the effect of inertia force bigger than droplet; Acceleration in gas flowfield is slow, and the coefficient of heat transfer between drop and the air-flow is low, and therefore large-sized drop also is in liquid phase state when arriving depositional plane.Tiny solid particle and bigger drop be high fast direction depositional plane simultaneously, clashes into depositional plane, and the bump of solid particle constantly is out of shape impact to sedimentary deposit just as shot peening strengthening, makes in the sedimentary deposit and can't form big arborescent structure; And that the drop of larger volume is deformed under high-speed impact is laminar attached to sedimentary deposit surface or sputter takes place form more tiny drop and carry out the secondary deposition or break away from deposit preform.The different molten drop high-speed impact depositor of this numerous coagulation grade surface in the depositor surface attachment, pile up, sprawl, fuse and form a thin semi liquid state layer and a consecutive solidification crystallization, progressively is deposited as the metal body of a large block compact.
Reaction-injection moulding is combined in the deposition of atomizing of liquid metal (rapid solidification) and atomizing molten drop (dynamically compact curing) in the step metallurgical operations and accomplishes; Not only reduce operation, have tangible 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, though such nozzle has reduced the risk of spray nozzle clogging, the metal drop size that atomizes out is bigger, influences the structural homogenity of high-alloying material.
Selecting suitable nozzle for use is the critical component that obtains desirable reaction-injection moulding high-alloying material structure.The factor that the reaction-injection moulding designs of nozzles need be considered comprises: (1) atomization gas can obtain big as far as possible outlet scattered-out beam and energy; (2) can form the rational ejector angle between atomizing medium and the metal bath; (3) working stability is difficult for stopping up.The characteristics of close coupling nozzle are that the outlet of atomizing inert gas exports near metal liquid stream; Make maximum gas energy aggtegation in liquid metal; Have only part energy seldom to be lost in the turbulent flow between gas vent to the flow; Add that atomization gas can adopt bigger angle to act on molten metal, so the gas kinetic energy rejection is less, can obtain the less drop of median particle diameter.But the outstanding problem that the close coupling nozzle exists is an easy blocking.Concrete reason is because the front end of mozzle receives the cooling of atomization gas, and molten metal possibly partly solidify before atomizing takes place, so the close coupling nozzle generally is used for the reaction-injection moulding of low-melting alloy, and the less materials with high melting point that is used for, like high temperature alloy etc.But adopt the grain size of high-alloying metal material of spray deposition processing preparation of close coupling nozzle thinner, organize more evenly, material mechanical performance is better.Therefore, if on preparation technology, obtain to break through, employing close coupling nozzle prepares dystectic alloy material such as high temperature alloy also is feasible.For example, the Beijing Research Inst. of Aeronautic Material adopts the spray deposition processing of close coupling nozzle to prepare high-temperature alloy turbine disc.The reaction-injection moulding high-temperature alloy turbine disc of preparing has following advantage: 1. there are not gross segregation and powder primary granule border (PPB), and structure refinement, oxygen content is low and do not have a thick carbide; 2. hot and cold processing characteristics and mechanical property significantly improve; 3. preparation section is few, and efficient is high, and production cost is low.Second kind is the free fall style atomizer.To begin interactional distance longer for atomization gas and molten metal in this kind nozzle because operating distance is long, the air-flow decay soon, capacity usage ratio is low, so the droplet size of jet deposition is thicker.
Domestic a kind of reciprocal reaction-injection moulding device of control (patent No.: CN03230878.7) for preparing big specification, multiple 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 the online accurate control is carried out in injection stream and substrate, and the alloy that is deposited on substrate surface cools off fast, obtains the deposit preform of dense structure and definite shape.This device adopts unrestricted formula (being the free-falling type) nozzle, and under same atomizing pressure condition, the size of atomized drop is bigger than close coupled type atomizer, adds that the flying speed of atomizing molten drop is lower, therefore causes the crystallite dimension in the deposit preform bigger.Make that the spray deposition processing that adopts unrestricted type nozzle is poorer than the high-alloying material composition uniformity of the spray deposition processing preparation of adopting the close coupling nozzle, 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 (the patent No.: CN200710041267.5) that propositions such as the Ren Sanbing of Baoshan Iron & Steel Co., Ltd are a kind of when preventing that reaction-injection moulding from preparing high temperature alloy; Calandria and heat-resisting crucible material are set in reaction-injection moulding equipment, and the calandria position is higher than depositor.And heat-resisting crucible material is positioned at calandria top, adds carbon property material granule above it; In fusion process and course of injection, all the time carbon property material granule is passed through and burn, the oxidation at high temperature of carbon property material granule generates protective gas in the time of consume oxygen, prevent that high temperature alloy from receiving oxidation in course of injection.But in concrete high temperature alloy reaction-injection moulding process, seldom adopt both at home and abroad heating carbon to generate to have reproducibility but the carbon monoxide that has toxicity simultaneously prevents the high temperature alloy oxidation, the technology operability is not strong.
Summary of the invention
The objective of the invention is to propose a kind of grain size that can improve the high-alloying material, the employing close coupling atomizer that reduces segregation prepares the negative pressure spray shaping technology of high-alloying metal material.
Technical solution of the present invention is:
(1) adopts 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) the reaction-injection moulding nozzle adopts supersonic speed close coupling atomizer; The gas pressure of spray deposition is 50～60atm;
(3) with the alloy melting kettle of packing into;
(4) vacuumize, send the electrical induction 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 send the electrical heating alloy material to alloy melting;
(5) vacuum induction melting: increase the power of vaccum sensitive stove, molten alloy in vacuum environment, treat that alloy melts fully after, refining 10～15 minutes makes the alloy material of fusing more even and purer;
(6) inflation: the alloy refining under high vacuum environment charges into high-purity argon gas to working chamber and spray chamber, purity＞99.9%wt, O after accomplishing
2＜2ppm, pressure are 0.95～1atm;
(7) negative pressure is taken out by the settling chamber: start the vacuum system of spray deposition chamber, vacuumize the settling chamber.The pressure reduction that keeps working chamber and spray deposition chamber through the vacuum unit between 0.25～0.5atm, i.e. P
The working chamber-P
The spray deposition chamber=0.3～0.4atm;
(8) negative pressure spray deposition: after the vacuum system of spray deposition chamber starts 3～5 seconds; Slowly pour in the tundish flow guide system that has heated by the speed of 20 kilograms of per minutes the uniform molten steel of refining in the induction melting crucible; After observing melt outflow mozzle lower end; Open the pressure gas valve of close coupling atomizer rapidly, the spray deposition alloy melt forms deposit preform with the molten drop jet deposition on the depositor of rotation; Atomization gas is a high-purity argon gas, purity＞99.99%wt, O
2＜2ppm, atomizing pressure are 80～100atm, and spray deposition is after 30 seconds, and the vacuum unit that keeps the settling chamber to be used to bleed is in running order, settling chamber's internal gas pressure is-0.2～-0.3atm;
(9) after spray deposition is accomplished, vacuumize working chamber and spray deposition chamber, make the high temperature deposition base be in vacuum state, vacuum is lower than 10
-2Pa, after the cooling of alloy preform temperature was lower than 200 ℃, vacuum breaker took out deposit preform.
Advantage of the present invention and effect:
The present invention fully combines 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; Negative pressure spray deposition technology through optimal design; Prepare the volume density height, the high-alloying material that crystal grain is tiny (high temperature alloy, high-speed steel) spray deposition base is for materials such as reaction-injection moulding high-temperature alloy turbine disc, reaction-injection moulding mould steel lay the first stone.
Advantage of the present invention also comprises: prevent that 1. the close coupling atomizer from stopping up.The blockage problem of close coupling supersonic gas atomizer is the difficult problem that domestic and international spray deposition processing is difficult to solution always.Negative pressure spray deposition technology has prevented that the alloy molten steel is long because of transmission range, and 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 atomizes; 2. reduce the gas content in the deposit preform.From the gases at high pressure of superonic flow nozzzle ejection under suction function; Increased 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 when improving molten metal and arriving the deposit preform top, the discharge of the atomization gas that helps entraining into or carry secretly improves the density of deposit preform; 3. reduce the inner crystallite dimension of deposit preform; Because nebulization efficiency improves, the median particle diameter of atomizing molten drop further reduces, and crystallite dimension is littler in the deposit preform.Therefore, the size of metallurgical imperfection and field trash also further reduces, and has improved the metallurgical quality of alloy deposition base.Research shows that the square root of the bending strength of high-speed steel and limit defective diameter is inversely proportional to, and therefore eliminating large-sized inclusions becomes one of fundamental way that improves high-speed steel intensity and quality.All spray forming high-speed steels all are made up of the carbide (tungsten carbide, molybdenum carbide or vanadium carbide etc.) and the martensitic matrix of tempering.If skewness on 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 inner carbide of spray forming high-speed steel distributes very evenly in high-speed steel inside, therefore; Material wear ability is better, longer service life; 4. the equipment operation safe is reliable.Inert gas through vacuum system entering settling chamber might cause the indoor pressure of spray deposition sharply to raise, and causes danger.Force to discharge through negative pressure system, improved the security when system operates.
The present invention helps to improve the metallurgical quality and the performance of China's reaction-injection moulding high-alloying material (comprising high temperature alloy, high-speed steel etc.); Promote China's high performance jetting shaping high-alloying Development of Materials; The gap of developed countries such as shortening and America and Europe; Solving the key issue that restriction reaction-injection moulding high-alloying material is applied, is advanced aviation of China and airspace engine technology, and the innovation of processing and manufacturing instrument and progressive provides technical support.
The specific embodiment
Technical scheme of the present invention may further comprise the steps:
(1) adopts vacuum induction melting high-alloying metal material; Melting kettle adopts the 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) the 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 and charging: select a kind of high-alloying metal material, like the alloy pig of high temperature alloy or mould steel, the alloy material crucible of packing into;
(4) vacuumize, send the electrical induction 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 send the electrical heating alloy material;
(5) vacuum induction melting: increase intermediate frequency power supply power, molten alloy in vacuum environment.After alloy melted fully, refining 10～15 minutes made the alloy material of fusing more even and purer;
(6) inflation: the alloy refining under high vacuum environment charges into high purity inert gas (＞99.9%wt, O to working chamber and spray chamber after accomplishing
2＜2ppm), pressure is 0.95～1atm;
(7) negative pressure is taken out by the settling chamber: start the vacuum system of spray deposition chamber, vacuumize the settling chamber.The pressure reduction that keeps working chamber and spray deposition chamber through the vacuum unit between 0.25～0.5atm, i.e. P
The working chamber-P
The spray deposition chamber=0.3～0.4atm.
(8) negative pressure spray deposition: after the vacuum system of spray deposition chamber starts 3～5 seconds; Slowly pour in the tundish flow guide system that has heated by the speed of 20 kilograms of per minutes the uniform molten steel of refining in the induction melting crucible; After observing melt outflow mozzle lower end; Open the pressure gas valve of close coupling atomizer rapidly, the spray deposition alloy melt forms deposit preform with the 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.Behind the spray deposition 30 seconds, it is in running order to remain the vacuum unit that the settling chamber is used to bleed, and settling chamber's internal gas pressure is-0.2～-0.3atm;
The major advantage of negative pressure spray deposition comprises: 1. prevent the close coupling spray nozzle clogging.The blockage problem of close coupling supersonic gas atomizer is the difficult problem that domestic and international spray deposition processing is difficult to solution always.Negative pressure spray deposition technology has prevented that the alloy molten steel is long because of transmission range, and 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 atomizes; 2. reduce the gas content in the deposit preform.From the gases at high pressure of superonic flow nozzzle ejection under suction function; Increased 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 when improving molten metal and arriving the deposit preform top, the discharge of the atomization gas that helps entraining into or carry secretly improves the density of deposit preform; 3. reduce the field trash 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. the equipment operation safe is reliable.Inert gas through vacuum system entering settling chamber might cause the indoor pressure of spray deposition sharply to raise, and causes danger.Force to discharge through negative pressure system, improved the security when system operates.
(9) after spray deposition is accomplished, vacuumize working chamber and spray deposition chamber, make the high temperature deposition base be in vacuum state, vacuum is lower than 10
-2Pa.After the cooling of alloy preform temperature was lower than 200 ℃, vacuum breaker took out deposit preform.
Embodiment
With the alloy material chemical composition is (wt%): C1.5; W12.3; Co4.66; V5.2; Cr4.16; Mo0.22; The high-alloying material of surplus Fe is an example, and how much weight of putting into alloy material is by the decision of crucible size.
The main operating process that reaction-injection moulding prepares the high-alloying material is: adopt vacuum induction melting high-alloying metal material; Melting kettle adopts the 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; The reaction-injection moulding nozzle adopts the supersonic speed close coupling atomizer of autonomous Design; The gas pressure of spray deposition is 50～60atm; The alloy material crucible of packing into; Vacuumize working chamber, spray chamber vacuum＜1 * 10
-2Pa.Slowly send the electrical heating alloy material; Increase intermediate frequency power supply power, molten alloy in vacuum environment.After alloy melts fully, refining 10～15 minutes.The alloy refining charges into high purity inert gas (＞99.9%wt, O to working chamber and spray chamber after accomplishing
2＜2ppm), pressure is 0.95～1atm; Start the vacuum system of spray deposition chamber, the pressure reduction that keeps working chamber and spray deposition chamber through the vacuum unit between 0.25～0.5atm, i.e. P
The working chamber-P
The spray deposition chamber=0.3～0.4atm.After the vacuum system of spray deposition chamber starts 3～5 seconds; Slowly pour in the tundish flow guide system that has heated by the speed of 20 kilograms of per minutes the uniform molten steel of refining in the induction melting crucible; After observing melt outflow mozzle lower end; Open the high-pressure atomization gas valve of close coupling atomizer, the spray deposition alloy melt forms deposit preform to the 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.Behind the spray deposition 30 seconds, remain settling chamber's internal gas pressure and be-0.2～-0.3atm.Spray deposition after accomplishing vacuumizes working chamber and spray deposition chamber, makes the high temperature deposition base be in vacuum state, and vacuum is lower than 10
-2Pa.After the cooling of alloy preform temperature was lower than 200 ℃, vacuum breaker took out deposit preform.
Claims (1)
1. a negative pressure spray deposition processing that adopts the close coupling nozzle to prepare the high-alloying material the steps include:
(1) adopt vacuum induction melting high-alloying metal material: melting kettle adopts the 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) the reaction-injection moulding nozzle adopts supersonic speed close coupling atomizer: the gas pressure of spray deposition is 50～60atm;
(3) with the alloy melting kettle of packing into;
(4) vacuumize, send the electrical induction 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 send the electrical heating alloy material to alloy melting;
(5) vacuum induction melting: increase the power of vaccum sensitive stove, molten alloy in vacuum environment, treat that alloy melts fully after, refining 10～15 minutes makes the alloy material of fusing more even and purer;
(6) inflation: the alloy refining under high vacuum environment charges into high-purity argon gas to working chamber and spray chamber, purity＞99.9%wt, O after accomplishing
2＜2ppm, pressure are 0.95～1atm;
(7) negative pressure is taken out by the settling chamber: start the vacuum system of spray deposition chamber, vacuumize the settling chamber.The pressure reduction that keeps working chamber and spray deposition chamber through the vacuum unit between 0.25～0.5atm, i.e. P
The working chamber-P
The spray deposition chamber=0.3～0.4atm;
(8) negative pressure spray deposition: after the vacuum system of spray deposition chamber starts 3～5 seconds; Slowly pour in the tundish flow guide system that has heated by the speed of 20 kilograms of per minutes the uniform molten steel of refining in the induction melting crucible; After observing melt outflow mozzle lower end; Open the pressure gas valve of close coupling atomizer rapidly, the spray deposition alloy melt forms deposit preform with the molten drop jet deposition on the depositor of rotation; Atomization gas is a high-purity argon gas, purity＞99.99%wt, O
2＜2ppm, atomizing pressure are 80～100atm, and spray deposition is after 30 seconds, and the vacuum unit that keeps the settling chamber to be used to bleed is in running order, settling chamber's internal gas pressure is-0.2～-0.3atm;
(9) after spray deposition is accomplished, vacuumize working chamber and spray deposition chamber, make the high temperature deposition base be in vacuum state, vacuum is lower than 10
-2Pa, after the cooling of alloy preform temperature was lower than 200 ℃, the equipment vacuum breaker took out deposit preform.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107481771A (en) * | 2017-07-24 | 2017-12-15 | 清华大学 | Metal mold nuclear fuel base substrate and preparation method thereof |
| CN109692953A (en) * | 2018-12-28 | 2019-04-30 | 西安欧中材料科技有限公司 | A kind of aero-engine high temperature alloy diskware preparation method |
| CN111390174A (en) * | 2020-04-16 | 2020-07-10 | 佛山市孔星材料应用研究院有限公司 | 3D printing metal spraying equipment, 3D printing device and control method thereof |
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|---|---|---|---|---|
| CN107481771A (en) * | 2017-07-24 | 2017-12-15 | 清华大学 | Metal mold nuclear fuel base substrate and preparation method thereof |
| CN109692953A (en) * | 2018-12-28 | 2019-04-30 | 西安欧中材料科技有限公司 | A kind of aero-engine high temperature alloy diskware preparation method |
| CN109692953B (en) * | 2018-12-28 | 2021-08-31 | 西安欧中材料科技有限公司 | Preparation method of high-temperature alloy disc for aircraft engine |
| CN111390174A (en) * | 2020-04-16 | 2020-07-10 | 佛山市孔星材料应用研究院有限公司 | 3D printing metal spraying equipment, 3D printing device and control method thereof |
| 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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