CN103224396B - Composite crucible liner for vacuum anti-gravity casting of titanium and titanium alloys, and manufacturing method thereof - Google Patents
Composite crucible liner for vacuum anti-gravity casting of titanium and titanium alloys, and manufacturing method thereof Download PDFInfo
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- CN103224396B CN103224396B CN201310125155.3A CN201310125155A CN103224396B CN 103224396 B CN103224396 B CN 103224396B CN 201310125155 A CN201310125155 A CN 201310125155A CN 103224396 B CN103224396 B CN 103224396B
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Abstract
The invention relates to a composite crucible liner for vacuum anti-gravity casting of titanium and titanium alloys, and a manufacturing method thereof, and relates to a composite crucible liner for titanium and titanium alloys, and a manufacturing method thereof. In the prior art, a composite crucible liner used during vacuum anti-gravity casting of titanium and titanium alloys easily generates problems such as easy cracking on the surface and shedding. With the crucible liner and the manufacturing method thereof, the problems in the prior art can be solved. The scheme 1 comprises that: the crucible liner comprises yttrium oxide, zirconium oxide and calcium oxide. The scheme 2 comprises that: 1, a mixing solution A and the yttrium oxide are subjected to ball milling and uniform mixing, and then are pressed in a mold to manufacture a yttrium oxide monomer inner layer, 2, a mixing powder material B and absolute alcohol are subjected to ball milling and uniform mixing, and the obtained mixed solution and the manufactured yttrium oxide monomer inner layer from the step 1 are pressed into a biscuit, 3, a mixed powder material X and the prepared biscuit from the step 2 are pressed into a new biscuit, and 4, the process of the step 3 is repeated according to requirements, the pressed biscuit is subjected to drying and roasting to obtain a liner monomer, and the liner monomer is combined to form the crucible liner. The composite crucible liner is used in the field of titanium and titanium alloy molding through vacuum anti-gravity casting.
Description
Technical field
The present invention relates to composite crucible liner and manufacture method thereof for a kind of titanium or titanium alloy.
Background technology
The advantage of titanium or titanium alloy vacuum antigravity casting forming technology displays gradually along with casting quality increase in demand, especially in fields such as Aeronautics and Astronautics, medicine equipment, automobiles.But the fusing point of titanium or titanium alloy is high, and under molten state, chemically reactive is very high, almost can all react with current existing engineering materials, so its melting difficulty is large especially.The titanium or titanium alloy melting mode of industrial application is mainly vacuum consumable electrode skull melting and vacuum permanent electrode Cold Crucible Melting mode (comprising the melting of Forced water cooling copper crucible and non-water-cooled oxide compound, nitride crucible for smelting) at present.For vacuum consumable electrode skull melting, owing to conflicting with vacuum antigravity forming process riser pipe position in the introducing position of electrode, therefore seldom application in actual titanium or titanium alloy vacuum antigravity is shaped.The power consumption of Forced water cooling Cold Crucible Melting titanium or titanium alloy melt is huge, capacity usage ratio is low, in crucible, the titanium or titanium alloy melt temperature difference is huge, head temperature is lower, and surface alloying layer melt overheat degree only has tens degree to one hundred degree left and right, and cooling very fast, melt lower superheating temperature in surface often causes riser pipe to enter after melt, through transfusion, freeze at top, and then cause completing whole antigravity shaping process, serious also can cause structure deteriorate.For addressing the above problem someone, propose to adopt lime crucible to carry out melting titanium or titanium alloy, but can exceed standard for high-quality foundry goods oxygen level.In order to reduce oxygen level people again at lime crucible external coating yttrium oxide coating or boron nitride coating, but due to process technology limit, coating is thinner, the coefficient of thermal expansion of coating and lime crucible there are differences, it is excessive that alloy melting process produces thermal stresses gradient, in addition vacuum antigravity casting need to keep larger molten bath for a long time, the souring of melt is strong, these all can cause coating cracking, come off, water the foundry goods casting out and easily produce inclusion defect, when serious, cause foundry goods to be scrapped, the state of the art of the crucible lining of the use of titanium or titanium alloy fusing at present cannot meet the processing requirement that vacuum antigravity casting is produced.
Therefore, manufacture applicable vacuum antigravity casting titanium or titanium alloy and there is great actual application value with crucible lining, particularly, under existing scientific and technological level and crucible technology of preparing condition, be necessary to develop new crucible lining and can keep pure alloying constituent to solve the problem that inner surface of crucible thermal stresses gradient is easy to crack greatly, come off simultaneously.The present invention introduces gradient thought, can solve the inside and outside stress gradient of titanium or titanium alloy vacuum antigravity casting forming process cold crucible huge, the problem that cause crucible surface cracking, comes off, adopt gradient liner of the present invention manufacture crucible cracking resistance, anti-come off, scouring capability is strong, non-caked crucible after alloy melting, alloying constituent is pure stable, can keep for a long time large molten bath, can meet the requirement of crucible lining for titanium or titanium alloy vacuum antigravity casting, manufacture craft is ripe, equipment is simple, stable performance.
Summary of the invention
The object of this invention is to provide composite crucible liner and manufacture method thereof for a kind of vacuum antigravity casting titanium or titanium alloy, the problem that the composite crucible using when solving current vacuum antigravity casting titanium or titanium alloy is prone to surface cracking, comes off.
The present invention solves the problems of the technologies described above the technical scheme of taking to be: scheme one: described crucible lining consists of yttrium oxide, zirconium white and calcium oxide, the described crucible lining from the inside to the outside mass percent of yttrium oxide is reduced to 20% successively by 100%, and the mass percent of zirconium white and calcium oxide is increased to 80% successively by 0%;
Scheme two: described method comprises the steps: step 1, dehydrated alcohol and polyvinyl alcohol are made into mixed liquor A, wherein dehydrated alcohol is (95-99) with the volume parts ratio of polyvinyl alcohol: (1-5), described mixed liquor A mixes with yttrium oxide ball milling, wherein the mass ratio of the volume of mixed liquor A and yttrium oxide powder is (1-100) ml: 100g, the granularity of yttrium oxide powder is 325-1000 order, in mould, be pressed into yttrium oxide monomer internal layer, thickness is at 1-3mm;
Step 2, yttrium oxide, zirconium white and calcium oxide powder are formed to mixed powder B, wherein to account for the mass percent of mixed powder B be 75-95% for zirconium white and calcium oxide, mixed powder B mixes with dehydrated alcohol ball milling, wherein the quality of mixed powder B and the volume ratio of dehydrated alcohol are 100g: (2-100) ml, does is the granularity of mixed powder B 275-1000 order? be pressed into biscuit with together with yttrium oxide monomer internal layer prepared in step 1, pressure is 5-20MPa, yttrium oxide monomer internal layer is interior, and new biscuit thickness increase is controlled within the scope of 1-1.5mm;
Step 3, yttrium oxide, zirconium white and calcium oxide powder are formed to mixed powder X, wherein to account for the mass percent of mixed powder X be to increase by 5%～25% in previous step for calcium oxide and zirconium white, mixed powder X is pressed into new biscuit together with the biscuit of preparing in previous step, the 5%-30% of the pressure using when wherein pressure is greater than previous step moulding, mixed powder X is distributed in the outermost layer of biscuit all the time, new biscuit thickness increase is controlled within the scope of 1-1.5mm, and the granularity of mixed powder X is 475-5 order;
Step 4, foundation need the technological process of repeating step three, until biscuit thickness meets design requirement;
Step 5, the biscuit drying suppressing, roasting obtain liner monomer, the biscuit final molding pressure range wherein suppressing is at 10MPa-100MPa, and bake out temperature is 120 ℃-180 ℃, and the time is 1-24 hour, maturing temperature is 420 ℃-680 ℃, and the time is 1-6 hour;
Step 6, the liner combination of monomers after sintering is formed to crucible lining.
The present invention has following beneficial effect: (1) gradient liner is from inside to outside by yttrium oxide, zirconium white and calcium oxide composition gradient structure, thermal stresses has been alleviated the unmatched problem of material coefficient of thermal expansion by Gradient distribution, be pressed into after crucible high temperature sintering, internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.
(2) gradient liner innermost layer is yttrium oxide, good with the chemical stability of titanium or titanium alloy.Alloying constituent is even, stable performance.
(3) the divisible assembling of gradient liner, has reduced the moulding difficulty of monocycle, makes follow-up crucible design more flexible, and required equipment is simple, and constant product quality is good, is applicable to producing in enormous quantities.
(4) gradient liner can be sintered to whole service life through a step and backing layer or supporting layer and significantly improves when making crucible.
Accompanying drawing explanation
Fig. 1 is the one-piece construction front view of crucible lining of the present invention, and Fig. 2 is the schema of the inventive method.
Embodiment
Embodiment one: the crucible lining of present embodiment consists of yttrium oxide, zirconium white and calcium oxide, the described crucible lining from the inside to the outside mass percent of yttrium oxide is reduced to 20% successively by 100%, and the mass percent of zirconium white and calcium oxide is increased to 80% successively by 0%.
Embodiment two: when the crucible lining thickness of present embodiment is 6mm, when thickness range is 0-3mm from the inside to the outside, the mass percent of yttrium oxide is 100%; The mass percent 90%-99% of yttrium oxide when thickness range is 3-4.5mm, the mass percent of zirconium white and calcium oxide is 1%-10%; The mass percent 80%-89% of yttrium oxide when thickness range is 4.5-6mm, the mass percent of zirconium white and calcium oxide is 11%-20%, the advantage of this method is that gradient liner is from inside to outside by yttrium oxide, zirconium white and calcium oxide composition gradient structure, thermal stresses has been alleviated the unmatched problem of material coefficient of thermal expansion by Gradient distribution, be pressed into after crucible high temperature sintering, internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other embodiment is identical with embodiment one.
Embodiment three: in conjunction with Fig. 1 and Fig. 2, present embodiment is described, the method for present embodiment comprises the steps:
Step 1, dehydrated alcohol and polyvinyl alcohol are made into mixed liquor A, wherein dehydrated alcohol is (95-99) with the volume parts ratio of polyvinyl alcohol: (1-5), described mixed liquor A mixes with yttrium oxide ball milling, wherein the mass ratio of the volume of mixed liquor A and yttrium oxide powder is (1-100) ml: 100g, the granularity of yttrium oxide powder is 325-1000 order, in mould, be pressed into yttrium oxide monomer internal layer, thickness is at 1-3mm;
Step 2, yttrium oxide, zirconium white and calcium oxide powder are formed to mixed powder B, wherein to account for the mass percent of mixed powder B be 75-95% for zirconium white and calcium oxide, mixed powder B mixes with dehydrated alcohol ball milling, wherein the quality of mixed powder B and the volume ratio of dehydrated alcohol are 100g: (2-100) ml, does is the granularity of mixed powder B 275-1000 order? be pressed into biscuit with together with yttrium oxide monomer internal layer prepared in step 1, pressure is 5-20MPa, yttrium oxide monomer internal layer is interior, and new biscuit thickness increase is controlled within the scope of 1-1.5mm;
Step 3, yttrium oxide, zirconium white and calcium oxide powder are formed to mixed powder X, wherein to account for the mass percent of mixed powder X be to increase 5%-25% in previous step for calcium oxide and zirconium white, mixed powder X is pressed into new biscuit together with the biscuit of preparing in previous step, the 5%-30% of the pressure using when wherein pressure is greater than previous step moulding, mixed powder X is distributed in the outermost layer of biscuit all the time, new biscuit thickness increase is controlled within the scope of 1-1.5mm, and the granularity of mixed powder X is 475-5 order;
Step 4, foundation need the technological process of repeating step three, until biscuit thickness meets design requirement;
Step 5, the biscuit drying suppressing, roasting obtain liner monomer 1, the biscuit final molding pressure range wherein suppressing is at 10MPa-100MPa, and bake out temperature is 120 ℃-180 ℃, and the time is 1-24 hour, maturing temperature is 420 ℃-680 ℃, and the time is 1-6 hour;
Step 6, the liner monomer after sintering 1 combination is formed to crucible lining.
Embodiment four: in conjunction with Fig. 2, present embodiment is described, the manufacture method of composite crucible liner for the vacuum antigravity casting titanium or titanium alloy of present embodiment, is characterized in that yttrium oxide powder used in step 1 is 425 orders.The advantage of this step is good with the chemical stability of titanium or titanium alloy, obtains alloying constituent even, and cast properties is stable.Other embodiment is identical with embodiment three.
Embodiment five: in conjunction with Fig. 2, present embodiment is described, in the step 1 of present embodiment, dehydrated alcohol is 95: 5 with the volume parts ratio of polyvinyl alcohol.The advantage of this step is can give full play to the bond effect of polyvinyl alcohol after absolute ethanol volatilizes.Other embodiment is identical with embodiment three.
Embodiment six: in conjunction with Fig. 2, present embodiment is described, in the step 1 of present embodiment, the mass ratio of the volume of mixed liquor A and yttrium oxide powder is 25ml: 100g.The advantage of this step is more easy-formation of subsequent process compacting yttrium oxide monomer.Other embodiment is identical with embodiment three.
Embodiment seven: in conjunction with Fig. 2, present embodiment is described, is pressed into yttrium oxide monomer internal layer in the step 1 of present embodiment after mixing in mould, thickness is 2mm, forming pressure 16MPa.The advantage of this step is the high and easy demoulding of the degree of packing more of yttrium oxide monomer internal layer.Other embodiment is identical with embodiment three.
Embodiment eight: in conjunction with Fig. 2, present embodiment is described, in the step 2 of present embodiment, the quality of mixed powder B and the volume ratio of dehydrated alcohol are 100g: 25ml.The advantage of this step is that mixed powder B is more prone to mix.Other embodiment is identical with embodiment three.
Embodiment nine: in conjunction with Fig. 2, present embodiment is described, in the step 2 of present embodiment, in yttrium oxide, zirconium white and calcium oxide, the ratio of quality and the number of copies of powder is 90: 8: 2.The advantage of this step is to form at yttrium oxide monomer internal layer the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.Other embodiment is identical with embodiment three.
Embodiment ten: in conjunction with Fig. 2, present embodiment is described, in the step 3 of present embodiment, yttrium oxide granularity is that 400 orders, zirconium white granularity are that 270 orders and calcium oxide granularity are 300 orders.The advantage of this step is that such size-grade distribution can obtain fine and close liner monomer.Other embodiment is identical with embodiment three.
Embodiment 11: present embodiment is described in conjunction with Fig. 2, the method of present embodiment comprises the steps: step 1, dehydrated alcohol and polyvinyl alcohol is made into mixed solution, dehydrated alcohol is 97: 3 with the volume parts ratio of polyvinyl alcohol, mixed solution ball milling together with 400 object yttrium oxide powder mixes, the ratio of the quality of the volume of mixed solution and yttrium oxide powder is 15ml: 100g, after mixing, in mould, be pressed into yttrium oxide monomer internal layer, thickness is 2.5mm, forming pressure 15MPa;
Step 2, yttrium oxide, zirconium white and calcium oxide powder are mixed with dehydrated alcohol ball milling, yttrium oxide, zirconium white and the quality of calcium oxide mixed powder and the volume ratio of dehydrated alcohol are 15ml: 100g, and in mixed powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is 90: 5: 5.The granularity of yttrium oxide is that 400 orders, zirconic granularity are that the granularity of 325 orders and calcium oxide is 325 orders, after mixing, is pressed into biscuit, forming pressure 18MPa with together with yttrium oxide monomer internal layer prepared in step 1.Yttrium oxide monomer internal layer is at innermost layer.New biscuit thickness increases 1.2mm;
In step 3, increase previous step, zirconium white and calcium oxide account for the degree of mixed powder, make the relative content of yttrium oxide reduce 10%, in powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is 80: 10: 10, the granularity of yttrium oxide is that 400 orders, zirconic granularity are that the granularity of 300 orders, calcium oxide is 270 orders, mix rear new ratio powder and be pressed into new biscuit together with the biscuit of preparing in previous step, the new powder mixing is distributed in the outermost layer of biscuit all the time.New biscuit thickness increases 1.0mm.Forming pressure 20MPa;
The technological process of step 4, repeating step 35 times, the relative proportion of yttrium oxide, zirconium white and calcium oxide in each powder (yttrium oxide: zirconium white: calcium oxide) be followed successively by 70: 12: 18,60: 18: 22,45: 24: 31,30: 30: 40,15: 35: 50.The granularity of yttrium oxide is the granularity that 400 orders, zirconic granularity are 300 orders, calcium oxide and respectively is 240 orders, 200 orders, 180 orders, 100 orders, 30 orders.Each new biscuit thickness increases 1.5mm.Each forming pressure respectively is 24MPa, 30MPa, 36MPa, 42MPa and 50MPa.
Step 5, the biscuit bake out temperature suppressing are 140 ℃-145 ℃, and the time is 1 hour, and maturing temperature is 650 ℃, and the time is 3 hours.Obtain the present invention's gradient liner.
Step 6, the liner combination of monomers after sintering is formed to the present invention's gradient liner.
The advantage of this method is: crucible lining monomer can freely be assembled, and makes follow-up crucible design more flexible, and monomer moulding difficulty is low, and required equipment is simple, and constant product quality is good, is applicable to producing in enormous quantities.Be pressed into after crucible high temperature sintering, internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.The high-temperature titanium alloys such as melting Ti600, Ti1100 and IMI834 are respond well, stable components.
Embodiment 12: present embodiment is different from embodiment three is that the ratio of quality and the number of copies of powder in yttrium oxide in step 2, zirconium white and calcium oxide is 90: 8: 2.The advantage of this step is to form at yttrium oxide monomer internal layer the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.Other are identical with embodiment three.
Embodiment 13: what present embodiment was different from embodiment three is that yttrium oxide, zirconium white and the quality of calcium oxide mixed powder and the volume ratio of dehydrated alcohol used in step 2 is 100g: 25ml, and in yttrium oxide, zirconium white and calcium oxide, the ratio of quality and the number of copies of powder is 90: 7: 3.The advantage of this step more easily mixes while being the mixed powder of such ratio.Other are identical with embodiment three.
Embodiment 14: what present embodiment was different from embodiment three is that in step 2, yttrium oxide is that 400 orders, zirconium white are that 300 orders and calcium oxide are 300 orders.The advantage of this step is to form at yttrium oxide monomer internal layer the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.。Other are identical with embodiment three.
Embodiment 15: what present embodiment was different from embodiment three is that in step 2, yttrium oxide is that 400 orders, zirconium white are that 270 orders and calcium oxide are 300 orders.The advantage of this step is to form at yttrium oxide monomer internal layer the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.Other are identical with embodiment three.
Embodiment 16: what present embodiment was different from embodiment three is that in step 2, yttrium oxide is that 400 orders, zirconium white are that 270 orders and calcium oxide are 300 orders.In yttrium oxide, zirconium white and calcium oxide, the ratio of quality and the number of copies of powder is 90: 6: 4.The advantage of this step is to form at yttrium oxide monomer internal layer the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.Other are identical with embodiment three.
Embodiment 17: what present embodiment was different from embodiment three is that in step 3, yttrium oxide is that 400 orders, zirconium white are that 270 orders and calcium oxide are 300 orders.The advantage of this step is that the biscuit of preparing in step 2 forms transition layer outward, makes each layer of follow-up transition even, fine and close.Other are identical with embodiment three.
Embodiment 18: what present embodiment was different from embodiment three is that in step 3, yttrium oxide is that 400 orders, zirconium white are that 270 orders and calcium oxide are 270 orders.The advantage of this step is to form transition layer outward at biscuit, makes each layer of follow-up transition even, fine and close.Other are identical with embodiment three.
Embodiment 19: what present embodiment was different from embodiment three is the relative content minimizing 8% of yttrium oxide in step 3, and in powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is 82: 8: 10.The advantage of this step is that biscuit forms the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.Other are identical with embodiment three.
Embodiment 20: present embodiment is different from embodiment three is that the ratio of quality and the number of copies of yttrium oxide in step 3, zirconium white and calcium oxide is 85: 8: 7.The advantage of this step is that biscuit forms the gradient layer that yttrium oxide reduces gradually outward, makes each layer of follow-up yttrium oxide gradient transition even.Other are identical with embodiment three.
Embodiment 21: present embodiment is different from embodiment three is that the ratio of quality and the number of copies of yttrium oxide in step 3, zirconium white and calcium oxide is 85: 8: 7, and yttrium oxide granularity is that 400 orders, zirconium white granularity are that 270 orders and calcium oxide granularity are 300 orders.The advantage of this step is that biscuit forms the gradient layer that yttrium oxide reduces gradually outward, and yttrium oxide gradient transition is even, the degree of packing is moderate to make follow-up each layer.Other are identical with embodiment three.
Embodiment 22: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, relative proportion (the yttrium oxide: zirconium white: calcium oxide) be followed successively by 70: 15: 15 of yttrium oxide, zirconium white and calcium oxide in each powder, 60: 16: 28,45: 24: 31,30: 30: 40,15: 35: 50.The advantage of this step is that the liner prepared is used while being applicable to compared with jogging speed melting titanium alloy, and during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 23: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, in each powder the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide be followed successively by 70: 18: 12,60: 18: 22,45: 24: 31,30: 28: 42,15: 35: 50.When the advantage of this step is the applicable fast speed melting titanium alloy of liner of preparing, use, during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 24: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, in each powder the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide be followed successively by 70: 15: 15,60: 18: 22,45: 24: 31,30: 28: 42,15: 35: 50.When the advantage of this step is the applicable moderate speed's melting titanium alloy of liner of preparing, use, during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 25: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, yttrium oxide granularity respectively is 400 orders, 375 orders, 325 orders, 300 orders, 300 orders, and zirconium white granularity is 300 orders and calcium oxide granularity respectively is 240 orders, 200 orders, 180 orders, 100 orders, 30 orders.The advantage of this step is that the liner prepared is applicable to fusing amount less, use during small power melting titanium alloy, and during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 26: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, yttrium oxide granularity respectively is 400 orders, 375 orders, 375 orders, 325 orders, 325 orders, and zirconium white granularity is 300 orders and calcium oxide granularity respectively is 240 orders, 200 orders, 180 orders, 100 orders, 30 orders.The advantage of this step is that the liner prepared is applicable to that fusing amount is medium, use during mid power melting titanium alloy, and during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 27: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, yttrium oxide granularity is respectively 400 orders, 375 orders, 375 orders, 325 orders, 325 orders for 5 times, zirconium white granularity is 325 orders for 5 times and calcium oxide granularity is respectively 240 orders 5 times, 200 orders, 180 orders, 100 orders, 30 orders.The advantage of this step is that the liner prepared is applicable to that fusing amount is medium, use during small power melting titanium alloy, and during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 28: present embodiment is different from embodiment three is the technological process 5 times of repeating step three in step 4, yttrium oxide granularity respectively is 400 orders, 375 orders, 375 orders, 375 orders, 325 orders, zirconium white granularity is 325 orders and calcium oxide granularity respectively is 240 orders, 200 orders, 150 orders, 100 orders, 40 orders.The advantage of this step is that the liner prepared is applicable to fusing amount less, use during high-power melting titanium alloy, and during fusing, thermal stresses can better be alleviated, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 29: present embodiment is different from embodiment three is the technological process 4 times of repeating step three in step 4, in each powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is followed successively by 70: 12: 18,60: 18: 22,45: 24: 31,30: 30: 40, yttrium oxide granularity respectively was 400 orders, 375 orders, 375 orders, 325 orders, zirconium white granularity is 325 orders and calcium oxide granularity respectively is 240 orders, 180 orders, 100 orders, 40 orders.Each new biscuit thickness increases 1.5mm.Each forming pressure respectively is 24MPa, 30MPa, 36MPa, 42MPa.The advantage of this step is that the liner prepared is applicable to that fusing amount is little, small power melting titanium alloy and vacuum antigravity compacting pressure are used when lower, and crucible lining preparation technology is simple, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 30: present embodiment is different from embodiment three is the technological process 4 times of repeating step three in step 4, in each powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is followed successively by 70: 15: 15,60: 20: 20,45: 24: 31,30: 30: 40.Yttrium oxide granularity is respectively 400 orders, 375 orders, 375 orders, 325 orders for 4 times, and zirconium white granularity is 325 orders for 4 times and calcium oxide granularity is respectively 240 orders, 180 orders, 100 orders, 40 orders for 4 times.Each new biscuit thickness increases 1.5mm.Each forming pressure is respectively 24MPa, 30MPa, 36MPa, 42MPa.The advantage of this step is that the liner prepared is applicable to that fusing amount is little, mid power melting titanium alloy and vacuum antigravity compacting pressure are used when lower, and crucible lining preparation technology is simple, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 31: present embodiment is different from embodiment three is the technological process 4 times of repeating step three in step 4, in each powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is followed successively by 70: 15: 15,60: 18: 22,45: 22: 33,30: 28: 42, yttrium oxide granularity is respectively 400 orders, 375 orders, 375 orders, 325 orders for 4 times, and zirconium white granularity is 325 orders for 4 times and calcium oxide granularity is respectively 270 orders, 180 orders, 100 orders, 60 orders for 4 times.Each new biscuit thickness increases 1.4mm.Each forming pressure is respectively 24MPa, 30MPa, 36MPa, 42MPa.The advantage of this step is that the liner prepared is applicable to little, the high-power melting titanium alloy of fusing amount and vacuum antigravity compacting pressure is used when lower, and crucible lining preparation technology is simple, and internal surface splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 32: present embodiment is different from embodiment three is the technological process 6 times of repeating step three in step 4, in each powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is followed successively by 70: 15: 15,60: 18: 22,45: 22: 33,30: 28: 42,15: 35: 50,5: 38: 57.Yttrium oxide granularity is respectively 400 orders, 375 orders, 375 orders, 325 orders, 325 orders, 325 orders for 6 times, and zirconium white granularity is 325 orders for 6 times and calcium oxide granularity is respectively 270 orders, 180 orders, 140 orders, 100 orders, 60 orders, 30 orders for 6 times.The each new biscuit thickness of front 3 circulation increases 1.4mm, and the each new biscuit thickness of rear 3 circulation increases 2mm.Each forming pressure is respectively 24MPa, 30MPa, 36MPa, 42MPa, 50MPa, 60MPa.The advantage of this step is that the liner prepared is applicable to medium, the high-power fusing high-temperature titanium alloy of fusing amount and vacuum antigravity compacting pressure is used when higher, and inner surface of crucible splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 33: present embodiment is different from embodiment three is the technological process 6 times of repeating step three in step 4, in each powder, the ratio of quality and the number of copies of yttrium oxide, zirconium white and calcium oxide is followed successively by 70: 15: 15,60: 20: 22,45: 22: 33,30: 28: 42,15: 35: 50,5: 35:60.Yttrium oxide is respectively 400 orders, 400 orders, 375 orders, 375 orders, 325 orders, 325 orders for 6 times, zirconium white is respectively 325 orders, 325 orders, 325 orders, 300 orders, 300 orders and 300 orders for 6 times, and calcium oxide is respectively 270 orders, 180 orders, 140 orders, 100 orders, 60 orders, 30 orders for 6 times.The each new biscuit thickness of front 3 circulation increases 1.4mm, and the each new biscuit thickness of rear 3 circulation increases 2mm.Each forming pressure is respectively 24MPa, 30MPa, 36MPa, 42MPa, 50MPa, 60MPa.The advantage of this step is that the liner prepared is applicable to large, the high-power melting titanium alloy of fusing amount and vacuum antigravity compacting pressure is used when higher, and inner surface of crucible splitting resistance is good, erosion resistibility is strong, and pot life is long.Other are identical with embodiment three.
Embodiment 34: what present embodiment was different from embodiment three is that the biscuit bake out temperature suppressing in step 5 is 120 ℃-130 ℃, and the time is 8 hours, and maturing temperature is 650 ℃, and the time is 3 hours.The advantage of this step is that the mechanical property of liner monomer is good.Other are identical with embodiment three.
Embodiment 35: what present embodiment was different from embodiment three is that the biscuit bake out temperature suppressing in step 5 is 150 ℃-160 ℃, and the time is 10 hours, and maturing temperature is 600 ℃, and the time is 4 hours.The advantage of this step is that mechanical property and the dimensional precision net effect of liner monomer is good.Other are identical with embodiment three.
Embodiment 36: what present embodiment was different from embodiment three is that the biscuit bake out temperature suppressing in step 5 is 130 ℃-140 ℃, and the time is 8 hours, and maturing temperature is 600 ℃, and the time is 4 hours.The advantage of this step is that the dimensional precision of liner monomer is high.Other are identical with embodiment three.
Claims (8)
1. a vacuum antigravity casting titanium or titanium alloy composite crucible liner, while it is characterized in that described crucible lining thickness is 6mm, when thickness range is 0-3mm from the inside to the outside, the mass percent of yttrium oxide is 100%; The mass percent 90%-99% of yttrium oxide when thickness range is 3-4.5mm, the mass percent of zirconium white and calcium oxide is 1%-10%; The mass percent 80%-89% of yttrium oxide when thickness range is 4.5-6mm, the mass percent of zirconium white and calcium oxide is 11%-20%.
2. the manufacture method of composite crucible liner for a vacuum antigravity casting titanium or titanium alloy, described crucible lining is by yttrium oxide, zirconium white and calcium oxide form, the described crucible lining from the inside to the outside mass percent of yttrium oxide is reduced to 20% successively by 100%, the mass percent of zirconium white and calcium oxide is increased to 80% successively by 0%, it is characterized in that described method comprises the steps: step 1, dehydrated alcohol and polyvinyl alcohol are made into mixed liquor A, wherein dehydrated alcohol is (95-99) with the volume parts ratio of polyvinyl alcohol: (1-5), described mixed liquor A mixes with yttrium oxide ball milling, wherein the mass ratio of the volume of mixed liquor A and yttrium oxide powder is (1-100) ml:100g, the granularity of yttrium oxide powder is 325-1000 order, in mould, be pressed into yttrium oxide monomer internal layer, thickness is at 1-3mm,
Step 2, yttrium oxide, zirconium white and calcium oxide powder are formed to mixed powder B, wherein to account for the mass percent of mixed powder B be 75% for zirconium white and calcium oxide, mixed powder B mixes with dehydrated alcohol ball milling, wherein the quality of mixed powder B and the volume ratio of dehydrated alcohol are 100g:(2-100) ml, the granularity of mixed powder B is 275-1000 order, be pressed into biscuit with together with yttrium oxide monomer internal layer prepared in step 1, pressure is 5-20MPa, yttrium oxide monomer internal layer is interior, and new biscuit thickness increase is controlled within the scope of 1-1.5mm;
Step 3, yttrium oxide, zirconium white and calcium oxide powder are formed to mixed powder X, wherein to account for the mass percent of mixed powder X be to increase by 5% in previous step for calcium oxide and zirconium white, mixed powder X is pressed into new biscuit together with the biscuit of preparing in previous step, the 5%-30% of the pressure using when wherein pressure is greater than previous step moulding, mixed powder X is distributed in the outermost layer of biscuit all the time, new biscuit thickness increase is controlled within the scope of 1-1.5mm, and the granularity of mixed powder X is 475-5 order;
Step 4, foundation need the technological process of repeating step three, until biscuit thickness meets design requirement;
Step 5, the biscuit drying suppressing, roasting obtain liner monomer (1), the biscuit final molding pressure range wherein suppressing is at 10MPa-100MPa, and bake out temperature is 120 ℃-180 ℃, and the time is 1-24 hour, maturing temperature is 420 ℃-680 ℃, and the time is 1-6 hour;
Step 6, liner monomer (1) combination after sintering is formed to crucible lining.
3. the manufacture method of composite crucible liner for vacuum antigravity casting titanium or titanium alloy according to claim 2, is characterized in that yttrium oxide powder used in step 1 is 425 orders.
4. the manufacture method of composite crucible liner for vacuum antigravity casting titanium or titanium alloy according to claim 2, it is characterized in that in step 1 dehydrated alcohol with the volume parts of polyvinyl alcohol than being 95:5.
5. the manufacture method of composite crucible liner for vacuum antigravity casting titanium or titanium alloy according to claim 2, is characterized in that the volume of mixed liquor A in step 1 and the mass ratio of yttrium oxide powder are 25ml:100g.
6. the manufacture method of composite crucible liner for vacuum antigravity casting titanium or titanium alloy is according to claim 2 pressed into yttrium oxide monomer internal layer after it is characterized in that mixing in step 1 in mould, and thickness is 2mm, forming pressure 16MPa.
7. the manufacture method of composite crucible liner for vacuum antigravity casting titanium or titanium alloy according to claim 2, is characterized in that in step 2 that the quality of mixed powder B and the volume ratio of dehydrated alcohol are 100g:25ml.
8. the manufacture method of composite crucible liner for vacuum antigravity casting titanium or titanium alloy according to claim 2, is characterized in that in step 3, yttrium oxide granularity is that 400 orders, zirconium white granularity are that 270 orders and calcium oxide granularity are 300 orders.
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