CN103071764B - For the CaZrO of titanium or titanium alloy hot investment casting 3the preparation method of shell - Google Patents
For the CaZrO of titanium or titanium alloy hot investment casting 3the preparation method of shell Download PDFInfo
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- CN103071764B CN103071764B CN201210499809.4A CN201210499809A CN103071764B CN 103071764 B CN103071764 B CN 103071764B CN 201210499809 A CN201210499809 A CN 201210499809A CN 103071764 B CN103071764 B CN 103071764B
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Abstract
The present invention discloses a kind of CaZrO for titanium or titanium alloy hot investment casting
3the preparation method of shell take calcium zirconate as filler, the binding agent that acetic acid zirconium or yttrium colloidal sol etc. do not react with titanium alloy, makes shell through operations such as pretreatment, shaping, sclerosis, sintering.This shell and the titanium or titanium alloy extent of reaction little, cast(ing) surface formed pickup layer thickness little; The intensity of calcium zirconate ceramics shell is high, cast(ing) surface highly polished; The not easily gelling of coating stabilization containing calcium zirconate, suspension is good, and the holding time is long.
Description
Technical field
The present invention relates to a kind of CaZrO for titanium or titanium alloy hot investment casting
3the preparation method of shell.
Background technology
Titanium or titanium alloy has that density is little, specific strength is high, corrosion-resistant, the characteristic of a series of excellence such as good biocompatibility, is widely used in the every field such as Aeronautics and Astronautics, chemical industry, medical treatment.But titanium is high chemically active metal, in the molten state, almost can with all known refractory material generation chemical reactions.This refractory material just needing Ti alloy casting to use and binding agent there is very high chemical stability.
The titanium alloy precision casting shell that current use is more, is broadly divided into: graphite shell, tungsten surface layer ceramic shell, New Oxide Ceramic Shell Mould etc.Wherein, graphite shell the foundry goods pouring into a mould out, have the α brittle layer of one deck carburizing from the teeth outwards, thickness is approximately 0.2 ~ 0.3mm, and it likely causes generation and the expansion of crackle under effect of stress.The heat endurance of graphite shell has certain limit, when graphite contacts with titanium liquid, under the condition reaching Activation energy, heat release chain reaction sharply likely occurs, therefore the complicated titanium alloy casting of the unsuitable casting large of graphite shell.In addition, the shrinkage factor of graphite shell is high, is the twice of common fusible pattern ceramic shell, and this have impact on the precision of fusible pattern graphite shell titanium alloy fine casting part.Time prepared by tungsten surface layer ceramic shell, tungsten powder uses as the filler in coating, and the quality of performance on shell of tungsten powder has great impact, the purity that tungsten powder answers tool higher, impurity content can not exceed specified standard, exceeding standard of oxygen, carbon content, will affect the quality of titanium casting.Tungsten surface layer investment shell must adopt solvent dewaxing, thus has very large injury to health, simultaneously also contaminated environment.The roasting under reducing atmosphere of tungsten surface shell, the mould material ash content be deposited on after dewaxing on shell surface is difficult to burn, and is easy to react with liquid titanium when pouring into a mould, and forms pore at cast(ing) surface.Mainly employ zirconia, yittrium oxide, calcium oxide etc. in the surface layer of New Oxide Ceramic Shell Mould and adjacent bed coating and react less oxide with titanium liquid, investment precoat casting character wherein using yittrium oxide as filler is better, but easily there is hydration in yittrium oxide, its slurry is very responsive to pH value change, easy gelling.New Oxide Ceramic Shell Mould cannot be avoided forming α pickup layer at cast(ing) surface in addition, and the thickness of α pickup layer is not from 0.02 ~ 0.2mm etc.
Summary of the invention
For the defect that prior art exists, the object of the present invention is to provide a kind of CaZrO for titanium or titanium alloy hot investment casting
3shell and preparation method thereof.
For achieving the above object, the present invention adopts following technical scheme:
A kind of CaZrO for titanium or titanium alloy hot investment casting
3shell, be made up of surface layer, secondary surface layer and backing layer, described surface layer is made up of surface layer filler and surface layer binding agent, described surface layer filler is calcium zirconate, described calcium zirconate is for being less than 200 object powder particles, described surface layer binding agent is the binding agent do not reacted with titanium alloy, and the weight proportion of surface layer filler and surface layer binding agent is 3:1 ~ 5:1; Described backing layer or secondary surface layer are made up of backing layer or secondary surface layer binding agent and backing layer or secondary surface layer filler.
Above-mentioned surface layer binding agent is the one of colloidal zirconia, colloidal yttria, acetic acid zirconium, zirconium nitrate or yttrium colloidal sol.
Above-mentioned backing layer or secondary surface layer binding agent are the one of waterglass, silicon melten gel or silester.
Above-mentioned backing layer or secondary surface layer filler are mullite powder.
A kind of CaZrO for titanium or titanium alloy hot investment casting
3the preparation method of shell, has following process and step:
The pretreatment of a calcium zirconate raw material: by levigate through ball milling for the calcium zirconate powder after pickling, obtains being less than 200 object calcium zirconate particles;
The preparation of b investment precoat: add through pretreated calcium zirconate in surface layer binding agent, and constantly stir with agitator, add additive in right amount; Additive is made up of surfactant and defoamer; The weight proportion of investment precoat is: 65 ~ 84.5wt% calcium zirconate, 15 ~ 35wt% surface layer binding agent, 0.1 ~ 0.5wt% surfactant and 0.1 ~ 0.5wt% defoamer form; No. 4 flow cups made in U.S.A are used to control to be coated with the viscosity of slip at 15 ~ 65s;
The preparation of c backing layer or secondary investment precoat: the weight proportion of backing layer or secondary investment precoat is: backing layer or secondary surface layer filler: backing layer or secondary surface layer binding agent=(3.5-4.5): 1;
The preparation of d shell: after coating prepares, wax-pattern is immersed in investment precoat, when unnecessary investment precoat gutters down, and investment precoat is coated with when hanging on wax-pattern equably carry out stucco, 80 ~ 120 object calcium zirconate powder are sprinkling upon equably and have been coated with on coating wax-pattern; After the fully dry and sclerosis of coating, then repeat 1-2 above-mentioned steps; And then being coated with backing layer or secondary investment precoat, its viscosity of the coating of composition controls at 10 ~ 20s, and then uses mullite powder stucco; Repeat 2-3 time; Then dry;
The dewaxing of e shell: dried shell is used high steam still or microwave dewaxing;
The sintering of f shell: the shell dewaxed is put into roaster and sinters in atmosphere, sintering temperature 850 ~ 1350 DEG C, sinters one hour, then at 300 DEG C, is incubated 2 ~ 3 hours, cools to room temperature with the furnace subsequently, obtain shell finished product.
Surfactant in above-mentioned steps b is the one as stearic acid or neopelex.
Defoamer in above-mentioned steps b is the one of dimethyl silicone polymer, silicone emulsion, the fatty acid ester compounded thing of higher alcohols, polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy propyl alcohol amidogen ether, polypropylene glycerol aether or polyoxypropylene.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant progress:
CaZrO
3caO---ZrO
2a kind of compound that in system, content is high and the most stable, it not only has good hydration resistance, also has very high fusing point.CaZrO
3investment shell intensity is high, and surperficial is highly polished, little with the titanium or titanium alloy extent of reaction, and the pickup layer thickness that cast(ing) surface is formed is little; Containing CaZrO
3coating stabilization not easily gelling, suspension is good, and the holding time is long.
Accompanying drawing explanation
Fig. 1 shell structural representation.
Shell (left rear, right for before cast for pouring into a mould) before and after Fig. 2 pours into a mould.
Fig. 3 knocks out the local of the alloy after part shell.
Fig. 4 removes the alloy of shell completely.
Detailed description of the invention
After specific embodiments of the invention being described in below in conjunction with accompanying drawing.
embodiment 1
The present embodiment is preparation process and the step of using calcium zirconate Shell Preparation TiAl alloy foundry goods:
(1) preparation of coating: add binding agent two acetic acid zirconium in calcium zirconate powder that is levigate, that cross 200 mesh sieves, constantly stir with agitator, control the viscosity of painting slip greatly about 30s, the weight ratio 4.5:1 of calcium zirconate powder and binding agent;
(2) preparation of shell: wax-pattern is immersed in the above-mentioned coating configured, stay a minute, when allowing coating be coated with equably to hang on wax-pattern, can stucco, be dispersed in equably by calcium zirconate dry powder and be coated with on coating wax-pattern, stucco process repeats 1 time; And then carry out backing layer coating; Backing layer coating binding agent used is ethyl silicate or Ludox, and filler used is mullite powder, and both weight proportions are 1:4; This backing layer paint slurry is coated on the skin of above-mentioned coating wax-pattern, carries out stucco with thicker mullite powder more subsequently; Backing layer coating is by this operation repetition 3 times; The gross thickness of final formation coating is 5mm.
(3) the above-mentioned wax-pattern with laminated coating is carried out drying, after sclerosis to be dried, remove wax-pattern, form shell.
(4) sintering of shell; The shell dewaxed is put into roaster roasting under nitrogen protection, sintering temperature 1250 DEG C, sinter 1 hour, in 300 DEG C of insulations 2 hours, cool to room temperature with the furnace subsequently, finally make the calcium zirconate ceramics shell for titanium or titanium alloy hot investment casting.
(5) cast of TiAl alloy: the high temperature TiAl alloy of coming out of the stove is injected the calcium zirconate shell made, removes shell i.e. obtained required TiAl alloy cast after cooling.
Through the Ti-Al alloy cast that this operation is poured into a mould, without significant reaction layer, any surface finish, alloy property is good.
embodiment 2
The present embodiment is preparation process and the step of using calcium zirconate Shell Preparation TiNi alloy foundry goods
(1) preparation of coating: add binding agent two acetic acid zirconium in calcium zirconate powder that is levigate, that cross 200 mesh sieves, constantly stir with agitator, control the viscosity of painting slip greatly about 30s, the weight ratio 3.5:1 of calcium zirconate powder and binding agent;
(2) preparation of shell: wax-pattern is immersed in the above-mentioned coating configured, stay a minute, when allowing coating be coated with equably to hang on wax-pattern, can stucco, calcium zirconate dry powder is dispersed in equably be coated with on coating wax-pattern, stucco process repeats 1 time; And then carry out backing layer coating; Backing layer coating binding agent used is ethyl silicate or Ludox, and filler used is mullite powder, and both weight proportions are 1:4; This backing layer paint slurry is coated on the skin of above-mentioned coating wax-pattern, carries out stucco with thicker mullite powder more subsequently; Backing layer coating is by this operation repetition 3 times; The gross thickness of final formation coating is 5mm.
(3) the above-mentioned wax-pattern with laminated coating is carried out drying, after sclerosis to be dried, remove wax-pattern, form shell.
(4) sintering of shell; The shell dewaxed is put into roaster roasting under nitrogen protection, sintering temperature 1100 DEG C, sinter 1 hour, in 300 DEG C of insulations 2 hours, cool to room temperature with the furnace subsequently, finally make the calcium zirconate ceramics shell for titanium or titanium alloy hot investment casting.
(5) cast of TiNi alloy: the high temperature TiNi alloy of coming out of the stove is injected the calcium zirconate shell made, removes shell i.e. obtained required TiNi alloy cast after cooling.
The Ti-Ni alloy foundry goods of this operation cast, without significant reaction layer, any surface finish, alloy property is good.
embodiment 3
The present embodiment is preparation process and the step of using calcium zirconate Shell Preparation Ti-6Al-4V alloy-steel casting
(1) preparation of coating: add binding agent two acetic acid zirconium in calcium zirconate powder that is levigate, that cross 200 mesh sieves, constantly stir with agitator, control the viscosity of painting slip greatly about 30s, the weight ratio 4:1 of calcium zirconate powder and binding agent;
(2) preparation of shell: wax-pattern is immersed in the above-mentioned coating configured, stay a minute, when allowing coating be coated with equably to hang on wax-pattern, can stucco, calcium zirconate dry powder is dispersed in equably be coated with on coating wax-pattern, stucco process repeats 1 time; And then carry out backing layer coating; Backing layer coating binding agent used is ethyl silicate or Ludox, and filler used is mullite powder, and both weight proportions are 1:4; This backing layer paint slurry is coated on the skin of above-mentioned coating wax-pattern, carries out stucco with thicker mullite powder more subsequently; Backing layer coating is by this operation repetition 3 times; The gross thickness of final formation coating is 5mm.
(3) the above-mentioned wax-pattern with laminated coating is carried out drying, after sclerosis to be dried, remove wax-pattern, form shell.
(4) sintering of shell; The shell dewaxed is put into roaster roasting under nitrogen protection, sintering temperature 1200 DEG C, sinter 1 hour, in 300 DEG C of insulations 2 hours, cool to room temperature with the furnace subsequently, finally make the calcium zirconate ceramics shell for titanium or titanium alloy hot investment casting.
(5) cast of Ti-6Al-4V alloy: the high temperature Ti-6Al-4V alloy of coming out of the stove is injected the calcium zirconate shell made, removes shell i.e. obtained required Ti-6Al-4V alloy casting part after cooling.
The Ti-6Al-4V alloy-steel casting of this operation cast, without significant reaction layer, cast(ing) surface is bright and clean, and alloy property is good.
Claims (3)
1. the CaZrO for titanium or titanium alloy hot investment casting
3the preparation method of shell, is characterized in that, has following process and step:
The pretreatment of a calcium zirconate raw material: by levigate through ball milling for the calcium zirconate powder after pickling, obtains being less than 200 object calcium zirconate particles;
The preparation of b investment precoat: add through pretreated calcium zirconate in surface layer binding agent, and constantly stir with agitator, add additive in right amount; Additive is made up of surfactant and defoamer; Investment precoat is made up of calcium zirconate, surface layer binding agent, surfactant and defoamer, and the weight proportion of investment precoat is: calcium zirconate: surface layer binding agent is 3:1 ~ 5:1, surfactant is investment precoat weight 0.1 ~ 0.5% and defoamer are 0.1 ~ 0.5% of investment precoat weight; No. 4 flow cups made in U.S.A are used to control to be coated with the viscosity of slip at 15 ~ 65s;
The preparation of c backing layer or secondary investment precoat: the weight proportion of backing layer or secondary investment precoat is: backing layer or secondary surface layer filler: backing layer or secondary surface layer binding agent=(3.5-4.5): 1;
The preparation of d shell: after coating prepares, wax-pattern is immersed in investment precoat, when unnecessary investment precoat gutters down, and investment precoat is coated with when hanging on wax-pattern equably carry out stucco, 80 ~ 120 object calcium zirconate powder are sprinkling upon equably and have been coated with on coating wax-pattern; After the fully dry and sclerosis of coating, then repeat 1-2 above-mentioned steps; And then being coated with backing layer or secondary investment precoat, its viscosity of the coating of composition controls at 10 ~ 20s, and then uses mullite powder stucco; Repeat 2-3 time; Then dry;
The dewaxing of e shell: dried shell is used high steam still or microwave dewaxing;
The sintering of f shell: the shell dewaxed is put into roaster and sinters in atmosphere, sintering temperature 850 ~ 1350 DEG C, sinters one hour, cools to room temperature with the furnace subsequently, obtain shell finished product.
2. the CaZrO for titanium or titanium alloy hot investment casting according to claim 1
3the preparation method of shell, is characterized in that, the surfactant in described step b is the one in stearic acid or neopelex.
3. the CaZrO for titanium or titanium alloy hot investment casting according to claim 1
3the preparation method of shell, it is characterized in that, the defoamer in described step b is the one in dimethyl silicone polymer, silicone emulsion, the fatty acid ester compounded thing of higher alcohols, polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy propyl alcohol amidogen ether, polypropylene glycerol aether or polyoxypropylene.
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| CN103611885B (en) * | 2013-11-26 | 2015-06-17 | 洛阳鹏起实业有限公司 | Method and device for dewaxing investment precision casting shell and flash burning dewaxing furnace |
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