CN101643360B - Method for manufacturing dentate special-shaped ceramic components by injection molding - Google Patents
Method for manufacturing dentate special-shaped ceramic components by injection molding Download PDFInfo
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- CN101643360B CN101643360B CN2009100906458A CN200910090645A CN101643360B CN 101643360 B CN101643360 B CN 101643360B CN 2009100906458 A CN2009100906458 A CN 2009100906458A CN 200910090645 A CN200910090645 A CN 200910090645A CN 101643360 B CN101643360 B CN 101643360B
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Abstract
The invention discloses a method for manufacturing dentate special-shaped ceramic components by injection molding, belonging to the technical field of high-performance ceramic preparation. The method comprises the following steps: evenly mixing 81wt% to 90wt% of ceramic powder and 10wt% to 19wt% of organic binders by weight percentage to obtain an injection-molding mixture, injection-molding the injection-molding mixture on an injection-molding machine with the injection temperature being 175 to 195 DEG C, to obtain a green body, and de-molding within 2 minutes after the injection, so as to obtain a molded green body; and then, subjecting the molded green body to water-extraction degreasing and thermal degreasing, sintering the degreased green body at 1,350 to 1,550 DEG C, holding for 1 to 4 hours and furnace-cooling to obtain the ceramic components. The invention has the advantages of high automation degree, high molding and degreasing efficiencies, even green body, high dimensional accuracy and surface smoothness of sintered products, and environment-friendly and energy-saving manufacture.
Description
Technical field
The invention belongs to the high-performance ceramic preparing technical field, particularly a kind of method of manufacturing dentate special-shaped ceramic components by injection molding.
Background technology
Multiple tooth oxide ceramic part is widely used in fields such as machinery, chemical industry and automobiles, for example zirconium white or alumina-ceramic gear and ceramic screw etc.Methods such as static pressure, dry-pressing, slip casting and injection moulding such as the present method of making this multiple tooth oxide ceramic part comprises.Though the dry-pressing formed efficient of pottery is higher, moulding product exists density variation, the uneven phenomenon of microstructure, and the while is easy-formation complicated shape and special-shaped product not; Cold isostatic compaction can obtain the molding blank of high-density and high uniformity, but is difficult to the complicated ceramic component of forming shape, and shaping efficiency is low many with manual operations.Though the plastic special-shaped product of ceramic grout moulding reaches near net-shape, molding blank be prone to produce density unevenness and component segregation, the compact dimensions precision low with product reliability under the degradation problem, and be shaped to manual operations and body drying efficient is low.The problem production cycle of hot die-casting molding maximum is long, is inefficiency, and organic binder bonds such as eliminating paraffin need dozens or even hundreds of hour, and are easy to generate defectives such as pore and cracking in the de-waxing process.
The ceramic injection forming technology comes from Plastics Injection Molding Technology, can realize quick, the accurate complicated shape ceramic component of making.In the ceramic injection forming, the flowability of ceramic particle is that the high-content organic binder bond that leans on particle surface to coat realizes that the content of organic binder bond (weight ratio) is between the 10-20% in the ceramic injection compound.These organic binder bonds in the molding blank must be got rid of before sintering, promptly need carry out degreasing.The past ceramic injection forming mainly adopts the method for slow heating to carry out degreasing; Organic binder bond is decomposed gradually get rid of, need more than tens hours even 100 hours, the time is long; Efficient is low; And in skimming processes, be easy to generate defectives such as cracking and distortion, therefore limited the application of ceramic injection forming, particularly will prepare very difficulty of multiple tooth shape non-conventional type ceramic series products.
Summary of the invention
The method that the purpose of this invention is to provide a kind of manufacturing dentate special-shaped ceramic components by injection molding.
A kind of method of manufacturing dentate special-shaped ceramic components by injection molding is characterized in that, this method steps is:
(1) hybrid ceramic powder and organic binder bond: ceramic powder and organic binder bond mixed obtain injection molding mixture; In the said injection molding mixture; The weight percentage of ceramic powder is 81-90%, and the weight percentage of organic binder bond is 10-19%;
Said ceramic powder is one or more in zirconium white, aluminum oxide or the mullite;
Said organic binder bond is made up of water-insoluble sticker, water-soluble binder, tensio-active agent, lower melting point organism and softening agent, and each composition weight percentage composition is: water-insoluble sticker: 15-30%; Water-soluble binder: 45-65%; Tensio-active agent: 1-5%; Lower melting point organism: 5-11%; Softening agent: 1-11%;
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate, and injection temperature injects behind the mould that the demoulding obtains molding blank in 2 minutes between 175-195 ℃;
(3) water extraction skim: the base substrate that injection molding obtains is put into water, and dissolving removes the portion water soluble organic binder, and the temperature of water is at 30-50 ℃, and degreasing time is at 6-8 hour, the thorough drying in baking oven of the base substrate behind the water extraction skim;
(4) hot degreasing: dried base substrate is put into electrical heater, carry out hot degreasing, remove water-insoluble sticker and remainder water soluble organic binder, be warming up to 550 ℃, be incubated 2-3 hour with the temperature rise rate of 5-8 ℃/min;
(5) sintering: the base substrate after the hot degreasing carries out sintering, and sintering temperature is incubated 1-4 hour between 1350-1550 ℃, and furnace cooling obtains ceramic component.
In the step (1), said hybrid ceramic powder and organic binder bond carry out on two roller mills or duplex Banbury mixer, and ceramic powder and water-insoluble sticker descended mixing 5-10 minute at 180-190 ℃; Temperature is reduced to 170 ℃ and is added tensio-active agent, mixing 5-10 minute; Temperature is reduced to 150 ℃, adds water-soluble binder and lower melting point organism, mixing 10-15 minute; Melting temperature is reduced to 120 ℃, adds softening agent, mixes 10-15 minute; Cool off fragmentation at last and obtain injection molding mixture, the particle after the compound fragmentation is less than 3mm.
Said water-insoluble sticker is the combination of two kinds of superpolymer, a kind of polyethylene terephthalate, polybutylene terephthalate of being selected from of said superpolymer, and another kind is selected from polymethylmethacrylate, polyvinyl butyral acetal.
Said water-soluble binder is polyoxyethylene glycol, Z 150PH or polyoxyethylene.
Said tensio-active agent is Triple Pressed Stearic Acid or oleic acid.
Said softening agent is dibutyl terephthalate, dioctyl terephthalate or terephthalic acid diamyl ester.
Said lower melting point organism is microcrystalline wax, POLISHING WAX-103 or beeswax.
In the step (3), said drying temperature is 40-60 ℃.
Said sintering carries out in the sintering oven of Si-Mo rod heating element or Sweet natural gas high temperature kiln.
Beneficial effect of the present invention is: the present invention proposes to adopt the fast injection forming method to make multiple tooth shape non-conventional type ceramic parts or product; Its thinking and basic fundamental route are to obtain multiple tooth shape non-conventional type ceramic base substrate through automatic injection moulding machine rapid shaping; The two step degreasing methods that adopt water extraction skim and hot degreasing to combine are then got rid of organic binder bond in the base substrate fast; Sintering in High Temperature Furnaces Heating Apparatus obtains fine and close all dentation non-conventional type ceramic products of even excellent performance then.The present invention can be efficiently, high precision is made the multiple tooth oxide ceramic part of high reliability, and multiple tooth oxide ceramic part thickness does not have distortion and cracking defect greater than 10mm in the manufacturing processed, and densified sintering product has the following advantages:
(1) level of automation is high, and to obtain base substrate be full-automatic process to filling the mould cooling from getting into injection moulding machine to be injected into moulding mixture, improved shaping efficiency greatly;
(2) the molding blank dimensional precision is high, surface smoothness is high, and it is very little that the product that final sintering obtains can not carry out mechanical workout or machining amount, reduced manufacturing cost;
(3) ceramic particle is uniformly dispersed in the base substrate, can reduce inhomogeneous in the final product structure, improves the safety of ceramic product;
(4) water extraction skim and compound degreasing method of two step of hot degreasing have improved degreasing efficient greatly, and degreasing time was reduced to more than 48-60 hour 8-11 hour by the traditional hot degreasing;
(5) water extraction skim and compound degreasing method of two step of hot degreasing can be used to make the bigger profile of tooth ceramic component of thickness; The base substrate of the about 8mm of maximum ga(u)ge that the traditional hot defatting technology can be made; Adopt the present invention can make the base substrate that thickness is about 16mm, be doubled.
Description of drawings
Fig. 1 is multiple tooth shape oxide ceramic part synoptic diagram;
Fig. 2 is a fast injection moulding process flow process;
Fig. 3 is the microstructural electron scanning micrograph of zirconia ceramics;
Fig. 4 is the microstructural electron scanning micrograph of alumina-ceramic.
Embodiment
Below in conjunction with accompanying drawing the present invention is described further:
Embodiment 1
In the present embodiment, ceramic powder is selected zirconia ceramics powder for use, Zirconium powder median size d
50=0.15 μ m, specific surface area is 8.5m
2/ g; Organic binder bond is made up of water-insoluble sticker, water-soluble binder, tensio-active agent, lower melting point organism and softening agent; Water-insoluble sticker is the combination of polyethylene terephthalate and polymethylmethacrylate, is water-soluble binder with the polyoxyethylene glycol, is tensio-active agent with the Triple Pressed Stearic Acid; With the dibutyl terephthalate is softening agent, is the lower melting point organism with the microcrystalline wax.
The method steps of manufacturing dentate special-shaped ceramic components by injection molding is following, and Fig. 2 is seen in technical process:
(1) hybrid ceramic powder and organic binder bond: 1000g zirconia ceramics powder and 12.4g polyethylene terephthalate, 22.9g polymethylmethacrylate are added two roller mills, descended mixing 10 minutes at 190 ℃; Temperature is reduced to 170 ℃ and is added Triple Pressed Stearic Acid 7.1g, mixing 10 minutes; Temperature is reduced to 150 ℃, adds polyoxyethylene glycol 102.4g and microcrystalline wax 14.1g, mixing 10 minutes; Melting temperature is reduced to 120 ℃, adds softening agent dibutyl terephthalate 17.6g, mixing 15 minutes; Cool off fragmentation at last and obtain compound, the compound granularity is less than 3mm;
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate; Base substrate is shaped as profile of tooth as shown in Figure 1; The number of multiple tooth shape special-shaped ceramic components tooth, the size of centre hole can change; Central hole size is determined by the core size; Can in the 0-22mm scope, change; The number of tooth is greater than 3; Component thickness is represented with H; Represent tip diameter with a; The root diameter of the multiple tooth shape parts of expression with
; Central hole size is expression with
, and the facewidth is represented with b, H=16mm in the present embodiment; B=5mm;
a=30,
are respectively 0mm, 5mm, 10mm, 15mm when
(be solid parts), are the multiple tooth shape parts of 4 teeth; Injection temperature is 175 ℃, injects behind the mould that the demoulding obtains molding blank in 2 minutes;
(3) water extraction skim: the base substrate that injection molding obtains is put into water; Dissolving removes the portion water soluble organic binder; The temperature of water is 38 ℃, and degreasing time is 7 hours, and 7 hours decreasing ratiies of polyoxyethylene glycol are 60-70%; (the remainder water soluble organic binder can be got rid of through thermolysis with water-insoluble organic binder bond in follow-up rapid heating process), the base substrate behind the water extraction skim is thorough drying in 40 ℃ of baking ovens;
(4) hot degreasing: dried base substrate is put into electrical heater, carry out hot degreasing, remove water-insoluble sticker and remainder water soluble organic binder, be warming up to 550 ℃, be incubated 3 hours with the temperature rise rate of 5 ℃/min;
(5) sintering: the base substrate after the hot degreasing carries out sintering, and sintering carries out in the sintering oven of Si-Mo rod heating element, and sintering temperature is 1550 ℃, is incubated 2 hours, and insulation is cut off the heating power supply furnace cooling later, obtains ceramic component.
Formed the connection pore behind the water extraction skim in the base substrate, remaining water-insoluble organic binder bond just can be in process furnace rapid heating get rid of and do not produce distortion and cracking.Base substrate after the degreasing carries out high temperature sintering in sintering oven, obtain the ceramic of compact of excellent performance.
Because of adopting identical raw material and method manufacturing, so four kinds of multiple tooth shape zirconium oxide ceramic component performances of the different central hole size of present embodiment gained are consistent: the sintered density of the product of above-mentioned preparation has reached 6.03g/cm
3, three-point bending resistance intensity 1090 ± 52MPa, fracture toughness property is 13.1 ± 2.2MPam
1/2, sintering oxidation zircon ceramic profile scanning electromicroscopic photograph is as shown in Figure 3, and visible uniform microstructure is fine and close, and average grain size is approximately 350nm, does not have pore and impurity, has guaranteed the HS and the H.T. of ceramic product.
The multiple tooth ceramic component of
for preparing is the solid parts that does not have centre hole; Thickness reaches 16mm, and this thickness is that traditional hot die casting and hot defatting technology can't be made.
Embodiment 2
In the present embodiment, ceramic powder is selected the alumina-ceramic powder for use, alumina powder jointed median size d
50=0.08 μ m, specific surface area is 13.5m
2/ g; Organic binder bond is made up of water-insoluble sticker, water-soluble binder, tensio-active agent, lower melting point organism and softening agent; Water-insoluble sticker is the combination of polyethylene terephthalate and polyvinyl butyral acetal, is water-soluble binder with the polyoxyethylene glycol, is tensio-active agent with the Triple Pressed Stearic Acid; With the dibutyl terephthalate is softening agent, is the lower melting point organism with the microcrystalline wax.
The method steps of manufacturing dentate special-shaped ceramic components by injection molding is:
(1) hybrid ceramic powder and organic binder bond: 1000g alumina-ceramic powder and 11.0g polyethylene terephthalate, 33.0g polyvinyl butyral acetal are added two roller mills, descended mixing 10 minutes at 190 ℃; Temperature is reduced to 170 ℃ and is added Triple Pressed Stearic Acid 8.8g, mixing 10 minutes; Temperature is reduced to 150 ℃, adds polyoxyethylene glycol 123g and microcrystalline wax 22g, mixing 10 minutes; Melting temperature is reduced to 120 ℃, adds softening agent dibutyl terephthalate 22g, mixing 15 minutes; Cool off fragmentation at last and obtain compound, the compound granularity is less than 3mm;
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate; Base substrate is shaped as profile of tooth as shown in Figure 1; H=16mm in the present embodiment; B=5mm;
a=30mm;
is the multiple tooth shape parts (base substrate is shaped as the multiple tooth shape that there is a circular hole at the center) of 4 teeth; Injection temperature is 180 ℃, injects behind the mould that the demoulding obtains molding blank in 2 minutes;
(3) water extraction skim: the base substrate that injection molding obtains is put into water, and dissolving removes the portion water soluble organic binder, and the temperature of water is 45 ℃, and degreasing time is 8 hours, the base substrate behind the water extraction skim in 40 ℃ of baking ovens dry 24 hours;
(4) hot degreasing: dried base substrate is put into electrical heater, carry out hot degreasing, remove water-insoluble sticker and remainder water soluble organic binder, be warming up to 550 ℃, be incubated 3 hours with the temperature rise rate of 8 ℃/min;
(5) sintering: the base substrate after the hot degreasing carries out sintering, and sintering carries out in the Sweet natural gas high temperature kiln, and sintering temperature is 1500 ℃, is incubated 2 hours, and furnace cooling obtains ceramic component then.
The alumina-ceramic density 3.97g/cm that obtains
3, bending strength 435 ± 30MPa, Vickers' hardness is 21GPa, and microstructure photograph is seen Fig. 4, and visible uniform microstructure is fine and close, and average grain size is approximately 0.5 μ m, does not have pore and impurity, makes this alumina ceramic product reach HS and high firmness.
Claims (7)
1. the method for a manufacturing dentate special-shaped ceramic components by injection molding is characterized in that, this method steps is:
(1) hybrid ceramic powder and organic binder bond: ceramic powder and organic binder bond mixed obtain injection molding mixture; In the said injection molding mixture; The weight percentage of ceramic powder is 81-90%, and the weight percentage of organic binder bond is 10-19%;
Said ceramic powder is one or more in zirconium white, aluminum oxide or the mullite;
Said organic binder bond is made up of water-insoluble sticker, water-soluble binder, tensio-active agent, lower melting point organism and softening agent, and each composition weight percentage composition is: water-insoluble sticker: 15-30%; Water-soluble binder: 45-65%; Tensio-active agent: 1-5%; Lower melting point organism: 5-11%; Softening agent: 1-11%;
Said lower melting point organism is microcrystalline wax, POLISHING WAX-103 or beeswax;
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate, and injection temperature injects behind the mould that the demoulding obtains molding blank in 2 minutes between 175-195 ℃;
(3) water extraction skim: the base substrate that injection molding obtains is put into water, and dissolving removes the portion water soluble organic binder, and the temperature of water is at 30-50 ℃, and degreasing time is at 6-8 hour, the thorough drying in baking oven of the base substrate behind the water extraction skim;
(4) hot degreasing: dried base substrate is put into electrical heater, carry out hot degreasing, remove water-insoluble sticker and remainder water soluble organic binder, be warming up to 550 ℃, be incubated 2-3 hour with the temperature rise rate of 5-8 ℃/min;
(5) sintering: the base substrate after the hot degreasing carries out sintering, and sintering temperature is incubated 1-4 hour between 1350-1550 ℃, and furnace cooling obtains ceramic component;
In the step (1), said hybrid ceramic powder and organic binder bond carry out on two roller mills or duplex Banbury mixer, and ceramic powder and water-insoluble sticker descended mixing 5-10 minute at 180-190 ℃; Temperature is reduced to 170 ℃ and is added tensio-active agent, mixing 5-10 minute; Temperature is reduced to 150 ℃, adds water-soluble binder and lower melting point organism, mixing 10-15 minute; Melting temperature is reduced to 120 ℃, adds softening agent, mixes 10-15 minute; Cool off fragmentation at last and obtain injection molding mixture, the particle after the compound fragmentation is less than 3mm.
2. the method for a kind of manufacturing dentate special-shaped ceramic components by injection molding according to claim 1; It is characterized in that; Said water-insoluble sticker is the combination of two kinds of superpolymer; A kind of polyethylene terephthalate, polybutylene terephthalate of being selected from of said superpolymer, another kind is selected from polymethylmethacrylate, polyvinyl butyral acetal.
3. the method for a kind of manufacturing dentate special-shaped ceramic components by injection molding according to claim 1 is characterized in that, said water-soluble binder is polyoxyethylene glycol, Z 150PH or polyoxyethylene.
4. the method for a kind of manufacturing dentate special-shaped ceramic components by injection molding according to claim 1 is characterized in that, said tensio-active agent is Triple Pressed Stearic Acid or oleic acid.
5. the method for a kind of manufacturing dentate special-shaped ceramic components by injection molding according to claim 1 is characterized in that, said softening agent is dibutyl terephthalate, dioctyl terephthalate or terephthalic acid diamyl ester.
6. the method for a kind of manufacturing dentate special-shaped ceramic components by injection molding according to claim 1 is characterized in that, in the step (3), said drying temperature is 40-60 ℃.
7. the method for a kind of manufacturing dentate special-shaped ceramic components by injection molding according to claim 1 is characterized in that, said sintering carries out in the sintering oven of Si-Mo rod heating element or Sweet natural gas high temperature kiln.
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