Forming process for silicon carbide reflector blank and expansion and contraction mold
Technical field: the invention belongs to the ceramic technical field, relate to a kind of body preparation method and moulding process of ceramic.
Background technology: SiC pottery is owing to its premium properties is used to make speculum.This speculum has military and civilian value, so the preparation technology of SiC speculum also receives much concern.
The technology of preparation SiC speculum has many kinds, and except hot pressed sintering, vapour deposition, what using value was arranged most is reaction sintering.The reaction sintering flow process is: at first utilize the SiC powder to make the base substrate of required form.This base substrate behind sintering under the Si atmosphere, after grinding, polishing just can be obtained the SiC speculum again.Most critical is how to prepare desirable base substrate in the whole technology.Desirable base substrate refers to: 1. can be by successful sintering; 2. there are not pore and crackle in the sintered body; 3. base substrate has lightweight structure.1 prescription that depends on technology wherein, 2,3 moulding, releasing processes that depend on base substrate.
Domestic is blank on this SiC reflector blank preparation technology, relates among the preparation technology of SiC ceramic material adopting the method for mixing various additives to carry out sintering mostly.This is worthless for the SiC speculum, because this will influence the polishing performance of SiC speculum, and mechanical property and thermal property etc.The forming method that adopts mostly is hot-forming, manual ramming or pressure extrusion etc. greatly, and the defective in the base substrate that this moulding process is made is inevitable.(referring to Chinese patent 00114425,99107877,99119733,98114247,97116581 etc.).
(U.S.) relevant patent retrieval (US Patent Database Search) abroad relates to the technology (referring to US patent5683028,6110283,5071596,4856887) of multinomial SiC ceramic, mentioned molding mode is mainly hot pressing, vapour deposition, gas-phase reaction in bibliographical information, only mentions as for the blank forming of reaction sintering and adopts gel slip casting.
The present invention solves hot-forming, manual ramming of prior art or pressure extrusion base substrate, the method that various additives are mixed in employing is carried out sintering influences polishing performance, and mechanical property and thermal property, the formed pollution of additive, demoulding base substrate is yielding and problems such as crackle are arranged.The present invention will provide a kind of novel forming process for silicon carbide reflector blank and expansion and contraction mold, have the desirable base substrate of the complicated shape of lightweight structure with preparation.
The present invention thes contents are as follows: propose a kind of new technical recipe; Proposition utilizes hyperacoustic method for densifying; New no active force release method and device are proposed.
Forming process for silicon carbide reflector blank of the present invention: the silicon carbide powder that at first select 95~99%, granularity is 1~5 μ m mixes with 1~5% graphite powder, more above-mentioned compound is added an amount of phenolic resins ethanolic solution and fully mix to make slurry; Above-mentioned slurry is carried out ultrasonic wave handle, eliminate the bubble that is trapped in the slurry, make the injection molding slurry, the injection molding slurry is injected mould form injection moulding blank; Again the injection moulding blank that injects mould is carried out drying processing, and operate expansion and contraction mold as described below and carry out the demoulding and mould is deviate from and formed demoulding base substrate; Demoulding base substrate is put into the baking oven intensification be baked to 250-350 ℃; Demoulding base substrate with baking places heating furnace to handle to 1000-1200 ℃ under protective atmosphere at last, makes the silicon carbide mirror molding blank.
Technology densification among the present invention: above-mentioned slurry is carried out ultrasonic wave handle, eliminate the bubble that is trapped in the slurry, through after the above-mentioned processing, again with the slurry injection molding.Ultrasonic wave energy effectively reduce the surface of bubble can will impel its overflow, the particle of slurry is uniformly dispersed is convenient to injection molding.But the present invention utilizes expansion and contraction mold to carry out the demoulding in the slurry drying process, and volume can shrink in the slurry exsiccation process.
Expansion and contraction mold among the present invention is to embed rigid support 6 for 1 li at the breathing parts.Rigid support 6 is made up of steel pole 2, connector 3, overcoat 4, interior bar 5.Several steel poles 2 are connected and form needed shape with several connectors 3, flexibly connect with several steel poles 2 respectively around the overcoat 4, one end of interior bar 5 and some steel poles 2 flexibly connect, and the other end of interior bar 5 and overcoat 4 places the outside of breathing parts 1 to be used for controlling the breathing of mould piece.
The course of work of apparatus of the present invention: but after outside the expansion and contraction mold piece, coating thin plastic, press the shape of base substrate and arrange, and inject slurry.When the slurry drying is handled and during drying shrinkage, only need interior bar is taken out outward, push away under the overcoat, rigid support will interiorly be received the entire die piece, therefore base substrate is not subjected to any active force in knockout course, reach the breathing of the breathing control mould piece that utilizes rigid support, thereby the mould piece is dwindled and realize not having the active force demoulding.
From above-mentioned employing technical recipe of the present invention as seen, de-carbon does not add any sinter additives that helps outward, has guaranteed the purity of gained SiC speculum to greatest extent, overcomes the harmful effect that the prior art additive brings.The carbon that the present invention adopts the phenolic resins pyrolysis to produce in fact just rises and helps agglomeration, because carbon can be converted into SiC in SiC atmosphere, so avoided the formed pollution of other additive.
The present invention carries out the demoulding synchronously when injection molding slurry drying shrinkage, solved existing release method when the intensity of slurry self is very low, make mould and injection molding slurry synchronous very difficult, mould then can not cause having in the demoulding base substrate crackle to occur with injection molding slurry synchronous, will destroy the problem of demoulding base substrate shape, the technology that adopts the present invention to carry out the demoulding in demoulding body drying process can guarantee that final products do not have the hole crackle.
The present invention adopts ultrasonic wave to handle and makes the densification of demoulding blank structure, solves the prior art polishing performance, the problem of mechanical property and thermal property difference.
The structure of bar, overcoat was dwindled the mould piece in but expansion and contraction mold of the present invention adopted, and demoulding base substrate is not subjected to any active force in the knockout course, has realized the unstressed demoulding, then makes the present invention can prepare the lightweight structure SiC reflector blank of different shape.Solve in the prior art problem that retractable die not can not prepare the lightweight structure SiC reflector blank of different shape.
Description of drawings:
Fig. 1 is a rigid support structural representation of the present invention.
Fig. 2 is the rigid support schematic diagram that the present invention shrinks.
Fig. 3 is the vertical view of rigid support of the present invention.
But Fig. 4, Fig. 5 are the use schematic diagrames of the present invention's expansion and contraction mold.
Fig. 6 is the cutaway view of expansion and contraction mold of the present invention.
Fig. 7 is a movable connecting mode schematic diagram of the present invention.
The specific embodiment: the present invention is embodiment as shown in drawings: the concrete size and dimension of rigid support structure can be determined according to actual needs among Fig. 1; When interior bar and sleeve pipe relative motion, will become state shown in Figure 2; Fig. 3 is the vertical view with the hexahedron rigid support; Fig. 4, Fig. 5 are the schematic diagrames in the actual use of expansion and contraction mold; Fig. 6 is the profile of expansion and contraction mold.The movable connecting mode of steel pole and steel pole, steel pole and interior bar, steel pole and outer inner room in Fig. 7 expansion and contraction mold, these parts can constitute multiple shape according to actual needs, as hexahedron, cuboid, tripartite body etc., can adopt metal material to make.Breathing parts 1 can be with sponge or other similar material.
Phenolic resins adopts thermoset phenolic resin among the present invention.Thermoset phenolic resin can be bonded to powder the base substrate with certain intensity, becomes the carbon of coated Si particle simultaneously after the thermoset phenolic resin pyrolysis, and carbon can be converted into SiC in SiC atmosphere.And the ethanol in the solution itself has the froth breaking effect.
Embodiment 1: preparation has the complicated shape base substrate of lightweight structure
(1), with 99%, particle diameter is that the SiC powder of 1~3 μ m mixes with 1% powdered graphite and adds the abundant ball milling of an amount of liquid phenolic resin again and mix, and becomes even injection molding slurry.
(2), the injection molding slurry carried out ultrasonic wave handled 5~10 minutes, eliminate to pour into behind the bubble and form injection moulding blank in the mould.
(3), the injection moulding blank drying is handled in the mould, injection moulding blank begins drying shrinkage;
(4), the demoulding of operation mould piece forms demoulding base substrate, it is dry to treat after the demoulding that demoulding base substrate continues;
(5), demoulding base substrate is put into baking oven, heat up and be baked to 350 ℃;
(6), processing is made the silicon carbide mirror molding blank to 1200 ℃ in heating furnace under protective atmosphere.
(7), the mould therefor piece is a hexagonal structure in this example, so can obtain having the base substrate of cellular lightweight structure.
Embodiment 2:
(1) is that the SiC powder of 1~3 μ m mixes with 5% powdered graphite and adds the abundant ball milling of an amount of liquid phenolic resin again and mix with a certain amount of particle diameter, becomes even injection molding slurry;
(2) the injection molding slurry is carried out ultrasonic wave and handled 5~10 minutes, eliminate to pour into behind the bubble and form injection moulding blank in the mould;
(3) identical among the embodiment 1;
(4) identical among the embodiment 1;
(5) demoulding base substrate is put into baking oven, heat up and be baked to 250 ℃;
(6) under protective atmosphere, in heating furnace, handle, make the silicon carbide mirror molding blank to 1000 ℃.
(7) the mould therefor piece is a cuboid in this example, so can obtain having the base substrate of latticed lightweight structure.
Embodiment 3:
(1) is that the SiC powder of 1~3 μ m mixes with 3% powdered graphite and adds the abundant ball milling of an amount of liquid phenolic resin again and mix with a certain amount of particle diameter, becomes uniform sizing material;
(2) identical among the embodiment 1;
(3) identical among the embodiment 1;
(4) identical among the embodiment 1;
(5) demoulding base substrate is put into baking oven, heat up and be baked to 300 ℃;
(6) under protective atmosphere, in heating furnace, handle, make the silicon carbide mirror molding blank to 1100 ℃.