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CN1201911C - Forming process for silicon carbide reflector blank and expansion and contraction mold - Google Patents

Forming process for silicon carbide reflector blank and expansion and contraction mold Download PDF

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Publication number
CN1201911C
CN1201911C CN 01117286 CN01117286A CN1201911C CN 1201911 C CN1201911 C CN 1201911C CN 01117286 CN01117286 CN 01117286 CN 01117286 A CN01117286 A CN 01117286A CN 1201911 C CN1201911 C CN 1201911C
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demoulding
expansion
silicon carbide
mold
contraction
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CN 01117286
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CN1364746A (en
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王君林
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Abstract

本发明属于陶瓷制品,涉及碳化硅反射镜坯体成型工艺方法及胀缩模具,由胀缩部件、钢杆、联接件、外套、内杆组成,采用本发明的装置可实现无应力脱模,可制备各种形状的轻量化结构SiC反射镜坯体。在坯体干燥过程中进行脱模保证最终产品无孔洞裂纹,超声波处理使结构致密,保证所得SiC反射镜的纯度克服添加剂的不良影响。采用内杆、外套的结构,使模具块缩小,脱模过程中脱模坯体未受到任何作用力,实现了无应力脱模,则使本发明可以制备各种形状的轻量化结构SiC反射镜坯体。The invention belongs to ceramic products, and relates to a silicon carbide reflector blank forming process and an expansion-contraction mold, which is composed of expansion-contraction parts, steel rods, couplings, jackets, and inner rods. The device of the invention can realize stress-free demoulding. Various shapes of lightweight structural SiC mirror blanks can be prepared. Demoulding is carried out during the drying process of the green body to ensure that the final product has no holes and cracks, and the ultrasonic treatment makes the structure compact, ensuring the purity of the obtained SiC mirror and overcoming the adverse effects of additives. The structure of the inner rod and the outer jacket is adopted to reduce the size of the mold block, and the demoulding blank is not subjected to any force during the demoulding process, and the stress-free demoulding is realized, so that the present invention can prepare various shapes of light-weight structure SiC reflectors body.

Description

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 ℃.

Claims (3)

1、碳化硅反射镜坯体成型的胀缩模具,其特征在于:包括可胀缩部件(1)和刚性支架(6),在可胀缩部件(1)里嵌入刚性支架(6)。1. An expansion-contraction mold for forming a silicon carbide mirror body, characterized in that it includes an expandable-contractable part (1) and a rigid support (6), and the rigid support (6) is embedded in the expandable-contractable part (1). 2、一种碳化硅反射镜坯体成型工艺方法,其特征在于:首先选择95~99%、粒度为1~5μm的碳化硅粉末与1~5%石墨粉混合,再将上述混合料加入适量的酚醛树脂乙醇溶液并充分混合均匀制成浆料;将上述浆料进行超声波处理,消除滞留在浆料中的气泡,制成注模浆料,将注模浆料注入模具形成注模坯体;再对注入模具中的注模坯体进行干燥处理时,操作如根据权利要求1所述的胀缩模具进行脱模使模具脱出并形成脱模坯体;将脱模坯体放入烘箱中升温烘烤至250-350℃;最后将烘烤的脱模坯体在保护气氛下置于加热炉中处理至1000-1200℃,制成碳化硅反射镜成型坯体。2. A process for forming a silicon carbide reflector body, characterized in that: first, 95-99% silicon carbide powder with a particle size of 1-5 μm is mixed with 1-5% graphite powder, and then an appropriate amount of the above-mentioned mixture is added phenolic resin ethanol solution and fully mixed to make a slurry; the above slurry is ultrasonically treated to eliminate the air bubbles trapped in the slurry to make an injection molding slurry, which is injected into the mold to form an injection molded body ; When drying the injection molded body injected into the mould, the expansion and contraction mold according to claim 1 is operated to carry out demoulding to make the mold come out and form a demoulding green body; the demoulding green body is put into an oven The temperature is raised to 250-350°C and baked; finally, the baked demoulding body is placed in a heating furnace under a protective atmosphere and treated to 1000-1200°C to make a silicon carbide mirror molding body. 3、根据权利要求1所述的碳化硅反射镜坯体成型的胀缩模具,其特征在于:刚性支架(6)由钢杆(2)、联接件(3)、外套(4)、内杆(5)组成,若干个钢杆(2)与若干个联接件(3)连接且组成所需要的形状,外套(4)的周围分别与若干个钢杆(2)活动连接,内杆(5)的一端与钢杆(2)活动连接,内杆(5)的另一端置于胀缩部件(1)的外部用来控制模具块的胀缩。3. The expansion and contraction mold for forming the silicon carbide mirror body according to claim 1, characterized in that: the rigid support (6) is composed of a steel rod (2), a coupling (3), a jacket (4), an inner rod (5) Composition, several steel rods (2) are connected with several connectors (3) and form the required shape, the surroundings of the overcoat (4) are respectively flexibly connected with several steel rods (2), and the inner rods (5 ) is flexibly connected to the steel rod (2), and the other end of the inner rod (5) is placed outside the expansion-contraction part (1) to control the expansion and contraction of the mold block.
CN 01117286 2001-04-28 2001-04-28 Forming process for silicon carbide reflector blank and expansion and contraction mold Expired - Fee Related CN1201911C (en)

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CN100462331C (en) * 2004-04-29 2009-02-18 西安交通大学 Normal temperature extrusion molding method of silicon carbide ceramics with phenolic resin as binder
CN1315754C (en) * 2004-11-16 2007-05-16 中国航空工业第一集团公司北京航空材料研究院 Method for precission shaping ceramic blank by semi-water-base injection-moulding gel process
CN100345007C (en) * 2005-06-29 2007-10-24 中国人民解放军国防科学技术大学 Reflection mirror with honeycomb sandwiched structure silicon carbide base composite material and its preparation method
CN1303038C (en) * 2005-12-12 2007-03-07 西安交通大学 Technical method for rapid shaping silicon carbide ceramic part utilizing laminated solid body
CN101941231B (en) * 2010-09-09 2012-02-08 中国科学院长春光学精密机械与物理研究所 Gel injection molding process of large-scale and complex-shaped silicon carbide ceramic green bodies
CN104400882B (en) * 2014-10-29 2016-08-24 中国科学院长春光学精密机械与物理研究所 Silicon carbide mirror mirror base preparation facilities and preparation method
CN106365418B (en) * 2016-08-30 2019-04-16 中国建筑材料科学研究总院 Lightweight quartz glass and preparation method thereof
CN106478106A (en) * 2016-10-09 2017-03-08 北京钢研新冶精特科技有限公司 Prepare the manufacture method of speculum silicon carbide granulating powder
WO2018189828A1 (en) * 2017-04-12 2018-10-18 三菱電機株式会社 Galvanomirror, galvanoscanner using galvanomirror, laser processing machine using galvanomirror, and method for manufacturing galvanomirror
CN110483001A (en) * 2019-08-19 2019-11-22 扬州霞光光学仪器有限公司 Silicon carbide optical frames and preparation method thereof
CN111390653A (en) * 2020-03-23 2020-07-10 中国科学院长春光学精密机械与物理研究所 Preparation method of off-axis aspheric silicon carbide lightweight reflector
CN113030916A (en) * 2021-03-17 2021-06-25 福州高意光学有限公司 Reflecting mirror for laser radar scanning

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