CN104030548A - Silicon carbide ceramic mold core for glass molding and manufacturing method thereof - Google Patents
Silicon carbide ceramic mold core for glass molding and manufacturing method thereof Download PDFInfo
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- CN104030548A CN104030548A CN201410314758.2A CN201410314758A CN104030548A CN 104030548 A CN104030548 A CN 104030548A CN 201410314758 A CN201410314758 A CN 201410314758A CN 104030548 A CN104030548 A CN 104030548A
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- silicon carbide
- carbide ceramics
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- protective membrane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention relates to a silicon carbide ceramic mold core for glass molding and a manufacturing method of the silicon carbide ceramic mold core for glass molding. The silicon carbide ceramic mold core for glass molding comprises a base material, a protection film and a metal transition layer between the base material and the protection film, wherein the base material is silicon carbide ceramic; the protection film is hard tungsten carbide alloy; the metal transition layer is titanium or chrome or tungsten.
Description
Technical field
The invention belongs to engineering ceramic material technical field, be specifically related to a kind of glass moulding silicon carbide ceramics die and preparation method thereof.
Background technology
Glass moulding technique is a kind of high-precision optical element manufacturing technology, and it is that softening opticglass is put into high-precision mould, is heating under pressurization and protective atmosphere, and disposable direct compression molding goes out to reach the optical element of service requirements.Its core technology is high precision die manufacturing process.The wherein qualification rate that is directly connected to eyeglass in surface optical quality, precision and work-ing life of die and and manufacturing cost.
Mould core for moulding glass need to possess following two principal characters:
(1) surperficial zero defect, can grind to form pore-free, smooth optical surface quality;
(2) under hot conditions, have high strength, hardness and good antioxidant property, surface quality is stable, and surface figure accuracy and smooth finish remain unchanged, and not with opticglass generation chemical reaction, occur bonding phenomenon, demolding performace is good.
Mould core for moulding glass is made up of base material and protective membrane.Wherein stainless steel and the large class of wolfram varbide two have mainly been experienced in the development of base material.Stainless steel hardness is not high, and resistance to elevated temperatures is poor, and form accuracy and surface quality, being repeatedly not easy to keep in circulating-heating process, cause the work-ing life of die not high., there is with it surface reaction but easily diffuse to opticglass under the element such as cobalt, nickel life-time service in its bonding agent in Wimet die processing characteristics excellence.Meanwhile, the thermal expansivity of Wimet is higher, and thermal conductivity is lower, and under high temperature thermal cycling, grain growth is obvious, causes die precision and surface quality to decline, and work-ing life is not high.
In order to improve the performance of die base material, progressively start to develop high performance ceramic material, as thyrite.Particularly solid-phase sintered silicon carbide ceramics has high heat conductance (100～130W/mK), low thermal coefficient of expansion (4.2 × 10
-6/ K), excellent anti-oxidant and thermal shock resistance, can significantly improve intensification and the speed of cooling of mould in glass moulding technique, reduces dimensional precision and surface quality under high temperature thermal cycling and changes, and is considered to the die base material of tool potentiality.
Mould core for moulding glass protective membrane system has also experienced amorphous carbon, quasi-diamond and noble metal film etc.Though amorphous carbon has good release property, low, the easy damage of intensity, oxidizable, work-ing life is limited.Diamond like carbon film cost is lower, and preparation temperature is low, but also exists the problem weak with base material bonding force, and work-ing life is limited.Precious metal is as the protective membrane taking platinum, iridium or ruthenium alloy as master; can improve the bonding force with base material; due to its reactionlessness; low with the surface reaction of opticglass; greatly improve die work-ing life; be the best mould cavity protective membrane of current result of use, but its cost is higher, aspect the model of high temp glass (more than 700 DEG C), there is certain limitation.WO2013141234A1 provides a kind of mould core for moulding glass.Itself and opticglass contact surface are vitreous carbon material, soak silicon technology original position generate silicon carbide ceramics as matrix by reaction.But silicon carbide ceramics and vitreous carbon bonding strength that this technique is manufactured are general, and vitreous carbon material as mould cavity protective membrane hardness and work-ing life limited.JP2002255570 provides a kind of silicon carbide ceramics die, adopts chemical vapor deposition method preparation.JP2005112672 provides a kind of silicon carbide ceramics die, but between its base material and film, adopts the technique of metal diffusing weldering to connect, and causes the larger thermal expansion mismatch of existence between the two, and thermal shock resistance is poor, and work-ing life is not high.CN200410052270.3 provides a kind of silicon carbide ceramics die, and its base material is silicon carbide, and surface modified membrane is platinoiridita, palladium iridium or its blending ingredients, and middle layer is silicon nitride or aluminium nitride.Because the thickness of transition layer is 1nm-5nm, this technique requires higher to the preparation of transition layer, complex process, and cost is high.CN02140644.8 provides a kind of mould core for moulding glass, and base material is wolfram varbide, and protective membrane is tantalum-tungsten alloy, has reduced manufacturing cost, and can be applicable to the model of high-temperature glass material.
In this field, further reduce the manufacturing cost of glass moulding silicon carbide ceramics die, improve its performance simultaneously, still there is objective demand.
Summary of the invention
The present invention is intended to overcome that existing glass moulding silicon carbide ceramics die preparation cost is high, the dissatisfactory defect of performance, the invention provides a kind of glass moulding silicon carbide ceramics die and preparation method thereof.
The invention provides a kind of glass moulding silicon carbide ceramics die; described silicon carbide ceramics die comprises base material, protective membrane and the intermediate metal between described base material and protective membrane; wherein; described base material is silicon carbide ceramics; protective membrane is carboloy, and described intermediate metal is titanium, chromium or tungsten.
Preferably, described carboloy is the Wimet being formed by wolfram varbide and metal adhesive Co, TaC, the common sintering of Ti, and the weight percentage that described wolfram varbide hard closes middle metal adhesive is 0.5～10%.
Preferably, the thickness of described intermediate metal is 0.05-0.2 μ m.
Preferably, the thickness of described protective membrane is 0.1-0.8 μ m.
Preferably, the surface roughness Ra value≤10nm of described base material, verticality and parallelism≤1.0, bottom surface μ m.
The present invention also provides a kind of method of preparing above-mentioned either carbon SiClx Ceramic mould core, and described method comprises:
1) adopt magnetron sputtering technique at pretreated substrate surface, plate intermediate metal;
2) adopt Assisted by Ion Beam gas-phase deposition, in step 1) on the intermediate metal of the substrate surface prepared, deposition protective membrane.
Preferably, step 1) in, described base material is silicon carbide ceramics, adopts solid phase, liquid phase or reaction sintering to obtain.
Preferably, step 1) in, the parameter of magnetron sputtering technique is: working gas is argon gas, base vacuum degree is 2～4 × 10
-3pa, operating air pressure is 0.2～1Pa, and substrate temperature is 100～200 DEG C, and operating voltage is 80～115V.
Preferably, step 2) in, the parameter of Assisted by Ion Beam gas-phase deposition is: total gas flow rate is 120～210L/ minute, and hydrogen flowing quantity is 1.5～5L/ minute, and vacuum tightness is 1～1 × 10
-5pa, radio frequency power is 5～15MHz, and temperature is 100～650 DEG C, and operating air pressure is 15～50Pa, and depositing time is 150～300 minutes.
Beneficial effect of the present invention:
1, select silicon carbide ceramics to do die core substrate material, thermal expansivity is little, thermal conductivity is high, high temperature resistant, antioxidant property good, and the work-ing life of die is of a specified duration;
2, preparing the magnetron sputtering technique that intermediate metal uses and the ion beam assisted depositing technique of preparing protective membrane is all very ripe preparation technology, and cost is low, and coating effects is good;
3, metallizing transition layer between substrate and protective membrane, can improve the bonding force between substrate and protective membrane like this, makes silicon carbide die intensity higher, improves die work-ing life;
4, the silicon carbide ceramics die prepared by this technical scheme is high temperature resistant, working accuracy is high, the life-span is long, is a kind of technical scheme that can expand application.
Brief description of the drawings
Fig. 1 is the microstructure that in an embodiment of the invention, normal pressure solid-phase sintered silicon carbide ceramics is substrate;
Fig. 2 is the figure of the AFM after normal pressure solid-phase sintered silicon carbide ceramics substrate polishing in an embodiment of the invention;
Fig. 3 is using Cr as transition metal and the die section SEM photo that adopts normal pressure solid-phase sintered silicon carbide ceramics to make as base material in an embodiment of the invention.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for the present invention is described, and unrestricted the present invention.
The invention belongs to engineering ceramic material technical field.The invention provides a kind of glass moulding silicon carbide ceramics die, mainly formed by base material and protective membrane.Wherein base material is silicon carbide ceramics, and surface deposition Wimet wolfram varbide is main protective membrane, and intermediate layer is titanium, chromium or tungsten etc.Adopt silicon carbide ceramics base material, can significantly improve warming and cooling rate in glass moulding process, improve eyeglass productivity.And the Wimet protective membrane that adopts transition layer combination can improve and the bonding strength of base material, improve and the demolding performace of opticglass, compared with precious metal protective membrane, can reduce eyeglass production cost.That the silicon carbide ceramics die that this invention provides has is high temperature resistant, high precision, long-life feature, particularly can be applicable to the model of high temp glass eyeglass, has range of application widely.This die can greatly improve the production efficiency of glass moulding and reduce production costs, and can be applicable to especially the model of high temp glass eyeglass, has range of application widely.
The invention provides a kind of glass moulding silicon carbide ceramics die, comprise base material, intermediate layer and protective membrane, base material is silicon carbide ceramics, and protective membrane is mainly carboloy, and transition layer is metal level.
Described glass moulding silicon carbide ceramics die, this base material is silicon carbide ceramics, can adopt solid phase, liquid phase sintering auxiliary agent or reaction sintering.
Described glass moulding silicon carbide ceramics die, has excellent suface processing quality, and roughness Ra value is less than 10nm.
Described glass moulding silicon carbide ceramics die, has excellent physical dimension precision, and verticality and bottom surface parallelism are less than 1.0 μ m.
Described glass moulding silicon carbide ceramics die, this protective membrane composition is mainly carboloy.Described carboloy is to be the Wimet being formed by wolfram varbide and metal adhesive Co, TaC, the common sintering of Ti, and the weight percentage that described wolfram varbide hard closes middle metal adhesive is 0.5～10.For example can adopt WC-Ta-Co, WC-Co Wimet.
Described glass moulding silicon carbide ceramics die, the thickness of this protective membrane is 0.1-0.8 μ m.
Described glass moulding silicon carbide ceramics die, exists intermediate metal between this protective membrane and base material, and the composition of this transition layer is titanium, chromium or tungsten.
Described glass moulding silicon carbide ceramics die, the thickness of this intermediate metal is 0.05～0.2 μ m.
The concrete steps that technical scheme of the present invention adopts are:
Step 1, employing silicon carbide ceramics are substrate, adopt grinding and polishing or aspherical mirror machining machine, in conjunction with MRF, substrate is carried out to surface finish processing, make the surface roughness Ra≤10nm of silicon carbide substrate;
Step 2, adopt magnetron sputtering technique can improve the metal of substrate and film bonding force at step 1 polished finish good silicon carbide metallizing transition layer Cr, Ti, W etc., and to control metal transition layer thickness be 0.05-0.2um; Groundwork control parameter is that working gas is argon gas, and base vacuum is 2～4 × 10
-3pa, operating air pressure is 0.2～1Pa, 100～200 DEG C of substrate temperatures, operating voltage 80～115V;
In the substrate that step 3, employing Assisted by Ion Beam gas-phase deposition are handled well in step 2, deposit wolfram varbide Wimet film, and to control film thickness be 120～210L/min at 0.1um-0.8um total gas flow rate, hydrogen flowing quantity is 1.5～5L/min, and vacuum tightness is 1～10 × 10
-6pa, radio frequency power is 5～15MHz, and temperature is 100～650 DEG C, and operating air pressure is 15～50Pa, and depositing time is 150～300min.
Feature of the present invention:
1, select silicon carbide ceramics to do die core substrate material, thermal expansivity is little, thermal conductivity is high, high temperature resistant, antioxidant property good, and the work-ing life of die is of a specified duration;
2, preparing the magnetron sputtering technique that intermediate metal uses and the ion beam assisted depositing technique of preparing protective membrane is all very ripe preparation technology, and cost is low, and coating effects is good;
3, metallizing transition layer between substrate and protective membrane, can improve the bonding force between substrate and protective membrane like this, makes silicon carbide die intensity higher, improves die work-ing life;
4, the silicon carbide ceramics die prepared by this technical scheme is high temperature resistant, working accuracy is high, the life-span is long, is a kind of technical scheme that can expand application.
Fig. 1 is the microstructure that in an embodiment of the invention, normal pressure solid-phase sintered silicon carbide ceramics is substrate;
Fig. 2 is the figure of the AFM after normal pressure solid-phase sintered silicon carbide ceramics substrate polishing in an embodiment of the invention;
Fig. 3 is using Cr as transition metal and the die section SEM photo that adopts normal pressure solid-phase sintered silicon carbide ceramics to make as base material in an embodiment of the invention.
Further exemplify embodiment below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter that following example is concrete etc. is only also an example in OK range, and those skilled in the art can be done in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1:
Step 1, do substrate with normal pressure solid-phase sintered silicon carbide ceramics, adopt varigrained diamond paste to carry out surface finish to silicon carbide ceramics, die surface is plane, and making its surface roughness Ra is 5nm, and verticality and bottom surface parallelism are 1.0 μ m;
Step 2, adopt magnetron sputtering technique in polished silicon carbide ceramics plane, to plate Ti intermediate metal in step 1, gauge control is 0.05 μ m;
On the intermediate metal that step 3, employing Assisted by Ion Beam gas-phase deposition have plated in step 2, deposit WC Wimet film, controlling thickness is 0.1 μ m.
Embodiment 2:
Step 1, do substrate with normal pressure liquid phase sintering silicon carbide ceramic, adopt varigrained diamond paste to carry out surface finish to silicon carbide ceramics, die surface is plane, and making its surfaceness reach Ra is 10nm, and verticality and bottom surface parallelism are 1.0 μ m;
Step 2, technique as identical in step 2 in embodiment 1 are at the ready silicon carbide substrate plating metal on surface of step 1 transition layer Ti, and the thickness of controlling intermediate metal is 0.2 μ m;
Step 3, the silicon carbide substrate protective film coating wolfram varbide preparing in step 2 as the identical step of step 3 in embodiment 1, and to control protective membrane Tungsten Carbide Thin Film thickness be 0.8 μ m.
Embodiment 3:
Step 1, do substrate with hot pressing solid-phase sintered silicon carbide ceramics, adopt the auxiliary MRF of aspherical mirror machining locomotive bed to carry out polishing, polished surface is sphere, and making its surfaceness reach Ra is 8nm, and verticality and bottom surface parallelism are 1.0 μ m;
Step 2, technique as identical in step 2 in embodiment 1 are at the ready silicon carbide substrate plating metal on surface of step 1 transition layer Cr, and the thickness of controlling intermediate metal is 0.05 μ m;
Step 3, the silicon carbide substrate protective film coating wolfram varbide preparing in step 2 as the identical step of step 3 in embodiment 1, and to control protective membrane Tungsten Carbide Thin Film thickness be 0.4 μ m;
In embodiment 3, adopt in Fig. 1 normal pressure solid-phase sintered silicon carbide ceramics as base material, after polished finish as shown in Figure 2, finally obtain taking Cr as transition metal and adopt the die material of normal pressure solid-phase sintered silicon carbide ceramics as substrate.
Embodiment 4:
Step 1, do substrate with hot pressing liquid phase sintering silicon carbide ceramic, adopt the auxiliary MRF of aspherical mirror machining locomotive bed to carry out polishing, polished surface is sphere, and making its surfaceness reach Ra is 5nm, and verticality and bottom surface parallelism are 0.5 μ m;
Step 2, technique as identical in step 2 in embodiment 1 are at the ready silicon carbide substrate plating metal on surface of step 1 transition layer Cr, and the thickness of controlling intermediate metal is 0.2 μ m;
Step 3, the silicon carbide substrate protective film coating wolfram varbide preparing in step 2 as the identical step of step 3 in embodiment 1, and the thickness of controlling protective membrane Tungsten Carbide Thin Film is 0.1 μ m.
Embodiment 5:
Step 1, do substrate with reaction sintering silicon carbide ceramic, adopt the auxiliary MRF of aspherical mirror machining locomotive bed to carry out polishing, polished surface is aspheric surface, and making its surfaceness reach Ra is 10nm, and verticality and bottom surface parallelism are 0.6 μ m;
Step 2, technique as identical in step 2 in embodiment 1 are at the ready silicon carbide substrate plating metal on surface of step 1 transition layer W, and the thickness of controlling intermediate metal is 0.05 μ m;
Step 3, the silicon carbide substrate protective film coating wolfram varbide preparing in step 2 as the identical step of step 3 in embodiment 1, and the thickness of controlling protective membrane Tungsten Carbide Thin Film is 0.8 μ m.
Embodiment 6:
Step 1, do substrate with reaction sintering silicon carbide ceramic, adopt the auxiliary MRF of aspherical mirror machining locomotive bed to carry out polishing, polished surface is aspheric surface, and making its surfaceness reach Ra is 8nm, and verticality and bottom surface parallelism are 0.5 μ m;
Step 2, technique as identical in step 2 in embodiment 1 are at the ready silicon carbide substrate plating metal on surface of step 1 transition layer W, and the thickness of controlling intermediate metal is 0.2 μ m;
Step 3, the silicon carbide substrate protective film coating wolfram varbide preparing in step 2 as the identical step of step 3 in embodiment 1, and the thickness of controlling protective membrane Tungsten Carbide Thin Film is 0.4 μ m.
Claims (9)
1. a glass moulding silicon carbide ceramics die; it is characterized in that; described silicon carbide ceramics die comprises base material, protective membrane and the intermediate metal between described base material and protective membrane; wherein; described base material is silicon carbide ceramics; protective membrane is carboloy, and described intermediate metal is titanium, chromium or tungsten.
2. silicon carbide ceramics die according to claim 1, it is characterized in that, described carboloy is the Wimet being formed by wolfram varbide and the common sintering of metal adhesive, the weight percentage that described wolfram varbide hard closes middle metal adhesive is 0.5～10%, wherein, the preferred Co of metal adhesive, TaC, Ti.
3. silicon carbide ceramics die according to claim 1 and 2, is characterized in that, the thickness of described intermediate metal is 0.05-0.2 μ m.
4. according to arbitrary described silicon carbide ceramics die in claim 1-3, it is characterized in that, the thickness of described protective membrane is 0.1-0.8 μ m.
5. according to arbitrary described silicon carbide ceramics die in claim 1-4, it is characterized in that the surface roughness Ra value≤10nm of described base material, verticality and parallelism≤1.0, bottom surface μ m.
6. a method of preparing arbitrary described silicon carbide ceramics die in claim 1-5, is characterized in that, described method comprises:
1) adopt magnetron sputtering technique at pretreated substrate surface, plate intermediate metal;
2) adopt Assisted by Ion Beam gas-phase deposition, on the intermediate metal of the substrate surface of preparing in step 1), deposition protective membrane.
7. method according to claim 6, is characterized in that, in step 1), described base material is silicon carbide ceramics, adopts solid phase, liquid phase or reaction sintering to obtain.
8. according to arbitrary described method in claim 6-7, it is characterized in that, in step 1), the parameter of magnetron sputtering technique is: working gas is argon gas, and base vacuum degree is 2-4 × 10
-3pa, operating air pressure is 0.2-1Pa, and substrate temperature is 100-200 DEG C, and operating voltage is 80-115V.
9. according to arbitrary described method in claim 6-8, it is characterized in that step 2) in, the parameter of Assisted by Ion Beam gas-phase deposition is: total gas flow rate is 120-210L/ minute, and hydrogen flowing quantity is 1.5-5L/ minute, and vacuum tightness is 1-1 × 10
-5pa, radio frequency power is 5-15MHz, and temperature is 100-650 DEG C, and operating air pressure is 15-50Pa, and depositing time is 150-300 minute.
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| CN201410314758.2A CN104030548A (en) | 2014-07-03 | 2014-07-03 | Silicon carbide ceramic mold core for glass molding and manufacturing method thereof |
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|---|---|---|---|
| CN201410314758.2A CN104030548A (en) | 2014-07-03 | 2014-07-03 | Silicon carbide ceramic mold core for glass molding and manufacturing method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113526961A (en) * | 2021-08-19 | 2021-10-22 | 南通三责精密陶瓷有限公司 | Manufacturing method of silicon carbide mold for glass molding and silicon carbide mold |
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