CN110981488A - Ultrahigh-hardness aspheric glass lens mold material and preparation method thereof - Google Patents
Ultrahigh-hardness aspheric glass lens mold material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an ultrahigh-hardness aspheric glass lens mold material and a preparation method thereof, wherein the mold material comprises, by weight, 0.1-0.5% of Co, 0.5-5% of TaC and 0.45-0.75% of Cr3C20.30 to 0.50 percent of VC, and the balance of WC; the preparation method comprises the steps of material preparation, wet grinding, wax doping, shaping, sintering and heat treatment. The invention limits the optimized technical conditions of each component in the raw materials and the optimized process conditions for preparing the product. The ultrahigh-hardness aspheric glass lens mold material has the WC average grain size of 0.13-0.25 mu m, the porosity of A02B00C00 and the HV102650-2750, has the advantages of good high-temperature stability, high wear resistance and good thermal shock resistance, and the manufactured optical glass mold core has high forming quality and multiple molding times, thereby reducing the aspheric surface glassThe production cost of the precision die pressing forming of the glass lens.
Description
Technical Field
The invention belongs to the field of precision die forming of aspheric optical glass, and particularly relates to an ultrahigh-hardness aspheric glass lens die material and a preparation method thereof.
Background
With the rapid development of high-end manufacturing technology, precision optical glass (mainly aspheric glass lenses) is more and more widely applied to civil and national defense fields such as satellite monitoring systems, laser radiation, microsystems, optical fiber communication, infrared night vision imaging and the like. With the continuous development of glass lenses to micro-volume, high precision and high imaging quality, the precision mould pressing forming technology becomes a key link for the development and application of aspheric lens glass. The technology has high requirements on the red hardness, the wear resistance, the heat conductivity, the thermal expansion coefficient and the chemical stability of the die material.
The glass precision press molding technology is a glass lens manufacturing technology which heats optical glass to a proper temperature above a transition temperature Tg, and copies the shape of a mold core to a glass prefabricated member by moving an upper mold and a lower mold. In essence, the accuracy of the lens is largely determined by the mold. The mold manufacture becomes the bottleneck of the development of the precision press molding technology, and the material of the mold needs to have the following characteristics: a. the high hardness and the high strength are kept at high temperature, the thermal expansion coefficient is as small as possible, and the chemical stability is good; b. the material has high compactness and no internal defect, and the surface roughness reaches below 10nm after processing; c. no adhesion phenomenon occurs with the glass material. In the glass molding apparatus used at present, the mold is generally made of superhard material, ceramic material and a coating film on the mold body.
WC-based composite ceramic materials (binderless tungsten carbide materials) refer to WC alloys that contain no or little metal binder (< 0.5% by mass). Compared with the traditional hard alloy, the WC-based composite ceramic material has more excellent high hardness, high temperature resistance, wear resistance, corrosion resistance and oxidation resistance, and when the WC-based composite ceramic material bears 200-2000N of pressure and 400-1400 ℃ of service temperature in the precision die forming process, the strength and toughness of the WC-based composite ceramic material also meet the requirements, so that the WC-based composite ceramic material is a reliable die core material for precision die forming.
At present, the domestic precision press molding die core for high-precision optical glass is mainly imported through die material processing or direct finished product import, and the die core HV thereof10Hardness of over 2650, domestic self-developed tungsten carbide mould material HV10The hardness is lower than 2600. Chinese patent CN 109692955A discloses a preparation method of pure tungsten carbide hard alloy and pure tungsten carbide hard alloy, the Vickers hardness is 2600-2700HV, the bending strength is 1400-1500MPa, the compression strength is 7000-8000MPa, the density of tungsten carbide material is 99%, more pores still exist in the material, and the surface roughness after processing can not reach the requirement of the performance of the mold core. To achieve tungsten carbide material hardness HV102650, A02B00C00, and further optimization of the tungsten carbide material components and preparation process are of great significance.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an ultrahigh-hardness aspheric glass lens mold material and a preparation method thereof in order to further improve the performance of a tungsten carbide material.
The invention adopts the following technical scheme:
the mold material for the ultrahigh-hardness aspheric glass lens is characterized by comprising the following ingredients in percentage by weight: 0.1 to 0.5 percent of Co, 0.5 to 5 percent of TaC and 0.45 to 0.75 percent of Cr3C20.3 to 0.5 percent of VC and the balance of WC.
The die material is characterized in that WC powder is subjected to classification treatment, the Fisher size of the WC powder is 0.1-0.2 μm, the Fisher size of the Co powder is 0.6-0.9 μm, and the Fisher size of the TaC powder is 0.4-0.6 μm;
the preparation method of the die material is characterized by comprising the following steps of:
(1) uniformly mixing ingredients Co, TaC and WC, and then placing the mixture into a rolling ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, deionized water (10-15):1, the liquid-solid ratio of the ball milling medium to the ingredients is 350mL/kg-450mL/kg, the ball-material ratio is (5-8):1, and the ball milling time is 96h-120h, so as to obtain a ball grinding material;
(2) drying the ball grinding material in a vacuum stirring dryer at the drying temperature of 80-90 ℃, screening, doping wax and screening to obtain a mixture, wherein the screening is carried out under the protection of nitrogen or argon, and the content of the doped paraffin is 0-1.5 wt% of the ingredients;
(3) preparing a formed blank by carrying out die pressing or cold isostatic pressing on the mixture, wherein the die pressing pressure is 5t-20t, the cold isostatic pressing pressure is 100MPa-150MPa, and the size of the formed blank is phi (5-30) mm x (5-15) mm;
(4) carrying out thermal degreasing on the formed blank under the protection of hydrogen atmosphere to remove the binder, wherein the degreasing temperature is 550-650 ℃, and the heat preservation time is 30-90 min; then, pre-sintering is carried out, the pre-sintering temperature is 850-950 ℃, and the heat preservation time is 30-60 min, so as to obtain a pre-sintered blank;
(5) placing the pre-sintered blank on a graphite boat coated with alumina or zirconia for vacuum sintering, wherein the sintering temperature is 1600-1650 ℃, and the heat preservation time is 45-60 min, so as to obtain a sintered blank; and carrying out hot isostatic pressing treatment on the sintered blank, wherein the heat treatment temperature is 1500-1600 ℃, the heat preservation time is 45-60 min, and the pressure is 150-200 MPa, so as to obtain the die material.
The preparation method is characterized in that in the step (1), ingredients Co, TaC and WC are pre-added with a binder and then placed in a rolling ball milling tank, wherein the binder accounts for 0-1.5 wt% of the ingredients; the binder is one or more of paraffin, methylcellulose, polyvinyl alcohol, glycerol and polyethylene glycol.
The invention has the following beneficial effects:
1. the aspheric glass lens mold material with ultrahigh hardness prepared by the invention is particularly suitable for optical glass lens mold cores, the average grain size of WC of the aspheric glass lens mold material is 0.13-0.25 mu m, the porosity of the aspheric glass lens mold material is A02B00C00, and HV102650-2750, and has the advantages of good high-temperature stability, high wear resistance and good thermal shock resistance.
2. According to the preparation method provided by the invention, superfine grading tungsten carbide, superfine cobalt powder and superfine tantalum carbide powder are used as raw materials, and the solution is pre-added with a binder to improve powder agglomeration, prevent powder oxidation and improve the uniformity of a mixture, so that the uniform distribution of a hardening agent and fine tungsten carbide grains are realized; meanwhile, the optimized process of presintering, vacuum sintering and hot isostatic pressing treatment is adopted to realize the grain size control of tungsten carbide and reduce the porosity of the material.
3. The invention adopts the methods of component optimization of the hardening agent, homogenization and anti-oxidation measures of the mixture, control of a grain growth mechanism and the like to reduce the grain size of the tungsten carbide and the porosity of the material, thereby improving the hardness and the wear resistance of the tungsten carbide material, further improving the mechanical property of the optical glass mold core and prolonging the service life.
4. The mold material for the aspheric glass lens with ultrahigh hardness, prepared by the invention, is processed into the mold core of the aspheric glass lens, has high surface smoothness, good glass lens forming quality, multiple molding times and good abrasion resistance of the surface of the mold core, and reduces the production cost of precise molding of the aspheric glass lens.
Drawings
FIG. 1 is a scanning electron microscope (BSE) microstructure of an ultra-high hardness aspherical glass lens mold material in example 1 of the present invention;
fig. 2 is a scanning electron microscope (BSE) microstructure of the ultra-high hardness aspheric glass lens mold material in example 2 of the present invention.
Detailed Description
The invention relates to an ultrahigh-hardness aspheric glass lens mold material, which comprises the following ingredients in percentage by weight: 0.1 to 0.5 percent of Co, 0.5 to 5 percent of TaC and 0.45 to 0.75 percent of Cr3C20.30 to 0.50 percent of VC and the balance of WC. The WC powder is subjected to grading treatment, the Fisher particle size of the WC powder is 0.1-0.2 mu m, the Fisher particle size of the Co powder is 0.6-0.9 mu m, and the Fisher particle size of the TaC powder is 0.4-0.6 mu m.
The preparation method of the die material comprises the following steps: (1) uniformly mixing ingredients Co, TaC and WC, and then placing the mixture into a rolling ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, deionized water (10-15):1, the liquid-solid ratio of the ball milling medium to the ingredients is 350mL/kg-450mL/kg, the ball-material ratio is (5-8):1, and the ball milling time is 96h-120h, so as to obtain a ball grinding material; preferably, ingredients Co, TaC and WC are pre-added with a binder and then placed in a rolling ball milling tank, wherein the binder accounts for 0-1.5 wt% of the ingredients; the binder is one or more of paraffin, methylcellulose, polyvinyl alcohol, glycerol and polyethylene glycol. (2) Drying the ball grinding material in a vacuum stirring dryer at the drying temperature of 80-90 ℃, screening, doping wax and screening to obtain a mixture, wherein the screening is carried out under the protection of nitrogen or argon, and the content of the doped paraffin is 0-1.5 wt% of the ingredients. (3) And preparing a formed blank by carrying out die pressing or cold isostatic pressing on the mixture, wherein the die pressing pressure is 5t-20t, the cold isostatic pressing pressure is 100MPa-150MPa, and the size of the formed blank is phi (5-30) mm x (5-15) mm. (4) Carrying out thermal degreasing on the formed blank under the protection of hydrogen atmosphere to remove the binder, wherein the degreasing temperature is 550-650 ℃, and the heat preservation time is 30-90 min; and then pre-sintering, wherein the pre-sintering temperature is 850-950 ℃, and the heat preservation time is 30-60 min, so as to obtain a pre-sintered blank. (5) Placing the pre-sintered blank on a graphite boat coated with alumina or zirconia for vacuum sintering, wherein the sintering temperature is 1600-1650 ℃, and the heat preservation time is 45-60 min, so as to obtain a sintered blank; and carrying out hot isostatic pressing treatment on the sintered blank, wherein the heat treatment temperature is 1500-1600 ℃, the heat preservation time is 45-60 min, and the pressure is 150-200 MPa, so as to obtain the die material.
Example 1
Adding the WC powder, the TaC powder, the Co powder and the pre-added binder into a rolling ball milling tank, wherein the ingredients comprise 0.1 wt% of Co powder (Fisher granularity is 0.9 mu m), 5 wt% of TaC (Fisher granularity is 0.6 mu m) and 0.45 wt% of Cr3C20.3 wt% of VC, and the balance of WC (Fisher size of 0.2 μm); the pre-added binder comprises: 0.25 wt% paraffin wax, 0.25 wt% polyethylene glycol. The ball milling medium is absolute alcohol and deionized water which are 15:1, the liquid-solid ratio is 450mL/kg, the ball material ratio of YG8 round balls (phi 6) is 8:1, the ball milling speed is 60r/min, and the ball milling is carried out for 96h to obtain the ball milling material. Drying the ball grinding material in a vacuum stirring dryer at 80 deg.C, sieving under argon protection (-320 mesh), adding wax in an amount of 1.5 wt% of the material, and sievingAnd (4) screening to (-200 meshes) to obtain a mixture. The mixture is molded to obtain a molding blank with the diameter of 10mm multiplied by 10mm, and the molding pressure is 5 t. Carrying out thermal degreasing on the formed blank under the protection of hydrogen atmosphere, wherein the thermal degreasing temperature is 600 ℃, and the heat preservation time is 60 min; and continuously heating for presintering, wherein the presintering temperature is 850 ℃, and the heat preservation time is 60min, so as to obtain a presintering blank. Placing the pre-sintered blank on a graphite boat coated with alumina for vacuum sintering to obtain a sintered blank, wherein the sintering temperature is 1650 ℃, and the heat preservation time is 45 min; and carrying out hot isostatic pressing treatment on the sintered blank, wherein the heat treatment temperature is 1500 ℃, the heat preservation time is 45min, and the pressure is 200 MPa.
FIG. 1 is a scanning electron microscope (BSE) microstructure of the ultra-high hardness aspherical glass lens mold material prepared in example 1, having a WC average grain size of 0.25 μm, a porosity of A02B00C00, HV102650.
Example 2
Adding the WC powder, the TaC powder, the Co powder and the pre-added binder into a rolling ball milling tank, wherein the ingredients comprise 0.5 wt% of Co powder (Fisher granularity is 0.6 mu m), 0.5 wt% of TaC (Fisher granularity is 0.4 mu m) and 0.75 wt% of Cr3C20.5 wt% VC, balance WC (Fisher size 0.1 μm); the pre-added binder comprises: 0.5 wt% of methyl cellulose, 0.25 wt% of glycerol and 0.25 wt% of polyvinyl alcohol. The ball milling medium is absolute alcohol and deionized water which are 10:1, the liquid-solid ratio is 350mL/kg, the ball material ratio of the YG8 round balls (phi 6) is 5:1, the ball milling speed is 60r/min, and the ball milling is carried out for 120h to obtain the ball milling material. And drying the ball grinding material in a vacuum stirring dryer at the drying temperature of 90 ℃, and then sieving the ball grinding material under the protection of argon gas to obtain a mixture, wherein the sieve is a (-200 meshes sieve). The mixture is subjected to cold isostatic pressing to form a formed blank with the diameter of 30mm multiplied by 15mm, and the pressure is 150 MPa. Carrying out thermal degreasing on the formed blank under the protection of hydrogen atmosphere, wherein the thermal degreasing temperature is 950 ℃, and the heat preservation time is 45 min; and continuously heating for presintering, wherein the presintering temperature is 950 ℃, and the heat preservation time is 30min, so as to obtain a presintering blank. Placing the pre-sintered blank on a graphite boat coated with alumina, and performing vacuum sintering to obtain a sintered blank, wherein the sintering temperature is 1600 ℃, and the heat preservation time is 60 min; hot isostatic pressing treatment is carried out on the sintered blank, the heat treatment temperature is 1600 ℃, and the heat preservation time isThe time is 60min and the pressure is 150 MPa.
FIG. 2 is a scanning electron microscope (BSE) microstructure of the ultra-high hardness aspherical glass lens mold material prepared in example 2, having a WC average grain size of 0.13 μm, a porosity of A02B00C00, HV10Is 2750.
Claims (4)
1. The mold material for the ultrahigh-hardness aspheric glass lens is characterized by comprising the following ingredients in percentage by weight: 0.1 to 0.5 percent of Co, 0.5 to 5 percent of TaC and 0.45 to 0.75 percent of Cr3C20.3 to 0.5 percent of VC and the balance of WC.
2. The die material according to claim 1, wherein the WC powder is subjected to classification treatment, the Fisher size of the WC powder is 0.1 to 0.2 μm, the Fisher size of the Co powder is 0.6 to 0.9 μm, and the Fisher size of the TaC powder is 0.4 to 0.6 μm.
3. The method for preparing a mold material according to any one of claims 1-2, comprising the steps of:
(1) uniformly mixing ingredients Co, TaC and WC, and then placing the mixture into a rolling ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, deionized water (10-15):1, the liquid-solid ratio of the ball milling medium to the ingredients is 350mL/kg-450mL/kg, the ball-material ratio is (5-8):1, and the ball milling time is 96h-120h, so as to obtain a ball grinding material;
(2) drying the ball grinding material in a vacuum stirring dryer at the drying temperature of 80-90 ℃, screening, doping wax and screening to obtain a mixture, wherein the screening is carried out under the protection of nitrogen or argon, and the content of the doped paraffin is 0-1.5 wt% of the ingredients;
(3) preparing a formed blank by carrying out die pressing or cold isostatic pressing on the mixture, wherein the die pressing pressure is 5t-20t, the cold isostatic pressing pressure is 100MPa-150MPa, and the size of the formed blank is phi (5-30) mm x (5-15) mm;
(4) carrying out thermal degreasing on the formed blank under the protection of hydrogen atmosphere to remove the binder, wherein the degreasing temperature is 550-650 ℃, and the heat preservation time is 30-90 min; then, pre-sintering is carried out, the pre-sintering temperature is 850-950 ℃, and the heat preservation time is 30-60 min, so as to obtain a pre-sintered blank;
(5) placing the pre-sintered blank on a graphite boat coated with alumina or zirconia for vacuum sintering, wherein the sintering temperature is 1600-1650 ℃, and the heat preservation time is 45-60 min, so as to obtain a sintered blank; and carrying out hot isostatic pressing treatment on the sintered blank, wherein the heat treatment temperature is 1500-1600 ℃, the heat preservation time is 45-60 min, and the pressure is 150-200 MPa, so as to obtain the die material.
4. The preparation method according to claim 3, wherein in the step (1), the ingredients Co, TaC and WC are placed in a rolling ball mill tank after pre-adding a binder, wherein the binder accounts for 0-1.5 wt% of the ingredients; the binder is one or more of paraffin, methylcellulose, polyvinyl alcohol, glycerol and polyethylene glycol.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115846668A (en) * | 2022-11-04 | 2023-03-28 | 安徽尚欣晶工新材料科技有限公司 | Hard alloy material for optical die and preparation method thereof |
| CN116145002A (en) * | 2022-12-27 | 2023-05-23 | 合肥工业大学 | Cemented carbide material for compression molding of precision glass lens and preparation method thereof |
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