Curved-surface transparent protective ceramic composite protective material for vehicle and preparation method of curved-surface transparent protective ceramic composite protective material

Abstract

The preparation method comprises the following steps: performing by adopting a dry pressing process, compacting by adopting a cold isostatic pressing process to prepare a curved-surface transparent ceramic biscuit, sintering at high temperature, performing CNC (Computer Numerical Control) precision machining, and polishing and grinding the surface to obtain curved-surface transparent ceramic; fixing the curved-surface transparent ceramic with the opening facing upwards, overlapping at least two layers of cut plain glass on the curved-surface transparent ceramic in sequence, spraying silicon dioxide between every two layers of glass and on the surface of the ceramic, and heating and softening in a bending furnace to be tightly attached to the surface of the curved-surface transparent ceramic; sequentially laminating the organic plate, the plurality of layers of plain glass and the curved transparent ceramic from top to bottom according to the adhesive sheets between the layers, sleeving the laminated sheets with a vacuum rubber ring, carrying out cold air pumping, transferring the laminated sheets into a high-pressure kettle, pressurizing and heating, exhausting and reducing pressure, and taking out the transparent ceramic composite FH material, so as to obtain the transparent ceramic composite FH material. And cutting off redundant films around to obtain the curved-surface transparent protective ceramic composite protective material for the vehicle.

Description

Technical Field

[0001] The invention discloses a vehicle curved surface transparent protective ceramic composite protective material and a preparation method thereof, belonging to the technical field of transparent protective ceramic composite protective materials. Background Art

[0002] At present, high-security protective glass adopts a multi-layer structure to achieve the protective effect. The glass is thick and heavy, and the vehicle's maneuverability is reduced. Transparent ceramic is a kind of ceramic with light-transmitting properties prepared by ceramic technology. It has the characteristics of good light transmittance, high hardness, corrosion resistance, high temperature resistance, and excellent protective performance. Compared with traditional protective glass, the composite protective material prepared by transparent ceramic can reduce weight by 50% and thickness by more than 40%.

[0003] Existing automotive glass, including front and rear windshields and door glass, has a certain curvature. Therefore, in terms of preparation technology, multi-layer protective glass is often produced by integral bending, which has high inter-layer matching accuracy and high production efficiency. However, transparent ceramics have a high melting point (>2000°C) and will not gradually soften with increasing temperature. The molding method mainly relies on sintering of the blank and subsequent processing, and cannot be integrally bent with the glass laminate.

[0004] Ceramics will shrink in size during the sintering process, and post-processing will also affect the actual size, thickness and curvature. Therefore, the finished transparent ceramic product will be significantly deformed compared to the blank, and the curvature of the matching glass is difficult to determine, which affects the subsequent assembly and causes a decline in optical performance, making it difficult to meet automotive requirements. Summary of the invention

[0005] The purpose of the present invention is to solve the problems existing in the existing glass protection configuration and to provide a vehicle curved surface transparent protective ceramic composite protective material and a preparation method thereof.

[0006] The problem to be solved by the present invention is achieved by the following technical solutions:

[0007] A method for preparing a curved transparent protective ceramic composite protective material for a vehicle, comprising:

[0008] Step S1, preforming by dry pressing process, and then compacting by cold isostatic pressing process to prepare curved transparent ceramic blank, sintering at high temperature, CNC precision machining, and surface polishing to obtain curved transparent ceramic;

[0009] Step S2, fix the curved ceramic with the opening facing upward, stack at least two layers of cut flat glass in order and place them on the curved transparent ceramic, spray silicon dioxide between each layer of glass and on the surface of the ceramic, heat and soften them in a bending furnace to closely adhere to the surface of the curved transparent ceramic;

[0010] Step S3, from top to bottom, the organic board, the multi-layer flat glass and the curved transparent ceramic layers are laminated with films, the laminated sheets are covered with vacuum rubber rings and cold air is extracted, transferred to an autoclave for pressurized heating, vented and depressurized, the transparent ceramic composite FH material is taken out, and the surrounding excess films are cut off to obtain the automotive curved transparent protective ceramic composite protective material.

[0011] Preferably, the transparent ceramic in step S1 is made of AlON ceramic, YAG ceramic or magnesium aluminum spinel ceramic material.

[0012] Preferably, in step S1, the dry pressing process pressure is 150 MPa to 500 MPa, the holding time is 1 min to 10 min, the sintering temperature is 1600° C. to 2000° C., and the sintering time is 10 to 30 h.

[0013] Preferably, in the step S1, the cold isostatic pressing process pressure is 100 MPa to 600 MPa, the holding time is 5 min to 30 min, the light transmittance of the curved transparent ceramic is at least 70%, and the thickness of the curved transparent ceramic is 4 mm to 10 mm.

[0014] Preferably, the bending temperature in step S2 is 500° C. to 800° C., and the time is 1 to 10 hours.

[0015] Preferably, in step S2, the thickness of the single glass layer is 3 mm to 8 mm.

[0016] Preferably, in step S3, the air is cold-extracted for 5 minutes or longer, and the mixture is transferred to an autoclave and pressurized and heated at a pressure of 0.5 MPa to 2 MPa and a temperature of 130° C. to 200° C. The mixture is vented and depressurized after 1 hour.

[0017] Preferably, in step S3, the thickness of the organic sheet is 2-4 mm, and the light transmittance of the organic sheet is greater than 80%.

[0018] Preferably, in step S3, the film is made of polyurethane material, and the thickness of the film is 0.5 mm to 1 mm.

[0019] A vehicle curved surface transparent protective ceramic composite protective material prepared by the above-mentioned preparation method.

[0020] The present invention has the following beneficial effects compared with the prior art:

[0021] The invention discloses a vehicle-use curved transparent protective ceramic composite protective material and a preparation method thereof. First, the curved transparent ceramic forming method adopts dry pressing process for preforming, and then adopts cold isostatic pressing process to compact the blank, and then CNC precision machining is performed after high temperature sintering, and the surface is polished and ground to achieve a transmittance of more than 70%. Secondly, the multi-layer glass bending method adopts the prepared curved transparent ceramic as a glass bending mold to ensure that the glass and the transparent ceramic are precisely matched, and the optical performance is good after the composite, while avoiding the separate mold opening in the glass forming process, reducing the production cost. Finally, the sheet-joining process method adopts transparent ceramic on the bullet-facing surface, and utilizes the high hardness of transparent ceramic to crush the projectile. The back plate is an organic plate to prevent fragments from flying, and the number of glass layers can be reduced to achieve thinning and weight reduction. The hot pressing process is adopted for compounding, which has simple process, high compounding precision and good product protection performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The present invention is a flow chart of a method for preparing a vehicle curved surface transparent protective ceramic composite protective material. DETAILED DESCRIPTION

[0023] The following is based on the attached Figure 1 The present invention is further described:

[0024] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] In the description of the present invention, it should be noted that the terms "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside", etc. indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limitations on the present invention.

[0026] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0027] The first embodiment of the present invention provides a method for preparing a vehicle curved surface transparent protective ceramic composite protective material based on the prior art, which specifically includes the following steps:

[0028] Step S1, preforming by dry pressing process, and then compacting by cold isostatic pressing process to prepare curved transparent ceramic blank, sintering at high temperature, CNC precision machining, surface polishing and grinding, to obtain curved transparent ceramic, the specific contents are as follows:

[0029] Transparent ceramics are made of AlON ceramics, YAG ceramics or magnesium aluminum spinel ceramic materials. Transparent ceramics use high-purity ultrafine high-dispersion powders, and dry pressing and isostatic pressing processes are used to prepare high-density large-size curved blanks. After high-temperature sintering and molding, curved transparent ceramics are obtained through post-treatment. The dry pressing process pressure is 150MPa~500MPa, and the holding time is 1min~10min. The cold isostatic pressing process pressure is 100MPa~600MPa, and the holding time is 5min~30min. The sintering temperature is 1600℃~2000℃, and the sintering time is 10~30h. The transmittance of curved transparent ceramics is more than 70%, and the thickness of curved transparent ceramics is 4mm~10mm.

[0030] The following is a detailed description using AlON ceramics and YAG ceramics as examples:

[0031] When the transparent ceramic is AlON ceramic, the above step S1 specifically includes:

[0032] The AlON powder was placed in a mold at a pressure of 200 MPa for 3 minutes. After the pre-formed curved shape, the cold isostatic pressing process at a pressure of 300 MPa was used to compact the blank to obtain a curved AlON transparent ceramic blank. The curved AlON transparent ceramic blank was sintered at a high temperature of 1900 ° C for 10 hours in a hydrogen atmosphere, and CNC precision machining was used, and the surface was polished to obtain a curved AlON transparent ceramic with a thickness of 4 mm.

[0033] When the transparent ceramic is YAG ceramic, the above step S1 specifically includes:

[0034] According to the stoichiometric ratio of each element in the chemical formula Y3Al5O12, Y2O3 powder and Al2O3 powder were weighed and placed in the mold at a pressure of 150MPa for 4 minutes. After the pre-forming of the curved surface, the green blank was compacted by cold isostatic pressing at a pressure of 280MPa to obtain a curved YAG transparent ceramic green blank.

[0035] The curved surface YAG transparent ceramic blank was sintered at a high temperature of 1600° C. for 10 hours, and was precisely processed by CNC, and the surface was polished and ground to obtain a curved surface YAG transparent ceramic with a thickness of 5 mm.

[0036] Step S2, fix the curved ceramic with the opening facing upward, stack at least two layers of cut flat glass in order and place them on the curved transparent ceramic, spray silicon dioxide between each layer of glass and on the surface of the ceramic, heat and soften in a bending furnace to closely adhere to the surface of the curved transparent ceramic, the specific steps are as follows:

[0037] The glass is formed by the bending process, and the bending mold is a curved transparent ceramic. The curved ceramic is fixed with the opening facing upward, and the cut multi-layer flat glass is stacked in order and placed on the curved ceramic surface. Silicon dioxide with a diameter of 0.8 microns is sprayed between each layer of glass and on the ceramic surface to prevent sticking during the bending process. After that, it is heated and softened in the bending furnace and tightly adhered to the ceramic surface by its own gravity. The bending temperature is 500℃~800℃, the time is 1~10h, and the thickness of the single layer of glass is 3mm~8mm.

[0038] The following is a detailed description using AlON ceramics and YAG ceramics as examples:

[0039] When the transparent ceramic is AlON ceramic, the above step S2 specifically includes:

[0040] The cut three layers of flat glass are stacked in order, with a glass thickness of 5mm, and placed on the curved transparent ceramic. Silicon dioxide with a diameter of 0.8 microns is sprayed between each layer of glass and on the ceramic surface to prevent sticking during the bending process. Then it is heated and softened in a bending furnace at a temperature of 680℃ for 3 hours, and fits tightly to the mold surface by its own gravity.

[0041] When the transparent ceramic is YAG ceramic, the above step S2 specifically includes:

[0042] The cut three layers of flat glass are stacked in order, with a glass thickness of 5mm, and placed on the curved transparent ceramic. Silicon dioxide with a diameter of 0.8 microns is sprayed between each layer of glass and on the ceramic surface to prevent sticking during the bending process. Then it is heated and softened in a bending furnace at a temperature of 680℃ for 3 hours, and fits tightly to the mold surface by its own gravity.

[0043] Step S3, from top to bottom, sequentially laminate the organic sheet, the multi-layer flat glass and the curved transparent ceramic layers with films between them, put a vacuum rubber ring on the laminated sheets and evacuate the air, transfer them to an autoclave for pressurized heating, exhaust the air and reduce the pressure, take out the transparent ceramic composite FH material, cut off the surrounding excess films to obtain the automotive curved transparent protective ceramic composite protective material, the specific steps are as follows:

[0044] According to the transparent ceramic at the bottom, the organic sheet at the top, the glass in the middle, the film between each layer, put on the vacuum rubber ring, and then cold-pump the glass to remove the air in the middle of the sheet, and the cold-pumping time should be no less than 5 minutes. In order to ensure that the sheet is firm and tight and the exhaust is sufficient, it is first preheated and pressed, and then transferred to the autoclave, pressurized and heated, the pressure is 0.5MPa~2MPa, the temperature is 130℃~200℃, and the pressure is reduced after 1h. The transparent ceramic composite FH material is taken out, and the excess film around it is cut off to obtain the automotive curved transparent protective ceramic composite protective material. The organic sheet is PC material, the thickness of the organic sheet is 2~4mm, the transmittance of the organic sheet is>80%, and the film is polyurethane material, and the film thickness is 0.5mm~1mm.

[0045] The following is a detailed description using AlON ceramics and YAG ceramics as examples:

[0046] When the transparent ceramic is AlON ceramic, the above step S3 specifically includes:

[0047] The transparent ceramic is at the bottom, the PC board is in the middle, and the layers are stacked together; a vacuum rubber ring is put on the laminate, and then the laminate is cold-drawn to expel the air in the middle of the laminate, and the cold-drawing time is 7 minutes; it is transferred to an autoclave, pressurized and heated to a pressure of 1MPa and a temperature of 150℃, and the pressure is reduced after 1 hour. The transparent ceramic composite FH material is taken out, and the excess film around it is cut off to obtain a curved AlON transparent ceramic composite protective material.

[0048] When the transparent ceramic is YAG ceramic, the above step S3 specifically includes:

[0049] The transparent ceramic is at the bottom, the PC board is in the middle, and the layers are stacked together; a vacuum rubber ring is put on the laminate, and then the laminate is cold-drawn to expel the air in the middle of the laminate, and the cold-drawing time is 8 minutes; it is transferred to an autoclave, pressurized and heated to a pressure of 1.2MPa and a temperature of 150℃, and the pressure is reduced after 1 hour. The transparent ceramic composite FH material is taken out, and the excess film around it is cut off to obtain a curved YAG transparent ceramic composite protective material.

[0050] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and the embodiments. It can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily realized. Therefore, without departing from the general concept defined by the claims and equivalent scope, the present invention is not limited to the specific details and the illustrations shown and described here.

Claims

1. A method for preparing a curved transparent protective ceramic composite protective material for a vehicle, characterized in that: include: Step S1, preforming by dry pressing process, and then compacting by cold isostatic pressing process to prepare curved transparent ceramic blank, sintering at high temperature, CNC precision machining, and surface polishing to obtain curved transparent ceramic; Step S2, fix the curved ceramic with the opening facing upward, stack at least two layers of cut flat glass in order and place them on the curved transparent ceramic, spray silicon dioxide between each layer of glass and on the surface of the ceramic, heat and soften them in a bending furnace to closely adhere to the surface of the curved transparent ceramic; Step S3, from top to bottom, the organic board, the multi-layer flat glass and the curved transparent ceramic layers are laminated with films, the laminated sheets are covered with vacuum rubber rings and cold air is extracted, transferred to an autoclave for pressurized heating, vented and depressurized, the transparent ceramic composite FH material is taken out, and the surrounding excess films are cut off to obtain the automotive curved transparent protective ceramic composite protective material.

2. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 1, characterized in that: In the step S1, the transparent ceramic is made of AlON ceramic, YAG ceramic or magnesium aluminum spinel ceramic material.

3. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 2, characterized in that: In the step S1, the dry pressing process pressure is 150MPa-500MPa, the pressure holding time is 1min-10min, the sintering temperature is 1600°C-2000°C, and the sintering time is 10-30h.

4. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 3, characterized in that: In the step S1, the cold isostatic pressing process pressure is 100 MPa to 600 MPa, the holding time is 5 min to 30 min, the light transmittance of the curved transparent ceramic is at least 70%, and the thickness of the curved transparent ceramic is 4 mm to 10 mm.

5. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 1, characterized in that: In step S2, the bending temperature is 500° C. to 800° C., and the time is 1 to 10 hours.

6. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 1 or 5, characterized in that: In step S2, the thickness of the single glass layer is 3 mm to 8 mm.

7. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 1, characterized in that: In the step S3, the air is cold-extracted for a time of greater than or equal to 5 minutes, and the mixture is transferred into an autoclave and pressurized and heated to a pressure of 0.5 MPa to 2 MPa and a temperature of 130° C. to 200° C. The mixture is vented and depressurized after 1 hour.

8. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 7, characterized in that: In step S3, the thickness of the organic sheet is 2-4 mm, and the light transmittance of the organic sheet is greater than 80%.

9. The method for preparing a vehicle curved surface transparent protective ceramic composite protective material according to claim 8, characterized in that: In step S3, the film is made of polyurethane material, and the thickness of the film is 0.5 mm to 1 mm.

10. A vehicle curved surface transparent protective ceramic composite protective material prepared by the preparation method according to any one of claims 1 to 9.

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