A curved transparent protective ceramic composite protective material for vehicles and a preparation method thereof

Abstract

The application discloses a kind of curved surface transparent protective ceramic composite protective material and its preparation method, comprising: using dry pressing process preforming, then using cold isostatic pressing process compaction preparation curved surface transparent ceramic body, CNC precision machining after high-temperature sintering, surface polishing, obtain curved surface transparent ceramic;With curved surface ceramic opening upwards fixed, cut good at least two layers of plane glass is placed in sequence on the curved surface transparent ceramic, between each layer of glass and ceramic surface spray silicon dioxide, in oven heating softening closely adhered to the surface of the curved surface transparent ceramic;From top to bottom in order according to organic plate, the multilayer plane glass and the curved surface transparent ceramic each layer between film is glued, the glued vacuum rubber ring is covered and is carried out cold air extraction, is transferred to autoclave after pressurizing and heating, exhaust decompression, remove transparent ceramic composite FH material, cut off surrounding excess film and obtain the vehicle curved surface transparent protective ceramic composite protective material.

Description

TECHNICAL FIELD

[0001] The application discloses a kind of curved surface transparent protective ceramic composite protective material for vehicle and preparation method thereof, belong to transparent protective ceramic composite protective material technical field. BACKGROUND

[0002] At present, high safety protective glass is realized by adopting multi-layer structure composite to achieve protection effect, and the glass is thick and heavy, and the vehicle maneuverability is reduced. Transparent ceramic is a kind of ceramic prepared by ceramic process, which has good light transmission, high hardness, corrosion resistance and high temperature resistance, and excellent protection performance. Compared with traditional protective glass, the composite protective material prepared by using transparent ceramic can reduce weight by 50% and reduce thickness by more than 40%.

[0003] The existing vehicle glass, including front and rear windshield glass and door glass, has a certain curvature, so in the preparation process, the multi-layer protective glass often adopts the whole baking bending mode, the interlayer matching precision is high, and the production efficiency is high; while the transparent ceramic has a high melting point (> 2000℃), and will not gradually soften with the increase of temperature, and the forming mode mainly relies on green body sintering forming and subsequent processing, which cannot be formed by whole baking bending of glass laminates.

[0004] During the sintering forming process of ceramic, size shrinkage will occur, and post-processing will also affect the actual size, thickness and curvature, so the transparent ceramic product will deform obviously compared with the green body, and the matching glass curvature is difficult to determine, which affects the subsequent lamination and causes the decline of optical performance, and it is difficult to meet the vehicle requirements. SUMMARY

[0005] The purpose of the present application is to solve the problems existing in the current glass protection configuration, and a kind of curved surface transparent protective ceramic composite protective material for vehicle and preparation method thereof are proposed.

[0006] The problem to be solved by the present application is realized by the following technical scheme:

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

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

[0009] Step S2, fix the curved surface ceramic with the opening upwards, place the cut at least two layers of plane glass in sequence on the curved surface transparent ceramic, spray silica between each layer of glass and the surface of the ceramic, and heat and soften in the baking furnace to tightly adhere to the surface of the curved surface transparent ceramic;

[0010] Step S3, the organic plate, the multi-layer flat glass and the adhesive sheet between the layers of the curved transparent ceramic are sequentially laminated from top to bottom, the laminated product is sleeved with a vacuum rubber ring and subjected to cold air suction, then is transferred into a autoclave for pressurization and heating, then is subjected to pressure reduction and exhaust, the transparent ceramic composite FH material is taken out, the surrounding excess adhesive sheet is cut off, and the curved transparent protective ceramic composite protective material for vehicles is obtained.

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

[0012] Preferably, the dry pressing process in step S1 is performed at a pressure of 150 MPa to 500 MPa, a pressure maintaining time of 1 min to 10 min, a sintering temperature of 1600 ℃ to 2000 ℃ and a sintering time of 10 to 30 h.

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

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

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

[0016] Preferably, the cold air suction time in step S3 is greater than or equal to 5 min, the product is transferred into an autoclave, pressurized and heated, the pressure is 0.5 MPa to 2 MPa, the temperature is 130 ℃ to 200 ℃, and the product is subjected to pressure reduction and exhaust after 1 h.

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

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

[0019] A curved transparent protective ceramic composite protective material for vehicles prepared by the preparation method.

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

[0021] The application discloses a kind of vehicle curved surface transparent protective ceramic composite protective material and preparation method thereof, first curved surface transparent ceramic forming method adopts dry pressing process preforming, then cold isostatic pressing process compaction blank, CNC precision machining after high temperature sintering, surface polishing grinding, it can realize transmittance 70% or more, second multilayer glass oven bending method uses the prepared curved surface transparent ceramic as glass oven bending mould, ensure that glass and transparent ceramic precision fit, after compounding, optical performance is good, simultaneously avoid glass forming process separately open mould, reduce production cost, finally piece process method, meet the face of transparent ceramic, utilize transparent ceramic high hardness broken bullet, backboard is organic board material, prevent broken piece scattering, can reduce glass layer, realize thinning and weight reduction.Compound using hot-pressing process, process is simple, compounding precision is high, and product protection performance is good. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 It is the flow chart of the preparation method of the vehicle curved surface transparent protective ceramic composite protective material of the application. DETAILED DESCRIPTION

[0023] The following will be according to the drawings Figure 1 Further illustrate the application:

[0024] The technical solutions of the application will be described clearly and completely below with reference to the drawings. Obviously, the described embodiments are part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the application.

[0025] In the description of the application, it should be noted that the orientations or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" and the like are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the application and simplifying the description, and therefore cannot be understood as indicating or implying that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the application.

[0026] In the description of the application, it should be noted that, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection" should be understood broadly, for example, it can be fixed connection, or detachable connection, or integrally connected, it can be mechanical connection, or electrical connection, it can be directly connected, or indirectly connected through intermediate medium, it can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the application can be understood according to specific circumstances.

[0027] The first embodiment of the present application provides a preparation method of a curved surface transparent protective ceramic composite protective material for vehicles on the basis of the prior art, and specifically comprises the following steps:

[0028] In step S1, a dry pressing process is used for preforming, and then a cold isostatic pressing process is used for compaction to prepare a curved surface transparent ceramic body, and after high temperature sintering, CNC precision machining, surface polishing and grinding, a curved surface transparent ceramic is obtained, and the specific content is as follows:

[0029] The transparent ceramic adopts AlON ceramic, YAG ceramic or magnesium aluminum spinel ceramic material, the transparent ceramic adopts high-purity ultra-fine high-dispersion powder, a high-density large-size curved surface body is prepared by a dry pressing and isostatic pressing process, and after high temperature sintering and forming, the curved surface transparent ceramic is prepared through post-processing. The dry pressing pressure is 150 MPa to 500 MPa, and the pressure holding time is 1 min to 10 min. The cold isostatic pressing pressure is 100 MPa to 600 MPa, and the pressure holding time is 5 min to 30 min. The sintering temperature is 1600 DEG C to 2000 DEG C, and the sintering time is 10 to 30 h. The light transmittance of the curved surface transparent ceramic is more than 70%, and the thickness of the curved surface transparent ceramic is 4 mm to 10 mm.

[0030] Next, AlON ceramic and YAG ceramic are taken as examples for specific description:

[0031] When the transparent ceramic adopts AlON ceramic, the specific content of step S1 includes:

[0032] The AlON powder is placed in a mold, the pressure is 200 MPa, the pressure holding time is 3 min, the curved surface shape is preformed, and then the cold isostatic pressing process with a pressure of 300 MPa is used to compact the body to obtain a curved surface AlON transparent ceramic body. The curved surface AlON transparent ceramic body is sintered at a high temperature of 1900 DEG C for 10 h in a hydrogen atmosphere, CNC precision machining is used, and surface polishing and grinding are performed to prepare a curved surface AlON transparent ceramic with a thickness of 4 mm.

[0033] When the transparent ceramic adopts YAG ceramic, the specific content of step S1 includes:

[0034] The Y2O3 powder and Al2O3 powder are weighed according to the stoichiometric ratio of each element in the chemical formula Y3Al5O12, and are placed in a mold, the pressure is 150 MPa, the pressure holding time is 4 min, the curved surface shape is preformed, and then the cold isostatic pressing process with a pressure of 280 MPa is used to compact the body to obtain a curved surface YAG transparent ceramic body;

[0035] The curved surface YAG transparent ceramic body is sintered at a high temperature of 1600 DEG C for 10 h, CNC precision machining is used, and surface polishing and grinding are performed to prepare a curved surface YAG transparent ceramic with a thickness of 5 mm.

[0036] Step S2, fix the curved ceramic opening upward, place the cut at least two layers of flat glass on the curved transparent ceramic in order, spray silica between each layer of glass and the ceramic surface, and heat and soften in the bending furnace to tightly 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 the curved transparent ceramic. Fix the curved ceramic opening upward, place the cut multiple layers of flat glass on the curved ceramic surface in order, spray silica with a diameter of 0.8 microns between each layer of glass and the ceramic surface to prevent sticking during the bending process, and then heat and soften in the bending furnace, and tightly adhere to the ceramic surface by its own gravity. The bending temperature is 500-800°C, the time is 1-10h, and the glass single layer thickness is 3-8mm.

[0038] The following will be described in detail with AlON ceramic and YAG ceramic as examples:

[0039] When the transparent ceramic adopts AlON ceramic, the specific content of the above step S2 includes:

[0040] Place the cut 3 layers of flat glass in order, with a glass thickness of 5mm, on the curved transparent ceramic, spray silica with a diameter of 0.8 microns between each layer of glass and the ceramic surface to prevent sticking during the bending process, and then heat and soften in the bending furnace, with a temperature of 680°C and a time of 3h, and tightly adhere to the mold surface by its own gravity.

[0041] When the transparent ceramic adopts YAG ceramic, the specific content of the above step S2 includes:

[0042] Place the cut 3 layers of flat glass in order, with a glass thickness of 5mm, on the curved transparent ceramic, spray silica with a diameter of 0.8 microns between each layer of glass and the ceramic surface to prevent sticking during the bending process, and then heat and soften in the bending furnace, with a temperature of 680°C and a time of 3h, and tightly adhere to the mold surface by its own gravity.

[0043] Step S3, sequentially glue the layers of organic plate material, multiple layers of flat glass, and curved transparent ceramic with glue film from top to bottom, cover the glued film with a vacuum rubber ring and perform cold air pumping, transfer to a high-pressure kettle for pressurization and heating, then exhaust and depressurize, take out the transparent ceramic composite FH material, cut off the excess glue film around to obtain the curved transparent protective ceramic composite protective material for vehicles. The specific steps are as follows:

[0044] According to the transparent ceramic is at the bottom, the organic plate is at the top, the middle is glass, the layers are glued together, the vacuum rubber ring is sleeved, then the glass is cold pumped to make the air in the middle of the composite clean, and the cold pumping time should be no less than 5 min. In order to ensure that the composite is firm and compact, the exhaust is sufficient, first, preheat and press, then transfer to the autoclave, pressurize and heat, the pressure is 0.5MPa-2MPa, the temperature is 130℃-200℃, 1h after exhaust and pressure reduction, the transparent ceramic composite FH material is taken out, the surrounding excess glue sheet is cut off to obtain the transparent protective ceramic composite protective material for vehicle curved surface. The organic plate is PC material, the thickness of the organic plate is 2-4mm, the light transmittance of the organic plate is >80%, the glue sheet is polyurethane material, the thickness of the glue sheet is 0.5mm-1mm.

[0045] Next, AlON ceramic and YAG ceramic are taken as examples to be specifically described:

[0046] When the transparent ceramic adopts AlON ceramic, the specific content of the above step S3 includes:

[0047] According to the transparent ceramic is at the bottom, the PC plate is at the top, the middle is multi-layer glass, the layers are glued together, the layers are stacked together; the composite is sleeved with a vacuum rubber ring, then the composite is cold pumped to make the air in the middle of the composite clean, the cold pumping time is 7min; transfer to the autoclave, pressurize and heat, the pressure is 1MPa, the temperature is 150℃, 1h after exhaust and pressure reduction, the transparent ceramic composite FH material is taken out, the surrounding excess glue sheet is cut off to obtain the curved surface AlON transparent ceramic composite protective material.

[0048] When the transparent ceramic adopts YAG ceramic, the specific content of the above step S3 includes:

[0049] According to the transparent ceramic is at the bottom, the PC plate is at the top, the middle is multi-layer glass, the layers are glued together, the layers are stacked together; the composite is sleeved with a vacuum rubber ring, then the composite is cold pumped to make the air in the middle of the composite clean, the cold pumping time is 8min; transfer to the autoclave, pressurize and heat, the pressure is 1.2MPa, the temperature is 150℃, 1h after exhaust and pressure reduction, the transparent ceramic composite FH material is taken out, the surrounding excess glue sheet is cut off to obtain the curved surface YAG transparent ceramic composite protective material.

[0050] Although the embodiments of the present application have been disclosed as above, it is not limited to the application listed in the specification and the embodiments. It can be fully applied to various fields suitable for the present application. For those skilled in the art, other modifications can be easily realized. Therefore, the present application is not limited to specific details and the figures shown and described herein without departing from the general concept defined by the claims and the equivalent scope.

Claims

1. A method for preparing a curved transparent protective ceramic composite protective material for automobiles, characterized in that, include: Step S1: Pre-formed using dry pressing process, then compacted using cold isostatic pressing process to prepare curved transparent ceramic blank, sintered at high temperature and then precision machined by CNC, and the surface polished to obtain curved transparent ceramic. Step S2: Fix the curved transparent ceramic with the opening facing upwards, and place at least two layers of cut flat glass on the curved transparent ceramic in sequence. Spray silica between each layer of glass and on the ceramic surface, and heat and soften in a bending furnace to tightly adhere to the surface of the curved transparent ceramic. Step S3: From top to bottom, the organic sheet, the multi-layer flat glass, and the curved transparent ceramic are sequentially joined together using the interlayer films. The joined sheets are then fitted with vacuum rubber rings and subjected to cold air extraction. After being transferred to an autoclave for pressurization and heating, the pressure is released and the transparent ceramic composite protective material is removed. Excess films around the material are then cut off to obtain the automotive curved transparent protective ceramic composite protective material.

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

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

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

5. The method for preparing a curved transparent protective ceramic composite protective material for automobiles according to claim 1, characterized in that, In step S2, the bending temperature is 500℃~800℃ and the time is 1~10h.

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

7. The method for preparing a curved transparent protective ceramic composite protective material for automobiles according to claim 1, characterized in that, In step S3, the cold air extraction time is greater than or equal to 5 minutes. The air is then transferred to a high-pressure autoclave, pressurized and heated at a pressure of 0.5 MPa to 2 MPa and a temperature of 130°C to 200°C. After 1 hour, the air is exhausted and the pressure is reduced.

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

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

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

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