CN114804903B - Production method of optical ceramic-based mold - Google Patents
Production method of optical ceramic-based mold Download PDFInfo
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- CN114804903B CN114804903B CN202210759079.0A CN202210759079A CN114804903B CN 114804903 B CN114804903 B CN 114804903B CN 202210759079 A CN202210759079 A CN 202210759079A CN 114804903 B CN114804903 B CN 114804903B
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Abstract
The invention discloses a production method of an optical ceramic-based mold, which comprises the following steps: mixing the mixture of carbon powder and silicon powder with carbon-containing liquid resin to obtain a resin matrix; compounding with carbon fiber, silicon carbide fiber or a mixture to obtain a resin composite material; and pressing and molding in a mold to obtain an optical ceramic matrix mold blank, carrying out de-bonding molding treatment on the optical ceramic matrix mold blank, polishing and cutting and molding to obtain an optical ceramic matrix mold semi-finished product, sintering at a high temperature to obtain an optical ceramic matrix mold base body, and coating the surface of the optical ceramic matrix mold semi-finished product with a composite brush plating solution to obtain an optical ceramic matrix mold finished product. The bending strength of the optical ceramic matrix mold material produced by the invention is 275-360 Mpa, and the impact toughness of the mold is 10-15 Mpa.m 1/2 The porosity of the die is 3-5%; the precision of the optical lens for the mobile phone and the camera produced by the method is less than 0.02mm, and the surface roughness of the mirror surface can reach 1-3 levels.
Description
Technical Field
The invention relates to a production method of a mold, in particular to a production method of an optical ceramic-based mold, and belongs to the field of production of optical ceramic-based molds.
Background
The key technology involved in the production of the optical ceramic-based mold is a ceramic-based composite material preparation technology, and the main technology comprises the following steps:
(1) Precursor impregnation cracking process (PIP)
And (3) dipping the fiber prefabricated member into the precursor solution or the molten liquid, solidifying under a certain condition, then carrying out pyrolysis, and finally repeating the dipping-pyrolysis process to obtain the fiber composite material.
The cracking temperature required by a precursor impregnation cracking method (PIP) is lower, and the mechanical damage and the thermal damage to the fiber are smaller; sintering aids are not required to be introduced, and the prepared material has good high-temperature performance; the precursor molecules can be designed, so that the composition, the structure and the performance of the ceramic matrix of the composite material can be controlled; can prepare ceramic matrix composite materials with more complex shapes.
(2) Reaction Melt Infiltration (RMI)
The metal or alloy is heated to molten state, and is made to permeate into porous prefabricated body by means of capillary force and react with the original matrix in the prefabricated body to produce new matrix.
The Reaction Melt Infiltration (RMI) has short production period, low cost, high material density and adjustable matrix composition; but are vulnerable to damage to the fibers.
(3) Mud method (SI)
Ceramic powder is made into slurry, the slurry is added into a fiber preform, and then high-temperature sintering is carried out to prepare the continuous fiber toughened ceramic matrix composite material, and the slurry impregnation method and the slurry brushing method are divided according to the introduction mode of the slurry.
The mud slurry method (SI) can promote the dispersion of ceramic powder to improve the comprehensive performance of the composite material, but the powder distribution in the mud slurry is difficult to homogenize, so that the defects of uneven mechanical property, poor oxidation resistance, easy phase separation and the like of the material are caused.
(4) Chemical Vapor Infiltration (CVI)
And (3) putting the fiber prefabricated part into a special furnace, diffusing the gas-phase precursor to the periphery of the prefabricated part along with pressure difference, diffusing the gas-phase precursor into the preformed part through pores, and reacting in the pores to generate a product to be deposited.
The Chemical Vapor Infiltration (CVI) method can prepare ceramic matrix composite materials with higher melting points at lower temperature; can be used for preparing ceramic matrix composite components with larger size and complex structure; the pressure is lower in the preparation process, and the mechanical damage to the fibers is smaller; can be used for preparing various ceramic matrixes and has wide application range.
Disclosure of Invention
The invention mainly aims to provide a production method of an optical ceramic-based mold, the optical ceramic-based mold produced by the production method has excellent bending strength and impact toughness, and optical lens products for mobile phone cameras and cameras produced by the optical ceramic-based mold have high precision and low mirror surface roughness.
The above object of the present invention is achieved by the following technical solutions:
a method of producing an optical ceramic-based mold, comprising: i, mixing carbon powder and silicon powder to obtain a mixture of the carbon powder and the silicon powder; II, mixing the mixture of the carbon powder and the silicon powder with carbon-containing liquid resin to obtain a resin matrix; III, compounding the resin matrix with carbon fibers, silicon carbide fibers or a mixture consisting of the carbon fibers and the silicon carbide fibers to obtain a resin composite material; IV, pressing and molding the resin composite material in a mold to obtain an optical ceramic matrix mold blank; v, carrying out debonding molding treatment on the optical ceramic-based mold blank, and then polishing and cutting the optical ceramic-based mold blank according to the design size of the optical ceramic-based mold to obtain a semi-finished product of the optical ceramic-based mold; VI, sintering the semi-finished product of the optical ceramic-based mold at a high temperature to prepare an optical ceramic-based mold matrix; and VII, coating the composite brush plating solution on the surface of the optical ceramic-based mold matrix to obtain the finished product of the optical ceramic-based mold.
As a preferred specific embodiment of the invention, in the step I, the carbon powder and the silicon powder are mixed according to the mass ratio of 0.5.
In a preferred embodiment of the invention, the carbon powder or silicon powder has a particle size of less than 75 microns and a purity of more than 99.99%.
According to a preferred embodiment of the invention, in the step II, the mass ratio of the silicon powder to the carbon-containing liquid resin in the mixture of the carbon powder and the silicon powder is controlled to be 0.5; the mixing time is preferably 1-5 h; the carbon-containing liquid resin includes, but is not limited to, phenolic resin or pitch resin. As a reference embodiment, the resin matrix can be obtained by thoroughly mixing a mixture of carbon powder and silicon powder with a carbon-containing liquid resin in a resin matrix storage tank.
In a preferred embodiment of the invention, the mass ratio of the resin matrix to the carbon fibers, the silicon carbide fibers or the mixture of the carbon fibers and the silicon carbide fibers in the step III is 1:2-1:1; wherein, the carbon fiber comprises but is not limited to viscose-based carbon fiber, polyacrylonitrile-based carbon fiber or asphalt-based carbon fiber, and the silicon carbide fiber comprises but is not limited to silicon carbide whisker or silicon carbide continuous fiber; in a more preferred embodiment, the compounding manner in step iii is to prepare a fiber cloth from carbon fibers, silicon carbide fibers or a mixture of carbon fibers and silicon carbide fibers, and impregnate and infiltrate the resin matrix into the fiber cloth to obtain the resin composite material.
As a preferred embodiment, the resin matrix can be impregnated into the fiber cloth by adopting a roller vacuum impregnation method to obtain the resin composite material, and the method comprises the following steps: a, uniformly winding fiber cloth on the outer part of a roller, wherein the inner part of the roller is vacuum, and small holes are uniformly formed in the wall of the roller; b, rotating the roller in a storage tank for storing resin matrix; during one circle of rotation of the roller, the fiber cloth can be immersed in the resin matrix storage tank for 1/3 of the time, and the fiber cloth can be immersed and permeated by utilizing vacuum in the roller for the rest of the time, so that the resin matrix is uniformly distributed and immersed in the fiber cloth; wherein, the roller preferably rotates at the speed of 0.05-0.15 r/min, the vacuum degree in the roller is controlled at 1000-2000 Pa, and the dipping time is controlled at 5-10 h. Compared with the traditional hand lay-up impregnation mode, the vacuum impregnation mode adopting the roller has the advantages of high degree of mechanization and simple operation, and thoroughly solves the problem of uneven coating in the impregnation process of the fiber cloth in the resin matrix in the hand lay-up impregnation process.
As a preferred embodiment, the press forming in step iv is preferably performed by cold press forming the resin composite material in a multifunctional mold with pressure control and temperature control, so that the resin composite material is tightly pressed to a compact structure, and an optical ceramic matrix mold blank with a certain shape and size is prepared. The cold press molding method is characterized in that the pressure and the temperature of cold press molding do not need to be specially selected, the cold press molding method is mainly used for determining the operation parameter range of a multifunctional mold used for producing a resin matrix composite material, the cold press molding operation time is determined by the resin matrix composite material used in the process, the cold press molding operation time is too short, and a produced molding blank body is insufficient in stability and easy to deform; the cold press molding operation time is too long, and unnecessary energy consumption of a green body molding process is increased. The pressure, temperature and time of cold press forming can be flexibly determined by those skilled in the art according to actual conditions, and the implementation of the invention is not influenced. As a reference implementation parameter, the pressure of the cold press molding can be 100-180 MPa, the time of the cold press molding can be 5-6 h, and the temperature of the cold press molding can be 15-25 ℃ of normal temperature.
As a preferred specific embodiment, the de-bonding molding treatment in step v is to perform pyrolysis treatment on the optical ceramic-based mold blank in the press molding mold under inert atmosphere and vacuum conditions (i.e., the optical ceramic-based mold blank is vacuumized in the cavity of the multifunctional mold device), wherein the inert atmosphere adopts argon or helium, the vacuum degree is preferably controlled to be 500 to 1000Pa, the pyrolysis temperature is preferably controlled to be 600 to 800 ℃, the pyrolysis treatment time is preferably controlled to be 3 to 5 hours, and the hot-pressing operation pressure is preferably controlled to be 100 to 180MPa.
The invention can realize the following effects by controlling the operation conditions of debonding molding treatment in inert atmosphere, vacuum degree at 500-1000 Pa and pyrolysis temperature at 600-800 ℃: a, ensuring that a carbon source is not oxidized to generate carbon dioxide in the de-bonding process of the formed blank body; b, pyrolyzing the carbon-containing liquid resin, carrying out pyrolysis oil gas out of the multifunctional mold by inert gas, and only remaining pyrolysis carbon in a molding blank body structure; and c, realizing the formation of a uniform structure of the pyrolytic carbon, the high-purity graphite powder and the silicon powder in the formed blank. The pyrolysis temperature is controlled to be 600-800 ℃ and the pyrolysis time is controlled to be 3-5 h, so that the carbon-containing resin can be converted into pyrolytic carbon, and other impurities which influence the reaction of carbon and silicon powder to generate silicon carbide do not exist; the thermal operation pressure is controlled to be 100-180 MPa, which is not only determined by the range of the operation parameters of the multifunctional mold, but also ensures that the optical ceramic matrix mold blank still has certain strength after pyrolysis and debonding under the pressure.
The green body forming process and the green body debonding process can be carried out in a multifunctional die with pressure control and temperature control, and can be operated in a forming and debonding sectional mode or in a forming and debonding continuous mode.
As a preferred embodiment, in the step v, after the optical ceramic-based mold blank is subjected to the de-bonding molding treatment, the optical ceramic-based mold blank is precisely polished and cut and molded on an automated precision apparatus (the automated precision apparatus belong to conventional equipment in the field) according to the design size of the optical ceramic-based mold to produce a semi-finished product of the optical ceramic-based mold, so that the dimensional error of the precisely processed semi-finished product of the optical ceramic-based mold is ensured to be within 0.05%.
As a preferred embodiment, the high-temperature sintering in step vi is to perform high-temperature sintering on the optical ceramic-based mold semi-finished product in a vacuum high-temperature furnace, wherein the high-temperature sintering is performed in an inert atmosphere, the sintering temperature is controlled to be 1500-2000 ℃, the vacuum degree is controlled to be 1000-1500 Pa, and it is ensured that the optical ceramic-based mold semi-finished product material is further melted and permeated at the temperature to form a surface-dense optical ceramic-based mold matrix; in order to achieve better sintering effect, sintering is preferably carried out by adopting a sintering mode of step temperature rise in the sintering mode, wherein the sintering mode of step temperature rise comprises the following steps; firstly, heating the semi-finished product of the optical ceramic-based mold from the normal temperature to 600-800 ℃, sintering at the constant temperature for 1-2 h, then heating to 1000-1200 ℃, sintering at the constant temperature for 2-4 h, finally heating to 1500-2000 ℃, and sintering at the constant temperature for 3-5 h.
The conventional silicon carbide powder is generated at about 2000 ℃, and the sintering operation under the vacuum condition can reduce the silicon carbide generation temperature to 1500-2000 ℃. Heating from normal temperature to 600-800 ℃ for sintering, namely, continuously repeating the pyrolysis and debonding operation temperature, so as to ensure that the heated material of the optical ceramic-based mold semi-finished product has a stable structure, and sintering at constant temperature for 1-2 h is used for further pyrolysis and debonding and ensuring that the internal temperature of the mold semi-finished product is uniform; the semi-finished product of the die is heated to 1000-1200 ℃ and sintered at constant temperature for 2-4 h, based on the consideration that alpha-phase and beta-phase crystal form changes exist in the semi-finished product material of the die in the sintering process, the crystal form transformation sintering of the material is completed; finally, the temperature is raised to 1500-2000 ℃, and alpha crystal phase can be generated by constant temperature sintering for 3-5 h.
And step VII, uniformly coating the chromium oxide, zirconium dioxide and titanium dioxide composite brush plating solution on the surface of the optical ceramic-based mold matrix by applying a composite electroplating technology, so that the surface wear resistance, hardness and service life of the matrix are greatly improved. As a preferred embodiment, the composite brush plating solution described in step VII consists essentially of Cr 2 O 3 、ZrO 2 And TiO 2 Forming; the invention discovers that Cr is mixed through experiments 2 O 3 、ZrO 2 And TiO 2 The mass ratio of (1). The thickness of the plating layer when the composite electric brush plating solution is coated on the surface of the optical ceramic matrix mold substrate has no special requirement, and the capabilityThe technical personnel can select or adjust the plating solution according to the actual situation and by referring to the related parameters of the conventional composite plating, which do not affect the realization of the invention, and as a reference implementation mode, the related process parameters of the composite brush plating solution when being coated on the surface of the optical ceramic matrix mold substrate can be as follows: the thickness of the plating layer is 0.01-0.02 mm. The working voltage of the composite electroplating is controlled to be 10-14V, the temperature of the composite brush plating solution is controlled to be 30-50 ℃, the relative movement speed of the automatic coating plating pen and the optical ceramic matrix is controlled to be 6-10 m/min, and the optical ceramic matrix coated by the coating is polished to meet the mirror requirement, so that the qualified optical ceramic matrix is produced.
The optical ceramic matrix mold produced by the invention has the following properties: the bending strength of the die material is 275-360 MPa; the impact toughness of the die is 10-15 Mpa.m 1/2 (ii) a The porosity of the die is 3-5%. The precision of the optical lens for mobile phones and cameras produced by applying the optical ceramic-based mold is less than 0.02mm, and the surface roughness of the mirror surface can reach 1-3 levels.
The main beneficial effects of the invention include:
(1) The optical ceramic-based mold finished product produced by the invention can realize the domestic substitution of the high-precision optical lens mold. In addition, the produced optical ceramic-based mold is used for replacing a tungsten steel mold in the existing market, and the produced optical lens products for mobile phone cameras and cameras have high precision (less than 0.02 mm) and low mirror surface roughness (1-3 levels).
(2) In the production process of the optical ceramic-based mold, high-purity carbon powder and carbon-containing liquid resin are used as double carbon sources and are subjected to in-situ melting reaction with silicon powder in the procedures of de-bonding and high-temperature sintering of a formed blank, so that the homogenization of the internal material of the optical ceramic-based mold is realized; the reinforced fiber cloth material is added into the resin matrix, so that the bending strength and the impact toughness of the produced optical ceramic matrix mold are improved; coating with Cr 2 O 3 -ZrO 2 -TiO 2 The composite brush plating solution also improves the service life of the produced optical ceramic matrix mould.
(3) According to the invention, the resin composite material matrix is produced by adopting roller vacuum impregnation in the production process of the optical ceramic matrix mold, so that the complete uniform penetration of the resin matrix in the reinforcing material is improved, and the defect of uneven coating of the resin matrix caused by the traditional hand lay-up forming technology is overcome; the production process adopts the coupling of the working procedures of cold press molding, hot press debonding pyrolysis, program high-temperature sintering and composite electroplating surface coating, reduces the porosity of the material of the optical ceramic matrix mold, and further improves the bending strength and the impact toughness performance of the mold.
Drawings
FIG. 1 is a flow chart of the production process of the optical ceramic mold.
Figure 2 schematic diagram of drum vacuum impregnation.
Detailed Description
The invention is further described below in conjunction with specific embodiments, the advantages and features of which will become apparent from the description. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be within the scope of the invention.
Example 1 preparation and Performance measurement of an optical ceramic-based mold
Chinese yam flour
Mixing carbon powder with the purity of more than 99.99 percent and silicon powder according to the mass ratio of 1:1, and grinding the mixture into powder with the particle size of less than 75 microns;
preparation of a resin-containing wall-catalyst component
Liquid phenolic resin is used as an adhesive, the mass ratio of silicon powder to the liquid resin is controlled to be 0.6;
⒊ resin composite material preparation
The polyacrylonitrile-based carbon fiber cloth is used as a reinforcing material, a resin matrix containing a carbon source and a silicon source and the polyacrylonitrile-based carbon fiber cloth are prepared according to the mass ratio of 1.5, a roller is used for vacuum impregnation at the speed of 0.08r/min, the vacuum degree is 1000-1200 Pa, and the impregnation time is 8 hours;
⒋ blank pressing forming
And cold press molding the resin matrix composite material in a multifunctional mold to prepare an optical ceramic matrix mold blank, wherein the operation pressure is 150MPa, and the cold press molding operation time is 5 hours.
⒌ formed blank debonding
And carrying out pyrolysis debonding treatment on the optical ceramic matrix mold blank in an argon-protected multifunctional mold, controlling the vacuum degree of the multifunctional mold to be 800Pa, controlling the pyrolysis debonding temperature to be 800 ℃, carrying out pyrolysis debonding treatment for 3h, and controlling the hot-pressing operation pressure to be 150MPa.
⒍ precision machining
And controlling the dimensional error of the semi-finished product of the optical ceramic-based mold after the optical ceramic-based mold blank is subjected to the debonding treatment and is precisely processed within 0.05 percent.
⒎ high temperature sintering
And (3) sintering the semi-finished product of the optical ceramic-based mold at a high temperature in a vacuum high-temperature furnace under the protection of argon to produce the optical ceramic-based mold matrix, wherein the sintering temperature is controlled at 1800 ℃ and the vacuum degree is 1000Pa. Sintering temperature control mode: firstly, heating the semi-finished product of the optical ceramic-based mold from normal temperature to 800 ℃, and sintering at constant temperature for 2 hours; then heating to 1200 ℃, and sintering for 4 hours at constant temperature; heating to 1800 ℃ and sintering for 3h at constant temperature.
⒏ surface coating
Preparation of Cr 2 O 3 -ZrO 2 -TiO 2 Composite brush plating solution, cr in brush plating solution 2 O 3 、ZrO 2 And TiO 2 The mass ratio of (1) to (1). Cr is carried out on optical ceramic matrix mold matrix by applying automatic composite electroplating technology 2 O 3 -ZrO 2 -TiO 2 The metal coating is coated to produce the optical ceramic-based mold, the coating working voltage is 12V, the temperature of the brush plating solution is 35 ℃, the relative movement speed is 8m/min, and the coating thickness of the prepared optical ceramic-based mold is 0.02mm.
The optical ceramic-based mold prepared in this example was used to measure the bending strength, the impact toughness and the porosity of the mold according to the following methods or standards, respectively:
the flexural strength is measured by adopting a flexural strength test method and an impact toughness test method of a GB/T4741-1999 ceramic material, the reference of the test method is GBT 14389-1993-engineering ceramic impact toughness test method, and the reference of the test method of the apparent porosity is GB/T25995-2010 test method of Fine ceramic Density and apparent porosity.
The bending strength of the optical ceramic-based mold for the mobile phone camera lens produced by the method is 330MPa; impact toughness of die 12.8 Mpa.m 1/2 (ii) a The mold porosity was 4.2%.
The lens precision and the mirror surface roughness of the lens produced by the optical ceramic-based mold prepared in the embodiment are respectively measured by the following measuring method or standard:
measuring the precision of the optical lens, namely the precision of the curvature radius by using a laser interferometer, wherein the precision error conforms to the GB/T1800.3-1998 standard; the surface roughness is measured by a stylus method, and the measurement result of the surface roughness refers to GB/T1031-2009 surface roughness parameters and values thereof by a surface structure profile method and GB/T131-2006 (ISO 1302).
The optical lens precision measuring method comprises the following steps:
the precision measurement of the optical lens, namely the precision measurement of the curvature radius depends on the accurate measurement of the curvature radius, and the specific method is as follows: the laser interferometer accurately judges the cat eye and the confocal position by testing interference fringes; the displacement from the cat eye to the confocal position is accurately recorded through a grating ruler or a laser range finder. The radius of curvature is equal to the displacement of the "cat eye" to the confocal position (or confocal to the "cat eye" position), plus the exact position compensation measured from the interference fringes at both positions by the interferometer. In the measuring process, the grating ruler or the laser range finder is operated to accurately record displacement change, and the measuring precision of the curvature radius is determined.
Surface roughness grade measurement method:
surface roughness grade determination is determined by surface roughness measurement, and the surface roughness grade can be determined by comparing the surface roughness parameter (profile parameter) value with a surface roughness decomposition table.
The surface roughness measurement refers to comparing a sample block (sample block for short) with the surface to be measured according to visual sense and touch sense, and judging that the roughness of the surface to be measured is equivalent to thatA value, or measuring the change in reflected light intensity, to assess surface roughness (see laser length measurement technique). The common methods are as follows:
comparison method: the method is a method for determining the roughness value of a measured surface by comparing the measured surface with a roughness sample plate marked with a certain value. The method that can be adopted when comparing: ra>Visual inspection is carried out at a thickness of 1.6 μm, and a magnifying glass, ra, is used at a thickness of Ra1.6-Ra0.4 μm<0.4 μm using a comparative microscope. The method is simple and convenient to measure, is used for on-site measurement in a workshop and is commonly used for measurement of medium or rough surfaces;
a contact pin method: the diamond contact pin with the curvature radius of 2 microns slides slowly along the surface to be measured, the up-down displacement of the diamond contact pin is converted into an electric signal by an electric length sensor, the surface roughness value is indicated by a display instrument after amplification, filtering and calculation, and a recorder can also be used for recording the profile curve of the section to be measured. A measuring tool capable of displaying only a surface roughness value is generally called a surface roughness measuring instrument, while a measuring tool capable of recording a surface profile is called a surface roughness profiler. The two measuring tools are provided with an electronic calculating circuit or an electronic computer, can automatically calculate the arithmetic mean deviation Ra of the profile, the height Rz of ten points of the micro-unevenness, the maximum height Ry of the profile and other various evaluation parameters, have high measuring efficiency and are suitable for measuring the surface roughness with the Ra of 0.025-6.3 microns;
a light cutting method: measuring the surface roughness by using a double-tube microscope, wherein the surface roughness can be used for Ry and Rz parameter evaluation, and the measurement range is 0.5 to 50;
an interference method: the shape error of the measured surface is displayed as interference fringe pattern by using light wave interference principle (see optical crystal and laser length measuring technology), and the interference fringe pattern is displayed by using microscope with high magnification (up to 500 times)And amplifying the microscopic part of the interference fringe and then measuring to obtain the roughness of the measured surface. The surface roughness measuring tool to which this method is applied is called an interference microscope. This method is suitable for measuring surface roughness with Rz and Ry of 0.025 to 0.8 microns.
The precision of an optical lens for a mobile phone camera, which is produced by applying the optical ceramic matrix mold disclosed by the invention, is less than 0.012mm, and the surface roughness of a mirror surface reaches 2 levels.
Example 2 preparation and Performance measurement of an optical ceramic-based mold
Powder prepared from Chinese medicinal herbs
Mixing carbon powder with the purity of more than 99.99% and silicon powder according to the mass ratio of 0.8 to perform ball milling until the particle size is less than 75 microns;
preparation of a resin-containing wall-catalyst component
Liquid asphalt resin is used as an adhesive, the mass ratio of silicon powder to the liquid resin is controlled to be 0.8;
⒊ resin composite material preparation
Silicon carbide fiber cloth is used as a reinforcing material, a resin matrix containing a carbon source and a silicon source and the silicon carbide fiber cloth are prepared according to the mass ratio of 1:2, a roller is used for vacuum impregnation at the speed of 0.12r/min, the vacuum degree is 1500-1600 Pa, and the impregnation time is 10 hours;
⒋ blank pressing forming
And cold press molding the resin matrix composite material in a multifunctional mold to prepare an optical ceramic matrix mold blank, wherein the operation pressure is 160MPa, and the cold press molding operation time is 5.5h.
⒌ formed blank debonding
And carrying out pyrolysis debonding treatment on the optical ceramic matrix mold blank in an argon-protected multifunctional mold, wherein the vacuum degree of the multifunctional mold is controlled to be 1000Pa, the pyrolysis debonding temperature is controlled to be 750 ℃, the pyrolysis debonding treatment is carried out for 4 hours, and the hot pressing operation pressure is 160MPa.
⒍ precision machining
And controlling the dimensional error of the semi-finished product of the optical ceramic-based mold after the optical ceramic-based mold blank is subjected to the debonding treatment and is precisely processed within 0.05 percent.
⒎ high temperature sintering
And (3) carrying out high-temperature sintering on the semi-finished product of the optical ceramic-based mold in a vacuum high-temperature furnace protected by argon to produce the substrate of the optical ceramic-based mold, wherein the sintering temperature is controlled at 1850 ℃, and the vacuum degree is 1300Pa. Sintering temperature control mode: firstly, heating the semi-finished product of the optical ceramic-based mold from normal temperature to 750 ℃, and sintering at constant temperature for 2 hours; then heating to 1300 ℃, and sintering for 3h at constant temperature; heating to 1850 ℃, and sintering for 5h at constant temperature.
⒏ surface coating
Preparation of Cr 2 O 3 -ZrO 2 -TiO 2 Composite brush plating solution, cr in brush plating solution 2 O 3 、ZrO 2 And TiO 2 The mass ratio of (1). Cr is carried out on optical ceramic matrix mold matrix by applying automatic composite electroplating technology 2 O 3 -ZrO 2 -TiO 2 The optical ceramic-based mold is produced by coating the metal coating, the coating working voltage is 10V, the temperature of the brush plating solution is 40 ℃, the relative movement speed is 6m/min, and the thickness of the coating of the prepared optical ceramic-based mold is 0.018mm.
Through detection, the bending strength of the optical ceramic-based mold produced by the implementation is 350MPa; impact toughness of die 13.6 Mpa.m 1/2 (ii) a The porosity of the mold was 3.6%. The precision of an optical lens for a camera produced by applying the optical ceramic matrix mold of the embodiment is less than 0.01mm, and the surface roughness of a mirror surface reaches 2 levels.
Claims (4)
1. A method of producing an optical ceramic-based mold, comprising: mixing carbon powder and silicon powder to obtain a mixture of the carbon powder and the silicon powder; II, mixing the mixture of the carbon powder and the silicon powder with carbon-containing liquid resin to obtain a resin matrix; III, compounding the resin matrix with carbon fibers, silicon carbide fibers or a mixture of the carbon fibers and the silicon carbide fibers to obtain a resin composite material; IV, pressing and molding the resin composite material in a mold to obtain an optical ceramic matrix mold blank; v, carrying out debonding molding treatment on the optical ceramic-based mold blank, and then polishing and cutting the optical ceramic-based mold blank according to the design size of the optical ceramic-based mold to obtain a semi-finished product of the optical ceramic-based mold; VI, sintering the semi-finished product of the optical ceramic-based mold at a high temperature to prepare an optical ceramic-based mold matrix; coating the composite brush plating solution on the surface of the optical ceramic-based mold matrix to obtain a finished product of the optical ceramic-based mold;
preparing carbon fibers, silicon carbide fibers or a mixture consisting of the carbon fibers and the silicon carbide fibers into fiber cloth, and impregnating a resin matrix into the fiber cloth to obtain a resin composite material; the method for impregnating and penetrating the resin matrix into the fiber cloth to obtain the resin composite material comprises the following steps: a, uniformly winding fiber cloth on the outer part of a roller, wherein the inner part of the roller is vacuum, and small holes are uniformly formed in the wall of the roller; b, rotating the roller in a storage tank for storing resin matrix; wherein, the roller rotates at the speed of 0.05-0.15 r/min, the vacuum degree in the roller is controlled to be 1000-2000 Pa, and the dipping time is controlled to be 5-10 h;
the step V of the debonding and forming treatment is to perform pyrolysis treatment on the optical ceramic matrix mold blank in the compression forming mold under inert atmosphere and vacuum conditions, wherein the inert atmosphere adopts argon or helium, the vacuum degree is controlled to be 500-1000 Pa, the pyrolysis temperature is controlled to be 600-800 ℃, the pyrolysis treatment time is controlled to be 3-5 h, and the hot pressing operation pressure is controlled to be 100-180 MP;
the high-temperature sintering in the step VI is carried out by adopting a sintering mode of step temperature rise, and the high-temperature sintering mode of step temperature rise comprises the following steps; firstly heating the semi-finished product of the optical ceramic-based mold from normal temperature to 600-800 ℃, sintering at the temperature for 1-2 h at constant temperature, then heating to 1000-1200 ℃, sintering at the temperature for 2-4 h at constant temperature, finally heating to 1500-2000 ℃, and sintering at the temperature for 3-5 h at constant temperature;
the composite electric brush plating solution in the step VII mainly comprises Cr2O3, zrO2 and TiO 2; wherein the mass ratio of Cr2O3, zrO2 and TiO2 is (1).
2. The method as claimed in claim 1, wherein in step I, the carbon powder and the silicon powder are mixed according to a mass ratio of 0.5 to 1:1, wherein the mixing is performed by ball milling.
3. The method according to claim 1, wherein the mass ratio of the silicon powder to the carbon-containing liquid resin in the mixture of carbon powder and silicon powder in the step II is controlled to be 0.5; the carbon-containing liquid resin includes but is not limited to phenolic resin or asphalt resin.
4. The method according to claim 1, wherein the mass ratio of the resin matrix to the carbon fibers, the silicon carbide fibers or the mixture of the carbon fibers and the silicon carbide fibers in step III is 1:2-1:1; the carbon fiber comprises but is not limited to viscose-based carbon fiber, polyacrylonitrile-based carbon fiber or asphalt-based carbon fiber, and the silicon carbide fiber comprises but is not limited to silicon carbide whisker or silicon carbide continuous fiber.
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