Disclosure of Invention
The technical problem solved by the invention is as follows: the production method of the sapphire camera window piece is high in piece quality, low in rejection rate and high in production efficiency.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a production method of a sapphire camera window film comprises the following specific steps:
step one, picking out a crystal bar; taking sapphire crystals in the A direction, the M direction or the C direction, and then using a bar drawing machine to draw bars, thereby obtaining crystal bars;
step two, crystal cutting; cutting the crystal bar by adopting diamond wire cutting equipment to obtain a wafer;
step three, grinding; grinding the wafer by a grinder; during grinding, adding grinding fluid, and pressurizing the wafer to 0.02-0.022 MPa by a grinding disc at the rotation speed of 1000-1200 r/min; cleaning with absolute ethyl alcohol after grinding; the grinding fluid comprises the following components: 0.5-2% of cubic boron nitride powder with the particle size of 10-20 microns, 14-16% of alkylphenol polyoxyethylene, 4-6% of glycerol, 9-11% of polypropylene glycol 400 and the balance of deionized water; stirring the grinding fluid;
step four, chamfering; chamfering the corners of the wafer by using a diamond grinding wheel of a numerical control machine;
step five, annealing; putting the wafer into an annealing furnace, heating at the speed of 180-220 ℃/h to raise the temperature to 1600 ℃, respectively preserving heat for 2-6 h at the temperature of 300 ℃, 800 ℃ and 1600 ℃ during heating, then cooling at the speed of 200 ℃/h, respectively preserving heat for 2-3 h at the temperature of 1000 ℃ and 500 ℃ during cooling, cooling to room temperature, and taking out;
sixthly, chemically polishing the two surfaces; firstly, cleaning a wafer by absolute ethyl alcohol, and then putting the cleaned wafer into a double-sided polishing machine for fixing; adding polishing solution during polishing, pressurizing the wafer to 0.12-0.15 Mpa by using a polishing disc, and cleaning the polished wafer by using absolute ethyl alcohol at the rotating speed of 1000-1500 r/min, and naturally cooling at room temperature; the polishing solution comprises the following components: 0.5-2% of cubic boron nitride powder with the particle size of 1-6 mu m, 14-16% of alkylphenol polyoxyethylene, 4-6% of glycerol, 9-11% of polypropylene glycol 400 and 0.5-2% of nano silicon dioxide, an alkaline solution for enabling the pH value of the polishing solution to be 11.0-13.0, and the balance of deionized water; continuously supplementing alkaline solution in the polishing process to maintain the pH value of the polishing solution;
step seven, laser film taking; putting the polished wafer into a laser cutting machine, introducing protective gas, and cutting the wafer into corresponding sizes as required;
step eight, coating a film; plating antireflection films on the front surface and the back surface of the wafer by using an optical vacuum coating machine, wherein the antireflection films are formed by coating low-refractive-index oxides and high-refractive-index oxides layer by layer, the number of the antireflection films is 4-8, the layer closest to the wafer adopts the low-refractive-index oxides, the low-refractive-index oxides are oxides of silicon or aluminum, and the high-refractive-index oxides are oxides of titanium or tantalum;
step nine, inking; covering the coated wafer with a hollow plate, brushing ink on the edge of the wafer, and repeatedly brushing three layers;
step ten, baking; and (4) putting the wafer coated with the printing ink into a hot drying machine for hot drying for 2-3 h, and then cooling the wafer to room temperature in air.
The improvement of the technical scheme is as follows: in the second step, the diameter of the diamond wire is 0.14-0.16 mm, the grain diameter of diamond on the diamond wire is 30-40 mu m, the diamond wire moves at the speed of 12-15 m/s during cutting, the moving speed of the crystal relative to the diamond wire is 0.2-0.3 mm/min, cutting fluid is continuously sprayed on the diamond wire during cutting, and the cutting fluid contains diamond grains with the grain diameter of 20-30 mu m and corundum grains with the grain diameter of 50-60 mu m.
The improvement of the technical scheme is as follows: in the third step, the grinding fluid contains alumina particles with the particle size of 3-6 μm.
The improvement of the technical scheme is as follows: in the fifth step, the temperature is kept for 2h at 300 ℃, 3h at 800 ℃ and 4h at 1600 ℃ during temperature rise.
The improvement of the technical scheme is as follows: in the sixth step, the alkaline solution is KOH.
The improvement of the technical scheme is as follows: in the sixth step, the pH value of the polishing solution is 12.0-13.0.
The improvement of the technical scheme is as follows: in the sixth step, the polishing disk presses the wafer to 0.135 Mpa.
The improvement of the technical scheme is as follows: in the seventh step, the diameter of the laser beam is 0.015-0.02 mm, and the cutting speed is 3-5 mm/s.
The improvement of the technical scheme is as follows: in the eighth step, the optical vacuum coating machine generates an electron beam by using an ion source, liquefies the low refractive index oxide or the high refractive index oxide, then solidifies the low refractive index oxide or the high refractive index oxide, and pre-melts the low refractive index oxide or the high refractive index oxide, and then gasifies and sprays the solidified low refractive index oxide or the solidified high refractive index oxide onto a crystal face to form a film.
The invention has the positive effects that:
(1) according to the production method of the camera window piece, grinding and polishing are carried out firstly, then laser piece taking is carried out, the production efficiency of grinding and polishing can be improved, large pressure must be applied during polishing due to high sapphire hardness, annealing before polishing is beneficial to eliminating internal stress generated by machining processes such as linear cutting, grinding and the like, so that a wafer is not prone to cracking during polishing, and the yield is effectively improved.
(2) The camera window piece production method strictly controls the grinding and polishing parameters and the components of the grinding liquid and the polishing liquid, is beneficial to improving the grinding and polishing efficiency and the grinding and polishing yield, and the prepared wafer has the advantages of complete structure, no physical damage, fine and smooth surface and small deformation. In the grinding liquid and the polishing liquid, a proper amount of cubic boron nitride powder is used as an abrasive, so that the hardness is high and the wear resistance is good; the suspension formed by the alkylphenol ethoxylates, the glycerol, the polypropylene glycol 400 and the deionized water has stable viscosity and interfacial film property, so that the abrasive is stable in suspension, good in uniformity and free from adhesion, and the grinding and polishing quality and efficiency are improved. The appropriate amount of alkylphenol polyoxyethylene is a nonionic surfactant, has stable property, has various performances of dispersion, emulsification, wetting and the like, and is the most main component for obtaining excellent performance of suspension; the glycerol has proper specific gravity, has good solubility with water and organic solution, and is very suitable to be used as an auxiliary dispersant; polypropylene (PP-II)The alcohol 400 has the functions of emulsification and wetting, can be effectively thickened, and effectively improves the viscosity and interfacial film property of the suspension. In addition, the polishing solution contains proper amount of nano SiO2Uniform granularity, good dispersity and high flattening efficiency. The polishing solution is alkaline due to the alkaline solution KOH, and the polishing is assisted by chemical corrosion, so that the polishing effect is better, and the polishing efficiency is better. In order to maintain the stability of the polishing solution and thus ensure the efficiency and quality of polishing, the alkaline solution must be continuously replenished to maintain the pH of the polishing solution substantially constant.
(3) According to the production method of the camera window sheet, disclosed by the invention, the light transmittance is increased and the reflectivity is reduced through a film coating process, so that the original 89% light transmittance of the sapphire wafer can be increased to more than 94%. In the coating process, the low refractive index oxide or the high refractive index oxide is liquefied and then solidified for pre-melting, so that the distribution of the oxide is more uniform, and the coating effect is improved.
(4) According to the production method of the camera window, the three layers of printing ink are coated and then dried, so that the edge of the wafer is light-tight, and light can be effectively prevented from entering from the side face of the wafer to influence imaging.
(5) The camera window sheet is made of sapphire serving as a base material, and the sapphire is high in hardness and good in wear resistance, so that the camera window sheet is not easy to wear and scratch. The window sheet manufactured by the method for producing the camera window sheet has the advantages of high finish, good light transmission, standard optical performance, high sheet quality, low rejection rate, high production efficiency and wide application prospect.
Detailed Description
Example 1
The preparation process of the sapphire camera window sheet of the embodiment comprises the following steps:
step one, picking out a crystal bar; taking sapphire crystals in the A direction, the M direction or the C direction, and then using a bar drawing machine to draw bars, thereby obtaining crystal bars;
step two, crystal cutting; cutting the crystal bar by adopting diamond wire cutting equipment to obtain a wafer;
step three, grinding; grinding the wafer by a grinder; during grinding, grinding fluid is added, a grinding disc pressurizes the wafer to 0.022Mpa, and the rotating speed of the grinding disc is 1200 r/min; cleaning with absolute ethyl alcohol after grinding; the grinding fluid comprises the following components: 2% of cubic boron nitride powder with the particle size of 20 mu m, 16% of alkylphenol polyoxyethylene ether, 6% of glycerol, 11% of polypropylene glycol 400 and the balance of deionized water;
step four, chamfering; chamfering the corners of the wafer by using a diamond grinding wheel of a numerical control machine;
step five, annealing; putting the wafer into an annealing furnace, heating up to 1600 ℃ at the speed of 220 ℃/h, preserving heat for 2h at 300 ℃, preserving heat for 3h at 800 ℃, preserving heat for 4h at 1600 ℃ during heating up, then cooling down at the speed of 200 ℃/h, preserving heat for 3h at 1000 ℃ and 500 ℃ respectively during cooling down, cooling to room temperature and taking out;
sixthly, chemically polishing the two surfaces; firstly, cleaning a wafer by absolute ethyl alcohol, and then putting the cleaned wafer into a double-sided polishing machine for fixing; during polishing, adding polishing liquid, pressurizing the wafer to 0.15Mpa by a polishing disc, and naturally cooling at room temperature after the polished wafer is cleaned by absolute ethyl alcohol, wherein the rotating speed of the polishing disc is 1500 r/min; the polishing solution comprises the following components: 2% of cubic boron nitride powder with the particle size of 6 microns, 14-16% of alkylphenol polyoxyethylene, 6% of glycerol, 11% of polypropylene glycol 400 and 2% of nano silicon dioxide, wherein the pH value of the polishing solution is 13.0 of alkaline solution, and the balance is deionized water; continuously supplementing alkaline solution in the polishing process to maintain the pH value of the polishing solution;
step seven, laser film taking; putting the polished wafer into a laser cutting machine, introducing protective gas, and cutting the wafer into corresponding sizes as required;
step eight, coating a film; plating antireflection films on the front surface and the back surface of the wafer by using an optical vacuum coating machine, wherein the antireflection films are formed by coating low-refractive-index oxides and high-refractive-index oxides layer by layer, the number of the antireflection films is 8, one layer closest to the wafer adopts the low-refractive-index oxides, the low-refractive-index oxides are oxides of silicon or aluminum, and the high-refractive-index oxides are oxides of titanium or tantalum;
step nine, inking; covering the coated wafer with a hollow plate, brushing ink on the edge of the wafer, and repeatedly brushing three layers;
step ten, baking; and (4) putting the wafer coated with the printing ink into a hot drying machine for hot drying for 2-3 h, and then cooling the wafer to room temperature in air.
Example 2
The preparation process of the sapphire camera window sheet of the embodiment comprises the following steps:
step one, picking out a crystal bar; taking sapphire crystals in the A direction, the M direction or the C direction, and then using a bar drawing machine to draw bars, thereby obtaining crystal bars;
step two, crystal cutting; cutting the crystal bar by adopting diamond wire cutting equipment to obtain a wafer;
step three, grinding; grinding the wafer by a grinder; during grinding, adding grinding fluid, and pressurizing the wafer to 0.02Mpa by a grinding disc at the rotation speed of 1000 r/min; cleaning with absolute ethyl alcohol after grinding; the grinding fluid comprises the following components: 0.5% of cubic boron nitride powder with the particle size of 10 mu m, 14% of alkylphenol polyoxyethylene, 4% of glycerol, 9% of polypropylene glycol 400 and the balance of deionized water;
step four, chamfering; chamfering the corners of the wafer by using a diamond grinding wheel of a numerical control machine;
step five, annealing; putting the wafer into an annealing furnace, heating up to 1600 ℃ at the speed of 180 ℃/h, preserving heat for 2h at 300 ℃ during heating up, preserving heat for 4h at 800 ℃, preserving heat for 5h at 1600 ℃, then cooling down at the speed of 200 ℃/h, preserving heat for 2h at 1000 ℃ and 500 ℃ respectively during cooling down, cooling to room temperature and taking out;
sixthly, chemically polishing the two surfaces; firstly, cleaning a wafer by absolute ethyl alcohol, and then putting the cleaned wafer into a double-sided polishing machine for fixing; during polishing, adding polishing liquid, pressurizing the wafer to 0.12Mpa by a polishing disc at the rotating speed of 1000r/min, cleaning the polished wafer by absolute ethyl alcohol, and naturally cooling at room temperature; the polishing solution comprises the following components: 0.5% of cubic boron nitride powder with the particle size of 1 mu m, 14% of alkylphenol polyoxyethylene, 4% of glycerol, 9% of polypropylene glycol 400 and 0.5% of nano silicon dioxide, so that the polishing solution is an alkaline solution with the pH value of 11.0, and the balance of deionized water; continuously supplementing alkaline solution in the polishing process to maintain the pH value of the polishing solution;
step seven, laser film taking; putting the polished wafer into a laser cutting machine, introducing protective gas, and cutting the wafer into corresponding sizes as required;
step eight, coating a film; plating antireflection films on the front surface and the back surface of the wafer by using an optical vacuum coating machine, wherein the antireflection films are formed by coating low-refractive-index oxides and high-refractive-index oxides layer by layer, the number of the antireflection films is 4, one layer closest to the wafer adopts the low-refractive-index oxides, the low-refractive-index oxides are oxides of silicon or aluminum, and the high-refractive-index oxides are oxides of titanium or tantalum;
step nine, inking; covering the coated wafer with a hollow plate, brushing ink on the edge of the wafer, and repeatedly brushing three layers;
step ten, baking; and (4) putting the wafer coated with the ink into a hot drying machine for hot drying for 2 hours, and then cooling the wafer to room temperature in air.
Example 3
The preparation process of the sapphire camera window sheet of the embodiment comprises the following steps:
step one, picking out a crystal bar; taking sapphire crystals in the A direction, the M direction or the C direction, and then using a bar drawing machine to draw bars, thereby obtaining crystal bars;
step two, crystal cutting; cutting the crystal bar by adopting diamond wire cutting equipment to obtain a wafer;
step three, grinding; grinding the wafer by a grinder; during grinding, grinding liquid is added, a grinding disc pressurizes the wafer to 0.02Mpa, and the rotating speed of the grinding disc is 11000 r/min; cleaning with absolute ethyl alcohol after grinding; the grinding fluid comprises the following components: 1% of cubic boron nitride powder with the particle size of 15 mu m, 15% of alkylphenol polyoxyethylene ether, 5% of glycerol, 10% of polypropylene glycol 400 and the balance of deionized water;
step four, chamfering; chamfering the corners of the wafer by using a diamond grinding wheel of a numerical control machine;
step five, annealing; putting the wafer into an annealing furnace, heating up to 1600 ℃ at the speed of 200 ℃/h, preserving heat for 2h at 300 ℃ during heating up, preserving heat for 3h at 800 ℃, preserving heat for 5h at 1600 ℃, then cooling down at the speed of 200 ℃/h, preserving heat for 2h at 1000 ℃ and 500 ℃ respectively during cooling down, cooling to room temperature and taking out;
sixthly, chemically polishing the two surfaces; firstly, cleaning a wafer by absolute ethyl alcohol, and then putting the cleaned wafer into a double-sided polishing machine for fixing; during polishing, adding polishing liquid, pressurizing the wafer to 0.13Mpa by a polishing disc at the rotation speed of 1200r/min, cleaning the polished wafer by absolute ethyl alcohol, and naturally cooling at room temperature; the polishing solution comprises the following components: 1% of cubic boron nitride powder with the particle size of 3 mu m, 15% of alkylphenol polyoxyethylene, 5% of glycerol, 10% of polypropylene glycol 400 and 1% of nano silicon dioxide, so that the pH value of the polishing solution is 12.0 of alkaline solution, and the balance is deionized water; continuously supplementing alkaline solution in the polishing process to maintain the pH value of the polishing solution;
step seven, laser film taking; putting the polished wafer into a laser cutting machine, introducing protective gas, and cutting the wafer into corresponding sizes as required;
step eight, coating a film; plating antireflection films on the front surface and the back surface of the wafer by using an optical vacuum coating machine, wherein the antireflection films are formed by coating low-refractive-index oxides and high-refractive-index oxides layer by layer, the number of the antireflection films is 6, one layer closest to the wafer adopts the low-refractive-index oxides, the low-refractive-index oxides are oxides of silicon or aluminum, and the high-refractive-index oxides are oxides of titanium or tantalum;
step nine, inking; covering the coated wafer with a hollow plate, brushing ink on the edge of the wafer, and repeatedly brushing three layers;
step ten, baking; and (4) putting the wafer coated with the ink into a hot drying machine for hot drying for 3 hours, and then cooling the wafer to room temperature in air.
The method for producing the sapphire camera window sheet is not limited to the specific technical scheme described in the embodiment, and all the technical schemes formed by adopting equivalent substitution are within the protection scope required by the invention.