CN111500198B - Composite polishing solution for blue glass optical filter and preparation method thereof - Google Patents
Composite polishing solution for blue glass optical filter and preparation method thereof Download PDFInfo
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- CN111500198B CN111500198B CN202010346831.XA CN202010346831A CN111500198B CN 111500198 B CN111500198 B CN 111500198B CN 202010346831 A CN202010346831 A CN 202010346831A CN 111500198 B CN111500198 B CN 111500198B
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Abstract
The invention discloses a composite polishing solution for a blue glass optical filter and a preparation method thereof. The preparation method comprises the steps of carrying out high-energy ball milling, drying granulation, calcination, high-energy ball milling and high-energy dispersion on aluminum hydroxide, zirconium hydroxide and silica sol to form dispersed materials, and then adding liquid alkali, a surfactant, a defoaming agent and water to prepare a stable composite polishing solution system.
Description
Technical Field
The invention relates to a glass polishing solution, in particular to a composite polishing solution for a blue glass optical filter and a preparation method thereof.
Background
The blue glass infrared cut-off filter is widely applied to the digital imaging field such as high-pixel mobile phone camera modules, monitoring lenses and the like, and is used for blocking the influence of infrared light on CCS/CMOS imaging and eliminating ghost and light spots. Compared with the common white glass infrared cut-off filter, the blue glass filter is used for more clear imaging, and the effective photosensitive angle can reach 30 degrees.
The blue glass is made of blue glass material (common optical filters are common optical glass), and the blue glass has the effect of filtering infrared light in an absorption mode. Because of the higher transmittance of blue light, the glass filter has better transmittance than red-orange glass filter, can filter infrared light above 630nm (but allows the rest light with wide wave band from ultraviolet to infrared light to pass through), and can filter thoroughly. However, since the blue glass does not have a main basic structure of silica-alumina as common glass and contains a large amount of phosphate and aluminate, the structure is weaker than that of common glass, the chemical activity is extremely strong, the blue glass is very easy to break and break in the polishing process, and meanwhile, the optical defects are caused because the blue glass is easy to form the Alar ratio, corrode white spots and white spots due to chemical instability in the processing process.
At present, the polishing process for blue glass mainly comprises two-step polishing, wherein in the first step, common rare earth polishing powder or zirconia polishing solution is used for firstly removing visible processing traces and scratches of the previous coarse grinding procedure; and in the second step, rare earth fine polishing liquid is used for deep processing. Generally, a plane double-side polishing machine is used for polishing, the Mohs hardness of rare earth oxide is usually between 4 and 6, while the hardness of blue glass is between 5 and 7, so that the processing is time-consuming and material-consuming, and the two-step method is adopted, the middle part needs to be fully cleaned, so that the processing through rate of the blue glass is very low, and the investment of the machine is not expensive.
Disclosure of Invention
In order to solve the technical problems, the invention provides a composite polishing solution for a blue glass optical filter and a preparation method thereof, so as to achieve the purposes of realizing the cutting rate of rough polishing and the surface quality of fine polishing while polishing in one step, along with simple process, cost saving and reduction of sewage discharge of a cleaning agent.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a composite polishing solution for a blue glass optical filter comprises aluminum hydroxide, zirconium hydroxide and silica sol, as well as liquid alkali, a surfactant, an antifoaming agent and water.
A preparation method of composite polishing solution for a blue glass optical filter comprises the following steps:
(1) adding aluminum hydroxide, zirconium hydroxide and silica sol into a stirring kettle, adding carboxymethyl cellulose and polyethylene glycol as a fusion agent, stirring, heating to 50-80 ℃, and keeping the temperature for 1 hour;
(2) stably pumping into a ball mill, circularly milling for 6-12 hours, and controlling the median particle size of the ball mill to be 1-4 microns;
(3) adding cellulose binder into the obtained mixed slurry, adjusting the viscosity to 20-200cps, spray drying and granulating, and controlling the median particle size of the granules to 20-100 μm;
(4) after granulation, the mixture is transferred into a kiln, the temperature rise speed is 1-10 ℃/min, the highest temperature is 1000-1200 ℃, and the calcination period is 22-24 hours;
(5) adding water into the calcined powder to adjust the mass ratio to 1: 1, ball milling the suspension, grinding the median particle size of the slurry to 0.4-1.0 μm, and controlling the particle size distribution D97 to be less than 5 μm;
(6) pumping the ball-milled slurry into a disc type dispersion machine, and dispersing until the particle size distribution D50 is 0.2-0.8 mu m and the D97 is less than 3 mu m;
(7) adding the dispersed materials into liquid alkali, surfactant, defoaming agent and water, stirring for 1-4 hours, filtering and packaging.
In the scheme, the liquid alkali is sodium hydroxide or strong potassium oxide.
In the scheme, the surfactant is glycol block polyether or sodium polyacrylate.
In the above scheme, the defoaming agent is an organic silicon defoaming agent.
In the above scheme, in the step (2), the ball mill needs to use alumina balls with a content of 95%, the ball diameter is 3mm, the rotation speed of the ball mill is adjusted to be 120-150rpm for grinding, the viscosity is monitored to be not higher than 500 in the process, the particle size is measured, and D50-1-4 um is taken as an end point.
In the scheme, centrifugal spray drying granulation is adopted in the step (3), natural gas is adopted as a drying heat source, the evaporation capacity is 100kg/h, the inlet temperature is adjusted to be 150-.
In the scheme, in the step (4), the calcining curve is set to be that the heating rate is 3-8 ℃/min from room temperature to 800 ℃, the temperature is kept for 1-6 hours at 800 ℃, the temperature is continuously increased to 1200 ℃ at 1000-4 ℃/min, the temperature is kept for 2-8 hours, and the temperature is naturally reduced to the room temperature.
In the above scheme, in the step (7), the mass ratios of the substances are respectively: 10-25% of dispersed material, 1-10% of liquid alkali, 1-10% of surfactant, 0.1-0.5% of defoaming agent and 60-80% of water.
In the scheme, the aluminum hydroxide is gamma-Al (OH)3Or gamma-AlOOH or alpha-Al (OH)3。
By the technical scheme, the composite polishing solution for the blue glass optical filter and the preparation method thereof provided by the invention have the following beneficial effects:
(1) according to the invention, hydroxides in the raw materials are processed into the three-component composite material of alumina, zirconia and silica after ball milling, drying and calcining, so that the surface quality of a polished part is effectively improved on the premise of ensuring high polishing efficiency, and the polished part has no surface defects, is easy to clean and has no residues.
(2) After the raw materials are mixed, the high-energy ball mill is used for adding the carboxymethyl cellulose and the polyethylene glycol, the effective adsorption of micropores in an alumina structure in the three-component composite slurry on zirconia particles is promoted by a physical crushing energizing and chemical fusing method, and simultaneously, the silica can be effectively wrapped in the alumina and the zirconia. Because the product is a micron and sub-nanometer material, the surface quality approaches the requirement of a final product on the basis of 20-50 percent higher than the cutting rate of a common product, and because the polishing process is deep, silicon oxide particles in the composite material structure are released, and the surface of a workpiece is repaired on the basis of realizing chemical mechanical polishing of micropores and other defects on the surface of the workpiece, so that the one-step polishing quality is far superior to two-step polishing.
(3) During calcination, the special calcination temperature curve is set, the phase ratio of alumina can be well controlled to reach the hardness close to that of blue glass, main physical grinding is provided, incomplete conversion of zirconia into tetragonal phase is controlled at high temperature, and meanwhile, the step (2) also ensures that the grain size is in a controllable range, so that the cutting rate is stably in a high-value state, the service life can be effectively prolonged to be close to 50%, and meanwhile, the unit workpiece processing time is saved by more than 50%.
(4) The composite material of the aluminum oxide, the zirconium oxide and the silicon oxide can provide the physical cutting rate higher than that of the existing two-step polishing, the zirconium oxide provides the chemical polishing capacity, and the silicon oxide provides CMP polishing and surface micro-defect repair, so that the product can realize the cutting rate of rough polishing and the surface quality of fine polishing while polishing in one step, the two-step method of rough polishing, cleaning and fine polishing in the original blue glass processing industry is optimized into a one-step method of polishing only once, 50% of polishing equipment and cleaning equipment are saved for customers, an intermediate cleaning step is saved, the non-process loss of blue glass is avoided, the cost is saved by 20%, the discharge of cleaning agent sewage is reduced, and the environmental benefit is very outstanding.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is an XRD pattern of a dispersed material obtained in step (6) disclosed in an embodiment of the present invention;
FIG. 2 is a surface state diagram of a product of an embodiment of the present invention after polishing blue glass;
fig. 3 is a schematic view of the surface state of the prior art finish-polished product after polishing blue glass.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The invention provides a composite polishing solution for a blue glass optical filter, which comprises aluminum hydroxide, zirconium hydroxide, silica sol, liquid alkali, a surfactant, a defoaming agent and water.
The invention also provides a preparation method of the composite polishing solution for the blue glass optical filter, which comprises the following steps:
(1) adding deionized water with the mass ratio of 5 percent into a reaction kettle, and adding aluminum hydroxide (gamma-Al (OH) with the mass ratio of 40 percent3Or gamma-AlOOH or alpha-Al (OH)3) After stirring for 20min, controlling the specific gravity between 1.1 and 1.2, slowly adding 30 percent by mass of zirconium hydroxide, after continuing stirring for 20min, adding 20 percent by mass of silica sol, adding 5 percent by mass of carboxymethyl cellulose and polyethylene glycol as fluxing agents, stirring, heating to 50-80 ℃, and keeping the temperature for 1 hour.
(2) And (2) stably pumping the mixed liquor obtained in the step (1) into a high-energy ball mill at a constant flow rate of 10L/min, wherein the ball mill needs to use alumina balls with the content of 95%, the ball diameter is 3mm, the rotating speed of the ball mill is adjusted to 130rpm for grinding, the viscosity is monitored to be not higher than 500 in the process, the grinding is carried out for 6-12 hours in a circulating manner, the granularity is measured, and D50-1-4 um is taken as an end point.
(3) Adding a cellulose binder into the obtained mixed slurry, adjusting the viscosity to be 20-200cps for later use, slowly pumping the mixed slurry into a centrifugal spray dryer for granulation by using a constant flow pump, carrying out spray drying granulation, wherein a drying heat source adopts natural gas, the evaporation capacity is 100kg/h, the inlet temperature is adjusted to be 180 ℃, the outlet temperature is adjusted to be 80 ℃ for spraying, the median particle size in the granulation is controlled to be 20-100 microns, and the shape of the particles is the best of a flying saucer shape or a spherical shape.
(4) Transferring the granulated particle powder into a kiln, setting the temperature rising rate to be 3-8 ℃/min from room temperature to 800 ℃ in a calcination curve, keeping the temperature at 800 ℃ for 5 hours, continuing to rise the temperature to 1000-1200 ℃, keeping the temperature at the rate of 1-4 ℃/min for 6 hours, and naturally cooling to the room temperature.
(5) Adding water into the calcined powder to adjust the mass ratio to 1: 1, ball milling the suspension by using a planetary mill, a pin type sand mill, a disc mill and a vibration mill, grinding the median particle size of the slurry to 0.4-1.0 mu m, and controlling the particle size distribution D97 to be less than 5 mu m; the grinding beads are yttrium-stabilized zirconia balls with the diameter of 0.4-1.2 mm.
(6) Pumping the ball-milled slurry into a disc type dispersion machine, and dispersing until the particle size distribution D50 is 0.2-0.8 mu m and the D97 is less than 3 mu m;
(7) and adding sodium hydroxide, a surfactant ethylene glycol block polyether, an organic silicon defoamer DC65 and water into the dispersed material, stirring for 1-4 hours, filtering by using a 5-micron PP filter element, and packaging. 15% of dispersed material, 8% of liquid alkali, 10% of surfactant, 0.2% of defoaming agent and 66.8% of water.
After drying the dispersed material obtained in step (6), the crystal structure and specific components of the product are tested by XRD, as shown in FIG. 1, it can be seen that alumina, zirconia and silica have formed a three-component composite system.
Comparing the cutting amount of the final product obtained in the step (7) with that of a rough polished product on the current market, and comparing the surface quality with that of a fine polished product on the current market, as shown in fig. 2 and 3.
The polishing process parameters are shown in table 1.
TABLE 1 polishing Process parameters
After the product of the invention is polished for 8 hours continuously, the cutting amount is obviously high, and the sold rough polishing product (rare earth polishing powder H500) is over 50 percent.
As shown in fig. 2 and 3, the surface of the blue glass is remarkably reduced in defects after the one-step polishing process of the present invention, and the smoothness and surface quality are remarkably improved compared with those of the existing finish-polished product.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The preparation method of the composite polishing solution for the blue glass optical filter is characterized by comprising the following steps of:
(1) adding aluminum hydroxide, zirconium hydroxide and silica sol into a stirring kettle, adding carboxymethyl cellulose and polyethylene glycol as a fusion agent, stirring, heating to 50-80 ℃, and keeping the temperature for 1 hour;
(2) stably pumping into a ball mill, circularly milling for 6-12 hours, and controlling the median particle size of the ball mill to be 1-4 microns;
(3) adding cellulose binder into the obtained mixed slurry, adjusting the viscosity to 20-200cps, spray drying and granulating, and controlling the median particle size of the granules to 20-100 μm;
(4) after granulation, the mixture is transferred into a kiln, the temperature rise speed is 1-10 ℃/min, the highest temperature is 1000-1200 ℃, and the calcination period is 22-24 hours; setting the calcining curve as the temperature rising rate of 3-8 ℃/min from room temperature to 800 ℃, keeping the temperature at 800 ℃ for 1-6 hours, continuing to rise the temperature to 1000-1200 ℃, keeping the temperature at the temperature rising rate of 1-4 ℃/min for 2-8 hours, and naturally cooling to room temperature;
(5) adding water into the calcined powder to adjust the mass ratio to 1: 1, ball milling the suspension, grinding the median particle size of the slurry to 0.4-1.0 μm, and controlling the particle size distribution D97 to be less than 5 μm;
(6) pumping the ball-milled slurry into a disc type dispersion machine, and dispersing until the particle size distribution D50 is 0.2-0.8 mu m and the D97 is less than 3 mu m;
(7) adding the dispersed materials into liquid alkali, a surfactant, a defoaming agent and water, stirring for 1-4 hours, filtering and packaging; the mass ratio of each substance is respectively as follows: 10-25% of dispersed material, 1-10% of liquid alkali, 1-10% of surfactant, 0.1-0.5% of defoaming agent and 60-80% of water.
2. The method of claim 1, wherein the liquid alkali is sodium hydroxide or strong potassium oxide.
3. The method of claim 1, wherein the surfactant is ethylene glycol block polyether or sodium polyacrylate.
4. The method for preparing the composite polishing solution for the blue glass filter according to claim 1, wherein the defoaming agent is a silicone defoaming agent.
5. The method as claimed in claim 1, wherein in the step (2), the ball mill is used with 95% alumina balls, the ball diameter is 3mm, the ball mill is adjusted to rotate at 120-150rpm, the viscosity is monitored to be not higher than 500, the particle size is measured, and D50-1-4 um is regarded as the end point.
6. The method as claimed in claim 1, wherein in the step (3), centrifugal spray drying granulation is adopted, natural gas is adopted as a drying heat source, the evaporation amount is 100kg/h, the inlet temperature is adjusted to be 150 ℃ and 300 ℃, and the outlet temperature is adjusted to be 60-90 ℃ for spraying.
7. The method of claim 1, wherein the aluminum hydroxide is γ -Al (OH)3Or gamma-AlOOH or alpha-Al (OH)3。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312789A (en) * | 1987-05-27 | 1994-05-17 | Minnesota Mining And Manufacturing Company | Abrasive grits formed of ceramic, impregnation method of making the same and products made therewith |
| CN1620490A (en) * | 2002-02-21 | 2005-05-25 | 3M创新有限公司 | Abrasive particles containing sintered, polycrystalline zirconia |
| CN102516882A (en) * | 2011-12-19 | 2012-06-27 | 德米特（苏州）电子环保材料有限公司 | Method for making resin lens polishing solution of alumina matrix |
| CN103183501A (en) * | 2013-03-13 | 2013-07-03 | 湖南大学 | Micro-nano spherical SG corundum abrasive and preparation method thereof |
| CN106479371A (en) * | 2016-08-15 | 2017-03-08 | 惠州市米特仑科技有限公司 | A kind of high precision composite polishing liquid and preparation method thereof |
| CN107936917A (en) * | 2017-12-13 | 2018-04-20 | 河北思瑞恩新材料科技有限公司 | A kind of micro mist performed polymer formula and preparation method thereof |
-
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- 2020-04-28 CN CN202010346831.XA patent/CN111500198B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312789A (en) * | 1987-05-27 | 1994-05-17 | Minnesota Mining And Manufacturing Company | Abrasive grits formed of ceramic, impregnation method of making the same and products made therewith |
| CN1620490A (en) * | 2002-02-21 | 2005-05-25 | 3M创新有限公司 | Abrasive particles containing sintered, polycrystalline zirconia |
| CN102516882A (en) * | 2011-12-19 | 2012-06-27 | 德米特（苏州）电子环保材料有限公司 | Method for making resin lens polishing solution of alumina matrix |
| CN103183501A (en) * | 2013-03-13 | 2013-07-03 | 湖南大学 | Micro-nano spherical SG corundum abrasive and preparation method thereof |
| CN106479371A (en) * | 2016-08-15 | 2017-03-08 | 惠州市米特仑科技有限公司 | A kind of high precision composite polishing liquid and preparation method thereof |
| CN107936917A (en) * | 2017-12-13 | 2018-04-20 | 河北思瑞恩新材料科技有限公司 | A kind of micro mist performed polymer formula and preparation method thereof |
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