CN111100559A - Water-based magnetorheological polishing solution and preparation method thereof - Google Patents
Water-based magnetorheological polishing solution and preparation method thereof Download PDFInfo
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- CN111100559A CN111100559A CN201911393574.9A CN201911393574A CN111100559A CN 111100559 A CN111100559 A CN 111100559A CN 201911393574 A CN201911393574 A CN 201911393574A CN 111100559 A CN111100559 A CN 111100559A
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Abstract
The invention belongs to the technical field of optical precision machining and manufacturing, and particularly relates to a water-based magnetorheological polishing solution and a preparation method thereof. The invention provides a water-based magnetorheological polishing solution which comprises: 77-88 wt% of magnetic particles; 0.01-8 wt% of non-magnetic polishing powder; 0.2-0.5 wt% of dispersion stabilizer; 0.5-1 wt% of a wetting agent; 0.1-0.4 wt% of a chelating agent; 0.01-0.02 wt% of an antioxidant; 0.2-0.5 wt% of a pH regulator; the solvent is water; the dispersion stabilizer is polyphosphate and/or citrate; the wetting agent is a polyol; the chelating agent is an aminocarboxylic acid compound and/or an organic phosphate. The water-based magnetorheological polishing solution provided by the invention has good dispersion stability and viscosity stability, low zero-magnetic-field viscosity and high material removal efficiency.
Description
Technical Field
The invention belongs to the technical field of optical precision machining and manufacturing, and particularly relates to a water-based magnetorheological polishing solution and a preparation method thereof.
Background
The magneto-rheological polishing technology is a new optical surface precision processing technology, integrates knowledge of electromagnetism, chemistry, contact mechanics and hydromechanics, is a processing method between contact and non-contact, and can carry out deterministic processing on optical elements made of various materials. Especially, the polishing agent is widely applied to polishing materials such as glass, ceramics and the like. The preparation technology of the magnetorheological polishing solution is one of key technologies for realizing magnetorheological polishing, and the magnetorheological polishing solution with excellent performance is also a necessary condition for realizing magnetorheological deterministic polishing. The magnetorheological polishing technology embodies the creative application of the magnetorheological fluid in the field of optical processing, wherein the main components of the magnetorheological polishing liquid are substantially similar to those of the magnetorheological fluid applied in the traditional field, but the component selection and the specific use requirements are greatly different.
Based on the requirements of actual optical processing, the magnetorheological polishing solution has the following performance characteristics: (1) good dispersion stability. The requirements are that the magnetorheological polishing solution does not settle in the using process, the consistency of liquid components in the polishing process is ensured, and the magnetorheological polishing solution can be redispersed by simple stirring after standing. (2) Lower zero field viscosity. This requires that the viscosity of the polishing solution is as low as possible in the absence of a magnetic field, so as to ensure stable circulation of the solution in the circulation system, while achieving a higher removal efficiency under the same polishing parameters. (3) Good rheological properties. The removal efficiency of the magnetorheological polishing material is in direct proportion to the shear yield stress of the polishing solution after the magnetorheological polishing solution generates rheology under a magnetic field. Therefore, in order to obtain higher material removal efficiency, the preparation of the magnetorheological polishing solution requires a lower zero magnetic field viscosity to ensure fluidity and a better rheological property. (4) Easy cleaning property. The magnetorheological polishing solution is added into the circulating system for polishing, the liquid is required to be discharged from the circulating system after polishing is finished, and then the liquid remaining in the circulating pipeline in the circulating system is cleaned, so that the cleanness of the circulating system is ensured, and new polishing solution added in next polishing is not influenced. Therefore, the ease of cleaning the magnetorheological polishing fluid is also very important. (5) Environment protection, no toxicity and simple preparation process.
The magnetorheological polishing solution comprises a water-based magnetorheological polishing solution and an oil-based magnetorheological polishing solution, and the water-based magnetorheological polishing solution is more suitable for optical processing due to the advantages of the water-based magnetorheological polishing solution in polishing efficiency, environmental protection, component control and the like compared with the oil-based magnetorheological polishing solution. At present, some research units at home and abroad research the magnetorheological polishing solution, and QED and rogegerster mainly research the magnetorheological polishing solution at home and abroad, wherein a water-based magnetorheological polishing solution patent (US 5804095) applied by QED has simple chemical components but insufficient dispersion stability, and cannot enable polishing and added magnetic particles to be well combined, so that the light efficiency is not high. In addition, the selection of magnetic particles and polishing powder particles is provided to improve the surface quality of the optical mirror surface after magnetorheological polishing, but specific components and a preparation method of the liquid are not provided. The patent of Rogers super university application introduces how to plate a ceramic film layer on the surface of carbonyl iron powder to improve the oxidation resistance and rust resistance of the magnetorheological polishing solution, and the same problems that the coated carbonyl iron powder can be mixed with a basic carrier liquid to prepare the magnetorheological polishing solution are that a specific preparation method of the magnetorheological polishing solution is not introduced, and the operation process is complicated.
The domestic research on the magnetorheological polishing solution is still in the starting stage at present, wherein the patent with the publication number of CN101139504A performs surface treatment on carbonyl iron powder by using a surfactant, and performs mixing and stirring in a ball milling mode to obtain the magnetorheological polishing solution, and then polishing powder is added for stirring to prepare the magnetorheological polishing solution. The process for obtaining the magnetorheological polishing solution by the method is complex, and the surface appearance and the particle size distribution of the carbonyl iron powder are damaged by adopting a ball milling method, so that the performance of the prepared magnetorheological polishing solution is influenced. In addition, the polishing powder is directly added into the magnetorheological fluid to prepare the magnetorheological polishing solution, the interaction between the polishing powder and carbonyl iron powder is not considered, and the prepared magnetorheological polishing solution has higher zero magnetic field viscosity. In another patent publication No. CN101250380A, a ball mill is also used to mix a dispersed phase of magnetic particles and polishing powder with a carrier liquid (continuous phase) of water-based complex ligand, which also has the problem of CN101250380 a. In addition, the thixotropic agent adopted in the formula has larger zero magnetic field viscosity and insufficient viscosity stability for long-time polishing use.
Disclosure of Invention
In view of the above, the present invention aims to provide a water-based magnetorheological polishing solution and a preparation method thereof, and the water-based magnetorheological polishing solution provided by the present invention has good dispersion stability and viscosity stability, low zero magnetic field viscosity, and high material removal efficiency.
The invention provides a water-based magnetorheological polishing solution, which comprises:
the dispersion stabilizer is polyphosphate and/or citrate;
the wetting agent is a polyol;
the chelating agent is an aminocarboxylic acid compound and/or an organic phosphate.
Preferably, the magnetic particles comprise one or more of unmodified carbonyl iron powder, phosphated carbonyl iron powder, reduced carbonyl iron powder and coated carbonyl iron powder;
median particle diameter D of the magnetic particles501 to 10 μm.
Preferably, the non-magnetic polishing powder comprises one or more of diamond powder, alumina powder and cerium oxide powder;
the median diameter D of the non-magnetic polishing powder5020nm to 3 mu m.
Preferably, the polyphosphate comprises one or more of sodium tripolyphosphate, sodium tetrapolyphosphate, ammonium polyphosphate, sodium pyrophosphate and sodium hexametaphosphate;
the citrate comprises one or more of potassium citrate, ammonium citrate and sodium citrate.
Preferably, the polyol comprises one or more of propylene glycol, glycerol, butylene glycol, sorbitol, polyglycerol and polypropylene glycol.
Preferably, the aminocarboxylic acid compounds comprise ethylene diamine tetraacetic acid salt and/or nitrilotriacetic acid;
the organophosphate comprises pentasodium aminotrimethylene phosphonate and/or tetrasodium aminotrimethylene phosphonate.
Preferably, the antioxidant comprises sodium nitrite and/or sodium benzoate.
Preferably, the pH adjuster includes one or more of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, phosphoric acid, and hydrochloric acid.
The invention provides a preparation method of the water-based magnetorheological polishing solution in the technical scheme, which comprises the following steps:
mixing magnetic particles, non-magnetic polishing powder, a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant and a pH regulator in water to obtain the water-based magnetorheological polishing solution.
Preferably, the mixing process specifically includes:
a) mixing a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant, a pH regulator and water to obtain a composite base carrier liquid; mixing the magnetic particles and the non-magnetic polishing powder to obtain a solid dispersion phase;
b) and rolling and stirring the composite base carrier liquid and the solid dispersion phase to obtain the water-based magnetorheological polishing solution.
Compared with the prior art, the invention provides a water-based magnetorheological polishing solution and a preparation method thereof. The invention provides a water-based magnetorheological polishing solution which comprises: 77-88 wt% of magnetic particles; 0.01-8 wt% of non-magnetic polishing powder; 0.2-0.5 wt% of dispersion stabilizer; 0.5-1 wt% of a wetting agent; 0.1-0.4 wt% of a chelating agent; 0.01-0.02 wt% of an antioxidant; 0.2-0.5 wt% of a pH regulator; the solvent is water; the dispersion stabilizer is polyphosphate and/or citrate; the wetting agent is a polyol; the chelating agent is an aminocarboxylic acid compound and/or an organic phosphate. According to the invention, the component formula of the water-based magnetorheological polishing solution is optimally designed, and particularly no macromolecular thickener or thixotropic agent is added, so that the zero magnetic field viscosity of the water-based magnetorheological polishing solution is obviously reduced, and the viscosity stability is higher, so that the water-based magnetorheological polishing solution is more suitable for use and control of magnetorheological polishing; by considering the action of the non-magnetic polishing powder and the magnetic particles, the using amount of the non-magnetic polishing powder in the polishing solution is reduced, the utilization efficiency of the non-magnetic polishing powder is improved, and the polishing efficiency is obviously improved; by adding a specific dispersion stabilizer, the dispersion stability and long-term effectiveness of the magnetorheological polishing solution can be ensured; by adding the specific wetting agent, the loss of water in the magnetorheological polishing process can be reduced, and the spreading of the dispersion stabilizer on the surface of the magnetic particles is promoted, so that the dispersing agent can better play a role; by adding the specific chelating agent, the non-magnetic polishing powder and the magnetic particles can be connected to enable the polishing powder to be associated with the surfaces of the magnetic particles, the utilization rate of the polishing powder is improved, the polishing efficiency is further improved, and the production cost is saved. Moreover, the magnetorheological polishing solution provided by the invention takes water as a base carrier liquid, so the magnetorheological polishing solution also has the advantages of environmental protection and easy cleaning. In addition, the water-based magnetorheological polishing solution has excellent universality, and the type and the particle size of the polishing powder can be adjusted according to different polishing materials and different polishing stages, so that different polishing requirements are met.
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, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a flow chart of a process for preparing a water-based magnetorheological polishing fluid according to an embodiment of the present invention;
FIG. 2 is a graph of the removal function of BK7 glass polished with the water-based magnetorheological polishing solution of example 1 provided by the present invention;
FIG. 3 is a graph of the removal function of the water-based magnetorheological polishing fluid of example 2 provided by the present invention for polishing RB-SiC materials;
FIG. 4 is a graph of the removal function of a water-based magnetorheological polishing fluid on a silicon carbide substrate modified silicon surface according to example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a water-based magnetorheological polishing solution, which comprises:
the dispersion stabilizer is polyphosphate and/or citrate;
the wetting agent is a polyol;
the chelating agent is an aminocarboxylic acid compound and/or an organic phosphate.
The water-based magnetorheological polishing solution provided by the invention comprises magnetic particles, nonmagnetic polishing powder, a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant, a pH regulator and water. The magnetic particles are used as the main component of the dispersed phase of the magnetorheological polishing solution, and preferably comprise one or more of unmodified carbonyl iron powder (namely common carbonyl iron powder), phosphated carbonyl iron powder, reduced carbonyl iron powder and coated carbonyl iron powder; median particle diameter D of the magnetic particles50Preferably 1 to 10 μm, and more specifically 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm, 8 μm, 8.5 μm, 9 μm, 9.5 μm or 10 μm. In the invention, the content of the magnetic particles in the water-based magnetorheological polishing solution is 77-88 wt%, specifically 77 wt%, 77.5 wt%, 78 wt%, 78.5 wt%, 79 wt%, 79.5 wt%, 80 wt%, 80.5 wt%, 81 wt%, 81.5 wt%, 82 wt%, 82.5 wt%, 83 wt%, 83.5 wt%, 84 wt%, 84.5 wt%, 85 wt%, 85.5 wt%, 86 wt%, 86.5 wt%, 87 wt%, 87.5 wt% or 88 wt%.
In the present invention, the non-magnetic polishing powder is a magnetic currentThe polishing solution can meet polishing conditions, and key components for removing materials are preferably selected from one or more of diamond powder, alumina powder and cerium oxide powder; the median diameter D of the non-magnetic polishing powder50Preferably 20nm to 3 μm, and more specifically 20nm, 50nm, 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1 μm, 1.2 μm, 1.5 μm, 1.7 μm, 2 μm, 2.3 μm, 2.5 μm, 2.7 μm or 3 μm. In the invention, the content of the non-magnetic polishing powder in the water-based magnetorheological polishing solution is 0.01 wt% to 8 wt%, specifically 0.01 wt%, 0.05 wt%, 0.1 wt%, 1 wt%, 5 wt%, 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, 5 wt%, 5.5 wt%, 6 wt%, 6.5 wt%, 7 wt%, 7.5 wt% or 8 wt%.
In the present invention, the dispersion stabilizer is polyphosphate and/or citrate. Wherein the polyphosphate preferably comprises one or more of sodium tripolyphosphate, sodium tetrapolyphosphate, ammonium polyphosphate, sodium pyrophosphate and sodium hexametaphosphate; the citrate salt preferably comprises one or more of potassium citrate, ammonium citrate and sodium citrate. In one embodiment provided by the invention, the dispersion stabilizer comprises sodium tripolyphosphate and sodium hexametaphosphate, and the mass ratio of the sodium tripolyphosphate to the sodium hexametaphosphate is preferably (2-3): 10, specifically 2:10, 2.1:10, 2.2:10, 2.3:10, 2.4:10, 2.5:10, 2.6:10, 2.7:10, 2.8:10, 2.9:10 or 3: 10. In the invention, the preferable dispersion stabilizer has better dispersion and stabilization effects on carbonyl iron powder, and has certain antirust and antioxidant effects. In the present invention, the dispersion stabilizer is contained in the water-based magnetorheological polishing fluid in an amount of 0.2 to 0.5 wt%, and specifically may be 0.2 wt%, 0.21 wt%, 0.22 wt%, 0.23 wt%, 0.24 wt%, 0.25 wt%, 0.26 wt%, 0.27 wt%, 0.28 wt%, 0.29 wt%, 0.3 wt%, 0.31 wt%, 0.32 wt%, 0.33 wt%, 0.34 wt%, 0.35 wt%, 0.36 wt%, 0.37 wt%, 0.38 wt%, 0.39 wt%, 0.4 wt%, 0.41 wt%, 0.42 wt%, 0.43 wt%, 0.44 wt%, 0.45 wt%, 0.46 wt%, 0.47 wt%, 0.48 wt%, 0.49 wt%, or 0.5 wt%.
In the present invention, the humectant is a polyhydric alcohol, which preferably includes one or more of propylene glycol, glycerin, butylene glycol, sorbitol, polyglycerol, and polypropylene glycol. In the present invention, the preferred wetting agent can reduce the water loss during the magnetorheological polishing process and promote the dispersion stabilizer to spread on the surface of the magnetic particles, so that the dispersion stabilizer can better perform the function. In the invention, the content of the wetting agent in the water-based magnetorheological polishing solution is 0.5-1 wt%, and specifically can be 0.5 wt%, 0.55 wt%, 0.6 wt%, 0.65 wt%, 0.7 wt%, 0.75 wt%, 0.8 wt%, 0.85 wt%, 0.9 wt%, 0.95 wt% or 1 wt%.
In the present invention, the chelating agent is an aminocarboxylic acid compound and/or an organophosphate. Wherein, the aminocarboxylic acid compounds preferably comprise ethylene diamine tetraacetic acid salt and/or nitrilotriacetic acid; the edetate is preferably sodium edetate; the organophosphate preferably comprises pentasodium aminotrimethylene phosphonate and/or tetrasodium aminotrimethylene phosphonate. In the invention, the preferable chelating agent can connect the non-magnetic polishing powder and the magnetic particles to enable the polishing powder to be associated with the surfaces of the magnetic particles, so that the utilization rate of the polishing powder is improved, the polishing efficiency is further improved, and the production cost is saved. In the invention, the content of the chelating agent in the water-based magnetorheological polishing solution is 0.1-0.4 wt%, and specifically can be 0.1 wt%, 0.12 wt%, 0.15 wt%, 0.17 wt%, 0.2 wt%, 0.23 wt%, 0.25 wt%, 0.27 wt%, 0.3 wt%, 0.32 wt%, 0.35 wt%, 0.37 wt%, or 0.4 wt%.
In the present invention, the antioxidant preferably comprises sodium nitrite and/or sodium benzoate; the content of the antioxidant in the water-based magnetorheological polishing solution is 0.01-0.02 wt%, and specifically can be 0.01 wt%, 0.011 wt%, 0.012 wt%, 0.013 wt%, 0.014 wt%, 0.015 wt%, 0.016 wt%, 0.017 wt%, 0.018 wt%, 0.019 wt% or 0.02 wt%.
In the present invention, the pH adjuster preferably includes one or more of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, phosphoric acid, and hydrochloric acid; the pH regulator is contained in the water-based magnetorheological polishing solution in an amount of 0.2 to 0.5 wt%, specifically 0.2 wt%, 0.21 wt%, 0.22 wt%, 0.23 wt%, 0.24 wt%, 0.25 wt%, 0.26 wt%, 0.27 wt%, 0.28 wt%, 0.29 wt%, 0.3 wt%, 0.31 wt%, 0.32 wt%, 0.33 wt%, 0.34 wt%, 0.35 wt%, 0.36 wt%, 0.37 wt%, 0.38 wt%, 0.39 wt%, 0.4 wt%, 0.41 wt%, 0.42 wt%, 0.43 wt%, 0.44 wt%, 0.45 wt%, 0.46 wt%, 0.47 wt%, 0.48 wt%, 0.49 wt%, or 0.5 wt%.
In the invention, the solvent of the water-based magnetorheological polishing solution is water, and the content of the water in the magnetorheological polishing solution is preferably the balance.
The invention also provides a preparation method of the water-based magnetorheological polishing solution in the technical scheme, which comprises the following steps:
mixing magnetic particles, non-magnetic polishing powder, a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant and a pH regulator in water to obtain the water-based magnetorheological polishing solution.
In the preparation method provided by the invention, the magnetic particles, the non-magnetic polishing powder, the dispersion stabilizer, the wetting agent, the chelating agent, the antioxidant and the pH regulator are directly and uniformly mixed in water to obtain the water-based magnetorheological polishing solution provided by the invention. Wherein, the specific process of mixing preferably comprises:
a) mixing a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant, a pH regulator and water to obtain a composite base carrier liquid; mixing the magnetic particles and the non-magnetic polishing powder to obtain a solid dispersion phase;
b) and rolling and stirring the composite base carrier liquid and the solid dispersion phase to obtain the water-based magnetorheological polishing solution.
In the above mixing process provided by the present invention, the composite base carrier liquid and the solid dispersion phase are prepared separately. Wherein, the composite base carrier liquid is preferably prepared according to the following steps:
a1) mixing a dispersion stabilizer with water to obtain a first mixed solution;
a2) mixing the first mixed solution with a wetting agent to obtain a second mixed solution;
a3) mixing the second mixed solution with a chelating agent to obtain a third mixed solution;
a4) mixing the third mixed solution with an antioxidant to obtain a fourth mixed solution;
a5) and mixing the fourth mixed solution with a pH regulator to obtain the composite base carrier liquid.
In the preparation step of the composite base carrier liquid provided by the invention, in the step a1), the mixing stirring speed is preferably 300-600 r/min, and specifically can be 300r/min, 350r/min, 400r/min, 450r/min, 500r/min, 550r/min or 600 r/min; the mixing temperature is preferably 22-25 ℃, and specifically can be 22 ℃, 23 ℃, 24 ℃ or 25 ℃; the mixing time is preferably 1-2 h, and specifically can be 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2 h.
In the preparation step of the composite base carrier liquid provided by the invention, in the step a2), the mixing stirring speed is preferably 300-600 r/min, and specifically can be 300r/min, 350r/min, 400r/min, 450r/min, 500r/min, 550r/min or 600 r/min; the mixing temperature is preferably 22-25 ℃, and specifically can be 22 ℃, 23 ℃, 24 ℃ or 25 ℃; the mixing time is preferably 0.5-1 h, and specifically can be 0.5h, 0.6h, 0.7h, 0.8h, 0.9h or 1 h.
In the preparation step of the composite base carrier liquid provided by the invention, in the step a3), the mixing stirring speed is preferably 300-600 r/min, and specifically can be 300r/min, 350r/min, 400r/min, 450r/min, 500r/min, 550r/min or 600 r/min; the mixing temperature is preferably 22-25 ℃, and specifically can be 22 ℃, 23 ℃, 24 ℃ or 25 ℃; the mixing time is preferably 1-2 h, and specifically can be 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2 h.
In the preparation step of the composite base carrier liquid provided by the invention, in the step a4), the mixing stirring speed is preferably 300-600 r/min, and specifically can be 300r/min, 350r/min, 400r/min, 450r/min, 500r/min, 550r/min or 600 r/min; the mixing temperature is preferably 22-25 ℃, and specifically can be 22 ℃, 23 ℃, 24 ℃ or 25 ℃; the mixing time is preferably 1-2 h, and specifically can be 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2 h.
In the preparation step of the composite base carrier liquid provided by the invention, in the step a5), the mixing stirring speed is preferably 300-600 r/min, and specifically can be 300r/min, 350r/min, 400r/min, 450r/min, 500r/min, 550r/min or 600 r/min; the mixing temperature is preferably 22-25 ℃, and specifically can be 22 ℃, 23 ℃, 24 ℃ or 25 ℃; the mixing time is preferably 1-2 h, and specifically can be 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2 h.
In the mixing process provided by the invention, the solid dispersion phase is formed by mixing magnetic particles and non-magnetic polishing powder, the specific mixing condition is not particularly limited, and the two components can be uniformly mixed.
In the mixing process provided by the invention, after the composite base carrier liquid and the solid dispersion phase are obtained, the composite base carrier liquid and the solid dispersion phase are stirred in a rolling manner. The specific operation process of the rolling stirring is as follows: filling the composite base carrier liquid and the solid dispersion phase into a container, then sealing the container, then putting the sealed container into a rolling stirring device, and finally starting the device to perform rolling stirring. In the invention, the volume of the container is preferably 2-3 times of the volume of the composite base carrier liquid and the solid dispersion mixture; the rotating speed of the rolling stirring is preferably 100-150 rpm, and specifically can be 100 rpm, 105 rpm, 110 rpm, 115 rpm, 120 rpm, 125 rpm, 130 rpm, 135 rpm, 140 rpm, 145 rpm or 150 rpm; the rolling stirring time is preferably 2-4 h, and specifically can be 2h, 2.5h, 3h, 3.5h or 4 h.
In the mixing process provided by the invention, the water-based magnetorheological polishing solution provided by the invention is obtained after rolling stirring is finished.
The water-based magnetorheological polishing solution has good dispersion stability and viscosity stability, low zero magnetic field viscosity and high material removal efficiency by optimally designing the component formula of the water-based magnetorheological polishing solution. More specifically, the magnetorheological polishing solution and the preparation method thereof provided by the invention at least have the following advantages:
1) according to the invention, no macromolecular thickener or thixotropic agent is added, so that the zero magnetic field viscosity of the water-based magnetorheological polishing solution is obviously reduced, and the viscosity stability is higher, so that the water-based magnetorheological polishing solution is more suitable for use and control of magnetorheological polishing;
2) the effect of the non-magnetic polishing powder and the magnetic particles is considered, so that the using amount of the non-magnetic polishing powder in the polishing solution is reduced, the utilization efficiency of the non-magnetic polishing powder is improved, and the polishing efficiency is obviously improved;
3) a specific dispersion stabilizer is added, so that the dispersion stability and long-term effectiveness of the magnetorheological polishing solution can be ensured; by adding the specific wetting agent, the loss of water in the magnetorheological polishing process can be reduced, and the spreading of the dispersion stabilizer on the surface of the magnetic particles is promoted, so that the dispersing agent can better play a role;
4) the specific chelating agent is added, so that the non-magnetic polishing powder and the magnetic particles can be connected to enable the polishing powder to be associated with the surfaces of the magnetic particles, the utilization rate of the polishing powder is improved, the polishing efficiency is further improved, and the production cost is saved;
5) the polishing powder has excellent universality, and the type and the particle size of the polishing powder can be adjusted according to different polishing materials and different polishing stages, so that different polishing requirements are met;
6) in the preferred technical scheme provided by the invention, the chemical reagent added into the water-based magnetorheological polishing solution has excellent water solubility, and after the polishing solution is used for polishing, only tap water is needed for cleaning a polishing circulation system, so that the cleaning process is convenient, the required time is short, and the cleaning is clean;
7) in the preferred technical scheme provided by the invention, a rolling stirring mode is adopted in the mixing process of the solid dispersion phase and the composite base carrier liquid, the mixing mode does not influence the addition components and the chemical action of the magnetorheological polishing liquid, and the operation is simple and convenient.
For the sake of clarity, the following examples are given in detail.
Example 1
1) Composition design
The specific components and contents of the water-based magnetorheological polishing solution provided in this embodiment are shown in table 1:
TABLE 1 EXAMPLE 1 ingredient information Table for magnetorheological polishing fluid
2) Referring to the component information in table 1, the water-based magnetorheological polishing solution is prepared according to the process shown in fig. 1, and the specific steps are as follows:
step 1, adding sodium citrate as a dispersion stabilizer into 250ml of deionized water, stirring for 1 hour, setting the rotating speed of a stirrer to be 400r/min, and controlling the temperature to be 22-25 ℃.
And 2, adding a wetting agent propylene glycol into the solution obtained in the step 1, and stirring for 0.5 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 3, adding chelating agent sodium ethylene diamine tetracetate into the solution obtained in the step 2, and stirring for 1.5 hours by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 4, adding an antioxidant sodium nitrite into the solution obtained in the step 3, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 5, adding a pH regulator sodium carbonate into the solution obtained in the step 4, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 6, because water is lost in the stirring process, supplementing the lost deionized water component, and stirring for 0.5 hour, wherein the rotating speed of a stirrer is set to be 500r/min, and the temperature is controlled to be between 22 and 25 ℃ to obtain the composite base carrier liquid.
And 7, uniformly mixing the common carbonyl iron powder and the cerium oxide powder to obtain a solid dispersion phase.
And step 8, taking the composite base carrier liquid as a continuous phase, adding the continuous phase and the solid dispersion phase into a round wide-necked bottle, sealing the bottle mouth, and stirring for 2.5 hours at 120 revolutions per minute in a rolling stirring device, wherein the volume of the wide-necked bottle is 2 times of the total volume of the continuous phase and the solid dispersion phase.
Example 2
1) Composition design
The specific components and contents of the water-based magnetorheological polishing solution provided in this embodiment are shown in table 1:
TABLE 2 EXAMPLE 2 ingredient information Table for magnetorheological polishing solutions
2) Referring to the component information in table 2, the water-based magnetorheological polishing solution is prepared according to the process shown in fig. 1, and the specific steps are as follows:
step 1, adding a dispersion stabilizer mixed by sodium tripolyphosphate and sodium hexametaphosphate into 250ml of deionized water, and stirring, wherein the rotating speed of a stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 2, adding a wetting agent sorbitol into the solution obtained in the step 1, and stirring for 0.5 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 3, adding chelating agent sodium ethylene diamine tetracetate into the solution obtained in the step 2, and stirring for 1.5 hours by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 4, adding an antioxidant sodium nitrite into the solution obtained in the step 3, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 5, adding a pH regulator potassium carbonate into the solution obtained in the step 4, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 6, because water is lost in the stirring process, supplementing the lost deionized water component, and stirring for 0.5 hour, wherein the rotating speed of a stirrer is set to be 500r/min, and the temperature is controlled to be between 22 and 25 ℃ to obtain the composite base carrier liquid.
And 7, uniformly mixing the common carbonyl iron powder and the diamond micro powder to obtain a solid dispersion phase.
And step 8, taking the composite base carrier liquid as a continuous phase, adding the continuous phase and the solid dispersion phase into a round wide-necked bottle, sealing the bottle mouth, placing the bottle mouth into a rolling stirring device, and stirring for 4 hours at 120 revolutions per minute to obtain the water-based magnetorheological polishing liquid, wherein the volume of the wide-necked bottle is 2 times of the total volume of the continuous phase and the solid dispersion phase.
Example 3
1) Composition design
The specific components and contents of the water-based magnetorheological polishing solution provided in this embodiment are shown in table 1:
TABLE 3 EXAMPLE 3 ingredient information Table for magnetorheological polishing fluid
| Name of composition | Composition information | Content (wt%) | Remarks for note |
| Ordinary carbonyl iron powder | D50＝4μm | 85 | Magnetic particles |
| Diamond micropowder | D50＝0.05μm | 0.1 | Non-magnetic polishing powder |
| Sodium hexametaphosphate | Analytical purity | 0.5 | Dispersion stabilizer |
| Glycerol | Analytical purity | 0.9 | Wetting agent |
| Amino trimethylene phosphonic acid pentasodium salt | Analytical purity | 0.3 | Chelating agents |
| Sodium nitrite | Analytical purity | 0.02 | Antioxidant agent |
| Sodium carbonate | Analytical purity | 0.5 | pH regulator |
| Water (W) | Deionized water | Balance of | Solvent(s) |
2) Referring to the component information in table 3, the water-based magnetorheological polishing solution was prepared according to the process shown in fig. 1, and the specific steps were as follows:
step 1, adding sodium hexametaphosphate serving as a dispersion stabilizer into 250ml of deionized water, and stirring, wherein the rotating speed of a stirrer is set to 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 2, adding a wetting agent glycerol into the solution obtained in the step 1, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 3, adding chelating agent aminotrimethylene phosphonic acid pentasodium into the solution obtained in the step 2, and stirring for 1.5 hours by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 4, adding an antioxidant sodium nitrite into the solution obtained in the step 3, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 5, adding a pH regulator sodium carbonate into the solution obtained in the step 4, and stirring for 1 hour by using a stirrer, wherein the rotating speed of the stirrer is set to be 400r/min, and the temperature is controlled to be between 22 and 25 ℃.
And 6, because water is lost in the stirring process, supplementing the lost deionized water component, and stirring for 0.5 hour, wherein the rotating speed of a stirrer is set to be 500r/min, and the temperature is controlled to be between 22 and 25 ℃ to obtain the water-based compound carrier liquid.
And 7, uniformly mixing the common carbonyl iron powder and the diamond micro powder to obtain a solid dispersion phase.
And step 8, taking the composite base carrier liquid as a continuous phase, adding the continuous phase and the solid dispersion phase into a round wide-necked bottle, sealing the bottle mouth, and stirring for 3 hours at 120 revolutions per minute in a rolling stirring device, wherein the volume of the wide-necked bottle is 2 times of the total volume of the continuous phase and the solid dispersion phase.
Evaluation of Performance
1) The water-based magnetorheological polishing solutions prepared in the embodiments 1, 2 and 3 are used for polishing materials, and the relevant processing parameters of the polishing operations are shown in table 4:
TABLE 4 polishing work processing parameters
| Control parameter | Size of polishing wheel | Depth of penetration | Rotational speed of polishing wheel |
| Parameter(s) | 160mm | 1mm | 120r/min |
Fig. 2 to 4 show removal functions obtained by polishing operation, fig. 2 is a graph of a removal function obtained by polishing BK7 glass with the water-based magnetorheological polishing solution according to example 1, fig. 3 is a graph of a removal function obtained by polishing RB-SiC material with the water-based magnetorheological polishing solution according to example 2, and fig. 4 is a graph of a removal function obtained by polishing silicon carbide substrate modified silicon surface with the water-based magnetorheological polishing solution according to example 3. Wherein, BK7 glass is a standard material; the RB-SiC material refers to a SiC material prepared by a reaction sintering method (RB); the silicon carbide substrate modified silicon surface is a Si modified layer with a certain thickness (about 10 mu m) formed on the surface of an RB-SiC material by deposition through a Physical Vapor Deposition (PVD) technology.
The peak value removing efficiency of the removing function can reach 4.6 mu m/min through calculation according to the figure 2; the peak value of the removal function can be calculated through the graph 3, and the removal efficiency can reach 1.2 mu m/min; it can be calculated from fig. 4 that the peak removal efficiency of the removal function can reach 1.5 μm/min.
After the continuous polishing operation is carried out for 6 hours, the removal efficiency change rates of the three water-based magnetorheological polishing solutions for polishing corresponding materials are respectively calculated, and the results are respectively as follows: 3 percent or less (the polishing solution in the embodiment 1), 4 percent or less (the polishing solution in the embodiment 2) and 3 percent or less (the polishing solution in the embodiment 3).
2) The zero magnetic field viscosity of the water-based magnetorheological polishing solutions prepared in example 1, example 2 and example 3 was respectively measured, and the results are respectively: 255 mPaS (example 1 polishing solution), 260 mPaS (example 2 polishing solution), and 280 mPaS (example 3 polishing solution).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A water-based magnetorheological polishing fluid comprising:
the dispersion stabilizer is polyphosphate and/or citrate;
the wetting agent is a polyol;
the chelating agent is an aminocarboxylic acid compound and/or an organic phosphate.
2. The water-based magnetorheological polishing solution of claim 1, wherein the magnetic particles comprise one or more of unmodified carbonyl iron powder, phosphated carbonyl iron powder, reduced carbonyl iron powder, and coated carbonyl iron powder;
in the magnetic particlesMedian particle diameter D501 to 10 μm.
3. The water-based magnetorheological polishing solution according to claim 1, wherein the non-magnetic polishing powder comprises one or more of diamond powder, alumina powder and cerium oxide powder;
the median diameter D of the non-magnetic polishing powder5020nm to 3 mu m.
4. The water-based magnetorheological polishing solution according to claim 1, wherein the polyphosphate comprises one or more of sodium tripolyphosphate, sodium tetrapolyphosphate, ammonium polyphosphate, sodium pyrophosphate and sodium hexametaphosphate;
the citrate comprises one or more of potassium citrate, ammonium citrate and sodium citrate.
5. The water-based magnetorheological polishing fluid of claim 1, wherein the polyol comprises one or more of propylene glycol, glycerol, butylene glycol, sorbitol, polyglycerol, and polypropylene glycol.
6. The water-based magnetorheological polishing solution according to claim 1, wherein the aminocarboxylic acid compounds comprise ethylenediaminetetraacetate and/or nitrilotriacetic acid;
the organophosphate comprises pentasodium aminotrimethylene phosphonate and/or tetrasodium aminotrimethylene phosphonate.
7. The water-based magnetorheological polishing fluid of claim 1, wherein the antioxidant comprises sodium nitrite and/or sodium benzoate.
8. The water-based magnetorheological polishing solution of claim 1, wherein the pH adjusting agent comprises one or more of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, phosphoric acid, and hydrochloric acid.
9. A preparation method of the water-based magnetorheological polishing solution according to any one of claims 1 to 8, comprising the following steps:
mixing magnetic particles, non-magnetic polishing powder, a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant and a pH regulator in water to obtain the water-based magnetorheological polishing solution.
10. The formulation method according to claim 9, wherein the mixing process comprises in particular:
a) mixing a dispersion stabilizer, a wetting agent, a chelating agent, an antioxidant, a pH regulator and water to obtain a composite base carrier liquid; mixing the magnetic particles and the non-magnetic polishing powder to obtain a solid dispersion phase;
b) and rolling and stirring the composite base carrier liquid and the solid dispersion phase to obtain the water-based magnetorheological polishing solution.
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| WO2021135568A1 (en) * | 2019-12-30 | 2021-07-08 | 中国科学院长春光学精密机械与物理研究所 | Water-based magnetorheological polishing liquid and preparation method therefor |
| CN113930164A (en) * | 2021-10-11 | 2022-01-14 | 温州大学 | Polishing solution for titanium alloy polishing and preparation method and application thereof |
| CN114752306A (en) * | 2022-04-19 | 2022-07-15 | 长沙埃福思科技有限公司 | Ferromagnetic polishing solution for integrated display screen and preparation method thereof |
| CN114958208A (en) * | 2022-07-07 | 2022-08-30 | 中国科学院长春光学精密机械与物理研究所 | Super-smooth magnetorheological polishing solution and preparation method thereof |
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