CN113563803A - Polishing solution containing alumina-boron carbide hybrid particles and preparation method thereof - Google Patents
Polishing solution containing alumina-boron carbide hybrid particles and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of polishing solution containing alumina-boron carbide hybrid particles, which comprises the following steps: s01: carrying out ultrasonic treatment on hexagonal boron carbide powder in deionized water by using an ultrasonic instrument to form boron carbide nanosheet dispersion liquid; s02: adding the boron carbide nanosheet dispersion into an aqueous suspension of alumina under stirring, adding 1 wt.% of polyethylene glycol (PEG) -400 after stirring, continuing to stir the mixed solution, and then performing ultrasonic dispersion, wherein the PEG-400 serves as a bridge between the boron carbide nanosheets and the alumina under the ultrasonic action, so that the alumina is directionally adsorbed on the boron carbide nanosheets to form an adsorption dispersion; s03: adding 3 wt.% of pH regulator into the adsorption dispersion liquid to obtain the polishing liquid containing the alumina-boron carbide hybrid particles. The invention can reduce alpha-Al2O3The agglomeration of the particles reduces the surface roughness of the polished workpiece; and can improve alpha-Al2O3Effective frictional contact between the particles and the sample surface, so that the polishing rate is greatly improvedHigh.
Description
Technical Field
The invention belongs to the field of zirconia ceramic polishing, and particularly relates to an alumina polishing solution for polishing a zirconia ceramic cover plate of a mobile phone and a preparation method thereof.
Technical Field
The application of the fifth generation mobile communication technology (5G) announces the arrival of the new era of mobile communication. The 5G network brings a revolution of the design of the mobile phone while increasing the technical requirements on the mobile phone communication. In several types of commonly used backplane materials, the hard defect of the metal material is that metal has an obvious shielding effect on millimeter waves, and the metal has conductivity, which brings difficulty to wireless charging of a mobile phone. The weaknesses of plastics and composite plastics are that they have poor wear resistance and heat dissipation properties, and that the aesthetic properties (especially hand and texture) are difficult to compare with other materials. Generally, glass has better comprehensive performance, but the falling resistance is required to be improved, and the heat dissipation performance is general. The tetragonal zirconia ceramics is a backboard material with great development prospect. The use of zirconia ceramics as a handset backplate requires an ultra-smooth surface and a high degree of flatness. However, zirconia ceramics have the characteristics of high hardness, high brittleness, high toughness, corrosion resistance and the like, and therefore, it is extremely difficult to perform ultra-precision machining on the surface.
Currently, inorganic particles such as cerium oxide, silicon oxide, aluminum oxide, and nanodiamond are generally used as the abrasive particles. Alumina has been widely used for surface polishing of devices such as integrated circuits, glass substrates, sapphire substrates, alloys, and ceramics by virtue of its advantages of high hardness, good stability, and the like. However, alumina is not well dispersed and tends to agglomerate, and the agglomeration of alumina in a polishing material is considered to be one of the sources of generation of polishing scratches. If the agglomeration of the alumina can be effectively reduced, the method is favorable for improving the material removal rate and the popularization and application of the alumina polishing solution.
Patent CN106147616A provides a preparation method of a solvent-based surface modified alumina polishing solution, which is based on the principle that-OH on the surface of alumina particles and acid in a modifier form covalent bonds and intermolecular forces with certain stability, thereby reducing agglomeration and improving dispersion stability. Patent CN106010297A provides a preparation method of silane coupling agent coated modified alumina, and the modified alumina polishing solution can achieve the polishing efficiency of the conventional unmodified alumina polishing solution at pH of 13 with less scratches when the pH is 9.5-10.5.
Although the polishing solution solves the problem that alumina is easy to agglomerate and precipitate to a certain extent, the alumina surface modification layer has the possibility of falling off under the impact of huge pressure in the polishing process, so that particles are agglomerated again and precipitated.
In order to overcome the defects in the prior art, the application provides a preparation method and application of a high-performance alumina-boron carbide hybrid particle polishing solution for polishing zirconia ceramics.
Disclosure of Invention
The invention aims to provide an alumina-boron carbide hybrid particle polishing solution and a preparation method thereof. The invention also aims to provide application of the alumina polishing solution in polishing of zirconia ceramics.
The invention adopts the following specific scheme for solving the technical problems: a method for preparing polishing solution containing alumina-boron carbide hybrid particles comprises the following steps:
s01: ultrasonic treatment is carried out on hexagonal boron carbide powder in deionized water by using an ultrasonic instrument, and the boron carbide powder is stripped into single-layer sheets and dispersed in the deionized water to form boron carbide nanosheet dispersion liquid;
s02: adding the boron carbide nanosheet dispersion into an aqueous suspension of alumina under stirring, adding 1 wt.% of polyethylene glycol (PEG) -400 after stirring, continuing to stir the mixed solution, and then performing ultrasonic dispersion, wherein the PEG-400 serves as a bridge between the boron carbide nanosheets and the alumina under the ultrasonic action, so that the alumina is directionally adsorbed on the boron carbide nanosheets to form an adsorption dispersion;
s03: adding 3 wt.% of pH regulator into the adsorption dispersion liquid, and regulating the pH of the solution to 10-12 to obtain the polishing liquid containing the alumina-boron carbide hybrid particles.
Further, the alumina in the step S02 is alpha-Al2O3The particle size of the aluminum oxide is 50-300 nm, and the mass concentration of the aluminum oxide is 3-10 wt.%.
Further, in the step S02, the mass ratio of the boron carbide nanosheets to the alumina is 1-3: 10.
further, in step S03, the pH adjusting agent is any one of sodium hydroxide, potassium hydroxide, sodium silicate, and triethanolamine.
Further, the particle size of the hexagonal boron carbide in step S01 is 2 μm.
Further, the polishing solution prepared by the method is included.
Compared with the prior art, the aluminum oxide-boron carbide hybrid particle polishing solution provided by the invention comprises hexagonal boron carbide (h-BN) nanosheets and alpha-Al2O3Due to the interaction generated by PEG induced hydrogen bonds between particles, the addition of the boron nitride nanosheet with the two-dimensional layered structure can improve alpha-Al2O3The stability and dispersibility of the abrasive can be reduced by reducing alpha-Al2O3The particles are agglomerated, so that the polishing precision is improved; on the other hand, the h-BN nanosheets can carry alpha-Al2O3The particles form directional arrangement in the slurry, and can promote alpha-Al2O3Effective frictional contact between particles and surface of polished workpiece, alpha-Al2O3The polishing efficiency of the abrasive is greatly improved.
Drawings
FIG. 1 is a schematic diagram of an alumina-boron carbide nanosheet hybrid particle structure;
reference numerals: 1 aluminum oxide, 2 boron carbide nanosheets.
Detailed Description
The aluminum oxide-boron carbide hybrid particle provided by the invention is a compound of a boron nitride nanosheet with the particle size of 50-300 nm and the particle size of 2 mu m, and the aluminum oxide is alpha-Al2O3The boron carbide nanosheets are hexagonal boron carbide powder (h-BN), h-BN and alpha-Al2O3The mass ratio of (A) to (B) is 1-3: 10. as shown in the attached figure 1, is a schematic structural diagram of the alumina-boron carbide nanosheet hybrid particle of the present invention.
The polishing solution containing alumina-boron carbide hybrid particles consists of alumina-boron carbide hybrid particles, a pH regulator, medium water and the like. The pH regulator is any one of sodium hydroxide, potassium hydroxide, sodium silicate, triethanolamine and the like.
A method for preparing polishing solution containing alumina-boron carbide hybrid particles comprises the following detailed preparation processes:
s01: and (3) ultrasonically treating the h-BN with the particle size of 2 microns in deionized water for 8 hours by using a 450W ultrasonic instrument, and stripping the h-BN powder into a single-layer sheet structure and dispersing the single-layer sheet structure in the deionized water.
S02: adding the boron carbide nanosheet dispersion prepared in the step S01 to alpha-Al under stirring2O3After stirring for 30 minutes, adding 1 wt.% of polyethylene glycol-400, continuing stirring the mixed solution for 30 minutes, and then performing ultrasonic dispersion for 0.5 hour, wherein the PEG400 serves as h-BN nano-sheets and alpha-Al under the action of ultrasonic waves2O3Bridge of alpha-Al between2O3Directionally adsorbing the nano-particles on the h-BN nano-sheets. Wherein the alumina is alpha-Al2O3The particle size is 30-300 nm, and the mass concentration of aluminum oxide is 3-10 wt.%; h-BN with alpha-Al2O3The mass ratio of (A) to (B) is 1-3: 10.
s03: and adding 3 wt.% of pH regulator into the dispersion liquid obtained in the step S02, and regulating the pH of the solution to 10-12 to obtain the high-performance alumina-boron carbide hybrid particle polishing liquid. The pH regulator is any one of sodium hydroxide, potassium hydroxide, sodium silicate, triethanolamine and the like.
The following is further explained and illustrated by means of specific examples:
example 1
Adding 3g of h-BN powder with the particle size of 2 mu m into 500mL of deionized water, and ultrasonically stripping for 8h to obtain h-BN dispersion liquid; weighing 15g of alumina powder with the particle size of 250nm, adding the alumina powder into the h-BN dispersion liquid under continuous stirring, stirring for 30 minutes, adding 5g of polyethylene glycol-400, stirring and dispersing for 0.5 hour, and then carrying out ultrasonic treatment for 0.5 hour; adjusting the pH value to 12 by using 3 wt.% sodium hydroxide solution to prepare h-BN and alpha-Al2O3The mass ratio is 2: 10. 500mL of polishing solution with an alumina concentration of 3 wt.%.
Example 2
Adding 4.5g of h-BN powder with the particle size of 2 mu m into 500mL of deionized water, and ultrasonically stripping for 8 h; weighing 15g of alumina powder with the particle size of 50nm, addingAdding 5g of polyethylene glycol-400 into the h-BN dispersion liquid, stirring and dispersing for 0.5h, performing ultrasonic treatment for 0.5h, adjusting the pH to 11 by using 3 wt.% sodium silicate solution, and preparing to obtain h-BN and alpha-Al2O3The mass ratio is 3: 10. 500mL of polishing solution with an alumina concentration of 3 wt.%.
Example 3
Adding 4g of h-BN powder with the particle size of 2 mu m into 500mL of deionized water, ultrasonically stripping for 8h, weighing 30g of alumina powder with the particle size of 50nm, adding the alumina powder into h-BN dispersion liquid, adding 5g of polyethylene glycol-400, ultrasonically stirring and dispersing for 0.5h, adjusting the pH to 12 by using 3 wt.% sodium silicate solution, and preparing to obtain h-BN and alpha-Al2O3The mass ratio is 1.3: 10. 500mL of polishing solution with an alumina concentration of 6 wt.%.
Example 4
Adding 2g of h-BN powder with the particle size of 2 mu m into 500mL of deionized water, ultrasonically stripping for 8h, weighing 15g of alumina powder with the particle size of 150nm, adding the alumina powder into h-BN dispersion, adding 5g of polyethylene glycol-400, ultrasonically stirring and dispersing for 0.5h, adjusting the pH to 11 by using 3 wt.% sodium silicate solution, and preparing to obtain h-BN and alpha-Al2O3The mass ratio is 1.3: 10. 500mL of polishing solution with an alumina concentration of 3 wt.%.
Example 5
Adding 2g of h-BN powder with the particle size of 2 mu m into 500mL of deionized water, ultrasonically stripping for 8h, weighing 15g of alumina powder with the particle size of 250nm, adding the alumina powder into h-BN dispersion liquid, adding 5g of polyethylene glycol-400, ultrasonically stirring and dispersing for 0.5h, adjusting the pH to 12 by using 3 wt.% of potassium hydroxide solution, and preparing to obtain h-BN and alpha-Al2O3The mass ratio is 1.3: 10. 500mL of polishing solution with an alumina concentration of 3 wt.%.
Example 6
Adding 5g of h-BN powder with the particle size of 2 mu m into 500mL of deionized water, ultrasonically stripping for 8h, weighing 50g of alumina powder with the particle size of 300nm, adding the alumina powder into h-BN dispersion liquid, adding 5g of polyethylene glycol-400, ultrasonically stirring and dispersing for 0.5h, adjusting the pH to 10 by using 3 wt.% of triethanolamine, and preparing to obtain h-BN and alpha-Al2O3The mass ratio is 1: 10. 500mL of polishing solution with an alumina concentration of 10 wt.%.
Comparative example 1
In 500mL of deionized water, 15g of alumina powder with the particle size of 250nm is weighed, 5g of polyethylene glycol-400 is added, the mixture is stirred and dispersed for 0.5h, ultrasonic treatment is carried out for 0.5h, 3 wt.% KOH solution is used for adjusting the pH value to 12, and 500mL of polishing solution with the alumina concentration of 3 wt.% is prepared.
Comparative example 2
In 500mL of deionized water, 50g of alumina powder with the particle size of 300nm is weighed, 5g of polyethylene glycol-400 is added, the mixture is stirred and dispersed for 0.5h, ultrasonic treatment is carried out for 0.5h, 3 wt.% sodium silicate solution is used for adjusting the pH value to 12, and 500mL of polishing solution with the alumina concentration of 10 wt.% is prepared.
Comparative example 3
In 500mL of deionized water, 30g of alumina powder with the particle size of 50nm is weighed, 5g of polyethylene glycol-400 is added, stirring and dispersing are carried out for 0.5h, ultrasonic treatment is carried out for 0.5h, 3 wt.% of triethanolamine is used for adjusting the pH value to 10, and 500mL of polishing solution with the alumina concentration of 6 wt.% is prepared.
Polishing test: the alumina polishing solution prepared in each of the above examples was used to perform a polishing test on a zirconia ceramic wafer under a certain polishing condition. The polishing conditions were as follows:
polishing machine: UNIPOL-1000S single-side polishing machine
Workpiece: zirconia ceramic plate with side length of 55 x 55mm
Polishing the pad: polyurethane material, RODEL production
Polishing pressure: 6 kg
Rotational speed of carrier plate (upper plate): 30rpm
Grinding and polishing disc (lower disc) rotating speed: 60rpm
Polishing time: 120 minutes
After polishing, cleaning and drying were carried out, and then the surface topography of the ceramic sheet was measured, and the surface average roughness (Ra) was measured with an Ambios XI-100 surface topography apparatus with a resolution of
The test range was 100. mu. m.times.100. mu.m. The weight of the ceramic wafer is weighed by an analytical balance, and the difference between the weight before and after polishing is divided by the polishing time to obtain the polishing rate.
The polishing effects of the polishing solutions of the examples are shown in Table 1. It can be seen that the polishing solutions containing the alumina-boron carbide nanosheet hybrid particles (examples 1, 2, 3, 4, 5, 6) improved the polishing rate and reduced the roughness of the surface of the zirconia ceramic sheet after polishing the zirconia ceramic sheet compared to each comparative example having the same alumina concentration.
TABLE 1 polishing effect of polishing solution of each example on zirconia ceramic sheet
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the structure of the present invention in any way. Any simple modification or modification of the above embodiments according to the technical spirit of the present invention should fall within the technical scope of the present invention.
Claims (6)
1. The preparation method of the polishing solution containing the alumina-boron carbide hybrid particles is characterized by comprising the following steps:
s01: ultrasonic treatment is carried out on hexagonal boron carbide powder in deionized water by using an ultrasonic instrument, and the boron carbide powder is stripped into single-layer sheets and dispersed in the deionized water to form boron carbide nanosheet dispersion liquid;
s02: adding the boron carbide nanosheet dispersion into an aqueous suspension of alumina under stirring, adding 1 wt.% of polyethylene glycol (PEG) -400 after stirring, continuing to stir the mixed solution, and then performing ultrasonic dispersion, wherein the PEG-400 serves as a bridge between the boron carbide nanosheets and the alumina under the ultrasonic action, so that the alumina is directionally adsorbed on the boron carbide nanosheets to form an adsorption dispersion;
s03: adding 3 wt.% of pH regulator into the adsorption dispersion liquid, and regulating the pH of the solution to 10-12 to obtain the polishing liquid containing the alumina-boron carbide hybrid particles.
2. The method of claim 1, wherein the method comprisesCharacterized in that the alumina in the step S02 is alpha-Al2O3The particle size of the aluminum oxide is 50-300 nm, and the mass concentration of the aluminum oxide is 3-10 wt.%.
3. The method of claim 1, wherein: in the step S02, the mass ratio of the boron carbide nanosheet to the alumina is 1-3: 10.
4. the method of claim 1, wherein: the pH adjusting agent in step S03 is any one of sodium hydroxide, potassium hydroxide, sodium silicate, and triethanolamine.
5. The method of claim 1, wherein: the particle size of the hexagonal boron carbide in the step S01 is 2 μm.
6. A polishing liquid containing alumina-boron carbide hybrid particles, comprising the polishing liquid obtained by the method according to any one of claims 1 to 5.
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