CN109054651B - Preparation method of rare earth polishing powder - Google Patents
Preparation method of rare earth polishing powder Download PDFInfo
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- CN109054651B CN109054651B CN201811013520.0A CN201811013520A CN109054651B CN 109054651 B CN109054651 B CN 109054651B CN 201811013520 A CN201811013520 A CN 201811013520A CN 109054651 B CN109054651 B CN 109054651B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
The invention relates to a preparation method of rare earth polishing powder, belonging to the technical field of polishing and grinding. In the invention, rare earth nitrate solution and stearic acid generate stearic acid rare earth precipitate under the catalytic action of sodium hydroxide, and wax powder, fluoride, petroleum sulfonate, alcohol substances and other auxiliary additives are added, so that the prepared polishing powder has good thermal stability and can not scratch the surface of glass; a small amount of petroleum sulfonate is added into the polishing powder, and a protective film can be formed on the polished surface after polishing, so that the polished surface is prevented from being corroded by hand sweat; a small amount of fluoride is added into the polishing powder, so that the polished surface can emit micro blue light; the proper amount of alcohol substances are added into the polishing powder, so that the uniformity of the whole polishing powder can be ensured, the brightness of the polished surface can be improved, and the animal and vegetable waxes are added into the polishing powder as auxiliary components of the polishing powder, so that the greasiness and greasiness of the polishing powder can be enhanced, the brightness of the polished surface can be enhanced, and the polishing effect is good.
Description
Technical Field
The invention relates to a preparation method of rare earth polishing powder, belonging to the technical field of polishing and grinding.
Background
At present, glass cover plates of electronic products such as mobile phones, tablet computers, liquid crystal displays and the like need to realize surface flattening through a chemical mechanical polishing process, and meanwhile, the surface finish is improved. With the continuous upgrading of the quality of electronic products, particularly the wide application of ITO glass, the requirements on the planarization and the smoothness of the glass surface are gradually improved, which puts higher technical requirements on the polishing of the glass surface.
The industrial glass polishing integral device is mainly formed by combining a workpiece carrier, a platform for placing a polishing pad and a slurry feeder. When the glass material is subjected to chemical mechanical polishing, a workpiece is driven by a carrier to rotate, a pressure head is also used for rotating the polishing pad under the action of certain pressure, and polishing slurry consisting of abrasive and chemical solution flows between the workpiece and the polishing pad. At this time, chemical substances and abrasives in the slurry cause chemical reactions such as hydrolysis and corrosion with the surface of the workpiece, and thus an oxide film which is easily removed is formed on the surface of the workpiece. The film is then removed by the mechanical action of the abrasive and polishing pad in the slurry and flows away with the polishing slurry, leaving the workpiece exposed to a new surface. And thereafter undergoes chemical etching and mechanical action of the slurry, and is removed again. And circularly performing the chemical mechanical action of the polishing slurry on the workpiece to finish the chemical mechanical polishing of the workpiece. The polishing efficiency is mainly determined by the polishing activity and precision of the abrasive, and the cerium-rich rare earth polishing powder is the most widely applied polishing abrasive in the glass polishing process in the industry at present.
The polishing characteristics of the cerium-rich rare earth polishing powder on glass materials are mainly determined by the chemical activity of the cerium-rich rare earth polishing powder and the mechanical grinding action in the polishing process, the cerium oxide contained in the cerium-rich rare earth polishing powder prepared under proper synthesis conditions has high chemical polishing activity on silicon oxide, and meanwhile, the mixed rare earth oxide in the polishing powder, such as lanthanum cerium oxyfluoride, has higher particle hardness, so that the stability of the particle size of the polishing powder under the mechanical grinding action in the polishing process is ensured, and the cycle service life of the polishing powder is prolonged.
At present, the application performance of polishing powder in the market mainly focuses on how to improve the polishing rate, the common method is to improve the particle size of the polishing powder and improve the polishing rate by increasing the mechanical action in the polishing process, and the traditional method for producing the rare earth cerium-based polishing powder has the defects of easy agglomeration, large average particle size, wide particle size distribution, poor sphericity, high production cost and the like. Therefore, the application defects that scratches are easily caused on the glass surface in the polishing process, polishing powder is easily settled in the polishing process and the like exist.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that the prior polishing powder is easy to scratch the surface of glass in the polishing process and has poor polishing effect, the preparation method of the rare earth polishing powder is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
respectively weighing 20-26 parts of rare earth nitrate solution, 30-40 parts of stearic acid, 5-15 parts of wax powder, 1-6 parts of fluoride, 1-3 parts of petroleum sulfonate with the mass fraction of 0.1%, 1-3 parts of alcohol substances and 0.1-0.6 part of sodium hydroxide aqueous solution with the concentration of 1.0mol/L, stirring the stearic acid, the wax powder, the fluoride, the petroleum sulfonate with the mass fraction of 0.1%, the alcohol substances and the rare earth nitrate aqueous solution to obtain a composite emulsion, dropwise adding the sodium hydroxide aqueous solution with the concentration of 1.0mol/L at a constant speed, keeping the temperature at 50-60 ℃ for 20-30 min to obtain a suspension, filtering while hot to obtain filter residue, washing the filter residue with deionized water for 3-5 times to obtain washed filter residue, carrying out vacuum filtration on the washed filter residue, drying the filter residue at the temperature of 80-90 ℃ for 1-2 h to obtain dried filter residue, carrying out drying and calcining treatment, and naturally cooling to room temperature to obtain the rare earth polishing powder.
The rare earth nitrate solution is a lanthanum cerium nitrate solution, wherein the mass ratio of lanthanum to cerium is 1: 4.
The wax powder is any combination of paraffin wax powder, microcrystalline wax powder, carnauba wax powder, insect white wax powder and Japanese wood wax powder.
The fluoride is one of ammonium fluoride, sodium fluoride or potassium fluoride.
The alcohol substance is one of methanol, ethanol, benzyl alcohol and ethylene glycol.
The stirring treatment comprises the steps of melting stearic acid at the temperature of 65-75 ℃ to obtain emulsion, adding wax powder, fluoride, petroleum sulfonate with the mass fraction of 0.1% and alcohol substances, stirring at the rotating speed of 100-160 r/min for 20-30 min to obtain mixed emulsion, adding rare earth nitrate solution, and stirring at the temperature of 65-75 ℃ and the rotating speed of 80-100 r/min for 20-30 min.
The calcining treatment is to calcine for 1-3 hours in a resistance furnace at the temperature of 600-900 ℃.
Compared with other methods, the method has the beneficial technical effects that:
(1) according to the invention, rare earth nitrate solution and stearic acid generate stearic acid rare earth precipitate under the catalytic action of sodium hydroxide, and wax powder, fluoride, petroleum sulfonate, alcohols and other auxiliary additives are added, so that the prepared polishing powder has good thermal stability, does not cause scratches on the surface of glass, has good polishing effect and good chemical stability, and does not cause chemical reaction between the abrasive and the polished surface at a working temperature; stearic acid has good lubricity, is also a good brightening agent, has good chemical stability at normal temperature, and can form a layer of protective film on the polished surface after polishing by adding a small amount of petroleum sulfonate into the polishing powder to prevent the polished surface from being corroded by hand sweat; a small amount of fluoride is added into the polishing powder, and the fluoride generates chemical reaction on the polished surface in the polishing process, so that the polished surface can emit micro blue light; the proper amount of alcohol substances are added into the polishing powder, so that the uniformity of the whole polishing powder can be ensured, and the brightness of the polished surface can be improved;
(2) the addition of the fluoride in the invention leads the particles to be refined, reduces agglomeration and forms spherical small particles, and because the fluorine element is combined with lanthanum atoms which are dissolved in cerium dioxide crystal lattices, lanthanum is separated out in cerium dioxide crystal cells, and small particles are formed in crystal boundaries or sub-crystal boundaries, thus hindering the agglomeration of cerium oxide particles.
Detailed Description
Respectively weighing 20-26 parts of rare earth nitrate solution, 30-40 parts of stearic acid, 5-15 parts of wax powder, 1-6 parts of fluoride, 1-3 parts of petroleum sulfonate with the mass fraction of 0.1%, 1-3 parts of alcohol substances and 0.1-0.6 part of sodium hydroxide aqueous solution with the concentration of 1.0mol/L, melting stearic acid at the temperature of 65-75 ℃ to obtain emulsion, adding the wax powder, the fluoride, the petroleum sulfonate with the mass fraction of 0.1% and the alcohol substances, stirring at the rotating speed of 100-160 r/min for 20-30 min to obtain mixed emulsion, adding the rare earth nitrate solution, stirring at the temperature of 65-75 ℃ and the rotating speed of 80-100 r/min for 20-30 min at a constant speed to obtain composite emulsion, dropwise adding the sodium hydroxide aqueous solution with the concentration of 1.0mol/L, stirring at the temperature of 50-60 ℃ for 20-30 min to obtain suspension, filtering while the suspension is hot, and washing the filter residue with deionized water for 3-5 times to obtain washed filter residue, carrying out vacuum filtration on the washed filter residue, drying the filter residue for 1-2 hours at the temperature of 80-90 ℃ to obtain dried filter residue, calcining the dried filter residue in a resistance furnace at the temperature of 600-900 ℃ for 1-3 hours, and naturally cooling to room temperature to obtain the rare earth polishing powder.
Example 1
Respectively weighing 20 parts of rare earth nitrate solution, 30 parts of stearic acid, 5 parts of wax powder, 1 part of fluoride, 1 part of petroleum sulfonate with the mass fraction of 0.1%, 1 part of alcohol substance and 0.1 part of sodium hydroxide aqueous solution with the concentration of 1.0mol/L, melting the stearic acid at the temperature of 65 ℃ to obtain emulsion, adding the wax powder, the fluoride, the petroleum sulfonate with the mass fraction of 0.1% and the alcohol substance, stirring at the rotating speed of 100r/min for 20min to obtain mixed emulsion, adding the rare earth nitrate solution, stirring at the temperature of 65 ℃ and the rotating speed of 80r/min for 20min to obtain composite emulsion, dropwise adding the sodium hydroxide aqueous solution with the concentration of 1.0mol/L at a constant speed, keeping the temperature at 50 ℃ for 20min to obtain suspension, filtering while hot to obtain filter residue, washing the filter residue for 3 times by deionized water to obtain washed filter residue, vacuum-filtering the washed filter residue, drying at the temperature of 80 ℃ for 1h, and (3) obtaining dried filter residue, calcining the dried filter residue in a resistance furnace at the temperature of 600 ℃ for 1h, and naturally cooling to room temperature to obtain the rare earth polishing powder.
Example 2
Weighing 23 parts of rare earth nitrate solution, 35 parts of stearic acid, 10 parts of wax powder, 3 parts of fluoride, 2 parts of petroleum sulfonate with the mass fraction of 0.1%, 2 parts of alcohol substances and 0.3 part of sodium hydroxide aqueous solution with the concentration of 1.0mol/L respectively, melting the stearic acid at the temperature of 70 ℃ to obtain emulsion, adding the wax powder, the fluoride, the petroleum sulfonate with the mass fraction of 0.1% and the alcohol substances, stirring at the rotating speed of 130r/min for 25min to obtain mixed emulsion, adding the rare earth nitrate solution, stirring at the temperature of 70 ℃ and the rotating speed of 90r/min for 25min to obtain composite emulsion, dropwise adding the sodium hydroxide aqueous solution with the concentration of 1.0mol/L at a constant speed, keeping the temperature of 55 ℃ for 25min to obtain suspension, filtering while hot to obtain filter residue, washing the filter residue for 4 times by deionized water to obtain filter residue after washing, vacuum-filtering the filter residue after washing, and drying at the temperature of 85 ℃ for 1.5h, and (3) obtaining dried filter residue, calcining the dried filter residue in a resistance furnace at the temperature of 750 ℃ for 2h, and naturally cooling to room temperature to obtain the rare earth polishing powder.
Example 3
Respectively weighing 26 parts of rare earth nitrate solution, 40 parts of stearic acid, 15 parts of wax powder, 6 parts of fluoride, 3 parts of petroleum sulfonate with the mass fraction of 0.1%, 3 parts of alcohol substances and 0.6 part of sodium hydroxide aqueous solution with the concentration of 1.0mol/L, melting the stearic acid at the temperature of 75 ℃ to obtain emulsion, adding the wax powder, the fluoride, the petroleum sulfonate with the mass fraction of 0.1% and the alcohol substances, stirring at the rotating speed of 160r/min for 30min to obtain mixed emulsion, adding the rare earth nitrate solution, stirring at the temperature of 75 ℃ and the rotating speed of 100r/min for 30min to obtain composite emulsion, dropwise adding the sodium hydroxide aqueous solution with the concentration of 1.0mol/L at a constant speed, keeping the temperature at 60 ℃ for 30min to obtain suspension, filtering while hot to obtain filter residue, washing the filter residue for 5 times by deionized water to obtain the filter residue after washing, vacuum-filtering the filter residue after washing, and drying at the temperature of 90 ℃ for 2h, and (3) obtaining dried filter residue, calcining the dried filter residue in a resistance furnace at the temperature of 900 ℃ for 3h, and naturally cooling to room temperature to obtain the rare earth polishing powder.
The rare earth polishing powder prepared by the invention and the commercially available polishing powder are detected, and the specific detection results are shown in the following table 1:
the detection method comprises the following steps:
all polishing powders are subjected to performance comparison under the same condition, 3 kilograms of polishing powder is added into 30L of water, stirred for 10 minutes, and filtered by a 200-mesh sieve, and then a polishing experiment is carried out on a mobile phone glass polishing production line in a certain factory in China. The model of the polishing machine station is 16B, the polishing glass is 5 inches of Corning GG4, the rotating speed is 200rpm, and the polishing time is 30 min. And (3) taking 101 th to 600 th polished 100 glass sheets of each sample, and comparing the cutting thickness, the scratching condition, the cleaning degree and the service life, wherein specific detection results are shown in table 1.
The cut thickness is the mean of the changes in glass thickness before and after polishing.
The yield is the surface quality, and the scratch is classified as bad. Namely, the yield of 500 pieces of glass in each group is detected and compared.
The cleaning is that the percent of defective rate detected after frequent ultrasonic cleaning accounts for 500 pieces of glass in each group.
The service life is the condition that the granularity of the polishing powder sample is reduced before and after the polishing experiment.
TABLE 1 characterization of rare earth polishing powder properties
As can be seen from Table 1, the rare earth polishing powder prepared by the method has the advantages of large cutting thickness, higher yield and improved polishing efficiency. Has wide market value and application prospect.
Claims (7)
1. A preparation method of rare earth polishing powder is characterized by comprising the following specific steps:
respectively weighing 20-26 parts of rare earth nitrate solution, 30-40 parts of stearic acid, 5-15 parts of wax powder, 1-6 parts of fluoride, 1-3 parts of petroleum sulfonate with the mass fraction of 0.1%, 1-3 parts of alcohol substances and 0.1-0.6 part of sodium hydroxide aqueous solution with the concentration of 1.0mol/L, stirring the stearic acid, the wax powder, the fluoride, the petroleum sulfonate with the mass fraction of 0.1%, the alcohol substances and the rare earth nitrate aqueous solution to obtain a composite emulsion, dropwise adding the sodium hydroxide aqueous solution with the concentration of 1.0mol/L at a constant speed, keeping the temperature at 50-60 ℃ for 20-30 min to obtain a suspension, filtering while hot to obtain filter residue, washing the filter residue with deionized water for 3-5 times to obtain washed filter residue, carrying out vacuum filtration on the washed filter residue, drying the filter residue at the temperature of 80-90 ℃ for 1-2 h to obtain dried filter residue, carrying out drying and calcining treatment, and naturally cooling to room temperature to obtain the rare earth polishing powder.
2. The method according to claim 1, wherein the rare earth nitrate solution is a lanthanum cerium nitrate solution, wherein the mass ratio of lanthanum to cerium is 1: 4.
3. The method of claim 1, wherein the wax powder is any combination of paraffin powder, microcrystalline wax powder, carnauba wax powder, insect white wax powder, and japanese wood wax powder.
4. The method according to claim 1, wherein the fluoride is one of ammonium fluoride, sodium fluoride and potassium fluoride.
5. The method according to claim 1, wherein the alcohol is one of methanol, ethanol, benzyl alcohol and ethylene glycol.
6. The method for preparing a rare earth polishing powder according to claim 1, wherein the stirring treatment comprises melting stearic acid at a temperature of 65 to 75 ℃ to obtain an emulsion, adding wax powder, fluoride, 0.1% by mass of petroleum sulfonate and alcohol, stirring at a rotation speed of 100 to 160r/min for 20 to 30min to obtain a mixed emulsion, adding a rare earth nitrate solution, and stirring at a temperature of 65 to 75 ℃ and a rotation speed of 80 to 100r/min for 20 to 30 min.
7. The method according to claim 1, wherein the calcination is carried out in a resistance furnace at 600 to 900 ℃ for 1 to 3 hours.
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| SU920060A1 (en) * | 1980-06-13 | 1982-04-15 | Предприятие П/Я Р-6670 | Method of producing polishing powder |
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| CN105505226A (en) * | 2015-12-02 | 2016-04-20 | 包头市新源抛光粉有限公司 | Rare earth polishing powder and preparation method thereof |
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| SU920060A1 (en) * | 1980-06-13 | 1982-04-15 | Предприятие П/Я Р-6670 | Method of producing polishing powder |
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