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CN114213977A - Polishing agent and preparation method thereof - Google Patents

Polishing agent and preparation method thereof Download PDF

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Publication number
CN114213977A
CN114213977A CN202111590559.0A CN202111590559A CN114213977A CN 114213977 A CN114213977 A CN 114213977A CN 202111590559 A CN202111590559 A CN 202111590559A CN 114213977 A CN114213977 A CN 114213977A
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China
Prior art keywords
particle size
cerium oxide
size range
polishing agent
less
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CN202111590559.0A
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Chinese (zh)
Inventor
丁杰
薛钦
钱宜刚
汤明明
陈�峰
顾登峰
马俊逸
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Zhongtian Technology Advanced Materials Co ltd
Jiangsu Zhongtian Technology Co Ltd
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Zhongtian Technology Advanced Materials Co ltd
Jiangsu Zhongtian Technology Co Ltd
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Priority to CN202111590559.0A priority Critical patent/CN114213977A/en
Publication of CN114213977A publication Critical patent/CN114213977A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The present application provides a polishing agent and a method of making the same. The polishing agent comprises granular cerium oxide and aluminum oxide, wherein the grain size of the granular cerium oxide is at least distributed in a first grain size range and a second grain size range, the first grain size range is 1000-2000 nm, the second grain size range is 2000-3000 nm, the amount of the cerium oxide distributed in the first grain size range accounts for at least 85% of the total amount of the cerium oxide, and the amount of the cerium oxide distributed in the second grain size range accounts for less than 5% of the total amount of the cerium oxide.

Description

Polishing agent and preparation method thereof
Technical Field
The application relates to the field of material chemical industry, in particular to a polishing agent and a preparation method thereof.
Background
The high-purity quartz glass is applied to a plurality of fields such as optics, laser, aerospace and the like, and is an extremely important basic material in the scientific and technological field. In the cold working process of the conventionally manufactured quartz glass, high requirements are put on the physical parameters of the quartz glass product, particularly the surface quality, the surface roughness and the like of the quartz glass. In order to obtain quartz glass having a good surface roughness, it is generally necessary to polish the quartz glass. The existing quartz glass polishing agent needs to be improved in components by introducing cerium oxide into a polishing agent so as to achieve a better polishing effect. However, rare earth raw materials are now very important strategic resources, are non-renewable, and it is necessary to consider how to reduce the amount of cerium oxide rare earth used and improve the glass polishing efficiency.
Moreover, the existing polishing agent still has the problems that a microscopic surface similar to a pit appears on the surface in the grinding process or the polishing efficiency is low. How to solve the above problems needs to be considered by those skilled in the art.
Disclosure of Invention
In order to solve the problems of the prior art, the present application provides a polishing agent and a method for preparing the same.
The embodiment of the application provides a polishing agent, which comprises granular cerium oxide and aluminum oxide, wherein the granular cerium oxide has particle sizes distributed in at least a first particle size range and a second particle size range, the first particle size range is 1300-2000 nm, the second particle size range is 2000-3000 nm, the amount of the cerium oxide distributed in the first particle size range accounts for at least 85% of the total amount of the cerium oxide, and the amount of the cerium oxide distributed in the second particle size range accounts for less than 5% of the total amount of the cerium oxide.
In one embodiment, the particle size of the particulate cerium oxide is further distributed in a third particle size range, the third particle size range is less than 1000 nanometers, and the amount of the cerium oxide distributed in the third particle size range accounts for less than 10% of the total amount of the polishing agent.
In one embodiment, the particle size range of the granular alumina is at least distributed in a fourth particle size range and a fifth particle size range, the fourth particle size range is 500-1500 nm, the fifth particle size range is 1500-2500 nm, the amount of the alumina distributed in the fourth particle size range accounts for at least 82% of the total amount of the alumina, and the amount of the alumina distributed in the fifth particle size range accounts for less than 8% of the total amount of the alumina.
In one embodiment, the particle size of the granular alumina is further distributed in a sixth particle size range, the sixth particle size range is less than 500 nanometers, and the amount of the cerium oxide distributed in the third particle size range accounts for less than 10% of the total amount of the cerium oxide.
In one embodiment, the maximum acute angle of the tip on the particulate alumina is less than or equal to 45 °, and the maximum acute angle of the tip on the particulate ceria is less than or equal to 30 °.
In one embodiment, the weight of cerium oxide in the polishing agent per unit weight is 10 to 30%, and the weight of aluminum oxide in the polishing agent per unit weight is 10 to 30%.
In one embodiment, the weight ratio of the cerium oxide to the aluminum oxide is (2-3): (0.5 to 1).
In one embodiment, the polishing agent further comprises 5 to 20% of a sodium phosphate salt, 8 to 12% of a polyether siloxane compound, 8 to 12% of a polyurethane compound, 25 to 35% of a polyol compound, and 2 to 8% of sodium chloride.
In one embodiment, the polishing agent has a water drop angle in the horizontal plane in the range of 12 ° to 15 °.
The embodiment of the application also provides a preparation method of the polishing agent, which is used for preparing the polishing agent, and comprises the following steps:
mixing the cerium oxide and the aluminum oxide in deionized water according to the ratio of 2:1, and stirring to obtain a first mixed solution;
continuously adding at least one of a sodium phosphate salt, a polyether siloxane compound, a polyurethane compound, a polyol compound and sodium chloride into the first mixed solution to obtain a second mixed solution;
heating the second mixed solution to 50 to 75 ℃ for 0.5 to 3 hours to obtain the polishing agent.
Compared with the prior art, the polishing agent and the preparation method thereof are disclosed. By mixing cerium oxide and aluminum oxide into the polishing agent, the use of cerium oxide can be reduced under the condition of ensuring a certain polishing effect, and the consumption of rare earth elements is further reduced. The polishing agent disclosed by the application has the advantages that the particle sizes and the proportions of cerium oxide and aluminum oxide are limited, so that the particle sizes of the granular cerium oxide are at least distributed in a first particle size range and a second particle size range, wherein the first particle size range is 1300-2000 nanometers, the cerium oxide distributed in the first particle size range accounts for at least 85% of the total amount of the cerium oxide, and the roughness of a ground finished product can be reduced under the particle sizes and proportions; the second particle size range is 2000 to 3000 nanometers, the amount of the cerium oxide distributed in the second particle size range accounts for less than 5 percent of the total amount of the cerium oxide, and under the particle size and proportion, the efficiency of grinding finished products can be increased; meanwhile, the polishing agent with the particle size and the proportion has extremely high removal efficiency.
Drawings
Fig. 1 is a schematic flow chart of a method for producing a polishing agent according to an example of the present application. The following detailed description will further illustrate the present application in conjunction with the above-described figures.
Detailed Description
The following description will refer to the accompanying drawings to more fully describe the present disclosure. There is shown in the drawings exemplary embodiments of the present application. This application may, however, be embodied in many different forms and should not be construed as limited to the exemplary embodiments set forth herein. These exemplary embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. Like reference numerals designate identical or similar components.
The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting of the application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. Further, as used herein, "comprises" and/or "comprising" and/or "having," integers, steps, operations, components, and/or components, but does not preclude the presence or addition of one or more other features, regions, integers, steps, operations, components, and/or groups thereof.
Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Furthermore, unless otherwise defined herein, terms such as those defined in commonly used dictionaries should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present application and will not be interpreted in an idealized or overly formal sense.
The following description of exemplary embodiments refers to the accompanying drawings. It should be noted that the components depicted in the referenced drawings are not necessarily shown to scale; and the same or similar components will be given the same or similar reference numerals or similar terms.
Embodiments of the present application will now be described in further detail with reference to the accompanying drawings.
The embodiment of the application provides a polishing agent, which comprises granular cerium oxide and aluminum oxide, wherein the grain size of the granular cerium oxide is at least distributed in a first grain size range and a second grain size range, wherein the first grain size range is 1300-2000 nm, the amount of the granular cerium oxide distributed in the first grain size range accounts for at least 85% of the total amount of the cerium oxide, the second grain size range is 2000-3000 nm, the amount of the granular cerium oxide distributed in the second grain size range accounts for less than 5% of the total amount of the cerium oxide, the grain size of the granular cerium oxide is also distributed in a third grain size range, the third grain size range is less than 1000 nm, and the amount of the granular cerium oxide distributed in the third grain size range accounts for less than 10% of the total amount of the cerium oxide.
Furthermore, by mixing cerium oxide and aluminum oxide into the polishing agent, the use of cerium oxide can be reduced under the condition of ensuring a certain polishing effect, and the consumption of rare earth elements is further reduced. The polishing agent disclosed by the application has the advantages that the particle sizes and the proportions of cerium oxide and aluminum oxide are limited, so that the particle sizes of the granular cerium oxide are at least distributed in a first particle size range and a second particle size range, wherein the first particle size range is 1300-2000 nanometers, the cerium oxide distributed in the first particle size range accounts for at least 85% of the total amount of the cerium oxide, and the roughness of a ground finished product can be reduced under the particle sizes and proportions; the second particle size range is 2000 to 3000 nanometers, the amount of the cerium oxide distributed in the second particle size range accounts for less than 5 percent of the total amount of the cerium oxide, and under the particle size and proportion, the efficiency of grinding finished products can be increased; meanwhile, the polishing agent with the particle size and the proportion has extremely high removal efficiency.
Further, the particle size of the granular cerium oxide is also distributed in a third particle size range, the third particle size range is less than 1000 nanometers, the amount of the cerium oxide distributed in the third particle size range accounts for less than 10 percent of the total amount of the cerium oxide, the use cost of the polishing agent can be reduced under the particle size and proportion, and the finished product obtained after polishing has better surface quality.
In one embodiment, the first particle size range of the cerium oxide may further be 1300 to 1400 nm, 1400 to 1500 nm, 1500 to 1600 nm, 1600 to 1700 nm, 1700 to 1800 nm, 1800 to 1900 nm, 1900 to 2000 nm. At this particle size and ratio, the efficiency of grinding the finished product can be increased and the polishing agent can be removed with a higher efficiency.
In one embodiment, the second particle size range of the cerium oxide may be further 2000 to 2100 nm, 2100 to 2200 nm, 2200 to 2300 nm, 2300 to 2400 nm, 2400 to 2500 nm, 2500 to 2600 nm, 2600 to 2700 nm, 2700 to 2800 nm, 2800 to 2900 nm, 2900 to 3000 nm. With this particle size and ratio, the roughness of the finished product can be reduced and the polishing agent can be removed with high efficiency.
In one embodiment, the third particle size range of the cerium oxide may be further 1300 to 1000 nm, 1000 to 700 nm, 700 to 600 nm, 600 to 500 nm, 500 to 400 nm, 400 to 300 nm. Under the condition of the particle size and the proportion, the use cost of the polishing agent can be reduced, and the finished product obtained after polishing has better surface quality.
In one embodiment, the particle size range of the granular alumina is at least distributed in a fourth particle size range and a fifth particle size range, the fourth particle size range is 500-1500 nm, the fifth particle size range is 1500-2500 nm, the amount of the alumina distributed in the fourth particle size range accounts for at least 82% of the total amount of the alumina, and the amount of the alumina distributed in the fifth particle size range accounts for less than 8% of the total amount of the alumina.
In one embodiment, the particle size of the granular alumina is further distributed in a sixth particle size range, the sixth particle size range is less than 500 nanometers, and the amount of the cerium oxide distributed in the third particle size range accounts for less than 10% of the total amount of the cerium oxide.
Furthermore, the particle size and the proportion of the alumina in the polishing agent are distributed in the range, so that the polishing effect of the polishing agent can be improved, and better surface quality can be obtained.
In one embodiment, the fourth particle size range of the aluminum oxide may be further 500 to 600 nm, 600 to 700 nm, 700 to 800 nm, 800 to 900 nm, 900 to 1000 nm, 1000 to 1100 nm, 1100 to 1200 nm, 1200 to 1300 nm, 1300 to 1400 nm, 1400 to 1500 nm.
In an embodiment, the fifth particle size range of the aluminum oxide may further be 1500 to 1600 nm, 1600 to 1700 nm, 1700 to 1800 nm, 1800 to 1900 nm, 1900 to 200 nm, 2000 to 2100 nm, 2100 to 2200 nm, 2200 to 2300 nm, 2300 to 2400 nm, 2400 to 2500 nm.
In an embodiment, the sixth particle size range of the aluminum oxide may further be 500 to 400 nm, 400 to 300 nm, 300 to 200 nm, 200 to 100 nm.
In one embodiment, the maximum acute angle of the tip on the particulate alumina is less than or equal to 45 °, and the maximum acute angle of the tip on the particulate ceria is less than or equal to 30 °. By controlling the angles of the tips of the granular alumina and the cerium oxide, scratches can be effectively prevented from occurring.
Further, during the preparation process of the aluminum oxide, the aluminum oxide can be subjected to micron-sized ball milling for more than 48 hours, and no acute angle smaller than or equal to 45 degrees is observed under a 50-time magnifying glass.
In one embodiment, the weight of cerium oxide in the polishing agent per unit weight is 10 to 30%, and the weight of aluminum oxide in the polishing agent per unit weight is 10 to 30%.
In one embodiment, the ratio of the amounts of the cerium oxide and the aluminum oxide is (2-3): (0.5 to 1).
In one embodiment, the polishing agent further comprises 5% to 20% of a sodium phosphate salt, 8% to 12% of a polyether siloxane compound, 8% to 12% of a polyurethane compound, 25% to 35% of a polyol compound, and 2% to 8% of sodium chloride.
In one embodiment, the sodium phosphate salt is a suspending agent; the polyether siloxane compound is used for increasing contact surface activity; the polyurethane compound is used for increasing adhesion; the polyol compound is used for increasing the chemical decomposition capacity of the polishing agent during grinding; the sodium chloride is used to increase the chemical activity of the polish.
In one embodiment, the polishing agent has a water drop angle in the horizontal plane in the range of 12 ° to 15 °. Further, when the angle between the water drop angle and the desktop is 12-15 degrees, the surface tension of the polishing agent is small, the polishing agent can easily enter the glass and the polishing pad, the contact area between the polishing agent and a polishing workpiece is increased, the polishing efficiency is improved, the water drop angle is more than 15 degrees or less than 12 degrees, the polishing agent cannot easily permeate into the polishing pad, and the polishing agent is easily thrown out and cannot play a polishing and grinding role.
As shown in fig. 1, the present application also provides a method for preparing a polishing agent, which is used for preparing the polishing agent, and comprises the following steps:
step S1: mixing the cerium oxide and the aluminum oxide in deionized water according to the ratio of 2:1, and stirring to obtain a first mixed solution;
step S2: continuously adding at least one of a sodium phosphate salt, a polyether siloxane compound, a polyurethane compound, a polyol compound and sodium chloride into the first mixed solution to obtain a second mixed solution;
step S3: heating the second mixed solution to 50 to 75 ℃ for 0.5 to 3 hours to obtain the polishing agent.
Example 1
And stirring the cerium oxide powder and the alumina powder in deionized water by adopting a high-speed multi-blade stirrer with the rotating speed of 800-1400 r/min, wherein the cerium oxide powder and the alumina powder are added according to the mass ratio of 2:1 in the stirring process. After stirring for 0.5h, adding other components of the polishing agent;
the quartz glass polishing agent is prepared from the following raw materials in percentage by mass:
20% of sodium phosphate;
12% of a polyether siloxane compound;
8% of a polyurethane compound;
25% of a polyol compound;
5% of sodium chloride;
20% of cerium oxide;
10% of aluminum oxide;
wherein the deionized water resistivity is more than 16M ohm; the raw materials are sequentially proportioned, the polishing agent is heated to 50 ℃, and the mixture is fully stirred for 1.5 hours; the polish was then tested for water droplets having a drop angle of about 13. And then, carrying out a polishing test, wherein the pressure of a polishing disc is 30kg, the rotating speed of an upper disc is 10r/min, the rotating speed of a lower disc is 8r/min, the sun gear is 5r/min, the temperature of a polishing agent is 25-27 ℃, a polishing pad is damping cloth, the friction coefficient is 0.15, and the equipment is polished for 3 hours.
Example 2
And stirring the cerium oxide powder and the alumina powder in deionized water by adopting a high-speed multi-blade stirrer with the rotating speed of 800-1400 r/min, wherein the cerium oxide powder and the alumina powder are added according to the mass ratio of 2:1 in the stirring process. After stirring for 0.5h, adding other components of the polishing agent;
the quartz glass polishing agent is prepared from the following raw materials in percentage by mass:
10% of sodium phosphate;
8% of polyether siloxane compound;
12% of a polyurethane compound;
28% of a polyol compound;
2% of sodium chloride;
27% of cerium oxide;
13% of aluminum oxide;
wherein the deionized water resistivity is more than 16M ohm; the raw materials are sequentially proportioned, the polishing agent is heated to 50 ℃, and the mixture is fully stirred for 1.5 hours; the polish was then tested for water droplets having a drop angle of about 15. And then, carrying out a polishing test, wherein the pressure of a polishing disc is 30kg, the rotating speed of an upper disc is 10r/min, the rotating speed of a lower disc is 8r/min, the sun gear is 5r/min, the temperature of a polishing agent is 25-27 ℃, a polishing pad is damping cloth, the friction coefficient is 0.15, and the equipment is polished for 3 hours.
Example 3
And stirring the cerium oxide powder and the alumina powder in deionized water by adopting a high-speed multi-blade stirrer with the rotating speed of 800-1400 r/min, wherein the cerium oxide powder and the alumina powder are added according to the mass ratio of 2:1 in the stirring process. After stirring for 0.5h, adding other components of the polishing agent;
the quartz glass polishing agent is prepared from the following raw materials in percentage by mass:
10% of sodium phosphate;
10% of polyether siloxane compound;
10% of a polyurethane compound;
30% of a polyol compound;
5% of sodium chloride;
23% of cerium oxide;
12% of alumina;
wherein the deionized water resistivity is more than 16M ohm; the raw materials are sequentially proportioned, the polishing agent is heated to 50 ℃, and the mixture is fully stirred for 1.5 hours; the polish was then tested for water droplets having a drop angle of about 14. And then, carrying out a polishing test, wherein the pressure of a polishing disc is 30kg, the rotating speed of an upper disc is 10r/min, the rotating speed of a lower disc is 8r/min, the sun gear is 5r/min, the temperature of a polishing agent is 25-27 ℃, a polishing pad is damping cloth, the friction coefficient is 0.15, and the equipment is polished for 3 hours.
Polished sample and workpiece dimensions in examples 1 to 3: 152 x 6.35mm quartz glass plate, the polishing effect was as follows:
name (R) Roughness (Ra) Scratch Time
Example 1 0.7~0.9nm 1.4um 3h
Example 2 0.4~0.8nm 1.2mm 3h
Example 3 0.1~0.2nm 0.9mm 3h
Hereinbefore, specific embodiments of the present application are described with reference to the drawings. However, those skilled in the art will appreciate that various modifications and substitutions can be made to the specific embodiments of the present application without departing from the scope of the present application. Such modifications and substitutions are intended to be within the scope of the present application.

Claims (10)

1. A polishing agent comprising a particulate cerium oxide and an aluminum oxide, wherein the particle size of the particulate cerium oxide is distributed at least in a first particle size range of 1300 to 2000 nm and in a second particle size range of 2000 to 3000 nm, the amount of the cerium oxide distributed in the first particle size range is at least 85% of the total amount of the cerium oxide, and the amount of the cerium oxide distributed in the second particle size range is less than 5% of the total amount of the cerium oxide.
2. The polishing composition of claim 1 wherein said particulate cerium oxide also has a particle size distribution in a third particle size range, said third particle size range being less than 1000 nanometers, and wherein said cerium oxide is distributed in said third particle size range in an amount less than 10 percent of the total amount of said cerium oxide.
3. The polishing composition of claim 2 wherein said particulate alumina has a particle size range at least in a fourth particle size range of 500 to 1500 nanometers and in a fifth particle size range of 1500 to 2500 nanometers, said alumina being present in said fourth particle size range in an amount of at least 82 percent of the total amount of said alumina, and said alumina being present in said fifth particle size range in an amount of less than 8 percent of the total amount of said alumina.
4. The polishing composition of claim 3 wherein said particulate aluminum oxide also has a particle size distribution in a sixth particle size range, said sixth particle size range being less than 500 nanometers, and wherein said cerium oxide is distributed in said third particle size range in an amount less than 10 percent of the total amount of said cerium oxide.
5. The polishing composition of claim 1 wherein the maximum acute angle of the tips on the particulate alumina is less than or equal to 45 ° and the maximum acute angle of the tips on the particulate ceria is less than or equal to 30 °.
6. The polishing abrasive according to claim 1, wherein the weight of said cerium oxide per unit weight of said abrasive is in the range of 10 to 30% and the weight of said aluminum oxide per unit weight of said abrasive is in the range of 10 to 30%.
7. The polishing composition according to claim 1, wherein the weight ratio of cerium oxide to aluminum oxide is (2-3): (0.5 to 1).
8. The polishing composition of claim 1 further comprising 5 to 20% sodium phosphate salt, 8 to 12% polyether siloxane compound, 8 to 12% polyurethane compound, 25 to 35% polyol compound, 2 to 8% sodium chloride.
9. The polishing composition of claim 1 wherein the polishing composition has a drop angle in the horizontal plane in the range of 12 ° to 15 °.
10. A method for producing a polishing agent, for producing a polishing agent according to any one of claims 1 to 9, comprising the steps of:
mixing the cerium oxide and the aluminum oxide in deionized water according to the ratio of 2:1, and stirring to obtain a first mixed solution;
continuously adding at least one of a sodium phosphate salt, a polyether siloxane compound, a polyurethane compound, a polyol compound and sodium chloride into the first mixed solution to obtain a second mixed solution;
heating the second mixed solution to 50 to 75 ℃ for 0.5 to 3 hours to obtain the polishing agent.
CN202111590559.0A 2021-12-23 2021-12-23 Polishing agent and preparation method thereof Pending CN114213977A (en)

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Application Number Priority Date Filing Date Title
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