CN114426809A - Silicon oxide modified nano diamond abrasive particles and preparation method and application thereof - Google Patents
Silicon oxide modified nano diamond abrasive particles and preparation method and application thereof Download PDFInfo
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- CN114426809A CN114426809A CN202210146853.0A CN202210146853A CN114426809A CN 114426809 A CN114426809 A CN 114426809A CN 202210146853 A CN202210146853 A CN 202210146853A CN 114426809 A CN114426809 A CN 114426809A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention provides a silicon oxide modified nano diamond abrasive particle and a preparation method and application thereof, wherein the preparation method comprises the following steps: dispersing the nano-diamond and the polyoxyethylene polyoxypropylene ether segmented copolymer in absolute ethyl alcohol, performing ultrasonic treatment, and stirring overnight; adding water and ammonia water, heating, dropwise adding the prepared tetraethyl orthosilicate-ethanol solution into the mixed solution, and continuing to react; centrifuging, washing and drying overnight; when the silicon oxide modified nano diamond abrasive grain polishing solution is applied to the chemical mechanical polishing of zirconia ceramics, compared with the original diamond abrasive grains, a softer hydration layer is generated through the solid-phase chemical reaction of silicon oxide and zirconia ceramics, and the mechanical grinding action of diamond is combined, namely, the chemical corrosion action of silicon oxide and the mechanical grinding action of diamond are combined, so that the surface roughness of a ceramic workpiece is effectively reduced, and the material removal rate is increased by up to 140% at the same ratio, thereby realizing better chemical mechanical polishing performance.
Description
Technical Field
The invention belongs to the technical field of surface polishing processing, and particularly relates to silicon oxide modified nano diamond abrasive particles and a preparation method thereof, which are applied to polishing of zirconia ceramic surfaces.
Background
The yttria-stabilized zirconia ceramic serving as a novel functional material has the excellent performances of low density, high hardness, high brittleness, high wear resistance, excellent corrosion resistance, excellent heat resistance and the like. The method has wide application prospect in the fields of aerospace, energy, semiconductors, computers, medical treatment and the like. Currently, with the arrival of the fifth generation mobile network era, zirconia ceramics have been applied to the rear cover of a 5G smart phone by virtue of excellent no-signal shielding, good heat dissipation performance and smooth touch. However, zirconia ceramics are difficult to process due to their inherent hard and brittle nature. The traditional main processing technology is grinding by using diamond abrasive grains. The processing precision can only reach micron level generally, and serious subsurface damage is easy to occur in the processing process, so that the nano-level planarization standard required by the industry is difficult to reach.
Therefore, it is required to precisely process it by using only the Chemical Mechanical Polishing (CMP) technique which can provide the global planarization technique. In the polishing solution, the abrasive particles are crucial to the influence of surface quality, the traditional diamond abrasive particles have the advantage of high polishing rate and are usually used as a rough polishing mode of the surface of a workpiece, but the diamond has high hardness and is easy to scratch the surface of the workpiece, so that subsurface damage is caused, and the surface quality is reduced.
Disclosure of Invention
In view of the defects in the prior art, the first purpose of the invention is to provide a preparation method of silicon oxide modified nano-diamond abrasive particles. Namely, the hydrolysis of tetraethyl orthosilicate is promoted by ammonia water to generate irregular silicon dioxide small particles, and then the silicon dioxide small particles are deposited on the surfaces of the nano-diamond particles to form coating layers, so that the silicon oxide modified nano-diamond abrasive particles are obtained. Compared with the original nano diamond, the addition of the silicon oxide improves the chemical corrosion effect in the CMP process, and the surface quality and the material removal rate are improved together by combining the chemical corrosion effect of the silicon oxide and the mechanical grinding effect of the diamond, so that the production efficiency of the processed workpiece is improved, and the transition from rough polishing to fine polishing is realized.
It is a second object of the present invention to provide the above silica-modified nanodiamond abrasive particles.
A third object of the present invention is to provide use of the above silica-modified nanodiamond abrasive particles.
In order to achieve the first object, the solution of the invention is:
a preparation method of silicon oxide modified nano-diamond abrasive particles comprises the following steps:
(1) dispersing the nano-diamond (ND) and the polyoxyethylene polyoxypropylene ether block copolymer (F127) in absolute ethyl alcohol, performing ultrasonic treatment to obtain F127-ND mixed liquor, and then stirring the F127-ND mixed liquor in a constant-temperature water bath for overnight;
(2) adding water and ammonia water into the F127-ND mixed solution stirred in the step (1), heating, dropwise adding a prepared tetraethyl orthosilicate (TEOS) -ethanol solution into the heated F127-ND mixed solution when the temperature reaches 60-65 ℃, and continuing to react after dropwise adding;
(3) and (3) centrifuging the product obtained in the step (2), alternately washing the product with ethanol and deionized water for several times, and drying the product at the temperature of between 60 and 65 ℃ overnight to obtain the silicon oxide modified ND abrasive grain.
As a preferred embodiment of the present invention, in the step (1), ND has an average particle diameter of 80 to 110 nm.
As a preferred embodiment of the present invention, in the step (1), the time for the ultrasonic treatment is 20 to 50 min.
As a preferred embodiment of the present invention, in the step (1), the temperature of the thermostatic waterbath is 20 to 25 ℃.
As a preferred embodiment of the present invention, in the step (1) and the step (2), the mass ratio of TEOS to ND in the TEOS-ethanol solution is (25-100): 5.
as a preferred embodiment of the present invention, in the step (2), the mass ratio of TEOS to ethanol in the TEOS-ethanol solution is (25-100): 60.
as a preferred embodiment of the present invention, in the step (2), the reaction is continued for 4 to 7 hours.
As a preferred embodiment of the present invention, in step (3), the rotation speed of the centrifugation is 3000-6000rpm, and the time of the centrifugation is 0.5-1 h.
In order to achieve the second object, the solution of the invention is:
the silicon oxide modified ND abrasive grain is obtained by the preparation method.
In order to achieve the third object, the solution of the invention is:
the application of the silica modified ND abrasive particle in zirconia ceramic polishing.
As a preferred embodiment of the present invention, deionized water is added to the silica-modified ND abrasive grain, the pH value is adjusted to be alkaline with a sodium hydroxide solution, and then ultrasonic processing is performed to obtain a silica-modified ND abrasive grain polishing solution, which is finally applied to zirconia ceramic polishing.
As a preferred embodiment of the invention, the pH is from 10 to 11.
As a preferred embodiment of the present invention, the time of the ultrasonic treatment is 1 to 2 hours.
As a preferred embodiment of the invention, the content of the silicon oxide in the silicon oxide modified ND abrasive grain polishing solution is 0.24-0.96mol/L, and the solid content is 1 wt%.
Due to the adoption of the scheme, the invention has the beneficial effects that:
first, when the silicon oxide modified nano diamond abrasive grain polishing solution is applied to the chemical mechanical polishing of zirconia ceramics, compared with the original diamond abrasive grains, a softer hydration layer is generated through the solid phase chemical reaction of silicon oxide and zirconia ceramics, and then the mechanical grinding action of diamond is combined, namely, the chemical corrosion action of silicon oxide and the mechanical grinding action of diamond are combined, so that the surface roughness of a ceramic workpiece is effectively reduced, and the material removal rate is increased by up to 140% at the same ratio, thereby realizing better chemical mechanical polishing performance.
Secondly, the silicon oxide modified nano-diamond abrasive particles are different from the pure mechanical action of the original diamond abrasive particles, and the polishing efficiency is jointly improved by utilizing the solid-phase chemical reaction of silicon oxide and zirconium oxide and combining the grinding action of diamond, so that the high-efficiency and high-precision polishing effect is achieved.
And thirdly, the preparation method of the silicon oxide modified nano-diamond abrasive particle is environment-friendly and simple, and has high repeatability.
Drawings
Fig. 1 is a transmission electron microscope photograph of silica-modified ND abrasive grains according to example 2 of the present invention.
Detailed Description
The invention provides a silicon oxide modified ND abrasive particle and a preparation method and application thereof.
< method for producing silica-modified ND abrasive grain >
The preparation method of the silicon oxide modified ND abrasive grain comprises the following steps of:
(1) dispersing ND and F127 into absolute ethyl alcohol, performing ultrasonic treatment to obtain F127-ND mixed solution, and then stirring the F127-ND mixed solution in a constant-temperature water bath for overnight;
(2) transferring the F127-ND mixed solution stirred in the step (1) into a three-neck flask, adding water and ammonia water, slowly heating, dropwise adding the prepared TEOS-ethanol solution to the heated F127-ND mixed solution when the temperature of the system reaches 60-65 ℃, and continuing to react after dropwise adding;
(3) and (3) centrifuging the product obtained in the step (2), alternately washing the product for 3 times by using ethanol and deionized water, and drying the product at the temperature of between 60 and 65 ℃ overnight to obtain the silicon oxide modified ND abrasive particles.
Among them, in the step (1), ND may have an average particle diameter of 80 to 110nm, preferably 100 nm.
In step (1), the time of sonication may be 20-50min, preferably 30 min.
In step (1), the temperature of the thermostatic water bath may be 20 to 25 ℃, preferably 25 ℃.
In the step (1) and the step (2), the mass ratio of TEOS and ND in the TEOS-ethanol solution may be (25 to 100): 5, preferably 50: 5.
In the step (2), the mass ratio of TEOS and ethanol in the TEOS-ethanol solution may be (25-100): 60, preferably 50: 60.
In step (2), the reaction may be continued for 4 to 7 hours, preferably 6 hours.
In step (2), the preparation process of the TEOS-ethanol solution is well known to those skilled in the art.
In step (3), the rotation speed of centrifugation may be 3000-6000rpm, preferably 5000 rpm; the time for centrifugation may be 0.5 to 1h, preferably 0.5 h.
< silica-modified ND abrasive grain >
The silica-modified ND abrasive grain of the present invention is obtained by the above-described production method.
< application of silica-modified ND abrasive grain >
Specifically, deionized water is added into the silica-modified ND abrasive grains, the pH value is adjusted to be alkaline by using a sodium hydroxide solution, then ultrasonic treatment is carried out to obtain the silica-modified ND abrasive grain polishing solution, and finally the polishing solution is applied to zirconia ceramic polishing.
Wherein the pH value can be 10-11, preferably 10.
The time of the ultrasound may be 1-2h, preferably 1 h.
The content of the silicon oxide in the silicon oxide modified ND abrasive grain polishing solution can be 0.24-0.96mol/L, and preferably 0.24 mol/L; the solids content was 1% by weight.
The application of the silicon oxide modified ND abrasive particles in polishing of the zirconia ceramics, namely the polishing solution prepared by the silicon oxide modified ND is applied to polishing of the zirconia ceramics cover plate, so that the polishing speed can be obviously improved, the surface roughness of the ceramic workpiece is reduced, and the purpose of efficient polishing is achieved.
The technical solution of the above scheme is further illustrated below by combining specific examples, and the preferred embodiments of the present invention are detailed as follows:
example 1:
the method for producing the silica-modified ND abrasive grain of the present example (i.e., producing the silica-modified ND abrasive grain by the TEOS hydrolysis method) includes the steps of:
(1) dispersing 5g of ND and 0.5g of F127 in 500g of absolute ethyl alcohol, carrying out ultrasonic treatment for 30min to obtain a F127-ND mixed solution, and then stirring the mixed solution in a thermostatic water bath at 25 ℃ overnight.
(2) And (2) transferring the stirred F127-ND mixed solution obtained in the step (1) to a three-neck flask, adding 40g of water and 10g of ammonia water, slowly heating, dropwise adding the prepared mixed solution of 25g of TEOS and 60g of ethanol to the reaction solution when the temperature of the system reaches 60 ℃, and continuing to react for 6 hours after dropwise adding.
(3) And (3) centrifuging the product obtained in the step (2) at 5000rpm for 0.5h, alternately washing the product with ethanol and deionized water for 3 times, and drying the product at 60 ℃ overnight to obtain the silica modified ND abrasive particles.
When the silica-modified ND abrasive grain of this embodiment is applied to polishing zirconia ceramics, specifically, deionized water is added to the silica-modified ND abrasive grain, a 3 wt% sodium hydroxide solution is used to adjust the pH value to 10, then ultrasound is performed for 1 hour to obtain a polishing solution of the silica-modified ND abrasive grain having a silica content of 0.24mol/L and a solid content of 1 wt%, and finally the polishing solution is applied to polishing zirconia ceramics. The polishing effect of the polishing liquid of this example on zirconia ceramics is shown in Table 1.
Example 2:
this example is substantially the same as example 1, and is characterized in that (only the mass of TEOS is increased):
the method for producing the silica-modified ND abrasive grain of the present example (i.e., producing the silica-modified ND abrasive grain by the TEOS hydrolysis method) includes the steps of:
(1) this step was the same as in example 1.
(2) And (2) transferring the stirred F127-ND mixed solution obtained in the step (1) to a three-neck flask, adding 40g of water and 10g of ammonia water, slowly heating, dropwise adding the prepared mixed solution of 50g of TEOS and 60g of ethanol into the reaction solution when the temperature of the system reaches 60 ℃, and continuing to react for 6 hours after dropwise adding.
(3) This step was the same as in example 1. The transmission electron microscope of this example is shown in FIG. 1.
When the silica-modified ND abrasive grain of this embodiment is applied to zirconia ceramic polishing, specifically, deionized water is added to the silica-modified ND abrasive grain, a 3 wt% sodium hydroxide solution is used to adjust the pH value to 10, then, 1 hour of ultrasound is performed to obtain a silica-modified ND abrasive grain polishing solution with a silica content of 0.48mol/L and a solid content of 1 wt%, and finally, the polishing solution is applied to zirconia ceramic polishing. The polishing effect of the polishing liquid of this example on zirconia ceramics is shown in Table 1.
Example 3:
this example is substantially the same as example 1, and is characterized in that (only the mass of TEOS is increased):
the method for producing the silica-modified ND abrasive grain of the present example (i.e., producing the silica-modified ND abrasive grain by the TEOS hydrolysis method) includes the steps of:
(1) this step was the same as in example 1.
(2) Transferring the stirred F127-ND mixed solution obtained in the step (1) into a three-neck flask, adding 40g of water and 10g of ammonia water, slowly heating, dropwise adding the prepared mixed solution of 75g of TEOS and 60g of ethanol into the reaction solution when the temperature of the system reaches 60 ℃, and continuing to react for 6 hours after dropwise adding.
(3) This step was the same as in example 1.
When the silica-modified ND abrasive grain of this embodiment is applied to zirconia ceramic polishing, specifically, deionized water is added to the silica-modified ND abrasive grain, a 3 wt% sodium hydroxide solution is used to adjust the pH value to 10, then, 1 hour of ultrasound is performed to obtain a silica-modified ND abrasive grain polishing solution with a silica content of 0.72mol/L and a solid content of 1 wt%, and finally, the polishing solution is applied to zirconia ceramic polishing. The polishing effect of the polishing liquid of this example on zirconia ceramics is shown in Table 1.
Example 4:
this example is substantially the same as example 1, and is characterized in that (only the mass of TEOS is increased):
the method for producing the silica-modified ND abrasive grain of the present example (i.e., producing the silica-modified ND abrasive grain by the TEOS hydrolysis method) includes the steps of:
(1) this step was the same as in example 1.
(2) And (2) transferring the stirred F127-ND mixed solution obtained in the step (1) to a three-neck flask, adding 40g of water and 10g of ammonia water, slowly heating, dropwise adding the prepared mixed solution of 100g of TEOS and 60g of ethanol to the reaction solution when the temperature of the system reaches 60 ℃, and continuing to react for 6 hours after dropwise adding.
(3) This step was the same as in example 1.
When the silica-modified ND abrasive grain of this embodiment is applied to zirconia ceramic polishing, specifically, deionized water is added to the silica-modified ND abrasive grain, a 3 wt% sodium hydroxide solution is used to adjust the pH value to 10, then, 1 hour of ultrasound is performed to obtain a silica-modified ND abrasive grain polishing solution with a silica content of 0.96mol/L and a solid content of 1 wt%, and finally, the polishing solution is applied to zirconia ceramic polishing. The polishing effect of the polishing liquid of this example on zirconia ceramics is shown in Table 1.
Comparative example:
this comparative example employed the original ND powder of example 1 diluted with a certain amount of deionized water, adjusted to pH 10 with 3 wt% sodium hydroxide solution, and then sonicated for at least 1h to obtain an ND polishing slurry with a solid content of 1 wt%.
The polishing effect of the polishing liquid of this comparative example on zirconia ceramics is shown in Table 1.
The polishing test was performed on the zirconia ceramics under certain polishing conditions using the polishing liquids of the above examples and comparative examples.
The polishing conditions for the polishing test were as follows:
polishing machine: UNIPOL-1000S automatic pressure grinding polisher.
Polishing the workpiece: a zirconia ceramic cover plate of 5.5cm x 5.5 cm.
Polishing the pad: a polyurethane polishing pad.
Polishing pressure: 6 kg.
Rotating speed of the upper disc and the lower disc: 30/60 rpm.
Steering of the upper and lower wheels: and (4) a positive direction.
Polishing time: and 2 h.
After polishing, the zirconium oxide ceramic wafer is sequentially subjected to ultrasonic cleaning by using acetone, a cleaning agent, deionized water and absolute ethyl alcohol, then the zirconium oxide ceramic wafer is dried, the mass difference of the zirconium oxide ceramic wafer before and after polishing is weighed by using a precision analytical balance, and the Material Removal Rate (MRR) is calculated according to a formula; in addition, the surface roughness (Sa: calculated number average height) of the zirconia ceramic sheet before and after polishing was observed by a 3D optical profiler (S neox 090v2), and the measured area was 500. mu. m.times.500. mu.m.
The polishing effects of the polishing solutions of the above examples and comparative examples on zirconia ceramics are shown in Table 1, respectively. As can be seen from table 1, from example 1 to example 4, as the mass of TEOS increases, the material removal rate appears to increase and decrease due to changes in particle hardness (step down) and particle chemical activity (step up). However, the silica-modified ND composite abrasive particles in examples 1 to 4 all improved the material removal rate and the surface quality significantly improved compared to the original ND abrasive particle in comparative example 1. The material removal rate of the zirconia ceramic polished by the silica-modified ND abrasive particles in example 2 was relatively increased by 140%, and the surface roughness reached the minimum value of 1.055 nm.
TABLE 1 comparison of polishing effects of polishing solutions of examples of the present invention and comparative examples on zirconia ceramic cover plates
In a word, compared with the original ND abrasive particles, when the silicon oxide modified ND abrasive particles are used for polishing the zirconia ceramic plate, the material removal rate can be obviously improved, the surface roughness can be greatly reduced, and the surface quality can be improved. Compared with the original ND abrasive particles, the silicon oxide modified ND abrasive particles generate softer hydration layers through the solid-phase chemical reaction of silicon oxide and zirconia ceramics, and are combined with the mechanical grinding action of diamond, so that the purpose of high-efficiency polishing is achieved, the material removal rate is increased by up to 140% in a same ratio, and better chemical mechanical polishing performance is realized.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the invention is in accordance with the purpose of the present invention, and shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.
Claims (10)
1. A preparation method of silicon oxide modified nano-diamond abrasive particles is characterized by comprising the following steps: which comprises the following steps:
(1) dispersing the nano-diamond and the polyoxyethylene polyoxypropylene ether block copolymer in absolute ethyl alcohol, performing ultrasonic treatment to obtain a mixed solution, and then stirring the mixed solution in a constant-temperature water bath overnight;
(2) adding water and ammonia water into the mixed solution stirred in the step (1), heating, dropwise adding the prepared tetraethyl orthosilicate-ethanol solution into the heated mixed solution when the temperature reaches 60-65 ℃, and continuing to react after dropwise adding;
(3) and (3) centrifuging the product obtained in the step (2), alternately washing the product with ethanol and deionized water for several times, and drying the product at the temperature of between 60 and 65 ℃ overnight to obtain the silicon oxide modified nano-diamond abrasive particles.
2. The method for producing the silicon oxide-modified nanodiamond abrasive grain according to claim 1, characterized in that: in the step (1), the average grain diameter of the nano-diamond is 80-110 nm; and/or the presence of a gas in the atmosphere,
in the step (1), the ultrasonic treatment time is 20-50 min; and/or the presence of a gas in the gas,
in the step (1), the temperature of the thermostatic water bath is 20-25 ℃.
3. The method for producing the silicon oxide-modified nanodiamond abrasive grain according to claim 1, characterized in that: in the step (1) and the step (2), the mass ratio of tetraethyl orthosilicate to nanodiamond in the tetraethyl orthosilicate-ethanol solution is (25-100): 5.
4. the method for producing the silica-modified nanodiamond abrasive grain according to claim 1, characterized in that: in the step (2), the mass ratio of tetraethyl orthosilicate to ethanol in the tetraethyl orthosilicate-ethanol solution is (25-100): 60.
5. the method for producing the silica-modified nanodiamond abrasive grain according to claim 1, characterized in that: in the step (2), the continuous reaction time is 4-7 h.
6. The method for producing the silicon oxide-modified nanodiamond abrasive grain according to claim 1, characterized in that: in the step (3), the rotation speed of the centrifugation is 3000-6000rpm, and the centrifugation time is 0.5-1 h.
7. A silicon oxide modified nano-diamond abrasive particle is characterized in that: which is obtained by the production method according to any one of claims 1 to 6.
8. Use of the silica-modified nanodiamond abrasive particles of claim 7 in zirconia ceramic polishing.
9. Use according to claim 8, characterized in that: adding deionized water into the silicon oxide modified nano-diamond abrasive particles, adjusting the pH value to be alkaline by using a sodium hydroxide solution, carrying out ultrasonic treatment to obtain a silicon oxide modified nano-diamond abrasive particle polishing solution, and finally applying the silicon oxide modified nano-diamond abrasive particle polishing solution to zirconia ceramic polishing.
10. Use according to claim 9, characterized in that: the pH value is 10-11; and/or the presence of a gas in the gas,
the ultrasonic time is 1-2 h; and/or the presence of a gas in the gas,
the content of silicon oxide in the silicon oxide modified nano diamond abrasive particle polishing solution is 0.24-0.96mol/L, and the solid content is 1 wt%.
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