CN107129762A - A kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof - Google Patents
A kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof Download PDFInfo
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- CN107129762A CN107129762A CN201710334987.4A CN201710334987A CN107129762A CN 107129762 A CN107129762 A CN 107129762A CN 201710334987 A CN201710334987 A CN 201710334987A CN 107129762 A CN107129762 A CN 107129762A
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
Abstract
The present invention relates to a kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof, belong to chemical Mechanical Polishing Technique field.Its cladded type silica/ceria composite abrasive grains 1%~10%, oxidant are that 0.1%~10%, dispersant is 0.1%~10%;It is 2~6 to adjust pH by pH adjusting agent, obtains the polishing fluid of carborundum chemically mechanical polishing.Operating method of the present invention is simple, reasonable, it is readily produced, add dispersant, so that polishing suspension good dispersion, the agglomeration of abrasive particle is avoided, while preparing cladded type silica/ceria core shell structure Compostie abrasive particles using homogeneous precipitation method, covered effect is improved, add potassium permanganate oxidant so that the polishing effect of polishing fluid is better.
Description
Technical field
The present invention relates to a kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof, belong to chemical machinery throwing
Light technical field.
Background technology
In recent years, as semi-conducting material is widely used in large scale integrated circuit, hard disc of computer, magnetic memory etc.
Field, semi-conducting material occupies increasingly consequence in the field such as advanced material science and new and high technology, to National Industrial
Progress has highly important effect.
It is that almost can uniquely realize the process for treating surface of leveling at present to chemically-mechanicapolish polish (CMP), extensively
The general planarizing process applied to surfaces such as hard disc of computer, optical glass, IC chips.
At present, in the CMP process such as optical glass, semiconductor wafer, polishing fluid abrasive particle is mainly from single
Silica abrasive particle or cerium oxide abrasive particle;Wherein silica abrasive particle has good dispersion, centralized particle diameter, manufacturing process ripe
The advantages of, but there is the shortcomings of material removing rate is low, hardness is higher in it;And single cerium oxide abrasive particle has clearance high, hard
Spend low advantage, but its there is also bad dispersibility, the strong difficult cleaning of adsorptivity, easily cause cut the shortcomings of;Due to single abrasive particle without
The need for method meets produce reality, therefore, this area occurs in that cerium oxide coats the Compostie abrasive particles of silica, improves carborundum
The effect of chemically mechanical polishing.
The content of the invention
It is an object of the present invention to overcome the above deficiencies, and there is provided a kind of polishing fluid of carborundum chemically mechanical polishing
And preparation method thereof, the clearance of carborundum chemically mechanical polishing is improved, silicon carbide quality is improved, reduces carbonization
The production cost of silicon polishing.
Technical scheme, a kind of polishing fluid of carborundum chemically mechanical polishing, it is characterized in that formula rate is pressed
Mass percent meter is as follows:Cladded type silica/ceria composite abrasive grains 1%~10%, oxidant are 0.1%~10%, divided
Powder is 0.1%~10%;It is 2~6 to adjust pH by pH adjusting agent.
The cladded type silica/ceria nucleocapsid Compostie abrasive particles are pulverulent solids, and particle diameter is 100~200nm.
The oxidant is one kind in potassium permanganate or hydrogen peroxide.
The dispersant is one kind in calgon or polyethylene glycol.
The pH adjusting agent is the KOH solution or HNO that mass concentration is 20%~60%3Solution.
The preparation method of the polishing fluid of the carborundum chemically mechanical polishing, step is as follows:Weigh cladded type silica/
Cladded type silica/ceria composite abrasive grains in the presence of magnetic agitation, are first dissolved in deionized water by ceria composite abrasive grains
In, suspension is formed, oxidant and dispersant is sequentially added so that cladded type silica/ceria composite abrasive grains concentration is
1%~10%, oxidant concentration 0.05%~2.0% and dispersant concentration are 0.5%~2.0%, finally using pH adjusting agent
The pH of suspension is adjusted to 2~6.
The cladded type silica/ceria composite abrasive grains preparation process is as follows by mass percentage:
(1) preparation of silicon suspension is aoxidized:Commercially available silicon dioxide polishing solution and deionized water are measured respectively, by the city measured
Sell silicon dioxide polishing solution be slowly added dropwise in the presence of magnetic agitation obtained into deionized water aoxidize silicon suspension, the oxygen
Silica in SiClx suspension is 2%~10%, magnetic agitation 10min, and pH is in the range of 10~10.5 for control;
(2) preparation of cerium solution:Six water cerous nitrates and hexa are taken, is dissolved in the presence of magnetic agitation
In ionized water, continue 10~20min of magnetic agitation, obtain cerium solution;Wherein, cerium ion concentration is 0.15~0.20mol/L,
The concentration of hexa is 0.5~1.0mol/L;
(3) mix:Step (2) is prepared into gained cerium solution uniform speed slow in the presence of magnetic agitation and instills step
(1) prepare in gained oxidation silicon suspension, obtain mixed solution, 10~20min of magnetic agitation;During mixing, SiO2:CeO2Quality
Than for 1:5~20;
(4) react:To mixed solution obtained by step (3), vigorous magnetic is stirred under 1000~3000r/min rotating speeds, 70~
100 DEG C of oil bath heatings, 2~3h of back flow reaction obtains dark brown suspension, then is cooled to room temperature, 3~5h of ripening,
Until there is lamination in the dark brown suspension;
(5) separate:The dark brown suspension for lamination occurred obtained by step (4) is centrifuged and washed,
In triplicate, dark brown sediment is obtained;
(6) post-process:Dark brown sediment obtained by step (5) is dried, drying temperature is 70~100 DEG C, drying
Time is 12~18h;Then the material after drying is tentatively ground, then continues to calcine 2~4h at 450~700 DEG C,
Lappingout is carried out to gained material again, cladded type silica/ceria nucleocapsid Compostie abrasive particles are obtained.
Beneficial effects of the present invention:Operating method of the present invention is simple, reasonable, it is easy to produce, and adds dispersant so that polishing
Suspension good dispersion, it is to avoid the agglomeration of abrasive particle, while prepare cladded type silica/ceria using homogeneous precipitation method
Core shell structure Compostie abrasive particles, improve covered effect, add potassium permanganate oxidant so that the polishing effect of polishing fluid is better
It is good.
Embodiment
Embodiment 1
A kind of preparation method of silicon carbide compound abrasive grain polishing solution, it comprises the following steps:
(1) cladded type silica/ceria nucleocapsid Compostie abrasive particles are prepared:
A, the preparation for aoxidizing silicon suspension:The commercial silica silicon polishing that 9mL particle diameter distributions are 60~100nm is measured respectively
Liquid and 18mL deionized waters, by 9mL commercial silicon dioxide polishing fluid in the presence of magnetic agitation, are uniformly slowly added dropwise to
In deionized water, magnetic agitation 10min obtains the oxidation silicon suspension that mass fraction is 10%;Simultaneously by adding thereto
Potassium hydroxide and dust technology control the suspension pH value of silica in the range of 10~10.5;
B, cerium solution preparation:Weigh respectively 20.9703g cerium ion concentrations for 0.15mol/L six water cerous nitrates and
33.9702g concentration is 0.5mol/L hexa, and its whole is dissolved in into 300mL in the presence of magnetic agitation
In ionized water, magnetic agitation 15min obtains cerium solution;
C, mixing:In the presence of magnetic agitation, obtained cerium solution uniform speed slow is instilled in oxidation silicon suspension,
Magnetic agitation 10min, obtains mixed solution;
D, reaction:Mixed solution is imported in three-neck flask, in the case where speed stirs for 1800r/min vigorous magnetic, with
100 DEG C of progress oil bath heatings, then 2h is heated at reflux, dark brown suspension is obtained, then room temperature is cooled to, ripening 3 is small
There is lamination in Shi Zhizhi;
E, separation:Dark brown suspension after layering is centrifuged, and with deionized water repeated washing 3 times, obtained
To dark brown sediment;
F, post processing:Then 80 DEG C of drying in vacuum drying chamber by it, are then ground, the powder after grinding are put
With 550 DEG C of temperature calcination 3 hours in Muffle furnace, light yellow powder is obtained, as cladded type silica/ceria nucleocapsid is answered
Close abrasive particle.
(2) novel silicon carbide composite abrasive grain polishing solution is prepared:1g Compostie abrasive particles are weighed, in the presence of magnetic agitation, according to
The secondary potassium permanganate oxidant by Compostie abrasive particles, 5wt% calgon dispersant and 5wt% is added in deionized water,
Obtain the polishing fluid that cumulative volume is 100mL so that Compostie abrasive particles concentration, calgon dispersant concentration and potassium permanganate oxidation
Agent concentration is respectively 1wt%, 0.5wt% and 0.158wt%, be eventually adding concentration be 60wt% pH adjusting agent (KOH solution or
Dilute nitric acid solution) pH value is adjusted to 2.
Embodiment 2
A kind of preparation method of silicon carbide compound abrasive grain polishing solution, it comprises the following steps:
(1) cladded type silica/ceria nucleocapsid Compostie abrasive particles are prepared:
A, the preparation for aoxidizing silicon suspension:The commercial silica silicon polishing that 9mL particle diameter distributions are 60~100nm is measured respectively
Liquid and 18mL deionized waters, by 9mL commercial silicon dioxide polishing fluid in the presence of magnetic agitation, are uniformly slowly added dropwise to
In deionized water, magnetic agitation 10min obtains the oxidation silicon suspension that mass fraction is 10%;Simultaneously by adding thereto
Potassium hydroxide and dust technology control the suspension pH value of silica in the range of 10~10.5;
B, cerium solution preparation:Weigh respectively 20.9703g cerium ion concentrations for 0.15mol/L six water cerous nitrates and
33.9702g concentration is 0.5mol/L hexa, and its whole is dissolved in into 300mL in the presence of magnetic agitation
In ionized water, magnetic agitation 15min obtains cerium solution;
C, mixing:In the presence of magnetic agitation, obtained cerium solution uniform speed slow is instilled in oxidation silicon suspension,
Magnetic agitation 10min, obtains mixed solution;
D, reaction:Mixed solution is imported in three-neck flask, in the case where speed stirs for 1800r/min vigorous magnetic, with
100 DEG C of progress oil bath heatings, then 2h is heated at reflux, dark brown suspension is obtained, then room temperature is cooled to, ripening 3 is small
There is lamination in Shi Zhizhi;
E, separation:Dark brown suspension after layering is centrifuged, and with deionized water repeated washing 3 times, obtained
To dark brown sediment;
F, post processing:Then 80 DEG C of drying in vacuum drying chamber by it, are then ground, the powder after grinding are put
With 550 DEG C of temperature calcination 3 hours in Muffle furnace, light yellow powder is obtained, as cladded type silica/ceria nucleocapsid is answered
Close abrasive particle.
(2) novel silicon carbide composite abrasive grain polishing solution is prepared:1g Compostie abrasive particles are weighed, in the presence of magnetic agitation, according to
It is secondary be 8wt% by Compostie abrasive particles, concentration calgon dispersant and concentration be 8wt% potassium permanganate oxidant be added to
In deionized water, obtain cumulative volume be 100ml polishing fluid so that Compostie abrasive particles concentration, calgon dispersant concentration and
Potassium permanganate oxidant concentration is respectively 1wt%, 0.5wt% and 0.79wt%, is eventually adding the pH that concentration is 60wt% and adjusts
Agent (KOH solution or dilute nitric acid solution) adjusts pH value to 2.
Embodiment 3
A kind of preparation method of silicon carbide compound abrasive grain polishing solution, it comprises the following steps:
(1) cladded type silica/ceria nucleocapsid Compostie abrasive particles are prepared:
A, the preparation for aoxidizing silicon suspension:The commercial silicon dioxide that 10mL particle diameter distributions are 60~100nm is measured respectively to throw
Light liquid and 40mL deionized waters, by 10mL commercial silicon dioxide polishing fluid in the presence of magnetic agitation, uniform slow drop
Add in deionized water, magnetic agitation 10min, obtain the oxidation silicon suspension that mass fraction is 6%;Simultaneously by adding thereto
Enter potassium hydroxide and dust technology to control the suspension pH value of silica in the range of 10~10.5;
B, cerium solution preparation:Weigh respectively 20.9703g cerium ion concentrations for 0.20mol/L six water cerous nitrates and
33.9702g concentration is 0.5mol/L hexa, and its whole is dissolved in into 300mL in the presence of magnetic agitation
In ionized water, magnetic agitation 15min obtains cerium solution;
C, mixing:In the presence of magnetic agitation, obtained cerium solution uniform speed slow is instilled in oxidation silicon suspension,
Magnetic agitation 10min, obtains mixed solution;
D, reaction:Mixed solution is imported in three-neck flask, in the case where speed stirs for 1800r/min vigorous magnetic, with
80 DEG C of progress oil bath heatings, then 2h is heated at reflux, dark brown suspension is obtained, then be cooled to room temperature, ripening 3 hours
Until there is lamination;
E, separation:Dark brown suspension after layering is centrifuged, and with deionized water repeated washing 3 times, obtained
To dark brown sediment;
F, post processing:Then 70 DEG C of drying in vacuum drying chamber by it, are then ground, the powder after grinding are put
With 650 DEG C of temperature calcination 2.5 hours in Muffle furnace, light yellow powder, as cladded type silica/ceria nucleocapsid are obtained
Compostie abrasive particles.
(2) novel silicon carbide composite abrasive grain polishing solution is prepared:2g Compostie abrasive particles are weighed, in the presence of magnetic agitation, according to
It is secondary be 8wt% by Compostie abrasive particles, concentration calgon dispersant and concentration be 10wt% potassium permanganate oxidant add
Into deionized water, the polishing fluid that cumulative volume is 100mL is obtained so that Compostie abrasive particles concentration, calgon dispersant concentration
It is respectively 2wt%, 0.5wt% and 1.58wt% with potassium permanganate oxidant concentration, is eventually adding the pH that concentration is 60wt% and adjusts
Save agent (KOH solution or dilute nitric acid solution) and adjust pH value to 2.
Embodiment 4
A kind of preparation method of silicon carbide compound abrasive grain polishing solution, it comprises the following steps:
(1) cladded type silica/ceria nucleocapsid Compostie abrasive particles are prepared:
A, the preparation for aoxidizing silicon suspension:The commercial silica silicon polishing that 9mL particle diameter distributions are 60~100nm is measured respectively
Liquid and 40mL deionized waters, by 10mL commercial silicon dioxide polishing fluid in the presence of magnetic agitation, uniform slow dropwise addition
Into deionized water, magnetic agitation 10min obtains the oxidation silicon suspension that mass fraction is 6%;Simultaneously by adding thereto
Potassium hydroxide and dust technology control the suspension pH value of silica in the range of 10~10.5;
B, cerium solution preparation:Weigh respectively 20.9703g cerium ion concentrations for 0.15mol/L six water cerous nitrates and
33.9702g concentration is 0.8mol/L hexa, and its whole is dissolved in into 300mL in the presence of magnetic agitation
In ionized water, magnetic agitation 15min obtains cerium solution;
C, mixing:In the presence of magnetic agitation, obtained cerium solution uniform speed slow is instilled in oxidation silicon suspension,
Magnetic agitation 10min, obtains mixed solution;
D, reaction:Mixed solution is imported in three-neck flask, in the case where speed stirs for 1600r/min vigorous magnetic, with
80 DEG C of progress oil bath heatings, then 3h is heated at reflux, dark brown suspension is obtained, then be cooled to room temperature, ripening 3 hours
Until there is lamination;
E, separation:Dark brown suspension after layering is centrifuged, and with deionized water repeated washing 3 times, obtained
To dark brown sediment;
F, post processing:Then 80 DEG C of drying in vacuum drying chamber by it, are then ground, the powder after grinding are put
With 650 DEG C of temperature calcination 3 hours in Muffle furnace, light yellow powder is obtained, as cladded type silica/ceria nucleocapsid is answered
Close abrasive particle.
(2) novel silicon carbide composite abrasive grain polishing solution is prepared:2g Compostie abrasive particles are weighed, in the presence of magnetic agitation, according to
It is secondary be 8wt% by Compostie abrasive particles, concentration calgon dispersant and concentration be 10wt% potassium permanganate oxidant add
Into deionized water, the polishing fluid that cumulative volume is 100mL is obtained so that Compostie abrasive particles concentration, calgon dispersant concentration
It is respectively 2wt%, 0.5wt% and 1.58wt% with potassium permanganate oxidant concentration, is eventually adding the pH that concentration is 40wt% and adjusts
Save agent (KOH solution or dilute nitric acid solution) and adjust pH value to 4.
Comparative example 1
The silicon dioxide polishing solution that 100mL commercial available qualities fraction is 30% is measured, is added in the presence of magnetic agitation
Enter into deionized water, then add 8wt% calgon dispersant and 10wt% potassium permanganate oxidant thereto, obtain
To the polishing fluid that cumulative volume is 1500ml so that silica concentration, calgon dispersant concentration and potassium permanganate oxidation
Agent concentration is respectively 2wt%, 0.5wt% and 1.58wt% suspension, is eventually adding the pH adjusting agent that concentration is 60wt% and adjusts
Save pH to 2.
Comparative example 2
The ceria polishing fluid that 100mL commercial available qualities fraction is 30% is measured, is added in the presence of magnetic agitation
Enter into deionized water, then add the calgon dispersant that concentration is 8wt% and the Gao Meng that concentration is 10wt% thereto
Sour potassium oxidant, obtain cumulative volume be 1500mL polishing fluid so that silica concentration, calgon dispersant concentration and
Potassium permanganate oxidant concentration is respectively 2wt%, 0.5wt% and 1.58wt% suspension, is eventually adding concentration for 60wt%
PH adjusting agent regulation pH to 2.
Above-described embodiment 1-4 and comparative example 1-2 the carborundum polishing fluid prepared are polished effect experiment, it is real
The polishing condition for testing process is as follows:2 inch silicon carbide wafers, polishing machine, polishing pad, polish pressure:3.5psi, upper disk rotating speed:
80rpm, lower wall rotating speed:80rpm, polishing flow velocity:100mL/min, polishing time:5min, polish temperature:Room temperature.
Table 1
As can be seen from Table 1, in novel silicon carbide composite abrasive grain polishing solution of the present invention, oxidant potassium permanganate
Concentration is higher, then material removing rate is bigger;Compostie abrasive particles concentration is higher, then material removing rate is bigger;PH value is bigger, then material is gone
Except rate is lower;Surface roughness very low super-smooth surface can be accessed simultaneously.
Novel silicon carbide composite abrasive grain polishing solution of the present invention, has more preferable removal than commercially available silicon dioxide polishing solution
Effect and surface roughness;Compared to commercially available ceria polishing fluid, removal effect is relatively low, but has a lower surface roughness,
Obtain nearly defect-free super-smooth surface.
Claims (7)
1. a kind of polishing fluid of carborundum chemically mechanical polishing, it is characterized in that formula rate is as follows by mass percentage:Bag
It is that 0.1%~10%, dispersant is 0.1%~10% to cover type silica/ceria composite abrasive grains 1%~10%, oxidant;Adjusted by pH
It is 2~6 to save agent regulation pH.
2. the polishing fluid of carborundum chemically mechanical polishing as claimed in claim 1, it is characterized in that:The cladded type silica/
Cerium oxide nuclear shell Compostie abrasive particles are pulverulent solids, and particle diameter is 100~200nm.
3. the polishing fluid of carborundum chemically mechanical polishing as claimed in claim 1, it is characterized in that:The oxidant is permanganic acid
One kind in potassium or hydrogen peroxide.
4. the polishing fluid of carborundum chemically mechanical polishing as claimed in claim 1, it is characterized in that:The dispersant is six inclined phosphorus
One kind in sour sodium or polyethylene glycol.
5. the polishing fluid of carborundum chemically mechanical polishing as claimed in claim 1, it is characterized in that:The pH adjusting agent is quality
KOH solution or HNO of the concentration for 20%~60%3Solution.
6. the preparation method of the polishing fluid of one of the claim 1-5 carborundum chemically mechanical polishings, it is characterized in that step
It is as follows:Cladded type silica/ceria composite abrasive grains are weighed, in the presence of magnetic agitation, first by cladded type silica/oxidation
Cerium Compostie abrasive particles are dissolved in deionized water, are formed suspension, are sequentially added oxidant and dispersant so that cladded type is aoxidized
Silicon/ceria composite abrasive grains concentration is 1%~10%, oxidant concentration 0.05%~2.0% and dispersant concentration is 0.5%~2.0%,
Finally the pH of suspension is adjusted to 2~6 using pH adjusting agent.
7. the preparation method of the polishing fluid of carborundum chemically mechanical polishing as claimed in claim 6, it is characterized in that the cladding
Type silica/ceria composite abrasive grains preparation process is as follows by mass percentage:
(1)Aoxidize the preparation of silicon suspension:Commercially available silicon dioxide polishing solution and deionized water are measured respectively, by measure commercially available two
Silica polishing fluid is slowly added dropwise in the presence of magnetic agitation to be obtained aoxidizing silicon suspension, the silica into deionized water
Silica in suspension is 2%~10%, magnetic agitation 10min, and pH is in the range of 10~10.5 for control;
(2)The preparation of cerium solution:Six water cerous nitrates and hexa are taken, deionization is dissolved in the presence of magnetic agitation
In water, continue 10~20min of magnetic agitation, obtain cerium solution;Wherein, cerium ion concentration is 0.15~0.20mol/L, and six is sub-
The concentration of tetramine is 0.5~1.0mol/L;
(3)Mixing:By step in the presence of magnetic agitation(2)Prepare gained cerium solution uniform speed slow and instill step(1)System
In standby gained oxidation silicon suspension, mixed solution, 10~20min of magnetic agitation are obtained;During mixing, SiO2:CeO2Mass ratio is 1:
5~20;
(4)Reaction:To step(3)Gained mixed solution vigorous magnetic under 1000~3000r/min rotating speeds is stirred, and 70~100
DEG C oil bath heating, 2~3h of back flow reaction obtains dark brown suspension, then is cooled to room temperature, 3~5h of ripening, until
There is lamination in the dark brown suspension;
(5)Separation:To step(4)The dark brown suspension that lamination has occurred in gained is centrifuged and washed, and repeats
Three times, obtain dark brown sediment;
(6)Post processing:To step(5)Gained dark brown sediment is dried, and drying temperature is 70~100 DEG C, drying time
For 12~18h;Then the material after drying is tentatively ground, then continues to calcine 2~4h at 450~700 DEG C, again
Lappingout is carried out to gained material, cladded type silica/ceria nucleocapsid Compostie abrasive particles are obtained.
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