CN104312441B - Silicon cerium polishing fluid and preparation method thereof - Google Patents
Silicon cerium polishing fluid and preparation method thereof Download PDFInfo
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- CN104312441B CN104312441B CN201410589847.8A CN201410589847A CN104312441B CN 104312441 B CN104312441 B CN 104312441B CN 201410589847 A CN201410589847 A CN 201410589847A CN 104312441 B CN104312441 B CN 104312441B
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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
Abstract
The present invention relates to a kind of silicon cerium polishing fluid, it contains micron order cerium dioxide powder, nanoscale cerium dioxide powder, cataloid, the water of succinate or salt, anionic dispersing agents, and surplus;The particle diameter of wherein described micron order cerium dioxide powder is 0.5 ~ 2.0 μm, and particle diameter is that less than 1.5 μm of micron order cerium dioxide powder accounts for more than 60%, and particle diameter is more than 1.8 μm and accounts for less than 5%;The particle diameter of the nanoscale cerium dioxide powder is 20 ~ 100 nm, and the nanoscale cerium dioxide powder that particle diameter is below 50nm accounts for 30 ~ 35%, and particle diameter accounts for 10 ~ 15% for more than 80nm's.The silicon cerium polishing fluid of the present invention, it can be used for high accuracy grinding and the glossing of glass, sapphire, resin lens and semiconductor chip, there is the advantages of polishing efficiency is high, polishing precision is high, and stock removal rate is high.
Description
Technical field
The present invention relates to the technical field of surface polishing, it is more particularly related to a kind of silicon cerium polishing fluid
And preparation method thereof.
Background technology
Chemically mechanical polishing (CMP) be it is a kind of be used for chemistry and mechanism by polishing fluid come smooth technology, its
It can be used for the planarization for including the surfaces such as glass, glasses or semiconductor wafer.The throwing that planarization or polishing substrate surface use
Light liquid is techniques known, and as a rule polishing fluid includes depositing abrasive material in aqueous.It is commonly known in the art
Abrasive material includes cerium oxide, silica, aluminum oxide, zirconium oxide and tin oxide etc..Have including the polishing fluid of polishing powder from rare earth
The advantages of polishing velocity is fast, precision is high.Since the invention forties in last century polishing powder from rare earth, output and application amount all by
It is cumulative to add.In recent years, with the fast development of optics and information industry, liquid crystal display, luminescent device and optical element etc.
It is more and more to the demand of polishing powder, polish required precision more and more higher.
Therefore, have studied in the prior art a variety of methods be used for improve traditional polishing fluid polishing efficiency and uniformly
Property, while the infringement of structure the defects of minimize polished surface and to lower face.For example, US5264010A discloses one kind
The polishing fluid of cerium oxide, pyrogenic silica and precipitated silica is included, it can significantly improve polishing efficiency.
US5543216A discloses a kind of preparation method for synthesizing cerium oxide particle, and the particle size of the cerium oxide is in 0.03~5um
Between, but the broad particle distribution of the cerium oxide, polishing efficiency and polishing effect still have much room for improvement.
It remains desirable, however, that one kind during polishing and planarized substrate, further improves polishing efficiency and processing
Precision.
The content of the invention
In order to solve above-mentioned technical problem of the prior art, it is an object of the invention to provide a kind of silicon cerium polishing fluid and
Its preparation method.
To achieve these goals, present invention employs following technical scheme:
A kind of silicon cerium polishing fluid, using nanoscale cerium dioxide powder, micron order cerium dioxide powder, cataloid
As grinding-material, it is characterised in that:Micron order cerium dioxide powder containing 3 ~ 6wt% in the polishing fluid, 1.20 ~
1.75wt% nanoscale cerium dioxide powder, 10 ~ 25wt% cataloid, 0.3 ~ 0.8wt% succinate or salt,
0.5 ~ 1.5wt% anionic dispersing agents, and the water of surplus;The particle diameter of wherein described micron order cerium dioxide powder is 0.5 ~ 2.0
μm, and the micron order cerium dioxide powder that particle diameter is less than 1.5 μm accounts for more than the 60% of micron order ceria powder weight,
Particle diameter is that more than 1.8 μm of micron order cerium dioxide powder accounts for less than the 5% of micron order ceria powder weight;Wherein, institute
The particle diameter for stating nanoscale cerium dioxide powder is 20 ~ 100 nm, and particle diameter is 50 below nm nanoscale cerium dioxide powder
The 30 ~ 35% of nanoscale ceria powder weight are accounted for, particle diameter is that 80 more than nm nanoscale cerium dioxide powder accounts for nanoscale
The 10 ~ 15% of ceria powder weight.
Wherein, the succinate or salt are preferably alkyl phenol ether sulfosuccinates, sulfosuccinic diethyl phthalate sodium salt,
And/or ethoxylated dodecyl alcohol mono sulfosuccinates.
Wherein, the anionic dispersing agents are acrylamide -2- acrylamide-2-methylpro panesulfonic acid copolymers(AM/
AMPS bipolymers).
Wherein, the nanoscale cerium dioxide powder passes through following surface treatment:
(1)The modifying agent that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder is added in deionized water, 800 ~
The first system for forming that concentration is 1.5 ~ 2.0wt% in 10 ~ 15min is stirred under 1000 rpm mixing speed;
(2)By nanoscale cerium dioxide powder, and the acryloyl that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder
Oxy-ethyl-trimethyl salmiac is distributed to GMA in the case where rotating speed is 800 ~ 1000 rpm mixing speed
In obtain second system;The quality of the GMA for nanoscale ceria powder weight 2.5 ~
3.0 again;
(3)By step(2)Obtained second system is added to step(1)In obtained the first system, 1800 ~ 2000
20 ~ 25 min are stirred under rpm mixing speed and obtain mixed liquor, and are transferred in reactor, in N2Under atmosphere protection, persistently stir
The dilauroyl peroxide for adding 0.5 ~ 1.0wt% of GMA quality is mixed, then in 80 ~ 85 DEG C of condition
2 hours of lower reaction, then it is filtered, washed and dried.
Wherein, the modifying agent is the compound with below general formula structure:
Also, R is the alkyl containing 10 ~ 15 carbon;R' is (CH2)nSO3Na, and n is 3 ~ 5 integer.
The second aspect of the present invention, further relate to the preparation method of above-mentioned silicon cerium polishing fluid, it is characterised in that:Methods described bag
Include following steps:
A. 10 ~ 25wt% cataloid is added in container, then add 0.3 ~ 0.8wt% succinate or
Salt simultaneously stirs, and obtains the first system;
B. 3 ~ 6wt% of addition micron order cerium dioxide powder in the first system obtained to step A, and 1.20 ~
1.75wt% nanoscale cerium dioxide powder simultaneously stirs, and obtains second system;And wherein described micron order ceria
The particle diameter of powder is 0.5 ~ 2.0 μm, and the micron order cerium dioxide powder that particle diameter is less than 1.5 μm accounts for micron order titanium dioxide
More than the 60% of cerium powder quality, particle diameter are that more than 1.8 μm of micron order cerium dioxide powder accounts for micron order cerium dioxide powder
Less than the 5% of quality;Wherein, the particle diameter of the nanoscale cerium dioxide powder is 20 ~ 100 nm, and particle diameter is 50 below nm
Nanoscale cerium dioxide powder account for the 30 ~ 35% of nanoscale ceria powder weight, particle diameter is 80 more than nm nanoscale
Cerium dioxide powder accounts for the 10 ~ 15% of nanoscale ceria powder weight;
C. 0.5 ~ 1.5wt% anionic dispersing agents are added in the second system obtained to step B, and add the water of surplus
It is uniformly dispersed using ultrasonic wave.
Wherein, the succinate or salt are preferably alkyl phenol ether sulfosuccinates, sulfosuccinic diethyl phthalate sodium salt,
And/or ethoxylated dodecyl alcohol mono sulfosuccinates.
Wherein, the anionic dispersing agents are acrylamide -2- acrylamide-2-methylpro panesulfonic acid copolymers(AM/
AMPS bipolymers).
Wherein, the nanoscale cerium dioxide powder passes through following surface treatment:
(1)The modifying agent that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder is added in deionized water, 800 ~
The first system for forming that concentration is 1.5 ~ 2.0wt% in 10 ~ 15min is stirred under 1000 rpm mixing speed;
(2)By nanoscale cerium dioxide powder, and the acryloyl that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder
Oxy-ethyl-trimethyl salmiac is distributed to GMA in the case where rotating speed is 800 ~ 1000 rpm mixing speed
In obtain second system;The quality of the GMA for nanoscale ceria powder weight 2.5 ~
3.0 again;
(3)By step(2)Obtained second system is added to step(1)In obtained the first system, 1800 ~ 2000
20 ~ 25 min are stirred under rpm mixing speed and obtain mixed liquor, and are transferred in reactor, in N2Under atmosphere protection, persistently stir
The dilauroyl peroxide for adding 0.5 ~ 1.0wt% of GMA quality is mixed, then in 80 ~ 85 DEG C of condition
2 hours of lower reaction, then it is filtered, washed and dried.
Wherein, the modifying agent is the compound with below general formula structure:
Also, R is the alkyl containing 10 ~ 15 carbon;R' is (CH2)nSO3Na, and n is 3 ~ 5 integer.
Compared with prior art, silicon cerium polishing fluid of the present invention and preparation method thereof has the advantages that:
The silicon cerium polishing fluid of the present invention, can be used for the high accuracy of glass, sapphire, resin lens and semiconductor chip
Grinding and glossing, there is the advantages of polishing efficiency is high, polishing precision is high, and stock removal rate is high, is not passivated, easy to operate.
Embodiment
Silicon cerium polishing fluid of the present invention and preparation method thereof is further explained below with reference to specific embodiment
State, to help those skilled in the art to have more complete, accurate and deep reason to inventive concept of the invention, technical scheme
Solution.
In embodiments of the invention and comparative example, micron order ceria powder is contained in described silicon cerium polishing fluid
The water of body, nanoscale cerium dioxide powder, cataloid, succinate or salt, anionic dispersing agents, and surplus;Wherein
The particle diameter of the micron order cerium dioxide powder is 0.5 ~ 2.0 μm, and particle diameter is less than 1.5 μm of micron order ceria
Powder accounts for the 72% of micron order ceria powder weight, and particle diameter is that more than 1.8 μm of micron order cerium dioxide powder accounts for micron
The 2.8% of level ceria powder weight;The particle diameter of the nanoscale cerium dioxide powder is 20 ~ 100 nm, and particle diameter is 50
Below nm nanoscale cerium dioxide powder accounts for the 32% of nanoscale ceria powder weight, and particle diameter is 80 more than nm nanometer
Level cerium dioxide powder accounts for the 12.2% of nanoscale ceria powder weight.The particle diameter distribution uses Mastersizer
3000 Particle Size Analyzers are tested to obtain, and it is the particle diameter distribution using the method test particle of laser diffraction.Below the present invention
Embodiment and comparative example in, the cataloid used is prepared using silicon dissolution method, be using inorganic base as
Catalyst, reacted with elemental silicon and pure water to prepare cataloid, SiO in the cataloid2Mass fraction
Can be 20 ~ 36%, particle diameter is 20 ~ 30 nm, and viscosity is 5 mPas.For the ease of comparing, in following examples and comparative example
SiO in the cataloid2Mass fraction be 35%.
Embodiment 1
The present embodiment is related to the surface treatment of nanoscale cerium dioxide powder, and it comprises the following steps
(1)The modifying agent that quality is nanoscale cerium dioxide powder 10wt% is added in deionized water, 800 ~ 1000
The first system for forming that concentration is 2.0wt% in 15min is stirred under rpm mixing speed;
(2)By nanoscale cerium dioxide powder, and the acryloyl-oxy second that quality is nanoscale cerium dioxide powder 8wt%
Base trimethyl ammonium chloride is distributed in GMA in the case where rotating speed is 800 ~ 1000 rpm mixing speed and obtained
To second system;The quality of the GMA is 3.0 times of nanoscale ceria powder weight;
(3)By step(2)Obtained second system is added to step(1)In obtained the first system, 1800 ~ 2000
25 min are stirred under rpm mixing speed and obtain mixed liquor, and are transferred in reactor, in N2Under atmosphere protection, lasting stirring
GMA quality 0.5wt% dilauroyl peroxide is added, then reacts 2 under conditions of 80 ~ 85 DEG C
Individual hour, then it is filtered, washed and dried;The modifying agent is the compound with below general formula structure:
Also, R is the alkyl containing 10 ~ 15 carbon;R' is (CH2)nSO3Na, and n is 3 ~ 5 integer.
Embodiment 2
Silicon cerium polishing fluid described in the present embodiment, the micron order cerium dioxide powder containing 3.0wt%, 1.20wt% nanometer
Level cerium dioxide powder, 15wt% cataloid, 0.5wt% alkyl phenol ether sulfosuccinates, 0.8wt% AM/
AMPS bipolymers, and the water of surplus.Its preparation method is as follows:Cataloid is added in container first, then
Add alkyl phenol ether sulfosuccinates and stir, obtain the first system;Then micron is separately added into the first system
Level cerium dioxide powder and nanoscale cerium dioxide powder simultaneously stir, and obtain second system;Added in the second last system
AM/AMPS bipolymers, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtain silicon cerium polishing fluid.
Embodiment 3
Silicon cerium polishing fluid described in the present embodiment, the micron order cerium dioxide powder containing 6.0wt%, 1.75wt% nanometer
Level cerium dioxide powder, 20wt% cataloid, 0.8wt% alkyl phenol ether sulfosuccinates, 1.5wt% AM/
AMPS bipolymers, and the water of surplus.Its preparation method is as follows:Cataloid is added in container first, then
Add alkyl phenol ether sulfosuccinates and stir, obtain the first system;Then micron is separately added into the first system
Level cerium dioxide powder and nanoscale cerium dioxide powder simultaneously stir, and obtain second system;Added in the second last system
AM/AMPS bipolymers, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtain silicon cerium polishing fluid.
Embodiment 4
Silicon cerium polishing fluid described in the present embodiment, the micron order cerium dioxide powder containing 4.0wt%, 1.39wt% nanometer
Level cerium dioxide powder, 18wt% cataloid, 0.6wt% alkyl phenol ether sulfosuccinates, 1.2wt% AM/
AMPS bipolymers, and the water of surplus.Its preparation method is as follows:Cataloid is added in container first, then
Add alkyl phenol ether sulfosuccinates and stir, obtain the first system;Then micron is separately added into the first system
Level cerium dioxide powder and nanoscale cerium dioxide powder simultaneously stir, and obtain second system;Added in the second last system
AM/AMPS bipolymers, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtain silicon cerium polishing fluid.
Embodiment 5
Silicon cerium polishing fluid described in the present embodiment, the micron order cerium dioxide powder containing 4.0wt%, 1.39wt% nanometer
Level cerium dioxide powder, 18wt% cataloid, 0.6wt% ethoxylated dodecyl alcohol sulfosuccinic acid monoesters disodium
Salt, 1.2wt% AM/AMPS bipolymers, and the water of surplus.Its preparation method is as follows:Cataloid is added first
Into container, then add ethoxylated dodecyl alcohol mono sulfosuccinates and stir, obtain the first system;
Then micron order cerium dioxide powder and nanoscale cerium dioxide powder are separately added into the first system and is stirred, is obtained
Second system;AM/AMPS bipolymers are added in the second last system, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave
It can obtain silicon cerium polishing fluid.
Embodiment 6
Silicon cerium polishing fluid described in the present embodiment, the micron order cerium dioxide powder containing 4.0wt%, 1.39wt% nanometer
Level cerium dioxide powder(By the surface treatment of embodiment 1), 18wt% cataloid, 0.6wt% alkyl phenol ether sulphur
Change succinate, 1.2wt% AM/AMPS bipolymers, and the water of surplus.Its preparation method is as follows:First by colloid dioxy
SiClx is added in container, is then added alkyl phenol ether sulfosuccinates and is stirred, obtains the first system;Then
Micron order cerium dioxide powder and nanoscale cerium dioxide powder are separately added into one system and is stirred, obtains the second body
System;AM/AMPS bipolymers are added in the second last system, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtained
To silicon cerium polishing fluid.
Comparative example 1
Silicon cerium polishing fluid described in this comparative example, the micron order cerium dioxide powder containing 4.0wt%, 1.39wt% nanometer
Level cerium dioxide powder, 18wt% cataloid, 1.2wt% AM/AMPS bipolymers, and the water of surplus.It is made
Preparation Method is as follows:Cataloid is added in container first and obtains the first system;Then add respectively in the first system
Enter micron order cerium dioxide powder and nanoscale cerium dioxide powder and stir, obtain second system;The second last system
Middle addition AM/AMPS bipolymers, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtain silicon cerium polishing fluid.
Comparative example 2
Silicon cerium polishing fluid described in this comparative example, the micron order cerium dioxide powder containing 4.0wt%, 1.39wt% nanometer
Level cerium dioxide powder, 18wt% cataloid, 1.2wt% aliphatic alcohol polyoxyvinethene phosphate, and the water of surplus.
Its preparation method is as follows:Cataloid is added in container first and obtains the first system;Then divide in the first system
It micron order cerium dioxide powder and nanoscale cerium dioxide powder and Jia Ru not stir, obtain second system;The second last
Aliphatic alcohol polyoxyvinethene phosphate is added in system, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtain silicon cerium
Polishing fluid.
Comparative example 3
Silicon cerium polishing fluid described in this comparative example, the micron order cerium dioxide powder containing 4.0wt%, 1.39wt% nanometer
Level cerium dioxide powder, 18wt% cataloid, 1.2wt% poly amic acid, and the water of surplus.Its preparation method is such as
Under:Cataloid is added in container first and obtains the first system;Then micron order is separately added into the first system
Cerium dioxide powder and nanoscale cerium dioxide powder simultaneously stir, and obtain second system;Added in the second last system poly-
Acrylic amine, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtain silicon cerium polishing fluid.
Comparative example 4
Silicon cerium polishing fluid described in this comparative example, the micron order cerium dioxide powder containing 5.5wt%, 18wt% colloid two
Silica, 0.6wt% alkyl phenol ether sulfosuccinates, 1.2wt% AM/AMPS bipolymers, and the water of surplus.It is made
Preparation Method is as follows:Cataloid is added in container first, alkyl phenol ether sulfosuccinates is then added and stirs
Uniformly, the first system is obtained;Then micron order cerium dioxide powder is added in the first system and is stirred, obtains the second body
System;AM/AMPS bipolymers are added in the second last system, and the water conservancy for adding surplus is uniformly dispersed with ultrasonic wave and can obtained
To silicon cerium polishing fluid.
The evaluation of polishing performance
Use SpeedFam-PW single side polishing machines and 3M polishing pads.The glass substrate being polished is a diameter of 2.5 inches
Disk glass-ceramic substrate.With cerium oxide base abrasive material pre-polish(ing) glass substrate.The surface roughness Ra of substrate through pre-polish(ing)
For 0.9nm.The charging rate of rare earth polishing is 120ml/min, and polish pressure is 60 g/cm2, polishing time is 30 minutes.
After the completion of polishing, polished glass substrate is cleaned, dried, and supersound washing is carried out to it with pure water.By by washing
Glass substrate is dried, and then tests following performance.Wherein, the change of quality before and after speed is polished by measurement is removed(Using point
Analyse balance)Determine the removal speed (nm/min) of glass substrate;Surface roughness is surveyed over the substrate surface with AFM
Measure glass substrate surface roughness (Ra);Surface defect and cut, with the polished glass substrate of the micro- sem observation of differential differential
Surface inspection attachment state, the cut that occurs, the inspection result of cut represents with the cut number observed on surface.As a result such as
Shown in table 1.
Table 1
Remove speed(nm/min) | Surface roughness(nm) | Cut number | |
Embodiment 2 | 360 | 0.36 | 25 |
Embodiment 3 | 720 | 0.44 | 29 |
Embodiment 4 | 520 | 0.43 | 23 |
Embodiment 5 | 520 | 0.41 | 21 |
Embodiment 6 | 530 | 0.23 | 11 |
Comparative example 1 | 430 | 0.76 | 38 |
Comparative example 2 | 390 | 0.73 | 41 |
Comparative example 3 | 380 | 0.77 | 42 |
Comparative example 4 | 510 | 0.58 | 40 |
For the ordinary skill in the art, simply the present invention is exemplarily described for specific embodiment,
Obviously present invention specific implementation is not subject to the restrictions described above, and is entered as long as employing the inventive concept and technical scheme of the present invention
The improvement of capable various unsubstantialities, or it is not improved by the present invention design and technical scheme directly apply to other occasions
, within protection scope of the present invention.
Claims (7)
1. a kind of silicon cerium polishing fluid, made using nanoscale cerium dioxide powder, micron order cerium dioxide powder, cataloid
For grinding-material, it is characterised in that:Contain 3 ~ 6wt% micron order cerium dioxide powder, 1.20 ~ 1.75wt% in the polishing fluid
Nanoscale cerium dioxide powder, 10 ~ 25wt% cataloid, 0.3 ~ 0.8wt% succinate or its salt, 0.5 ~
1.5wt% anionic dispersing agents, and the water of surplus;The particle diameter of wherein described micron order cerium dioxide powder is 0.5 ~ 2.0 μm;
The particle diameter of the nanoscale cerium dioxide powder is 20 ~ 100 nm;Wherein, the nanoscale cerium dioxide powder passes through following table
Face is handled:
(1)The modifying agent that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder is added in deionized water, in 800 ~ 1000 rpm
Mixing speed under stir 10 ~ 15min in formed concentration be 1.5 ~ 2.0wt% the first system;
(2)By nanoscale cerium dioxide powder, and the acrylyl oxy-ethyl that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder
Trimethyl ammonium chloride is distributed in GMA in the case where rotating speed is 800 ~ 1000 rpm mixing speed and obtained
Second system;The quality of the GMA is 2.5 ~ 3.0 times of nanoscale ceria powder weight;
(3)By step(2)Obtained second system is added to step(1)In obtained the first system, in 1800 ~ 2000 rpm
Mixing speed under 20 ~ 25 min of stirring obtain mixed liquor, and be transferred in reactor, in N2Under atmosphere protection, lasting stirring
0.5 ~ 1.0wt% of GMA quality dilauroyl peroxide is added, then under conditions of 80 ~ 85 DEG C
2 hours are reacted, are then filtered, washed and dried;The modifying agent is the compound with below general formula structure:
Also, R is the alkyl containing 10 ~ 15 carbon;R' is (CH2)nSO3Na, n are 3 ~ 5 integer.
2. silicon cerium polishing fluid according to claim 1, it is characterised in that:Particle diameter is less than 1.5 μm of micron order titanium dioxide
Cerium powder accounts for more than the 60% of micron order ceria powder weight, and particle diameter is more than 1.8 μm of micron order cerium dioxide powder
Account for less than the 5% of micron order ceria powder weight;Particle diameter is that 50 below nm nanoscale cerium dioxide powder accounts for nanoscale
The 30 ~ 35% of ceria powder weight, particle diameter are that 80 more than nm nanoscale cerium dioxide powder accounts for nanoscale ceria
The 10 ~ 15% of powder quality.
3. silicon cerium polishing fluid according to claim 1, it is characterised in that:The succinate or its salt are alkyl phenol ether sulphur
Change succinate, sulfosuccinic diethyl phthalate sodium salt, and/or ethoxylated dodecyl alcohol mono sulfosuccinates.
4. silicon cerium polishing fluid according to claim 1, it is characterised in that:The anionic dispersing agents are acrylamide -2-
Acrylamide-2-methylpro panesulfonic acid copolymer.
A kind of 5. preparation method of silicon cerium polishing fluid, it is characterised in that:It the described method comprises the following steps:
A. 10 ~ 25wt% cataloid is added in container, then add 0.3 ~ 0.8wt% succinate or its
Salt simultaneously stirs, and obtains the first system;
B. 3 ~ 6wt% of addition micron order cerium dioxide powder in the first system obtained to step A, and 1.20 ~ 1.75wt%
Nanoscale cerium dioxide powder simultaneously stirs, and obtains second system;And the grain of wherein described micron order cerium dioxide powder
Footpath is 0.5 ~ 2.0 μm, and the micron order cerium dioxide powder that particle diameter is less than 1.5 μm accounts for micron order ceria powder constitution
More than the 60% of amount, particle diameter are that more than 1.8 μm of micron order cerium dioxide powder accounts for the 5% of micron order ceria powder weight
Below;Wherein, the particle diameter of the nanoscale cerium dioxide powder is 20 ~ 100 nm, and particle diameter is 50 below nm nanoscale
Cerium dioxide powder accounts for the 30 ~ 35% of nanoscale ceria powder weight, and particle diameter is 80 more than nm nanoscale ceria
Powder accounts for the 10 ~ 15% of nanoscale ceria powder weight;
0.5 ~ 1.5wt% anionic dispersing agents are added in the second system obtained to step B, and the water conservancy for adding surplus is used and surpassed
Sound wave is uniformly dispersed;
Surface treatment of the nanoscale cerium dioxide powder Jing Guo following steps:
(1)The modifying agent that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder is added in deionized water, 800 ~ 1000
The first system for forming that concentration is 1.5 ~ 2.0wt% in 10 ~ 15min is stirred under rpm mixing speed;The modifying agent be with
The compound of below general formula structure:
Also, R is the alkyl containing 10 ~ 15 carbon;R' is (CH2)nSO3Na, and n is 3 ~ 5 integer;
(2)By nanoscale cerium dioxide powder, and the acryloyl-oxy second that quality is 8 ~ 10wt% of nanoscale cerium dioxide powder
Base trimethyl ammonium chloride is distributed in GMA in the case where rotating speed is 800 ~ 1000 rpm mixing speed and obtained
To second system;The quality of the GMA is the 2.5 ~ 3.0 of nanoscale ceria powder weight
Times;
(3)By step(2)Obtained second system is added to step(1)In obtained the first system, in 1800 ~ 2000 rpm
Mixing speed under 20 ~ 25 min of stirring obtain mixed liquor, and be transferred in reactor, in N2Under atmosphere protection, lasting stirring
0.5 ~ 1.0wt% of GMA quality dilauroyl peroxide is added, then under conditions of 80 ~ 85 DEG C
2 hours are reacted, are then filtered, washed and dried.
6. the preparation method of silicon cerium polishing fluid according to claim 5, it is characterised in that:The succinate or salt are alkane
Base phenolic ether sulfosuccinates, sulfosuccinic diethyl phthalate sodium salt, and/or ethoxylated dodecyl alcohol sulfosuccinic acid monoesters two
Sodium salt.
7. the preparation method of silicon cerium polishing fluid according to claim 5, it is characterised in that:The anionic dispersing agents are third
Acrylamide -2- acrylamide-2-methylpro panesulfonic acid copolymers.
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EP0133102A1 (en) * | 1983-07-29 | 1985-02-13 | Rhone-Poulenc Chimie | Polishing composition based on cerium and process for making it |
CN1301288A (en) * | 1998-03-18 | 2001-06-27 | 卡伯特微电子公司 | Chemical mechanical polishing slurry useful for copper substrates |
CN102533126A (en) * | 2010-12-21 | 2012-07-04 | 盟智科技股份有限公司 | Abrasive composition and use thereof |
CN103992743A (en) * | 2014-05-09 | 2014-08-20 | 杰明纳微电子股份有限公司 | Polishing solution containing ceric oxide powder/colloid silicon dioxide mixed abrasive and preparing process thereof |
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EP0133102A1 (en) * | 1983-07-29 | 1985-02-13 | Rhone-Poulenc Chimie | Polishing composition based on cerium and process for making it |
CN1301288A (en) * | 1998-03-18 | 2001-06-27 | 卡伯特微电子公司 | Chemical mechanical polishing slurry useful for copper substrates |
CN102533126A (en) * | 2010-12-21 | 2012-07-04 | 盟智科技股份有限公司 | Abrasive composition and use thereof |
CN103992743A (en) * | 2014-05-09 | 2014-08-20 | 杰明纳微电子股份有限公司 | Polishing solution containing ceric oxide powder/colloid silicon dioxide mixed abrasive and preparing process thereof |
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Effective date of registration: 20200121 Address after: 014000 No.8 Jinger Road, application Industrial Park, Baotou Rare Earth Development Zone, Inner Mongolia Autonomous Region Patentee after: Baotou Zhongke Yuhang polishing materials Co., Ltd Address before: Anyang City, Henan province 455000 longan District Ma Jian Xiang Shang Mao Cun Yijian Patentee before: ANYANG FANGYUAN ABRASIVE SUBSTANCE CO., LTD. |