CN109929460A - A kind of glass polishing water base cerium oxide polishing slurry and preparation method thereof - Google Patents
A kind of glass polishing water base cerium oxide polishing slurry and preparation method thereof Download PDFInfo
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Abstract
The present invention provides glass polishing water base cerium oxide polishing slurries and preparation method thereof, including cerium oxide milling 20~55%；Built surfactant 0.1~3%；Dispersing agent 1~8%；Lubricant 0.1~2%；Complexing agent 0.01~3%；Grinding aid 0.01~5%；PH adjusting agent 0.01~1%；Preservative 0.01~2%；Excess water；Built surfactant is the compounding of nonionic and anionic surfactant；Nonionic surfactant is one of polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and fatty glyceride or a variety of；Anionic surfactant is one of neopelex, sodium laurate, odium stearate and sodium succinate or a variety of；Dispersing agent is one of sodium oxalate, calgon, sodium pyrophosphate, sodium nitrate, Sodium Polyacrylate and lauryl sodium sulfate or a variety of.Polishing fluid suspended dispersed is good, and product yield is high after polishing.
Description
Technical field
The present invention relates to polishing fluid technical field more particularly to a kind of glass polishing water base cerium oxide polishing slurry and its systems
Preparation Method.
Background technique
Chemically mechanical polishing (CMP) technology has the chemical attack effect of the mechanical abrasive action of nanoparticle and polishing fluid
It is combined together to machine, Precision Machining is carried out to material surface.Now, chemical Mechanical Polishing Technique is acknowledged as unique overall situation
Flattening technique is widely used in the manufacture of the advanced electronic product such as hard disc of computer, integrated circuits silicon wafers, optical glass.
And polishing fluid in the market, excellent chemical mechanical polishing liquid depends on the import in the U.S., Japan and other countries, home products
Mainly based on polishing powder, and the good polishing fluid of suspended dispersed stability not yet forms large-scale production, this severely limits
The development of China's Ultraprecision Machining.Therefore preparation Costco Wholesale is low, and the excellent polishing fluid of service performance is extremely urgent.
Cerium oxide (CeO2) nanoparticle polishing fluid as a kind of good polishing material, is usually used in aeronautical glasses, integrated
Circuit substrate, liquid crystal display, optical glass and various sapphire polishings.In polishing material application field, nano Ce O2
Itself has excellent performance, and hardness is low, scratch less, can be with the advantages such as silicon dioxde reaction and polishing velocity be fast.But it receives
Rice CeO2Particle polishing powder partial size is small, has quantum size effect and skin effect, therefore particle is easily reunited.And powder point
It dissipates in water by mechanical functions such as electrostatic attraction, Van der Waals force, particle capillary forces, is very easy to that secondary agglomeration occurs.Therefore
The performance of the polishing performance of nano-cerium oxide rely on its powder dispersion situation, while in process polish after workpiece surface damage
Wound, shows as that surface roughness is big, surface scratch, removal amount numerous disadvantages such as not enough mostly.Therefore how to reduce the reunion of powder
And twice dispersing problem is the bottleneck for preparing stable cerium oxide polishing slurry, and the research hotspot in current micro mist field.
The Chinese patent of Publication No. CN 2009101608097A discloses a kind of chemically mechanical polishing nano-cerium oxide
Slurries and preparation method thereof, slurry constituents are as follows: 10~25 parts of acidic ph modifier, 0.1~0.8 part of dispersing agent, nano oxidized
74.2~89.8 parts of cerium powder, surplus is decentralized medium.Finished product made from the form of slurries has selectivity high in polishing, system
Product advantage with high accuracy, but the contact area in the slurries made simultaneously between nano-cerium oxide particle greatly increases, and product hangs
Floating dispersion effect cannot obtain good guarantee in use, in addition, the holding time of slurries is shorter, in the effect of external environment
Under be easy to happen particle aggregation and agglomeration the phenomenon that.Which has limited its popularizations and application in technique production.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of glass polishing water base cerium oxide polishing slurries and its preparation side
Method, the polishing fluid suspended dispersed is preferable, and product yield is higher after polishing.
The present invention provides a kind of water base cerium oxide polishing slurries of glass polishing, based on mass fraction, including following components:
Cerium oxide milling 20.0~55.0%；Built surfactant 0.1~3.0%；Dispersing agent 1~8%；Lubricant
0.1~2%；Complexing agent 0.01~3%；Grinding aid 0.01~5.0%；PH adjusting agent 0.01~1.0%；Preservative 0.01~
2%；Surplus is water；
The built surfactant is the compounding of nonionic surface active agent and anionic surfactant；Institute
It states nonionic surface active agent and is selected from polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and rouge
One of fatty acid glyceride is a variety of；Anionic surfactant is selected from neopelex, sodium laurate, tristearin
One of sour sodium and sodium succinate are a variety of；
The dispersing agent is selected from sodium oxalate, calgon, sodium pyrophosphate, sodium nitrate, Sodium Polyacrylate and dodecyl
One of sodium sulphate is a variety of.
Preferably, nonionic surface active agent and anionic surfactant in the built surfactant
Mass ratio is 1:0.9~1.1.
Preferably, the lubricant in polyethylene glycol 200, polyethylene glycol 400, Macrogol 600 and glycerol one
Kind is a variety of.
Preferably, the complexing agent is selected from ethylenediamine tetra-acetic acid, sodium gluconate, malic acid, sodium lactate and potassium citrate
One of or it is a variety of.
Preferably, the grinding aid is selected from one of potassium bromide, sodium bromide, potassium chloride, sodium chloride and potassium iodide or more
Kind.
Preferably, the preservative is selected from one of benzotriazole, potassium borate and Boratex or a variety of.
Preferably, the pH adjusting agent is selected from ethanol amine, tetraethyl ammonium hydroxide, diethanol amine, triethanolamine, tetramethyl
One of base ammonium hydroxide, tetrabutylammonium hydroxide, sodium hydroxide and potassium hydroxide are a variety of.
The present invention provides a kind of preparation method of water base cerium oxide polishing slurry of glass polishing described in above-mentioned technical proposal,
The following steps are included:
Water, built surfactant and mix lubricant is uniform, obtain the first mixture；
By first mixture and cerium oxide milling mixing, stirs, stand, obtain the second mixture；
Second mixture and dispersing agent, complexing agent, preservative and grinding aid are uniformly mixed, third mixing is obtained
Object；
The third mixture and pH adjusting agent are mixed, obtain glass polishing with water base polishing fluid.
Preferably, the dispersing agent, complexing agent, preservative and grinding aid are added with the speed of 1.0~2.0L/min.
The present invention provides a kind of water base cerium oxide polishing slurries of glass polishing, in terms of mass fraction, including following components:
Cerium oxide milling 20.0~55.0%；Built surfactant 0.1~3.0%；Dispersing agent 1~8%；Lubricant 0.1~
2%；Complexing agent 0.01~3%；Grinding aid 0.01~5.0%；PH adjusting agent 0.01~1.0%；Preservative 0.01~2%；
Surplus is water；The built surfactant is the compounding of nonionic surface active agent and anionic surfactant；
The nonionic surface active agent be selected from polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and
One of fatty glyceride is a variety of；Anionic surfactant is selected from neopelex, sodium laurate, hard
One of resin acid sodium and sodium succinate are a variety of；The dispersing agent is selected from sodium oxalate, calgon, sodium pyrophosphate, nitric acid
One of sodium, Sodium Polyacrylate and lauryl sodium sulfate are a variety of.The present invention by using above-mentioned content component, they
Mutual compatibility, so that the suspended dispersed of polishing fluid is preferable, and product yield is higher after polishing.The results showed that the polishing
The layer height of liquid is lower, and the delamination of powder and liquid is able to maintain and is basically unchanged in the case where long-time is stood；Overall average is good
Rate is 88.01%~95.6%.
Specific embodiment
The present invention provides a kind of water base cerium oxide polishing slurries of glass polishing, based on mass fraction, including following components:
Cerium oxide milling 20.0~55.0%；Built surfactant 0.1~3.0%；Dispersing agent 1~8%；Lubricant
0.1~2%；Complexing agent 0.01~3%；Grinding aid 0.01~5.0%；PH adjusting agent 0.01~1.0%；Preservative 0.01~
2%；Surplus is water；
The built surfactant is the compounding of nonionic surface active agent and anionic surfactant；Institute
It states nonionic surface active agent and is selected from polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and rouge
One of fatty acid glyceride is a variety of；Anionic surfactant is selected from neopelex, sodium laurate, tristearin
One of sour sodium and sodium succinate are a variety of；
The dispersing agent is selected from sodium oxalate, calgon, sodium pyrophosphate, sodium nitrate, Sodium Polyacrylate and dodecyl
One of sodium sulphate is a variety of.
Component of the present invention by using above-mentioned content, their mutual compatibilities, so that the suspended dispersed of polishing fluid is preferable,
And product yield is higher after polishing.
Polishing fluid provided by the invention includes cerium oxide milling 20.0~55.0%, preferably 30~55%, more preferably
50~55%.The mass content of cerium oxide is 97~98% or more in the cerium oxide milling；In the cerium oxide milling preferably
It further include one of cerium lanthanum oxide milling, silica milling and chromium oxide milling or a variety of.In the present invention, the cerium oxide
The partial size of milling is preferably 50nm~5 μm.The particle diameter distribution of the cerium oxide milling is uniform, can be improved the surface of polished product
The problems such as quality, the scuffing of reduction product, chipping.
The present invention provide polishing fluid includes built surfactant 0.1~3.0%, preferably 0.5~2.5%, more
Preferably 0.8~2.3%.The built surfactant is nonionic surface active agent and anionic surfactant
Compounding；The mass ratio of nonionic surface active agent and anionic surfactant is excellent in the built surfactant
It is selected as 1:0.9~1.1, more preferably 1:1.It is poly- that the nonionic surface active agent is selected from polyvinylpyrrolidone, alkyl phenol
One of ethylene oxide ether, fatty alcohol polyoxyethylene ether and fatty glyceride are a variety of；Be preferably selected from polyvinylpyrrolidone,
One of fatty alcohol polyoxyethylene ether and alkyl phenol polyoxyethylene ether are a variety of；It is more preferably selected from polyvinylpyrrolidone；Yin
Ionic surfactant is selected from one of neopelex, sodium laurate, odium stearate and sodium succinate or more
Kind；It is preferably selected from one of neopelex, odium stearate and sodium laurate or a variety of, is more preferably selected from dodecane
Base benzene sulfonic acid sodium salt.In a specific embodiment of the present invention, the built surfactant is neopelex and gathers
The mixture of vinylpyrrolidone.Built surfactant makes in polishing fluid between particle while playing the role of steric hindrance
It is acted on electrostatic stabilization, so that the suspension effect of powder is more preferable.
Polishing fluid provided by the invention includes dispersing agent 1~8%, preferably 3~8%.The dispersing agent is preferably selected from grass
One of sour sodium, calgon, sodium pyrophosphate, sodium nitrate, Sodium Polyacrylate and lauryl sodium sulfate are a variety of, more excellent
Choosing is selected from one of calgon, sodium pyrophosphate and Sodium Polyacrylate or a variety of.The dispersing agent of the inorganic of mentioned kind
The electrostatic stabilization effect between particle can be enhanced, so that polishing fluid is capable of the holding stably dispersing state of long period,
Have the advantages that simultaneously nontoxic, environmentally friendly.
Polishing fluid provided by the invention includes lubricant 0.1~2%, preferably 0.5~1.5%；The lubricant is selected from
One of polyethylene glycol 200, polyethylene glycol 400, Macrogol 600 and glycerol are a variety of；It is more preferably selected from polyethylene glycol 400
And/or glycerol.
Polishing fluid provided by the invention includes complexing agent 0.01~3%, preferably 0.5~1%.The complexing agent preferably selects
From one of ethylenediamine tetra-acetic acid, sodium gluconate, malic acid, sodium lactate and potassium citrate or a variety of, it is more preferably selected from second
Ethylenediamine tetraacetic acid (EDTA) (EDTA).The addition of complexing agent increases the polishing speed of glass surface in polishing process, improves production effect
Rate.
Polishing fluid provided by the invention includes grinding aid 0.01~5.0%, preferably 1~4%.The grinding aid preferably selects
From one of potassium bromide, sodium bromide, potassium chloride, sodium chloride and potassium iodide or a variety of, it is more preferably selected from potassium bromide and sodium bromide.
Polishing fluid provided by the invention includes pH adjusting agent 0.01~1.0%.The pH adjusting agent is preferably selected from second
Hydramine, tetraethyl ammonium hydroxide, diethanol amine, triethanolamine, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, sodium hydroxide
With one of potassium hydroxide or a variety of, it is more preferably selected from diethanol amine and triethanolamine.
Polishing fluid provided by the invention includes preservative 0.01~2%, preferably 1.0~1.5%；The preservative is preferred
Selected from one of benzotriazole, potassium borate and Boratex or a variety of, it is more preferably selected from potassium borate and Boratex.
The present invention provide polishing fluid includes water, preferably deionized water.
The present invention provides a kind of preparation methods of water base polishing fluid of glass polishing described in above-mentioned technical proposal, including with
Lower step:
Water, built surfactant and mix lubricant is uniform, obtain the first mixture；
By first mixture and cerium oxide milling mixing, stirs, stand, obtain the second mixture；
Second mixture and dispersing agent, complexing agent, preservative and grinding aid are uniformly mixed, third mixing is obtained
Object；
The third mixture and pH adjusting agent are mixed, obtain glass polishing with water base polishing fluid.
In the present invention, the water, built surfactant, lubricant, cerium oxide milling, dispersing agent, complexing agent, anti-
Water described in rotten agent, the type of grinding aid and pH adjusting agent, dosage and source and above-mentioned technical proposal, Compositional type surface-active
Agent, lubricant, cerium oxide milling, dispersing agent, complexing agent, preservative, grinding aid and pH adjusting agent type, dosage and source
Unanimously, details are not described herein.
Preferably dispersing agent, complexing agent, preservative and grinding aid is added with the rate of 1.0~2.0L/min in the present invention.
Present invention preferably employs pH adjusting agents to be adjusted to 8~11 with the pH value of water base polishing fluid for glass polishing.
In the present invention, the glass polishing is preferably 20~30 with the temperature of the whole preparation process of water base polishing fluid
℃。
The present invention provides a kind of water base cerium oxide polishing slurries of glass polishing, in terms of mass fraction, including following components:
Cerium oxide milling 20.0~55.0%；Built surfactant 0.1~3.0%；Dispersing agent 1~8%；Lubricant 0.1~
2%；Complexing agent 0.01~3%；Grinding aid 0.01~5.0%；PH adjusting agent 0.01~1.0%；Preservative 0.01~2%；
Surplus is water；The built surfactant is the compounding of nonionic surface active agent and anionic surfactant；
The nonionic surface active agent be selected from polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and
One of fatty glyceride is a variety of；Anionic surfactant is selected from neopelex, sodium laurate, hard
One of resin acid sodium and sodium succinate are a variety of；The dispersing agent is selected from sodium oxalate, calgon, sodium pyrophosphate, nitric acid
One of sodium, Sodium Polyacrylate and lauryl sodium sulfate are a variety of.The present invention by using above-mentioned content component, they
It cooperates, so that the suspended dispersed of polishing fluid is preferable, and product yield is higher after polishing.The results showed that the polishing
The layer height of liquid is lower, and the delamination of powder and liquid is able to maintain and is basically unchanged in the case where long-time is stood；Overall average is good
Rate is 88.01%~95.6%.
In order to further illustrate the present invention, below with reference to embodiment to the water base polishing fluid of glass polishing provided by the invention
And preparation method thereof be described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
It is formulated (weight percent):
Preparation process:
A. deionized water is added in the container of certain capacity, is separately added into built surfactant and lubricant, and with
300~700rpm continues stirring until evenly dispersed；
B. it is then slowly added into cerium oxide milling, stops stirring, solution left standstill 5h after stirring 1h；
C. stirring is opened, dispersing agent, complexing agent, preservative and grinding aid is separately added into, is stirred until homogeneous dispersion；
D. pH adjusting agent is added, pH value is adjusted to 8~11, is stirred until homogeneous dispersion, obtains glass polishing with water base
Polishing fluid.
It is commonly milled at present in technique for a kind of polishing, model: manufacturer: XJH-1008 newly praises boat abrasive material in Shenzhen
Grinding tool Co., Ltd.
Product is flat after the suspended dispersed and polishing of the water base polishing fluid of the glass polishing that the present invention prepares embodiment 1
The polishing milling that equal yield and current technique use carries out analysis contrast test, and tests its removal rate and roughness:
(1) observation of polishing fluid suspended dispersed
By polishing fluid obtained above, take a certain amount of polishing fluid sample into the 25mL pipe of standard, respectively by it is quiet
12h is set, for 24 hours, 48h, 72h observe the delamination of its powder and liquid, then sample is repeatedly shaken up to observation 12h again, for 24 hours,
After 48h, 72h, 96h, the delamination of powder and liquid in sample is observed again, as shown in table 1；
The polishing fluid suspended dispersed test result of 1 embodiment 1 of table preparation
The polishing milling suspended dispersed test result that the current technique of table 2 uses
By table 1 and table 2 it can be seen that the layer height of the polishing fluid under the formula of embodiment 1 is lower, and for a long time
The delamination of powder and liquid, which is able to maintain, under (72h) is stood is basically unchanged, the polishing milling precipitate height that technique uses at present
It is higher than under formula, illustrates that the suspended dispersed of the polishing fluid made from example 1 and redispersibility are better than current technique
It uses.
(2) the verifying analysis of the overall average yield of product, removal rate and roughness after polishing
Experimental facilities and condition
Machine table: double-face circular disc returns grinding and polishing ray machine；Upper disk material: capillary brush；Pedestal material: plane resin grinds skin；Mill
Liquid: polishing fluid made from embodiment 1 (is recycled) under certain density；Tonnage: 200KG；The speed of mainshaft: 30rpm adds
Chemical product: mobile phone glass screen；Process time: 240s；Subsequent processing: product needs to impregnate in water, cleans, is dry laggard after polishing
The quasi- quality testing of rower.
Test method:
It is fast in the hope of removal amount and removal with the thickness and record of the Thickness measuring instrument measurement processing front and back product of high standard
Rate；With the roughness of roughness tester test product；The overall average yield of product is thickness test, removal amount test and product
Surface quality reaches summarizing under Eligibility requirements.
It is total that the product after the polishing milling that current technique provides is polished with the polishing fluid that embodiment 1 provides is respectively adopted
Average yield analysis comparison, the results are shown in Table 2:
What the current technique of table 3 provided polishes the production after the polishing fluid that milling is provided with embodiment 1 is polished
Product overall average yield result
As shown in Table 3, it is provided using average total more current technique of yield of the polishing product of polishing fluid made from embodiment 1
Polishing fluid polishing after product yield height close to 6%, illustrate the yield of polishing product of polishing fluid provided by the present application compared with mesh
Preceding technique is greatly improved and reaches the product yield requirement of production.
The test of average removal rate and roughness
Product 10pcs after randomly selecting above scheme polishing respectively, every takes a point in roughness measuring instrument at random
On tested, every at random take a region removal flowmeter on tested, the results are shown in Table 4:
The removal rate of product and the test result of roughness after the polishing of 4 embodiment of table, 1 polishing fluid
| Serial number | Roughness Sa/nm | Removal amount/μm | Removal rate (μm/min) |
| 1 | 0.545 | 7.0 | 1.75 |
| 2 | 0.554 | 7.24 | 1.81 |
| 3 | 0.563 | 7.32 | 1.83 |
| 4 | 0.532 | 7.28 | 1.82 |
| 5 | 0.533 | 7.4 | 1.85 |
| 6 | 0.534 | 7.12 | 1.78 |
| 7 | 0.525 | 7.4 | 1.85 |
| 8 | 0.532 | 6.96 | 1.74 |
| 9 | 0.534 | 6.88 | 1.72 |
| 10 | 0.562 | 7.16 | 1.79 |
| Average value | 0.541 | 7.17 | 1.79 |
From 4 data of table: the mean roughness Sa value of product is 0.541nm after the polishing fluid polishing that embodiment 1 provides；
Average removal rate is 1.79 μm/min；This satisfies the quality of the performance requirement that producing line uses polishing fluid, while product also to accord with
Symphysis produces.
Embodiment 2
Formula
Preparation process:
A. deionized water is added in the container of certain capacity, is separately added into built surfactant and lubricant, and with
It is continued stirring until between 300~700rpm evenly dispersed；
B. it is then slowly added into cerium oxide milling, stops stirring, solution left standstill 5h after stirring 1h；
C. stirring is opened, dispersing agent, complexing agent, preservative and grinding aid is separately added into, is stirred until homogeneous dispersion；
D. pH adjusting agent is added, pH value is adjusted to 8~11, is stirred until homogeneous dispersion, obtains glass polishing with water base
Polishing fluid.
Product is flat after the suspended dispersed and polishing of the water base polishing fluid of the glass polishing that the present invention prepares embodiment 2
Equal yield, removal rate and roughness are tested:
(1) observation of polishing fluid suspended dispersed
By polishing fluid obtained above, take a certain amount of polishing fluid sample into the 25mL pipe of standard, respectively by it is quiet
12h is set, for 24 hours, 48h, 72h observe the delamination of its powder and liquid, then sample is repeatedly shaken up to observation 12h again, for 24 hours,
After 48h, 72h, 96h, the delamination of powder and liquid in sample is observed again, as shown in table 5；
The polishing fluid suspended dispersed test result of 5 embodiment 2 of table preparation
As can be seen from Table 5: the layer height of polishing fluid is lower, and long-time stand under powder and liquid layering feelings
Condition, which is able to maintain, to be basically unchanged, and illustrates that the suspended dispersed of the polishing fluid made from example 2 is preferable.
(2) the verifying analysis of the overall average yield of product, removal rate and roughness after polishing
Experimental facilities and condition
Machine table: double-face circular disc returns grinding and polishing ray machine；Upper disk material: capillary brush；Pedestal material: plane resin grinds skin；Mill
Liquid: polishing fluid (being recycled under certain density) prepared by embodiment 2；Tonnage: 200KG；The speed of mainshaft: 25rpm adds
Chemical product: mobile phone glass screen；Process time: 160s；Subsequent processing: product needs to impregnate in water, cleans, is dry laggard after polishing
The quasi- quality testing of rower.
Test method is similar with embodiment 1, and the method that it is detected for different types of glass product is different, product
Test philosophy is the same, and the parameter of test changes.
It is total that the product after the polishing milling that current technique provides is polished with the polishing fluid that embodiment 2 provides is respectively adopted
Average yield analysis comparison, the results are shown in Table 6:
What the current technique of table 6 provided polishes the production after the polishing fluid that milling is provided with embodiment 2 is polished
Product overall average yield result
As shown in Table 6: being averaged total more current process program of yield using the product that polishing fluid obtained tries out process program
Yield it is slightly higher, illustrate that the yield of the polishing liquid product obtained of embodiment 2 reaches the product yield requirement of production, meet producing line
Production technology use.
The test of average removal rate and reliability
Product 10pcs after randomly selecting above scheme polishing respectively, every takes a point in roughness measuring instrument at random
On tested, every at random take a region removal flowmeter on tested, the results are shown in Table 7:
The removal rate of product and the test result of roughness after the polishing of 7 embodiment of table, 2 polishing fluid
| Serial number | Removal amount/μm | Removal rate (μm/min) |
| 1 | 12.02 | 4.50 |
| 2 | 13.27 | 4.97 |
| 3 | 15.21 | 5.69 |
| 4 | 13.24 | 4.95 |
| 5 | 12.21 | 4.57 |
| 6 | 12.36 | 4.62 |
| 7 | 12.42 | 4.65 |
| 8 | 12.32 | 4.61 |
| 9 | 12.43 | 4.65 |
| 10 | 12.54 | 4.69 |
| Average value | 12.80 | 4.79 |
As shown in Table 7: use polishing liquid made from embodiment 2 polish product average removal rate for 4.79 μm/
Min meets the performance requirement that producing line uses polishing fluid, while the quality of product also complies with production.
The present invention polishes product to embodiment 2 and carries out related trusted test, and test result is shown in Table 8:
The related trusted test result of the polishing product of 8 embodiment 2 of table
| Test item | Quantity (PCS) | As a result |
| Static pressure test | 100 | OK |
| Sand paper steel ball falls | 100 | OK |
| 4PB | 100 | OK |
| Falling sphere test | 100 | OK |
As shown in Table 8, test item OK have met and have required on the quality reliability of production.
Embodiment 3
Formula
Preparation process:
A. deionized water is added in the container of certain capacity, is separately added into built surfactant and lubricant, and with
It is continued stirring until between 300~700rpm evenly dispersed；
B. it is then slowly added into cerium oxide milling, stops stirring, solution left standstill 5h after stirring 1h；
C. stirring is opened, dispersing agent, complexing agent, preservative and grinding aid is separately added into, is stirred until homogeneous dispersion；
D. pH adjusting agent is added, pH value is adjusted to 8~11, is stirred until homogeneous dispersion, obtains glass polishing with water base
Polishing fluid.
Product is flat after the suspended dispersed and polishing of the water base polishing fluid of the glass polishing that the present invention prepares embodiment 3
Equal yield, removal rate and roughness are tested:
(1) observation of polishing fluid suspended dispersed
By polishing fluid obtained above, take a certain amount of polishing fluid sample into the 25mL pipe of standard, respectively by it is quiet
12h is set, for 24 hours, 48h, 72h observe the delamination of its powder and liquid, then sample is repeatedly shaken up to observation 12h again, for 24 hours,
After 48h, 72h, 96h, the delamination of powder and liquid in sample is observed again, as shown in table 9；
The polishing fluid suspended dispersed test result of 9 embodiment 3 of table preparation
As can be seen from Table 9: the layer height of polishing fluid is lower, and long-time stand under powder and liquid layering feelings
Condition, which is able to maintain, to be basically unchanged.
(2) the verifying analysis of the overall average yield of product, removal rate and roughness after polishing
Experimental facilities and condition
Machine table: double-face circular disc returns grinding and polishing ray machine；Upper disk material: capillary brush；Pedestal material: plane resin grinds skin；Mill
Liquid: polishing fluid (being recycled under certain density) prepared by embodiment 3；Tonnage: 200KG；The speed of mainshaft: 25rpm adds
Chemical product: mobile phone glass screen；Process time: 160s；Subsequent processing: product needs to impregnate in water, cleans, is dry laggard after polishing
The quasi- quality testing of rower.
Test method is similar with embodiment 3, and the method that it is detected for different types of glass product is different, product
Test philosophy is the same, and the parameter of test changes.
It is total that the product after the polishing milling that current technique provides is polished with the polishing fluid that embodiment 3 provides is respectively adopted
Average yield analysis comparison, the results are shown in Table 10:
After the polishing fluid that the polishing milling and embodiment 3 that the current technique of table 10 provides provide is polished
Product overall average yield result
As shown in Table 10: be averaged total yield and current process program using the product that polishing fluid obtained tries out process program
Yield remain basically stable, illustrate that the yield of the polishing liquid product obtained of embodiment 3 reaches the product yield requirement of production, meet
The production technology of producing line uses.
The test of average removal rate and reliability
Product 10pcs after randomly selecting above scheme polishing respectively, every takes a point in roughness measuring instrument at random
On tested, every at random take a region removal flowmeter on tested, as a result as shown in table 11:
The removal rate of product and the test result of roughness after the polishing of 11 embodiment of table, 3 polishing fluid
| Serial number | Removal amount/μm | Removal rate (μm/min) |
| 1 | 2.41 | 3.42 |
| 2 | 3.32 | 3.24 |
| 3 | 5.24 | 3.74 |
| 4 | 3.34 | 3.65 |
| 5 | 2.62 | 3.78 |
| 6 | 2.42 | 3.96 |
| 7 | 2.37 | 3.73 |
| 8 | 2.83 | 3.42 |
| 9 | 2.41 | 3.67 |
| 10 | 2.56 | 3.42 |
| Average value | 2.95 | 3.60 |
As shown in Table 11: use polishing liquid made from embodiment 3 polish product average removal rate for 2.95 μm/
Min meets the performance requirement that producing line uses polishing fluid, while the quality of product also complies with production.
As seen from the above embodiment, the present invention provides a kind of water base polishing fluids of glass polishing, in terms of mass fraction, packet
Include following components: cerium oxide milling 20.0~55.0%；Built surfactant 0.1~3.0%；Dispersing agent 1~8%；Profit
Lubrication prescription 0.1~2%；Complexing agent 0.01~3%；Grinding aid 0.01~5.0%；PH adjusting agent 0.01~1.0%；Preservative
0.01~2%；Surplus is water；The built surfactant is nonionic surface active agent and anionic surface activity
The compounding of agent；The nonionic surface active agent is selected from polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxy
One of vinethene and fatty glyceride are a variety of；Anionic surfactant is selected from neopelex, the moon
One of sodium metasilicate, odium stearate and sodium succinate are a variety of；The dispersing agent is selected from sodium oxalate, calgon, burnt phosphorus
One of sour sodium, sodium nitrate, Sodium Polyacrylate and lauryl sodium sulfate are a variety of.The present invention is by using above-mentioned content
Component, their mutual compatibilities, so that the suspended dispersed of polishing fluid is preferable, and product yield is higher after polishing.Experimental result table
Bright: the layer height of the polishing fluid is lower, and the delamination of powder and liquid is able to maintain and is basically unchanged in the case where long-time is stood；
Overall average yield is 88.01%~95.6%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of water base cerium oxide polishing slurry of glass polishing, based on mass fraction, including following components:
Cerium oxide milling 20.0~55.0%；Built surfactant 0.1~3.0%；Dispersing agent 1~8%；Lubricant 0.1
~2%；Complexing agent 0.01~3%；Grinding aid 0.01~5.0%；PH adjusting agent 0.01~1.0%；Preservative 0.01~
2%；Surplus is water；
The built surfactant is the compounding of nonionic surface active agent and anionic surfactant；It is described non-
Ionic surfactant is selected from polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and fatty acid
One of glyceride is a variety of；Anionic surfactant is selected from neopelex, sodium laurate, odium stearate
With one of sodium succinate or a variety of；
The dispersing agent is selected from sodium oxalate, calgon, sodium pyrophosphate, sodium nitrate, Sodium Polyacrylate and dodecyl sulphate
One of sodium is a variety of.
2. the water base cerium oxide polishing slurry of glass polishing according to claim 1, which is characterized in that the Compositional type surface
The mass ratio of nonionic surface active agent and anionic surfactant is 1:0.9~1.1 in activating agent.
3. the water base cerium oxide polishing slurry of glass polishing according to claim 1, which is characterized in that the lubricant is selected from
One of polyethylene glycol 200, polyethylene glycol 400, Macrogol 600 and glycerol are a variety of.
4. the water base cerium oxide polishing slurry of glass polishing according to claim 1, which is characterized in that the complexing agent is selected from
One of ethylenediamine tetra-acetic acid, sodium gluconate, malic acid, sodium lactate and potassium citrate are a variety of.
5. the water base cerium oxide polishing slurry of glass polishing according to claim 1, which is characterized in that the grinding aid is selected from
One of potassium bromide, sodium bromide, potassium chloride, sodium chloride and potassium iodide are a variety of.
6. the water base cerium oxide polishing slurry of glass polishing according to claim 1, which is characterized in that the preservative is selected from
One of benzotriazole, potassium borate and Boratex are a variety of.
7. the water base cerium oxide polishing slurry of glass polishing according to claim 1, which is characterized in that the pH adjusting agent
Selected from ethanol amine, tetraethyl ammonium hydroxide, diethanol amine, triethanolamine, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, hydrogen
One of sodium oxide molybdena and potassium hydroxide are a variety of.
8. the preparation method of the water base cerium oxide polishing slurry of glass polishing described in a kind of claim 1~7 any one, including with
Lower step:
Water, built surfactant and mix lubricant is uniform, obtain the first mixture；
By first mixture and cerium oxide milling mixing, stirs, stand, obtain the second mixture；
Second mixture and dispersing agent, complexing agent, preservative and grinding aid are uniformly mixed, third mixture is obtained；
The third mixture and pH adjusting agent are mixed, obtain glass polishing with water base polishing fluid.
9. preparation method according to claim 8, which is characterized in that described in the speed addition with 1.0~2.0L/min
Dispersing agent, complexing agent, preservative and grinding aid.
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| CN110499102A (en) * | 2018-05-20 | 2019-11-26 | 深圳市得益达电子科技有限公司 | A kind of cerium oxide liquid suspension polishing liquid for glass polishing |
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| CN111423819A (en) * | 2020-04-17 | 2020-07-17 | 深圳市朗纳研磨材料有限公司 | Polishing solution and preparation method thereof |
| CN111647357A (en) * | 2020-06-18 | 2020-09-11 | 江苏可润光电科技有限公司 | Multipurpose polishing solution main liquid |
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| CN115141548A (en) * | 2021-03-15 | 2022-10-04 | 拓米(成都)应用技术研究院有限公司 | High-suspension cerium oxide polishing solution and polishing process and application thereof |
| CN115785818A (en) * | 2022-11-10 | 2023-03-14 | 湖北五方光电股份有限公司 | Polishing solution and preparation method and application thereof |
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| CN110499102A (en) * | 2018-05-20 | 2019-11-26 | 深圳市得益达电子科技有限公司 | A kind of cerium oxide liquid suspension polishing liquid for glass polishing |
| CN110951400A (en) * | 2019-11-18 | 2020-04-03 | 河北工业大学 | Polishing solution for reducing surface defects in CMP (chemical mechanical polishing) of multilayer cobalt interconnection barrier layer and preparation method thereof |
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| CN111647357A (en) * | 2020-06-18 | 2020-09-11 | 江苏可润光电科技有限公司 | Multipurpose polishing solution main liquid |
| CN115141548A (en) * | 2021-03-15 | 2022-10-04 | 拓米(成都)应用技术研究院有限公司 | High-suspension cerium oxide polishing solution and polishing process and application thereof |
| CN115141548B (en) * | 2021-03-15 | 2023-12-05 | 拓米(成都)应用技术研究院有限公司 | High-suspension cerium oxide polishing solution and polishing process and application thereof |
| CN113817413A (en) * | 2021-09-30 | 2021-12-21 | 苏州博洋化学股份有限公司 | High-performance glass cover plate polishing solution |
| CN114231183A (en) * | 2022-01-11 | 2022-03-25 | 广东富行洗涤剂科技有限公司 | Nano cerium oxide suspension for grinding and polishing glass and preparation method thereof |
| CN115785818A (en) * | 2022-11-10 | 2023-03-14 | 湖北五方光电股份有限公司 | Polishing solution and preparation method and application thereof |
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| CN116004122A (en) * | 2022-12-27 | 2023-04-25 | 嘉庚创新实验室 | Cerium dioxide polishing solution and preparation method thereof |
| CN117327451A (en) * | 2023-09-28 | 2024-01-02 | 中建材光芯科技有限公司 | Polishing mixture for polishing polymer optical fiber panel and preparation method and application thereof |
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