CN106479371A - A kind of high precision composite polishing liquid and preparation method thereof - Google Patents
A kind of high precision composite polishing liquid and preparation method thereof Download PDFInfo
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- CN106479371A CN106479371A CN201610670232.7A CN201610670232A CN106479371A CN 106479371 A CN106479371 A CN 106479371A CN 201610670232 A CN201610670232 A CN 201610670232A CN 106479371 A CN106479371 A CN 106479371A
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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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Abstract
A kind of high precision composite polishing liquid that the present invention is provided, is made up of following weight percent composition：Grinding agent 0.1%～50%, dispersant 0.01%～20%, suspending agent 0.01%～15%, corrosion inhibiter 0.1%～5%, balance of deionized water solvent, the polishing fluid are can achieve the two-forty to base material and polish mainly based on mechanical removal；And the preparation method has the advantages that production efficiency is high, continuity is strong, low cost, product fineness are high, while size distribution and homogeneity no requirement (NR) of the method to the raw material for grinding agent, the range of choice of grinding agent raw material is widened, as long as the powder body material for meeting particle mean size requirement is all applicable.
Description
Technical field
The present invention relates to Ultraprecise polished technical field, and in particular to a kind of high precision composite polishing liquid and its preparation side
Method.
Background technology
Be different from the finishing method of traditional purely mechanic or pure chemistry, chemically-mechanicapolish polish (CMP) by chemistry and machine
The comprehensive function of tool, polishes, so as to avoid the surface damage caused by simple mechanical polishing and by pure chemistry, the throwing for easily causing
Ray velocity is slow, surface smoothness and the shortcomings of polishing uniformity difference, thus is widely used in integrated circuit (IC), ultra-large collection
Become circuit (ULSI), hard disc of computer and optical glass surface Ultraprecise polished in, be gradually applied to mobile phone, flat board in recent years
The surface fine polishing of the metalworks such as shell, frame Deng electronic product.
Polishing fluid is one of key element of CMP, and the performance of polishing fluid directly affects the quality of surface of polished.Polishing fluid
General by ultrafine solids particle grinding agent (such as SiO2, α-Al2O3, CeO2 of micro/nano level etc.), surfactant, stabilizer,
Oxidant etc. constitutes.The species, physicochemical properties, particle size of polishing fluid abrasive material, particle dispersion and stability etc. all with
Polishing effect is closely related.
At present, the polishing fluid overwhelming majority for being sold on market only with the addition of a kind of grinding agent of component, but for same
A kind of base material, the composite polishing liquid for adding multicomponent grinding agent tend to obtain unexpected effect, such as
A kind of sial composite polishing liquid for sapphire polishing is described in CN201410255977.8, is thrown with respect to single silica
Light liquid, the polishing fluid can make workpiece improve polishing velocity while obtaining certain surface state；And for example patent
A kind of medal polish composite polishing liquid and preparation method thereof is described in CN201610039894.4, and the composite polishing liquid is in gold
Polishing efficiency is remarkably improved in category polishing, prevents abrasive material from producing in surface of workpiece and inlay, workpiece brightness is improved, is reduced
The intractability of next process, is suitable for promoting the use of；And for example patent No. CN201410308864.X describes a kind of new multiple
Metal-polishing liquid and preparation method thereof is closed, liquid energy meets each product, the polishing of parts is required for polishing, improve polishing effect
Rate height, cleaning performance, surface accuracy etc.；While also patent No. CN201410852457.5, CN201480049117.7,
CN201110298605.X etc..In composite polishing liquid, the grinding agent of different performance can play different effects, phase for workpiece
When in gradually being polished with the single polishing fluid of the grinding agent containing different performance to same workpiece, thus larger improve polishing effect
How rate, as the other grinding agent of micro/nano level has serious agglomeration in itself, ensure multicomponent grinding agent in polishing fluid
In dispersed come, be obtain high-quality composite polishing liquid difficult point, the dispersed of abrasive particles should be ensured, again
Ensure the dispersed of each grinding agent composition, be difficult to using the dispersed with stirring employed in above-mentioned patent.
It is presently used in the polishing fluid of high accuracy polishing, granularity to grinding agent powder, pattern and its particle size distribution
More and more higher is required, abrasive size is less, and size distribution is narrower, and homogeneity is better, could realize the overall situation of work piece surface
Planarization or even mirror effect, due to the performance requirement more and more higher for grinding agent powder, thus must purchase high-quality
Powder body material, not only increases the purchase cost of grinding agent, has also limited to the purchase channel of grinding agent raw material, therefore needs into one
Step ground is improved.
Content of the invention
The technical problem to be solved be for above-mentioned the deficiencies in the prior art and providing one kind has high dispersive, height
Stable, long-time is not settled, the high precision composite polishing liquid of high yield rate and preparation method thereof.
The present invention is that the adopted technical scheme that solves the above problems is：
The present invention provides a kind of high precision composite polishing liquid, is made up of following weight percent composition：
Grinding agent 0.1%～50%,
Dispersant 0.01%～20%,
Suspending agent 0.01%～15%,
Corrosion inhibiter 0.1%～5%,
Balance of deionized water solvent.
Further, the grinding agent be silica that average grain diameter is 0.1～5um, zirconium oxide, cerium oxide, aluminum oxide,
One or more in magnesia, titanium oxide.
Further, the dispersant be sodium metasilicate, sodium tripolyphosphate, calgon and sodium pyrophosphate, triethyl group oneself
Base phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyglycol ethylene glycol
One or more in ester.
Further, the suspending agent is methylcellulose, hydroxypropyl methyl cellulose, sodium carboxymethylcellulose, hydroxyl second
One or more in one or more in base cellulose and xanthans, sodium alginate, gum arabic, soybean protein glue are pressed
Mass ratio is 1：0.1～1 mixture for being formed.
Further, the corrosion inhibiter is chromate, molybdate, tungstates, vanadate, borate, Quadrafos, zinc
One or more in salt, phosphonic acids (salt), phosphine carboxylic acid, coloured glaze base benzothiazole, BTA, lignosulfonate；
A kind of preparation method of high precision composite polishing liquid, it is characterised in that comprise the following steps：
(1) by a certain percentage grinding agent and deionized water are added in sand mill, are ground by certain rotating speed and divide
Dissipate and process；
(2) after the slurry obtained in step (1) reaches certain dispersion effect, dispersant is added；
(3) slurry obtained through grinding, dispersion in step (2) is added and is stirred in homogenizer, and press one
Certainty ratio adds suspending agent, corrosion inhibiter；
(4) obtained slurry in step (3) is placed 24h nothing precipitation.
Further, described in described step (1), the mass percent of grinding agent and deionized water is：0.01～1：1.
Further, sand mill described in described step (1) is any in basket type, turbine type or rod pin-type sand mill
A kind of；The sand mill abrasive media is the zirconia ball of a diameter of 0.1～0.5mm；The sand mill rotating speed be 5000～
8000r/min；Milling time is 0.5～3h.
Further, in described step (2), in slurry, the size distribution of abrasive particles is 2D10≥D50≤0.5D90.
Further, homogenizer described in described step (3), its stirring slurry are the tooth-like dispersion impeller of periphery, stirring speed
Spend for 500～1000r/min, mixing time is 0.5～3h.
The beneficial effects of the present invention is：
Provided by the present invention a kind of for high precision composite polishing liquid, wide variety of oxide abrasive particle aerobic
Change titanium, cerium oxide, colloidal silica, zirconium oxide, aluminum oxide etc., its Mohs' hardness is followed successively by 5～6,7,7,8.5,9, from than
The soft oxide abrasive particle of polished base material matter is polished, and physical removal effect is weak and chemism is strong, polishing process
In main removed with chemical solution based on, can achieve the polishing of good to base material low rate, surface quality and low damage；From than polished
The hard oxide abrasive particle of base material matter is polished, and mainly based on mechanical removal, can achieve the two-forty to base material and throws
Light；
And the preparation method is ground decentralized processing, sand mill by introducing sand mill to the grinding agent in polishing fluid
Compared with the milling apparatus such as ball mill, roller mill, colloid mill, with production efficiency high, continuity is strong, low cost, product are thin
The advantages of spending high, using the shear action of the high rotary speed of sand mill and the shear action of thin abrasive media, Ke Yi
In the shorter time, the larger particles in grinding agent are crushed, the aggregate of relatively fine particle is opened, reduce the grain of abrasive particles
Degree distribution, while different abrasive particles are fully dispersed uniform, thus can prepare to add and appoints according to the needs of different substrate materials
Anticipate multiple different performances grinding agent composite polishing liquid, be simultaneously introduced new dispersant and suspending agent, so can guarantee that the throwing
Light liquid has high dispersive, high stable, and long-time is not settled, the feature of high yield rate, while the method is to the original for grinding agent
The size distribution of material and homogeneity no requirement (NR), have widened the range of choice of grinding agent raw material, as long as meeting particle mean size requirement
Powder body material is all applicable.
Specific embodiment
Lower mask body illustrates embodiments of the present invention, being only given for illustrative purposes of these embodiments, and
It is not intended that limitation of the invention, only for reference and explanation use, do not constitute the restriction to scope of patent protection of the present invention,
Because without departing from the spirit and scope of the present invention, many changes can be carried out to the present invention.
Embodiment 1
By silica (D10=2um, D50=3um, D90=10um), aluminum oxide (D10=1.8um, D50=3um, D90=
7um) by mass percentage 1:1 ratio is mixed into grinding agent, and with deionized water in mass ratio 0.5：1 adds in sand mill,
After stirring, with abrasive media as 0.2mm zirconia ball, 7000r/min rotating speed grinding distribution 2h, obtain polishing fluid slurry grain
Degree is distributed as D10=1.5um, D50=2.6um, D90=3.5um, addition are made into by calgon and lauryl sodium sulfate
Dispersant, dispersant addition are the 1% of grinding agent quality；Slurry good for grinding distribution is added in homogenizer, rotating speed
For 800r/min, add by hydroxypropyl methyl cellulose and xanthans in mass ratio 1 by grinding agent quality 2% first：0.5 is made into
Suspending agent, then add the corrosion inhibiter being made into by borate and coloured glaze base benzothiazole by grinding agent quality 2%, after stirring 1h,
24h nothing precipitation is placed, product is most long to be placed January and do not precipitate, and pH value is 7.5, and in alkalescent, Long-Time Service will not be to workpiece
Corrosion damage is caused with equipment surface.
Embodiment 2
By cerium oxide (D10=0.8um, D50=1um, D90=12um), aluminum oxide (D10=0.6um, D50=1um, D90=
3um), zirconium oxide (D10=0.5um, D50=1um, D90=6um) by by mass percentage 1:1：1 ratio is mixed into grinding agent,
And with deionized water in mass ratio 0.2：1 adds in sand mill, after stirring, with abrasive media as 0.2mm zirconia ball,
7500r/min rotating speed grinding distribution 3h, it is D to obtain polishing fluid slurry size distribution10=0.5um, D50=0.8um, D90=
1.2um, adds the dispersant being made into by sodium tripolyphosphate, calgon and triethyl group hexyl phosphoric acid, and dispersant addition is
The 2% of grinding agent quality；Slurry good for grinding distribution is added in homogenizer, rotating speed is 1000r/min, first by grinding
Agent quality 3% is added by hydroxyethyl cellulose and xanthans, soybean protein glue in mass ratio 1：0.8 suspending agent being made into, then
The corrosion inhibiter being made into by Quadrafos, zinc salt and lignosulfonate is added by grinding agent quality 3%, after stirring 2h, places 24h nothing
Precipitation, product is most long to be placed January and does not precipitate, and pH value is 6, and in faintly acid, Long-Time Service will not be made to workpiece and equipment surface
Become corrosion damage.
Embodiment 3
By magnesia (D10=0.2um, D50=0.5um, D90=2um), titanium oxide (D10=0.18um, D50=0.5um,
D90=3um) by by mass percentage 1:1 ratio is mixed into grinding agent, and with deionized water in mass ratio 0.6：1 adds sand milling
In machine, after stirring, with abrasive media as 0.2mm zirconia ball, 8000r/min rotating speed grinding distribution 2.5h, obtain polishing
Slurry material granularity is distributed as D10=0.16um, D50=0.3um, D90=0.5um, adds by sodium pyrophosphate, methyl anyl alcohol and fat
The dispersant that acid polyethylene glycol ester is made into, dispersant addition are the 0.5% of grinding agent quality；The good slurry of grinding distribution is added
Enter in homogenizer, rotating speed is 1000r/min, adds by methylcellulose, hydroxypropyl methyl by grinding agent quality 6% first
Cellulose and xanthans in mass ratio 1：1 suspending agent being made into, is then added by phosphine carboxylic acid and coloured glaze base benzene by grinding agent quality 4%
And the corrosion inhibiter that thiazole is made into, after stirring 3h, 24h nothing precipitation is placed, product is most long to be placed January and does not precipitate, and pH value is 6, is in
Faintly acid, Long-Time Service will not cause corrosion damage to workpiece and equipment surface.
Provided by the present invention a kind of for high precision composite polishing liquid, wide variety of oxide abrasive particle aerobic
Change titanium, cerium oxide, colloidal silica, zirconium oxide, aluminum oxide etc., its Mohs' hardness is followed successively by 5～6,7,7,8.5,9, from than
The soft oxide abrasive particle of polished base material matter is polished, and physical removal effect is weak and chemism is strong, polishing process
In main removed with chemical solution based on, can achieve the polishing of good to base material low rate, surface quality and low damage；From than polished
The hard oxide abrasive particle of base material matter is polished, and mainly based on mechanical removal, can achieve the two-forty to base material and throws
Light；
And the preparation method is ground decentralized processing, sand mill by introducing sand mill to the grinding agent in polishing fluid
Compared with the milling apparatus such as ball mill, roller mill, colloid mill, with production efficiency high, continuity is strong, low cost, product are thin
The advantages of spending high, using the shear action of the high rotary speed of sand mill and the shear action of thin abrasive media, Ke Yi
In the shorter time, the larger particles in grinding agent are crushed, the aggregate of relatively fine particle is opened, reduce the grain of abrasive particles
Degree distribution, while different abrasive particles are fully dispersed uniform, thus can prepare to add and appoints according to the needs of different substrate materials
Anticipate multiple different performances grinding agent composite polishing liquid, be simultaneously introduced new dispersant and suspending agent, so can guarantee that the throwing
Light liquid has high dispersive, high stable, and long-time is not settled, the feature of high yield rate, while the method is to the original for grinding agent
The size distribution of material and homogeneity no requirement (NR), have widened the range of choice of grinding agent raw material, as long as meeting particle mean size requirement
Powder body material is all applicable.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, other any Spirit Essences without departing from the present invention and the change that is made under principle, modification, replacement, combine, simplify,
Equivalent substitute mode is all should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of high precision composite polishing liquid, it is characterised in that consist of the following components in percentage by weight：
Grinding agent 0.1%～50%,
Dispersant 0.01%～20%,
Suspending agent 0.01%～15%,
Corrosion inhibiter 0.1%～5%,
Balance of deionized water solvent.
2. a kind of high precision composite polishing liquid according to claim 1, it is characterised in that：The grinding agent is average grain diameter
For one or more in the silica of 0.1～5um, zirconium oxide, cerium oxide, aluminum oxide, magnesia, titanium oxide.
3. a kind of high precision composite polishing liquid according to claim 1, it is characterised in that：The dispersant be sodium metasilicate,
Sodium tripolyphosphate, calgon and sodium pyrophosphate, triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose
One or more in derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
4. a kind of high precision composite polishing liquid according to claim 1, it is characterised in that：The suspending agent is Methyl cellulose
One or more in element, hydroxypropyl methyl cellulose, sodium carboxymethylcellulose, hydroxyethyl cellulose and xanthans, alginic acid
One or more in sodium, gum arabic, soybean protein glue are 1 in mass ratio：0.1～1 mixture for being formed.
5. a kind of high precision composite polishing liquid according to claim 1, it is characterised in that：The corrosion inhibiter be chromate,
Molybdate, tungstates, vanadate, borate, Quadrafos, zinc salt, phosphonic acids (salt), phosphine carboxylic acid, coloured glaze base benzothiazole, benzo three
One or more in azoles, lignosulfonate.
6. a kind of preparation method of high precision composite polishing liquid, it is characterised in that comprise the following steps：
(1) by a certain percentage grinding agent and deionized water are added in sand mill, be ground by certain rotating speed and dispersion at
Reason；
(2) after the slurry obtained in step (1) reaches certain dispersion effect, dispersant is added；
(3) slurry obtained through grinding, dispersion in step (2) is added and is stirred in homogenizer, and by certain than
Example adds suspending agent, corrosion inhibiter；
(4) obtained slurry in step (3) is placed 24h nothing precipitation.
7. a kind of high precision composite polishing liquid preparation method according to claim 5, it is characterised in that：Step (1)
Described in the mass percent of grinding agent and deionized water be：0.01～1：1.
8. a kind of high precision composite polishing liquid preparation method according to claim 5, it is characterised in that：Step (1)
Described in sand mill be basket type, turbine type or rod pin-type sand mill in any one；The sand mill abrasive media is straight
Footpath is the zirconia ball of 0.1～0.5mm；The sand mill rotating speed is 5000～8000r/min；Milling time is 0.5～3h.
9. a kind of high precision composite polishing liquid preparation method according to claim 5, it is characterised in that：Step (2)
In middle slurry, the size distribution of abrasive particles is 2D10≥D50≤0.5D90.
10. a kind of high precision composite polishing liquid preparation method according to claim 5, it is characterised in that：Step (3)
Described in homogenizer, its stirring slurry is the tooth-like dispersion impeller of periphery, and mixing speed is 500～1000r/min, and mixing time is
0.5～3h.
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