CN109294450A - A kind of mechanical dispersion process for mixed polishing solution - Google Patents
A kind of mechanical dispersion process for mixed polishing solution Download PDFInfo
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- CN109294450A CN109294450A CN201811414683.XA CN201811414683A CN109294450A CN 109294450 A CN109294450 A CN 109294450A CN 201811414683 A CN201811414683 A CN 201811414683A CN 109294450 A CN109294450 A CN 109294450A
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- polishing solution
- mixed polishing
- abrasive material
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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- Organic Chemistry (AREA)
- Grinding-Machine Dressing And Accessory Apparatuses (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
A kind of mechanical dispersion process for mixed polishing solution.Under the premise of no added chemical dispersant, based on mixing, both middle low frequency and high frequency ultrasound combined and abrasive material in mixed polishing solution were effectively disperseed；The selection of mixing frequencies can be dispersed into the reunion abrasive material of some tens of pm to a few micrometers in the abrasive material of hundreds of nanometers of partial sizes wherein mixing low and medium frequency is 25~45KHz；High frequency ultrasound frequency be 600~900KHz, to by low-mid-frequency ultrasonic disperse abrasive material disperse again, form the polish abrasive of individual particle；By stirring, so that the polish abrasive after dispersion is distributed in mixed polishing solution；It is converted into thermal energy for the prolonged mechanical-stretching motion mechanical energy of amplitude transformer in ultrasonic transducer, mixed polishing solution operating temperature is caused to increase, controls solenoid valve, it is cooling that recirculated cooling water is introduced ultrasonic water in real time, it is ensured that mixed polishing solution is in 22~28 DEG C；To mixed polishing solution object definition, including ontology and capacity.
Description
Technical field
The present invention relates to physical dispersion field of nanoparticles, are used for mixed polishing solution more particularly, to one kind needed for CMP
Mechanical dispersion process.
Background technique
CMP and photoetching, plated film and etching collectively constitute the big fundamental technology of semiconductor four.CMP technique is started in 20th century 80
Age is proposed by IBM Corporation of the U.S. earliest.In the semiconductor technologies at tip, CMP has become essential crucial work
Skill is flattening method most direct and maximally efficient at present.Main consumptive material needed for CMP process includes polishing pad and polishing fluid
Two kinds.Workpiece/device surface passes through after CMP process, and why surface roughness can be greatly lowered, and be mainly based upon
The principle of CMP " buffing is hard "
Main consumptive material needed for CMP process includes polishing fluid and polishing pad.Presently the most common polishing fluid is with SiO2Make
For abrasive material polishing fluid based on, commonly use abrasive size be 50~150nm.The pH value of the polishing fluid of the type be 9.8~10.5 it
Between, with this condition, the abrasive material form in polishing fluid is the most stable, and suitable dispersing agent and suspending agent are added in polishing fluid, can
Effectively avoid abrasive material that cluster and precipitating occurs.SiO2Polishing fluid has been obtained in the substrate polish such as Si, dielectric layer, sapphire
It is extensive to use, but for hard substrate, inert metal, polymer and using Ge as the polishing of the photoelectric material of representative, at present
There is no mature polishing fluid is available in the market.For the polishing of above-mentioned special material, mainly to existing SiO2Polishing fluid
It is modified to form new mixed polishing solution, for example hard substrate is polished, it can be in SiO2Appropriate hard abrasive material is added in polishing fluid, such as
Diamond or alumina abrasive, hard abrasive material help to improve polishing speed, and SiO2Mild abrasives then assist in removing residual
Stay in the Micro scratching on surface；It, can be in SiO to Ge substrate polish2Proper amount of hydrogen peroxide (H is added in polishing fluid2O2) and micro phosphorus
Acid (H3PO4)；It can be in SiO to polyimides (Polyimide, PI)2Appropriate ethylenediamine is added in polishing fluid.
Mixed polishing solution destroys original SiO due to the addition of new abrasive material or new chemical reagent2The chemistry of polishing fluid
Balance is formed a few micrometers or even the particle of some tens of pm magnitude partial size so that cluster and precipitating occur for abrasive material.According to
(T.G.Bifano, T.Dow.Ductile-regime grinding a new the technology for such as T.G.Bifano
Machining brittle materials [J] .Transaction of ASME, Vol.113, pp.185-189,1991) modeling
Shape Grinding Theory, when abrasive size reaches a few micrometers of magnitudes, then there is parts with brittle fracture in special material polishing process
Mechanism removing method, then the defects of polished surface will necessarily generate severe dell and depth scratch.Since mixing polishes
The diversity of liquid, therefore it is difficult to find that general, suitable, matched suspending agent and dispersing agent, so that all abrasive materials in mixed polishing solution
In the state for suspending, dispersing.Other than chemical reagent disperses abrasive material, mechanical ultrasound cavitation effect also contributes to mixing and throws
Abrasive material in light liquid is in dispersity.So-called ultrasonic cavitation refers to the physical action due to ultrasonic wave in a liquid, certainly
The rectangular temporary negative pressuren zone at part forms small vacuole or gas so as to cause liquid or the fracture of liquid-solid interface
Bubble.Cavitation bubbles can release huge energy when collapsing, and generates speed and be about 110m/s, have the micro- of strong impact power to penetrate
Stream, makes collision density be up to 1.5kg/cm2.By the huge destructive power that ultrasonic cavitation is contained, therefore can be in polishing fluid
Particle broken up, destroy the hard aggregation of abrasive material, and effectively control the size and distribution of particle.
Based on ultrasound cavitation effect, the abrasive material in polishing fluid is dispersed, extensive utilization has been obtained.Publication number
For CN102911606A patent application in a kind of sapphire polishing liquid and preparation method, be mentioned to deionized water solution,
SiO2Abrasive material, dispersing agent, complexing agent and pH adjusting agent keep abrasive material dispersion complete after mixing using ultrasound；(Li Ying, Lee such as Li Ying
Become dawn, Zhao Mengyue waits Nano diamond in aqueous medium to disperse behavioral study [J] superhard material engineering, 2010,22 (2): 5-
9) it uses op-10 as dispersing agent in diamond polishing liquid, and is aided with ultrasonication, finally obtain 0.788 μ of average grain diameter
M, the most suspension of fine grain 350nm.In polishing fluid, by the effective ionization equilibrium of chemical dispersant, then it is aided with ultrasonic sky
Change effect, the abrasive material less than 100nm and uniform particle sizes can be obtained really.But correlative study also indicates that, if do not had in polishing fluid
Have comprising chemical dispersant, the simple ultrasound cavitation effect for relying on low and medium frequency, is to be difficult to realize abrasive material in polishing fluid uniformly to divide
Scattered.(Wang Pei, Zhu Feng, Wang Zhiqiang ultrasonic wave and dispersing agent disperse behavior to Nano diamond to Wang Pei etc. in an aqueous medium
Influence [J] superhard material engineering, 2010,22 (2): 5-9) by relevant description of test, under low-mid-frequency ultrasonic dispersion,
Diamond abrasive average grain diameter is larger in polishing fluid, and partial size normal distribution is focused primarily upon in sub-micron to grain between micron dimension
Diameter, with this condition, if carrying out CMP process to workpiece, it will leave severe dell and depth scratch etc. in workpiece surface and lack
It falls into.
Supersonic frequency currently used for polishing fluid dispersion is generally 40KHz middle low frequency below, empty under this working frequency
Bubble growth time is long, and volume is big, and cavitation is strong, can rapidly make to be agglomerated into a few micrometers or even some tens of pm polish abrasive,
Under the action of the strong impact power caused by cavitation bubble moment closure vanishes, dispersion forms the polishing mill of hundreds of nanometers of partial sizes
Material.But under low-mid-frequency ultrasonic, cavitation bubble diameter in some tens of pm between hundreds of microns magnitude, when closure vanishes, institute
Although the microjet impact force of generation is strong, diameter is also more than a few micrometers of magnitudes, it is difficult to be embedded into be dispersed it is hundreds of
Between the polish abrasive gap of nanometer particle size, can not the polish abrasive of hundreds of nanometers of partial sizes, redisperse formed partial size 150nm with
Under polish abrasive.
Summary of the invention
The chemical dispersant for being difficult to find that a kind of General adaptive the purpose of the present invention is being directed to solution mixed polishing solution, or in
The problem of low frequency ultrasound can not be effectively disperseed the abrasive material in mixed polishing solution, one kind needed for providing CMP is for mixing
The mechanical dispersion process of polishing fluid.
The present invention the following steps are included:
1) under the premise of no added chemical dispersant, based on mixing, both middle low frequency and high frequency ultrasound were combined for mixed
Abrasive material in polishing fluid is closed to be effectively disperseed；
In step 1), the ontology polishing fluid of the mixed polishing solution can be SiO2Polishing fluid, pH value are 9.8~10.5；
The partial size of the abrasive material can be 80~150nm, can be modified to ontology polishing fluid, or hard abrasive material is added, or oxidation is added
The chemical reagent such as agent, corrosion inhibiter form mixed polishing solution；
2) about the selection of mixing frequencies, wherein mixing low and medium frequency is 25~45KHz, it can be fast and effeciently tens of micro-
Rice is dispersed into the abrasive material of hundreds of nanometers of partial sizes to a few micrometers of reunion abrasive material；High frequency ultrasound frequency is 600~900KHz, to
Abrasive material through being dispersed by low-mid-frequency ultrasonic is dispersed again, forms the polish abrasive of individual particle；
In step 2), the ultrasonic power of low frequency can be 0~400W in the mixing；The ultrasonic power of the high frequency can be
0~600W.
3) by stirring, so that the polish abrasive after dispersion is uniformly distributed in mixed polishing solution；
In step 3), electric stirring is can be used in the stirring, and the revolving speed of electric stirring can be 50~200rpm, every batch of
It after mixed polishing solution need to first pass through 2~5min of mechanism of mixing and stirring, can use, every batch of mixed polishing solution capacity
It can be 2~4L.
4) for the prolonged mechanical-stretching movement of amplitude transformer in ultrasonic transducer, mechanical energy is converted into thermal energy, causes to mix
The problem of closing the raising of polishing fluid operating temperature controls solenoid valve by programmable controller and opens and closes, in real time will circulation
Cooling water introduces ultrasonic water surrounding and is cooled down, it is ensured that mixed polishing solution is between 22~28 DEG C；
5) mixed polishing solution object is defined, including ontology and capacity.
Compared with prior art, technological progress of the invention, which is embodied in, replaces chemical dispersant using frequency mixing technique, has
Effect solves mixed polishing solution due to diversity, it is difficult to the chemical dispersant for finding a kind of General adaptive, in mixed polishing solution
Abrasive material the problem of being dispersed.Polish abrasive after ensuring to disperse in combination with auxiliary stirring is uniformly distributed in mixed polishing solution
In, and temperature control technology is combined to ensure that mixed polishing solution is in good chemical stabilization state.It is thrown based on above-mentioned mechanical mixing
The dispersing method of light liquid can effectively reduce device/workpiece surface generated severe dell and depth scratch etc. during CMP
Defect.
Detailed description of the invention
Fig. 1 is to be dispersed using frequency mixing ultrasonic to abrasive material in mixed polishing solution.
Fig. 2 is a kind of mechanical dispersion process for mixed polishing solution.
Fig. 3 is the temperature control schematic diagram based on PLC.
Specific embodiment
Following embodiment will the present invention is further illustrated in conjunction with attached drawing.
In the prior art, for mixed polishing solution, it is difficult to find the good chemical dispersant of suitability, low-mid-frequency ultrasonic without
Method is effectively disperseed abrasive material, and the present invention proposes a kind of based on mixing, auxiliary stirring and the mechanical mixing of temperature control throwing
Light liquid abrasive material dispersing method.So-called mixing is combined based on middle low frequency and high frequency, and collective effect is in mixed polishing solution
Abrasive material is dispersed.With the increase of frequency, cavitation bubble volume is gradually reduced, when supersonic frequency is greater than 600KHz, cavitation bubble
Volume less than 10 μm, the diameter for the microjet that when closure generates is effectively embedded into mixed polishing solution mill between hundreds of nanometers
Expect gap in, to by low-mid-frequency ultrasonic disperse abrasive material disperse again, formed single particle polish abrasive, such as
Shown in Fig. 1.In addition, the cavitation yield of mixed polishing solution will dramatically increase using frequency mixing ultrasonic, increased amplitude is greater than each frequency
The superposition of acoustic cavitation yield, and then improve the dispersion efficiency of abrasive material in mixed polishing solution.It is further enhanced with cavitation yield mixed
The interaction between polishing fluid cavitation bubble is closed, leads to the quick implosion of small particle cavitation bubble, further increases the energy of ultrasonic disperse
Power.Auxiliary stirring is the precipitating for avoiding a small amount of abrasive material, it is ensured that the abrasive material uniformity of dispersion is split in mixed polishing solution.Mixing is thrown
The chemical solvent of light liquid, especially complexing agent and corrosion inhibiter as the temperature rises, understand accelerated decomposition and volatilization, therefore polishing fluid
It usually works in room temperature.But the prolonged mechanical-stretching movement of amplitude transformer, mechanical energy are converted into thermal energy in ultrasonic transducer,
It will cause the raising of mixed polishing solution operating temperature.To ensure that mixed polishing solution is in the stable working condition of temperature, in machinery
Temperature-controlling system is introduced while dispersion.That is: it is 24~26 DEG C that temperature, which is arranged, in PLC, when temperature sensor detects ultrasonic water temperature
When degree is more than setting temperature, PLC controls solenoid valve and opens, and recirculated cooling water introduces ultrasonic water surrounding and cooled down.When ultrasonic water
Temperature detection be less than setting temperature, solenoid valve close, recirculated cooling water input stop, so that it is guaranteed that mixed polishing solution be in 22~
28 DEG C of working condition.
A kind of mechanical dispersion process for mixed polishing solution proposed by the invention, is primarily adapted for use in the polishing of small lot
In liquid.This is because ultrasonic wave is longitudinal wave, propagated along the height of mixed polishing solution, if the height of mixed polishing solution is more than
30cm, ultrasonic amplitude are obviously decayed, and cavitation intensity significantly reduces, therefore the present invention is mainly suitable for the mixing that capacity is 2~4L
The abrasive material of polishing fluid disperses.
A kind of mechanical dispersion process for mixed polishing solution proposed by the invention is suitable for small lot, with SiO2It throws
Mixed polishing solution of the light liquid as ontology efficiently solves what single abrasive material or compound abrasive in mixed polishing solution were difficult to disperse
Problem, available temperature is constant, the finely dispersed mixed polishing solution of abrasive material, to throw by adding surfactant with traditional
Abrasive material in light liquid is in the methods of dispersion and suspended state and compares, and has many advantages, such as easy to operate, wide adaptation range.
Referring to fig. 2 with 3, by taking polishing fluid Ge substrate as an example.
(1) in Fig. 2, room temperature cooling water first is supplemented in 2 surrounding of shell, cooling water entrance need to be with Fig. 3 cooling system phase
Even；
(2) in Fig. 2, it is added the ultrasonic deionized water of 1L, thermocouple 3 is by the temperature of real-time detection ultrasound deionized water；
(3) in Fig. 2, low-mid-frequency ultrasonic energy converter 4, frequency 40KHz, power 250W are opened, and at the same time opening
High-frequency transducer 6, frequency 800KHz, power 450W；
(4) in Fig. 2, in the container 8 for containing mixed polishing solution, the SiO after being watered first is added2Polishing fluid, volume is about
For 2.5L；
(5) stirring motor 11 (stirring motor is fixed on support base 7 by support rod 9 and support rod 10), stirring are opened
Motor 11 is connect by stirring rod 12 with blade 5, and band movable vane piece rotates, revolving speed 80rpm；
(6) SiO after above-mentioned be watered2In polishing fluid, suitable H is added2O2With micro H3PO4, total volume is about
2.8L, pH value is obtained to be reduced to about 8.8 after mixing from 10.2 before originally mixing, after abundant ultrasonic and stirring 3min, by compacted
Dynamic pump mixed polishing solution is introduced into CMP tool；
(7) polishing fluid temperature controls.Such as Fig. 3, PLC set temperature is 26 DEG C.Thermocouple 10 in real time passes ultrasonic coolant-temperature gage
Defeated to arrive temperature transmitter 9, when ultrasonic coolant-temperature gage is more than 26 DEG C, temperature transmitter 9 exports high level to PLC, by PLC
CPU operation, since both ends level signal is there are difference, PLC controls solenoid valve 2 and opens.It by check valve 1 and is opened by hot cooling water
The solenoid valve 2 opened be flowed into cooling system (cooling system include closed loop cooler 3, closed cycle water pump 4, condenser 5,
The components such as water circulating pump 6 and check valve 8), the cooling water flowed out from cooling system is introduced in ultrasonic water four by check valve 7
Zhou Jinhang is cooling.When ultrasonic coolant-temperature gage is detected less than 26 DEG C, temperature transmitter 9 exports low level and controls solenoid valve 2 to PLC, PLC
It closes, recirculated cooling water input stops, it is ensured that mixed polishing solution is in 26 ± 2 DEG C；
Based on the dispersing method of above-mentioned mechanical mixed polishing solution, produced by the surface Ge can be effectively reduced during CMP
Severe dell and depth scratch the defects of, surface of polished roughness be less than 1nm.
Claims (5)
1. a kind of mechanical dispersion process for mixed polishing solution, it is characterised in that the following steps are included:
1) under the premise of no added chemical dispersant, based on mixing, both middle low frequency and high frequency ultrasound, which had combined, throws mixing
Abrasive material is effectively disperseed in light liquid；
2) about the selection of mixing frequencies, wherein mixing low and medium frequency is 25~45KHz, can fast and effeciently some tens of pm extremely
A few micrometers of reunion abrasive material, is dispersed into the abrasive material of hundreds of nanometers of partial sizes；High frequency ultrasound frequency is 600~900KHz, to having led to
The abrasive material for crossing low-mid-frequency ultrasonic dispersion is dispersed again, forms the polish abrasive of individual particle；
3) by stirring, so that the polish abrasive after dispersion is uniformly distributed in mixed polishing solution；
4) for the prolonged mechanical-stretching movement of amplitude transformer in ultrasonic transducer, mechanical energy is converted into thermal energy, mixing is caused to be thrown
The problem of raising of light liquid operating temperature, controls solenoid valve by programmable controller and opens and closes, in real time by circulating cooling
Water introduces ultrasonic water surrounding and is cooled down, it is ensured that mixed polishing solution is between 22~28 DEG C；
5) mixed polishing solution object is defined, including ontology and capacity.
2. a kind of mechanical dispersion process for mixed polishing solution as described in claim 1, it is characterised in that in step 1), institute
The ontology polishing fluid for stating mixed polishing solution is SiO2Polishing fluid, pH value are 9.8~10.5.
3. a kind of mechanical dispersion process for mixed polishing solution as described in claim 1, it is characterised in that in step 1), institute
The partial size for stating abrasive material is 80~150nm, is modified to ontology polishing fluid, or hard abrasive material is added, or oxidant, inhibition is added
Agent chemical reagent forms mixed polishing solution.
4. a kind of mechanical dispersion process for mixed polishing solution as described in claim 1, it is characterised in that in step 2), institute
The ultrasonic power for stating low frequency in mixing is 0~400W；The ultrasonic power of the high frequency is 0~600W.
5. a kind of mechanical dispersion process for mixed polishing solution as described in claim 1, it is characterised in that in step 3), institute
Stirring is stated using electric stirring, the revolving speed of electric stirring is 50~200rpm, every batch of mixed polishing solution need to first pass through mixing and
It after 2~5min of mechanism of stirring, can use, every batch of mixed polishing solution capacity is 2~4L.
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| CN205613356U (en) * | 2016-01-15 | 2016-10-05 | 天津西美半导体材料有限公司 | Aluminium oxide polish configuration device |
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2018
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|---|---|---|---|---|
| CN102173426A (en) * | 2011-01-06 | 2011-09-07 | 清华大学 | Preparation method for SiO2 sol with high evenness degree |
| CN103980819A (en) * | 2014-05-28 | 2014-08-13 | 南京航空航天大学 | Method for preparing high-dispersion ultrafine alumina polishing solution |
| CN205613356U (en) * | 2016-01-15 | 2016-10-05 | 天津西美半导体材料有限公司 | Aluminium oxide polish configuration device |
| WO2018079334A1 (en) * | 2016-10-28 | 2018-05-03 | 株式会社トクヤマ | Fumed silica and production method therefor |
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