CN109294450B - Mechanical dispersion method for mixing polishing solution - Google Patents
Mechanical dispersion method for mixing polishing solution Download PDFInfo
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- CN109294450B CN109294450B CN201811414683.XA CN201811414683A CN109294450B CN 109294450 B CN109294450 B CN 109294450B CN 201811414683 A CN201811414683 A CN 201811414683A CN 109294450 B CN109294450 B CN 109294450B
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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
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- 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
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Abstract
A mechanical dispersion method for mixing polishing liquid. On the premise of no chemical dispersant, the grinding materials in the mixed polishing solution are effectively dispersed by combining the medium-low frequency ultrasonic with the high-frequency ultrasonic based on mixing; the mixing frequency is selected, wherein the low frequency in the mixing is 25-45 KHz, and the agglomerated abrasive materials with the particle size of tens of micrometers to several micrometers can be dispersed into abrasive materials with the particle size of hundreds of nanometers; the high-frequency ultrasonic frequency is 600-900 KHz, and the abrasive materials which are dispersed by the medium-low frequency ultrasonic are dispersed again to form single-particle polishing abrasive materials; the dispersed polishing abrasive is distributed in the mixed polishing solution by stirring; aiming at the problem that the mechanical energy of long-time mechanical telescopic movement of an amplitude transformer in an ultrasonic transducer is converted into heat energy to cause the working temperature of the mixed polishing solution to rise, an electromagnetic valve is controlled, circulating cooling water is introduced into ultrasonic water cooling in real time, and the mixed polishing solution is ensured to be at 22-28 ℃; a mixed slurry object is defined, including a body and a volume.
Description
Technical Field
The invention relates to the field of physically dispersing nano particles, in particular to a mechanical dispersing method for mixing polishing liquid, which is required by CMP.
Background
CMP and photoetching, film plating and etching together form a semiconductor four-base process. CMP technology began in the 80 s of the 20 th century and was first proposed by IBM corporation in the united states. CMP has become an indispensable critical process in sophisticated semiconductor technology, the most direct and effective planarization method at present. The main consumables required for the CMP process include both polishing pad and polishing liquid. After the surface of the workpiece/device is subjected to the CMP process, the surface roughness of the workpiece/device can be greatly reduced, mainly based on the principle of CMP of' soft grinding and hardening
The main consumables required for the CMP process include a polishing liquid and a polishing pad. The most commonly used polishing solution is SiO 2 As the polishing liquid of the abrasive, the particle size of the abrasive is 50-150 nm. The pH value of the polishing solution is 9.8-10.5, under the condition, the form of the abrasive in the polishing solution is most stable, and a proper amount of dispersing agent and suspending agent are added into the polishing solution, so that the occurrence of clusters and precipitation of the abrasive can be effectively avoided. SiO (SiO) 2 Polishing solutions have been widely used for polishing substrates such as Si, dielectric layers, and sapphire, but no mature polishing solutions are currently available on the market for polishing hard substrates, inert metals, polymers, and photovoltaic materials typified by Ge. For the special materialsIs mainly used for polishing the prior SiO 2 The polishing solution is modified to form a new mixed polishing solution, such as polishing a hard substrate, which can be used in SiO 2 The polishing solution is added with a proper amount of hard abrasive such as diamond or alumina abrasive, the hard abrasive helps to improve the polishing rate, and SiO 2 The soft abrasive is helpful to remove micro scratches remained on the surface; polishing Ge substrate, can be performed on SiO 2 Adding proper hydrogen peroxide (H) into the polishing solution 2 O 2 ) And a trace amount of phosphoric acid (H) 3 PO 4 ) The method comprises the steps of carrying out a first treatment on the surface of the For Polyimide (PI) can be prepared on SiO 2 And adding proper amount of ethylenediamine into the polishing solution.
The mixed polishing solution damages the original SiO due to the addition of new abrasive materials or new chemical reagents 2 The chemical balance of the polishing solution causes the abrasive to be clustered and precipitated to form particles with the particle size of several micrometers to tens of micrometers. According to T.G.Bifano et al (T.G.Bifano, T.Dow.Ductile-regime grinding a new technology for machining brittle materials [ J)]Transaction of ASME, vol.113, pp.185-189,1991) the grinding theory of shaping, when the grain size of the abrasive reaches several micrometers, the mechanical action removing mode of brittle fracture exists in the polishing process of special materials, and the polished surface inevitably has defects such as severe pits, deep scratches and the like. Because of the variety of mixed polishing solutions, it is difficult to find a general, suitable, matched suspending and dispersing agent, so that all the abrasive materials in the mixed polishing solution are in a suspended, dispersed state. In addition to dispersing the abrasive by the chemical agent, the mechanical ultrasonic cavitation effect also helps to disperse the abrasive in the mixed slurry. Ultrasonic cavitation is the formation of local temporary negative pressure areas in a liquid due to the physical action of ultrasonic waves, thereby causing the liquid or liquid-solid interface to break and form tiny cavitation bubbles or air bubbles. The cavitation bubbles or bubbles can release huge energy when collapsing, and generate micro-jet with a speed of about 110m/s and strong impact force, so that the collision density is as high as 1.5kg/cm 2 . Because of the huge destructive power of ultrasonic cavitation, particles in the polishing solution can be scattered, hard agglomeration of the abrasive is destroyed, and the size and distribution of the particles are effectively controlled.
Based on the ultrasonic cavitation effect, the abrasive in the polishing solution is dispersed, and the method has been widely used. In a sapphire polishing solution and preparation method, patent application publication No. CN102911606A mentions that the polishing solution is prepared by a method comprising the steps of dissolving in deionized water and SiO 2 The grinding material, the dispersing agent, the complexing agent and the pH regulator are mixed and then completely dispersed by adopting ultrasonic; li Ying et al (Li Ying, li Bianxiao, zhao Mengyue, et al. Study of nanodiamond dispersion behavior in aqueous Medium [ J)]Superhard material engineering 2010,22 (2): 5-9) using op-10 as dispersing agent in diamond polishing solution, and ultrasonic treatment to obtain suspension with average particle size of 0.788 μm and minimum particle size of 350 nm. In the polishing solution, the grinding material with the particle size smaller than 100nm and uniform particle size can be truly obtained through effective ionization balance of a chemical dispersing agent and the assistance of ultrasonic cavitation effect. However, related researches also show that if the polishing solution does not contain chemical dispersing agents, uniform dispersion of the abrasive in the polishing solution is difficult to achieve by simply relying on ultrasonic cavitation effect at medium and low frequencies. Wang Pei et al (Wang Pei, zhu Feng, wang Zhijiang. Effect of ultrasonic waves and dispersants on the dispersing behavior of nanodiamonds in aqueous media [ J]The ultra-hard material engineering 2010,22 (2): 5-9) shows that under the condition of medium-low frequency ultrasonic dispersion, the average grain diameter of diamond abrasive in the polishing solution is larger, the normal grain diameter distribution is mainly concentrated on the grain diameter between submicron and micron level, and under the condition, if the CMP process is carried out on a workpiece, the defects such as heavy pits, deep scratches and the like are left on the surface of the workpiece.
At present, the ultrasonic frequency used for dispersing the polishing solution is generally lower than the medium frequency of 40KHz, at the working frequency, the cavitation bubbles grow for a long time, have large volume and strong cavitation, can quickly agglomerate polishing abrasive materials with a plurality of micrometers to tens of micrometers, and disperse to form polishing abrasive materials with a particle size of hundreds of nanometers under the action of strong impact force generated by instant closing and breaking of the cavitation bubbles. However, in the case of medium-low frequency ultrasound, the cavitation bubble diameter is in the order of tens of micrometers to hundreds of micrometers, and when the device is closed and broken, the generated microjet has strong impact force, but the diameter is in the order of more than several micrometers, so that the microjet is difficult to be embedded into gaps of already dispersed polishing abrasives with the particle size of hundreds of nanometers, and the polishing abrasives with the particle size of hundreds of nanometers cannot be redispersed to form the polishing abrasives with the particle size of less than 150nm.
Disclosure of Invention
The invention aims at solving the problem that a general adaptive chemical dispersing agent is difficult to find in mixed polishing solution or the problem that medium-low frequency ultrasonic cannot effectively disperse abrasive materials in the mixed polishing solution, and provides a mechanical dispersing method for the mixed polishing solution, which is required by CMP.
The invention comprises the following steps:
1) On the premise of no chemical dispersant, the grinding materials in the mixed polishing solution are effectively dispersed by combining the medium-low frequency ultrasonic with the high-frequency ultrasonic based on mixing;
in step 1), the bulk polishing liquid of the mixed polishing liquid may be SiO 2 The pH value of the polishing solution is 9.8-10.5; the grain size of the abrasive can be 80-150 nm, the bulk polishing liquid can be modified, or hard abrasive is added, or chemical reagents such as oxidant, corrosion inhibitor and the like are added to form mixed polishing liquid;
2) Regarding the selection of mixing frequency, wherein the low frequency in the mixing is 25-45 KHz, the agglomerated abrasive materials of tens of micrometers to several micrometers can be rapidly and effectively dispersed into abrasive materials with the particle size of hundreds of nanometers; the high-frequency ultrasonic frequency is 600-900 KHz, and the abrasive materials which are dispersed by the medium-low frequency ultrasonic are dispersed again to form single-particle polishing abrasive materials;
in the step 2), the ultrasonic power of the low frequency in the mixing can be 0-400W; the high frequency ultrasonic power may be 0 to 600W.
3) The dispersed polishing abrasive is uniformly distributed in the mixed polishing solution by stirring;
in the step 3), the stirring can be electric stirring, the rotating speed of the electric stirring can be 50-200 rpm, each batch of mixed polishing solution can be used after the mechanical action of mixing and stirring is carried out for 2-5 min, and the capacity of each batch of mixed polishing solution can be 2-4L.
4) Aiming at the problem that the working temperature of the mixed polishing solution is raised due to the long-time mechanical telescopic movement of the amplitude transformer in the ultrasonic transducer, the electromagnetic valve is controlled to be opened and closed by the programmable controller, and circulating cooling water is introduced into the periphery of ultrasonic water for cooling in real time, so that the mixed polishing solution is ensured to be between 22 and 28 ℃;
5) A mixed slurry object is defined, including a body and a volume.
Compared with the prior art, the invention has the advantages that the technology progress is realized by adopting the mixing technology to replace the chemical dispersing agent, so that the problem that the mixed polishing solution is difficult to find a universal adaptive chemical dispersing agent due to diversity and the abrasive in the mixed polishing solution is dispersed is effectively solved. Meanwhile, the dispersed polishing abrasive is ensured to be uniformly distributed in the mixed polishing liquid by combining auxiliary stirring, and the mixed polishing liquid is ensured to be in a good chemical stable state by combining a temperature control technology. Based on the dispersion method of the mechanical mixed polishing solution, the defects of severe pit, deep scratch and the like generated in the CMP process of the surface of a device/workpiece can be effectively reduced.
Drawings
FIG. 1 illustrates the dispersion of abrasive materials in a mixed polishing solution using mixed ultrasound.
Fig. 2 is a mechanical dispersion method for mixing polishing solutions.
Fig. 3 is a schematic diagram of PLC-based temperature control.
Detailed Description
The invention will be further illustrated by the following examples in conjunction with the accompanying drawings.
In the prior art, aiming at the mixed polishing solution, a chemical dispersing agent with good suitability is difficult to find, and medium-low frequency ultrasonic cannot effectively disperse the abrasive, the invention provides a mechanical mixed polishing solution abrasive dispersing method based on mixing, auxiliary stirring and temperature control. The mixing is based on a combination of low and medium frequencies and high frequencies, which act together to disperse the abrasive in the mixed slurry. Along with the increase of the frequency, the volume of cavitation bubbles gradually decreases, when the ultrasonic frequency is larger than 600KHz, the volume of cavitation bubbles is smaller than 10 mu m, the diameter of microjet generated during closing is hundreds of nanometers, the microjet is effectively embedded into a gap between the abrasive materials of the mixed polishing solution, and the abrasive materials which are dispersed by medium-low frequency ultrasonic are dispersed again to form single-particle polishing abrasive materials, as shown in figure 1. In addition, by adopting mixing ultrasound, the cavitation yield of the mixed polishing solution is obviously increased, and the increased amplitude is larger than the superposition of the acoustic cavitation yields of all frequencies, so that the dispersion efficiency of the abrasive in the mixed polishing solution is improved. Meanwhile, the cavitation yield further enhances the interaction between the cavitation bubbles of the mixed polishing solution, so that the cavitation bubbles with small particle size are quickly implosion, and the ultrasonic dispersion capacity is further improved. The auxiliary stirring is to prevent a small amount of abrasive from precipitating and ensure the uniformity of the dispersed abrasive to be placed in the mixed polishing solution. Chemical solvents, particularly complexing agents and corrosion inhibitors, that mix with the polishing slurry accelerate decomposition and volatilization as the temperature increases, so the slurry typically operates at room temperature. However, the long-time mechanical telescopic movement of the amplitude transformer in the ultrasonic transducer can cause the working temperature of the mixed polishing solution to rise by converting mechanical energy into heat energy. In order to ensure that the mixed polishing solution is in a working state with stable temperature, a temperature control system is introduced while mechanical dispersion is carried out. Namely: the PLC sets the temperature to be 24-26 ℃, and when the temperature sensor detects that the ultrasonic water temperature exceeds the set temperature, the PLC controls the electromagnetic valve to be opened, and circulating cooling water is introduced into the periphery of the ultrasonic water for cooling. When the ultrasonic water temperature detection is smaller than the set temperature, the electromagnetic valve is closed, and the input of circulating cooling water is stopped, so that the mixed polishing solution is ensured to be in a working state of 22-28 ℃.
The mechanical dispersion method for mixing the polishing solution is mainly suitable for small batches of polishing solutions. This is because ultrasonic waves are longitudinal waves, and propagate along the height of the mixed polishing liquid, and if the height of the mixed polishing liquid exceeds 30cm, the ultrasonic amplitude is significantly attenuated and the cavitation intensity is significantly reduced, so that the invention is mainly suitable for dispersing the abrasive of the mixed polishing liquid with the capacity of 2-4L.
The mechanical dispersion method for mixing the polishing solution is suitable for small batches and uses SiO 2 The mixed polishing solution taking the polishing solution as the body effectively solves the problem that single abrasive or mixed abrasive in the mixed polishing solution is difficult to disperse, can obtain the mixed polishing solution with constant temperature and uniform abrasive dispersion, and is compared with the traditional mixed polishing solution which is prepared by adding a surfactantCompared with the methods of dispersing and suspending the abrasive, the method has the advantages of simple operation, wide application range and the like.
Referring to fig. 2 and 3, a polishing solution Ge substrate is taken as an example.
(1) In fig. 2, normal temperature cooling water is replenished around the shell 2, and the cooling water inlet and outlet are connected with the cooling system of fig. 3;
(2) In fig. 2, 1L of ultrasonic deionized water is added, and the thermocouple 3 detects the temperature of the ultrasonic deionized water in real time;
(3) In fig. 2, the mid-low frequency ultrasonic transducer 4 is turned on at 40KHz with power of 250W, and the high frequency ultrasonic transducer 6 is turned on at 800KHz with power of 450W;
(4) In FIG. 2, siO after adding water is added into a container 8 for containing the mixed polishing solution 2 The volume of the polishing solution is about 2.5L;
(5) The stirring motor 11 is started (the stirring motor is fixed on the supporting seat 7 through the supporting rod 9 and the supporting rod 10), the stirring motor 11 is connected with the blade 5 through the stirring rod 12 to drive the blade to rotate, and the rotating speed of the stirring motor is 80rpm;
(6) SiO after the water is added 2 Adding a proper amount of H into the polishing solution 2 O 2 And trace amount of H 3 PO 4 The total volume is about 2.8L, the pH value is reduced from 10.2 before the original mixing to about 8.8 after the mixing, and after the full ultrasonic treatment and stirring for 3min, the mixed polishing solution is introduced into the CMP equipment by a peristaltic pump;
(7) And controlling the temperature of the polishing solution. As shown in fig. 3, the plc set temperature was 26 ℃. The thermocouple 10 transmits the ultrasonic water temperature to the temperature transmitter 9 in real time, when the ultrasonic water temperature exceeds 26 ℃, the temperature transmitter 9 outputs high level to the PLC, and the PLC controls the electromagnetic valve 2 to be opened due to the difference value of level signals at two ends through CPU operation in the PLC. The heated cooling water flows into a cooling system (the cooling system comprises a closed circulation cooler 3, a closed circulation water pump 4, a condenser 5, a circulation water pump 6, a one-way valve 8 and the like) through a one-way valve 1 and an opened electromagnetic valve 2, and the cooling water flowing out of the cooling system is introduced into the periphery of ultrasonic water for cooling through a one-way valve 7. When the ultrasonic water temperature detection is less than 26 ℃, the temperature transmitter 9 outputs a low level to the PLC, the PLC controls the electromagnetic valve 2 to be closed, the input of circulating cooling water is stopped, and the mixed polishing solution is ensured to be at 26+/-2 ℃;
based on the dispersion method of the mechanical mixed polishing solution, the defects of severe pit, deep scratch and the like generated in the CMP process of the Ge surface can be effectively reduced, and the surface roughness after polishing is less than 1nm.
Claims (2)
1. A mechanical dispersion method for mixing polishing solutions, characterized by comprising the steps of:
1) On the premise of no chemical dispersant, the grinding materials in the mixed polishing solution are effectively dispersed by combining the medium-low frequency ultrasonic with the high-frequency ultrasonic based on mixing; the bulk polishing solution of the mixed polishing solution is SiO 2 The pH value of the polishing solution is 9.8-10.5; the grain diameter of the abrasive is 80-150 nm, the bulk polishing liquid is modified, or hard abrasive is added, or oxidant and corrosion inhibitor chemical reagent are added to form mixed polishing liquid;
2) Regarding the selection of mixing frequency, wherein the low frequency in the mixing is 25-45 KHz, the agglomerated abrasive materials of tens of micrometers to several micrometers can be rapidly and effectively dispersed into abrasive materials with the particle size of hundreds of nanometers; the high-frequency ultrasonic frequency is 600-900 KHz, and the abrasive materials which are dispersed by the medium-low frequency ultrasonic are dispersed again to form single-particle polishing abrasive materials;
3) The dispersed polishing abrasive is uniformly distributed in the mixed polishing solution by stirring; the stirring adopts electric stirring, the rotating speed of the electric stirring is 50-200 rpm, each batch of mixed polishing solution can be used after being subjected to the mechanical action of mixing and stirring for 2-5 min, and the capacity of each batch of mixed polishing solution is 2-4L;
4) Aiming at the problem that the working temperature of the mixed polishing solution is raised due to the long-time mechanical telescopic movement of the amplitude transformer in the ultrasonic transducer, the electromagnetic valve is controlled to be opened and closed by the programmable controller, and circulating cooling water is introduced into the periphery of ultrasonic water for cooling in real time, so that the mixed polishing solution is ensured to be between 22 and 28 ℃;
5) A mixed slurry object is defined, including a body and a volume.
2. The mechanical dispersion method for mixed polishing solutions as claimed in claim 1, wherein in the step 2), the ultrasonic power of the low and medium frequencies in the mixing is 0 to 400W; the ultrasonic power of the high frequency is 0-600W.
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| CN108687669A (en) * | 2018-05-10 | 2018-10-23 | 太原理工大学 | A kind of liquid circulating apparatus of ultrasonic cavitation auxiliary stirring Magnetorheologicai polishing liquid |
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| CN102173426B (en) * | 2011-01-06 | 2012-11-14 | 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 |
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| 《双频哨声空化模型的研究》;于云虎 等;《声学技术》;20101231;第29卷(第6期);第200-201页 * |
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