CN1113945C - Method for preparing metallic oxides sludge for chemical mechanical polishing for semiconductor - Google Patents
Method for preparing metallic oxides sludge for chemical mechanical polishing for semiconductor Download PDFInfo
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- CN1113945C CN1113945C CN99800657A CN99800657A CN1113945C CN 1113945 C CN1113945 C CN 1113945C CN 99800657 A CN99800657 A CN 99800657A CN 99800657 A CN99800657 A CN 99800657A CN 1113945 C CN1113945 C CN 1113945C
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- metal oxide
- sio
- pressure pump
- dispersion
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000004065 semiconductor Substances 0.000 title abstract description 8
- 238000005498 polishing Methods 0.000 title description 29
- 239000000126 substance Substances 0.000 title description 2
- 239000010802 sludge Substances 0.000 title 1
- 239000002002 slurry Substances 0.000 claims abstract description 43
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 229960001866 silicon dioxide Drugs 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 230000005540 biological transmission Effects 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 27
- 239000006185 dispersion Substances 0.000 abstract description 23
- 238000009826 distribution Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002955 isolation Methods 0.000 abstract description 3
- 239000003989 dielectric material Substances 0.000 abstract 2
- 239000011229 interlayer Substances 0.000 abstract 1
- 230000003449 preventive effect Effects 0.000 abstract 1
- 238000006748 scratching Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012530 fluid Substances 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 235000012431 wafers Nutrition 0.000 description 5
- 230000001133 acceleration Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
There is disclosed a process for preparing a metal oxide CMP slurry suitable for semiconductor devices, wherein a mixture comprising 1 to 50% by weight of a metal oxide and 50 to 99% by weight of water is mixed in a pre-mixing tank, transferred to a dispersion chamber with the aid of a transfer pump, allowed to have a flow rate of not less than 100 m/sec by pressurization with a high pressure pump, and subjected to counter collision for dispersion through two orifices in the dispersion chamber. The slurry has particles which are narrow in particle size distribution, showing an ultrafine size ranging from 30 to 500 nm. Also, the slurry is not polluted at all during its preparation and shows no tailing phenomena, so that it is preventive of mu -scratching. Therefore, it can be used in the planarization for shallow trench isolation, interlayer dielectrics and intermetal dielectrics through a CMP process.
Description
Background of invention
Invention field
The present invention relates generally to be used for the preparation method of the metal oxide paste of chemical-mechanical polishing of semiconductor (CMP), be particularly related to and utilize by metal oxide paste is collided with the opposite direction of injecting from two apertures at a high speed, and make this metal oxide paste except that the μ that demonstrates a kind of unusual minimizing-cut occurrence rate, can also have narrow particle size dispersion and superior dispersion stability and polishing speed.
Prior art
The CMP method is a kind of lithography, can be used in the semi-conductive manufacturing.When semi-conductor became microminiaturization along with more intensive multilayered structure, the complanation that can obtain by the CMP method was indispensable for highly integrated semi-conductor.
Generally, concerning metal oxide paste useful in the CMP method, except that requiring to have the high purity, also requiring to have good dispersibility and polishing speed and permission has the least possible defective after polishing, as μ-cut.
Except that purity, above-mentioned all requirements are all closely related with the granular size and the distribution of metal oxide.For granular size, smaller particles is preferred, because smaller particles can show better dispersion stability, and can provide μ-cut still less.But smaller particles is unfavorable for polishing efficiency, because particle is more little, polishing speed is slow more.Certainly, aspect particle size dispersion, particle preferably is distributed in the narrow size range.In other words, granular size is even more, will bring good more polish results.For example, when use had the slurry of granular size of wide region, the planeness on the surface of fretting corrosion was poor, and has a large amount of surperficial μ-cuts.
Therefore, when selecting to be used for the granular size of CMP slurry and distributing, must calculate polishing speed, dispersion stability and μ-cut occurrence rate.
United States Patent (USP) 5,382,272 disclose the preparation method of the polishing composition that shows high polishing speed.Said composition is based on silicon-dioxide and is used for the polished silicon wafer.Said composition is by silicon-dioxide is mixed in high-speed mixer with deionized water, and mixture is stirred in the stirring runner milling that contains a kind of medium of milling (ball).The matrix abrasive is by a kind of second kind of positively charged ion such as the Ce that add
4+And Zr
4+And be activated to strengthen polishing speed.The disclosed method of this patent has shortcoming.In the dispersion process of being finished by the collision between abrasive and the described ball, described ball tarnishes inevitably.In addition, the generation of tailing phenomenon makes that producing its particle has the slurry of narrow size distribution to become difficult.Say that further described ball suffers erosion and makes their dispersive ability descend in process of lapping.In fact, because slurry granular size to each other that is produced and distribution is obvious different, can not wish to obtain constant polishing ability from described slurry.
In another known preparation method, the rotary drum high speed that a kind of fluid is sold at German IKA is rotated and is collided with stator.Although this technology has been strengthened United States Patent (USP) 5,382,272 method still has a problem, is exactly that the result of wall collision corrodes stator and makes dispersive ability reduce significantly.
The granular size that all these known technology are produced is 1 micron.These particles can not be used for CMP too greatly.Particularly these particles if μ-cut occurred in isolation processes, will cause fatal infringement because there is μ-cut can not be used for the isolation of shallow ridges as the CMP slurry to the function and the output of semiconducter device.
Another technology that relates to the CMP slurry is disclosed among the WO patent No.9747430.Along with the use in the polished silicon wafer, the paste compound of this patent contains silicon-dioxide as a kind of abrasive, as the monoethanolamine of pH regulator agent with such as NH
4+, Cs
+And Ba
2+Additive.The pH regulator agent has been got rid of as KOH or NH
4The conventional pH regulator agent of OH may diffuse into the neutralized possibility of effect of pollutent of wafer in polishing process.But these slurries show low relatively scope from 1500～2500 dusts/minute polishing speed.In addition, do not mention the dispersing method of CMP slurry in this technology.
United States Patent (USP) 5,342,609 have described the method and apparatus that forms milk sap, wherein with the collision between the oil, cavatition and shearing stress in conjunction with utilization.Described device is called a kind of minisize fluid machine, is to become known for various purposes, in particular for emulsifying effect.But it is not used for the particles dispersed as metal oxide.
Use the example of minisize fluid machine referring to United States Patent (USP) 5,342,609 in the prior art.According to this patent, contain calcium and oxide anion granular mixture and in a minisize fluid machine, disperse to have the composition that granular size is 5 nanometers with production.Yet this composition is used for testing goal such as MRI, X-ray and ultrasonic, is not used in polished semiconductor.
Summary of the invention
Therefore an object of the present invention is to overcome existing problem in the prior art, and provide a kind of preparation method who is used for the metal oxide paste of chemical-mechanical polishing of semiconductor (CMP), can make metal oxide paste except that the μ that demonstrates a kind of unusual minimizing-cut occurrence rate by this method, can also have narrow particle size distribution and superior dispersion stability and polishing speed.
According to the present invention, the preparation method of the metal oxide chemical mechanical polishing slurry that is applicable to semiconducter device that described purpose can be passed through to be provided realizes, wherein will contain the metal oxide of 1～50 heavy % and the water of 50～99 heavy % mixes in a premix tank, by means of transmission pump by being forced into 50 normal atmosphere with high-pressure pump so that flow velocity is not less than 100 meter per seconds, mixture is transferred in the dispersing chamber, and in dispersing chamber, carry out the opposite direction collision and disperse by two apertures.
The simple description of accompanying drawing
The description of above and other objects of the present invention and the aspect embodiment by with reference to the accompanying drawings and will become obvious.
Fig. 1 represents according to the present invention the dispersion process synoptic diagram of metal oxide paste;
Fig. 2 is that the expression fluid passes through two apertures conceptual diagram of opposite direction collisions each other in dispersing chamber.
Detailed description of the present invention
To understand the preferred embodiment of the present patent application better with reference to accompanying drawing.
Fig. 1 represents according to the present invention the dispersion process synoptic diagram of metal oxide paste.As shown in the figure, metal oxide is with after water mixes equably in premix tank 1, and in the pipeline that metal oxide paste is introduced with high-pressure pump 3 links to each other, high-pressure pump 3 has assists transmission pump 2.By the acceleration of high-pressure pump 3, make flow velocity be not less than 100 meter per seconds, this slurry is injected dispersing chamber 4 by two apertures, in dispersing chamber 4, slurry disperses as the collision of fluidic wall, cavatition and shearing by the opposite direction collision of complexity.In the method for the invention, design is disperseing the back to keep diameter should reclaim so that final slurry is stable by a kind of way of recycling greater than the particle of 500 nanometers by collision.Check valve 5 is installed in before or after the high-pressure pump 3 to avoid backflow of slurry.
In general, the dispersion of metal oxide depends on its surface area.Surface-area is big more, and the metal oxide dispersiveness is good more.When carrying out oxidation under 1000 ℃ or higher temperature, the present invention can obtain any metal oxide that surface area is 20～300 meters squared per gram that has.Preferably be selected from by SiO
2, CeO
2, ZrO
2Or a kind of in the group formed of its mixture.
The metal oxide of selecting is mixed with water in premix tank, and the blended mode is that to make resulting metal oxide paste have solid content be 1～50 heavy %, preferred 5～30 heavy %.If premixed slurry has the solid content that is lower than 1 heavy %, then can not reach satisfied dispersion effect.On the other hand,, can cause the thixotroping phenomenon, cause the viscosity pole the earth to increase if solid content surpasses 50 heavy %.
Before being used for the CMP process, with this slurry dilution.The solid content of metal oxide paste that for example will be used for the dilution of CMP technology is to SiO
2Be controlled at 10～14 heavy %, to CeO
2Be controlled at 1～5 heavy %, to ZrO
2Be controlled in the scope of 4～8 heavy %, help polishing performance and material cost.
In the present invention, the degree of scatter of metal oxide and the fluid velocity of acceleration are proportional, and fluidic speed is proportional with the pressure in the high-pressure pump at orifice diameter place.Therefore, have the metal oxide paste of various particle size dispersion can be simply pressure by the control high-pressure pump obtain.
According to the present invention, its flow velocity of fluid that quickens by the pressure effect of high-pressure pump 3 is higher than 100 meter per seconds, preferred 350 meter per seconds.For reaching this flow velocity, requiring 3 pairs of flow velocitys of high-pressure pump is that 100 meter per seconds pressurize under 50 normal atmosphere, is that 350 meter per seconds pressurize under 500 normal atmosphere to flow velocity.Therefore any pressure pump is as long as pressure is 50 normal atmosphere or highlyer all can be used for the present invention.
As mentioned above, by two apertures that are provided with at dispersing chamber 4, will be introduced in the dispersing chamber 4 by the fluid that high-pressure pump is quickened, in dispersing chamber 4, fluid carries out complicated opposite direction collision as wall collision and cavatition, to form ultra-fine grain.Described aperture is to be made by engineering plastics, glass-reinforced plastic, carbon steel, stainless steel, pottery or diamond.Consider preferably ceramic or diamond from weather resistance.But these examples only are in order to illustrate rather than limit the present invention.
Consider and the tolerability of high-pressure pump and the dispersion efficiency of slurry that aperture 6 should have 0.05～0.5 millimeter, preferred 0.1～0.3 millimeter diameter.For example, if the diameter in aperture 6 is lower than 0.05 millimeter, under certain pressure condition, owing to increase the effect of acceleration, and the dispersion that metal oxide paste is obtained; But, therefore caused the productivity result of difference owing to reduced the turnout of unit time.On the other hand, if the diameter in aperture 6 greater than 0.5 millimeter, productivity has increased, but owing to need to keep the high-pressure pump of desired flow velocity, is worthless economically.
As shown in Figure 2, the aperture is tubulose and is designed to exit diameter (I
1) less than inlet diameter (I
2), improved the effect of the acceleration under certain pressure condition like this.As exit diameter (I
1) reduce to inlet diameter (I
2) a half, flow velocity is increased to 4 times.On mathematics, the production of the slurry of unit time is directly proportional with the square root of the sum of squares institute applied pressure of the exit diameter in aperture.When design dispersing technology system, the diameter in aperture and the pressure of high-pressure pump can decide by the treatment rate of considering slurry.
Consider the degree of scatter (super-refinement) of metal oxide, the pressure of this degree of scatter and high-pressure pump 3 and opposite direction collision frequency are proportional.In other words, when pressure increased, when collision frequency increased, the particle of metal oxide was littler, and the distribution of granular size is narrower and more even.
For the SiO that extremely is widely used for the CMP method
2Slurry, for example, when in case is being 0.2 millimeter by two diameters, pressure is to carry out one under the flow velocity of 350 meter per seconds in 500 atmospheric two apertures when colliding in the other direction, can obtain to be applicable to the particle that mean sizes is 140～150 nanometers that has of CMP.Certainly, be higher than 500 atmospheric pressure effects and produce littler particle, make particle size dispersion narrower.Yet, be higher than the same polishing effect of slurry that the slurry that is obtained under 500 normal atmosphere demonstrates and obtained under 500 normal atmosphere, as polishing speed and μ-cut occurrence rate.Therefore, if there is not difference on polish results, selecting alap pressure is favourable aspect Energy efficiency.On the other hand, compare, be lower than at pressure that prepared slurry has identical high polishing speed under 300 normal atmosphere, but produce more μ-cut with slurry prepared under 500 normal atmosphere.
Below listed embodiment be illustrated more clearly in principle of the present invention and practice to the person skilled in the art.These embodiment are not restriction the present invention, but to the explanation of some preferred embodiment of the present invention.
Embodiment 1
With surface area be 200 meters squared per gram 130 gram silicon-dioxide (as can trade mark " Aerosil 200 " by name be purchased from Degussa), the potassium hydroxide solution of 18 grams 20%, with 860 the gram deionized waters a volume be 1 cubic metre with the teflon-coating premix tank in mix, and this mixture transferred in the dispersing chamber with transmission pump (1～50 normal atmosphere of diaphram), in dispersing chamber, be that 0.4 millimeter and exit diameter are two apertures of 0.2 millimeter by inlet diameter, and by means of high-pressure pump (intensifier booster pump, 50-1,500 normal atmosphere) carry out the opposite direction collision with 500 atmospheric pressure, can obtain to be applicable to the slurry of CMP.Use the granular size analyzer,, measure granular size, particle size dispersion and the mean particle size of the sample of dispersing chamber as the analyzer of the trade mark " Zetasizer " by name sold by Malvern.The results are shown in Table 1.
Embodiment 2～6
Repeat the step of embodiment 1, the pressure of the high-pressure pump shown in the table 1 that different are to use.The results are shown in Table 1.
Embodiment 7
Repeat the step of embodiment 1, different is to use cerium dioxide (CeO
2, surface area 30 meters squared per gram) and replacement silicon-dioxide.The results are shown in Table 1.
Embodiment 8
Repeat the step of embodiment 1, different is to use zirconium dioxide (ZrO
2, surface area 30 meters squared per gram) and replacement silicon-dioxide.The results are shown in Table 1.
Embodiment 9～13
Repeat the step of embodiment 1, different is to use the pressure of the high-pressure pump shown in the table 1 and the number of times that collides in the other direction.The results are shown in Table 1.
Embodiment 14
Repeat the step of embodiment 1, different is not use 20% potassium hydroxide solution.
Table 1
Comparative Examples 1～9
| The embodiment sequence number | Metal oxide | Pressure (normal atmosphere) | Collision frequency | Solid content (%) | The pH value | Size distribution (nanometer) | Mean particle size (nanometer) |
| 1 | SiO 2 | 500 | 1 | 13 | 10.7 | 40～390 | 150 |
| 2 | SiO 2 | 300 | 1 | 13 | 10.9 | 50～520 | 170 |
| 3 | SiO 2 | 800 | 1 | 13 | 10.7 | 30～370 | 150 |
| 4 | SiO 2 | 1000 | 1 | 13 | 10.7 | 30～350 | 145 |
| 5 | SiO 2 | 1200 | 1 | 13 | 10.7 | 30～350 | 145 |
| 6 | SiO 2 | 1500 | 1 | 13 | 10.6 | 30～320 | 130 |
| 7 | CeO 2 | 500 | 1 | 13 | 6.8 | 40～550 | 178 |
| 8 | ZrO 2 | 500 | 1 | 13 | 7.3 | 40～500 | 180 |
| 9 | SiO 2 | 500 | 2 | 13 | 10.8 | 30～350 | 143 |
| 10 | SiO 2 | 500 | 5 | 13 | 10.6 | 30～280 | 135 |
| 11 | SiO 2 | 500 | 10 | 13 | 10.5 | 30～250 | 120 |
| 12 | SiO 2 | 1200 | 5 | 13 | 10.5 | 30～300 | 125 |
| 13 | SiO 2 | 2500 | 10 | 13 | 10.5 | 30～250 | 110 |
| 14 | SiO 2 | 500 | 1 | 13 | 4.5 | 40～390 | 153 |
| 15 | SiO 2 | 500 | 1 | 18 | 10.5 | 30～370 | 148 |
| 16 | SiO 2 | 500 | 1 | 25 | 10.5 | 30～360 | 145 |
| 17 | SiO 2 | 500 | 1 | 30 | 10.5 | 30～340 | 143 |
130 gram silicon-dioxide with commercially available surface area 200 meters squared per gram, the potassium hydroxide solution of 18 grams 20%, with 860 gram deionized waters be that 2 millimeters glass sphere joins in 2 liters the Dynomill shredder with 300 gram sizes, and under rate of dispersion shown in the table 2 and time conditions, disperse.The results are shown in Table 2.Comparative Examples 10
Repeat the step of Comparative Examples 1, different is uses cerium dioxide (CeO not existing under the condition of 20% potassium hydroxide solution
2, surface area is 30 meters squared per gram) and replacement silicon-dioxide.The results are shown in Table 2.Comparative Examples 11
Repeat the step of Comparative Examples 1, different is to use zirconium dioxide (ZrO
2, surface area is 30 meters squared per gram) and replacement silicon-dioxide.The results are shown in Table 2.
Table 2
Test case
| The Comparative Examples sequence number | Metal oxide | Rate of dispersion (commentaries on classics/per minute) | Jitter time (hour) | The pH value | Particle size dispersion (nanometer) | Mean particle size (nanometer) |
| 1 | SiO 2 | 1000 | 1 | 10.9 | 50～1200 | 456 |
| 2 | SiO 2 | 1500 | 1 | 10.9 | 500～1200 | 450 |
| 3 | SiO 2 | 2000 | 1 | 10.9 | 50～1100 | 450 |
| 4 | SiO 2 | 2500 | 1 | 10.8 | 50～950 | 430 |
| 5 | SiO 2 | 3000 | 1 | 10.7 | 50～800 | 420 |
| 6 | SiO 2 | 2000 | 2 | 10.8 | 50～1100 | 420 |
| 7 | SiO 2 | 2000 | 5 | 10.9 | 50～1100 | 400 |
| 8 | SiO 2 | 3000 | 2 | 10.7 | 50～750 | 370 |
| 9 | SiO 2 | 3000 | 5 | 10.7 | 50～750 | 350 |
| 10 | CeO 2 | 2000 | 1 | 7.3 | 70～1300 | 570 |
| 11 | ZrO 2 | 2000 | 1 | 6.7 | 80～1550 | 680 |
With embodiment 1,2,7,8 and Comparative Examples 1,10,11 in the slurry that the obtained testing experiment that carries out the polishing performance assessment.6 inches thick naked wafers that p-TEOS is applied are polishing with described slurry in Strabaugh 6EC type polishing machine under the following grinding condition:
Chassietype: IC1000/Suba IV Stacked (Rodel)
Press nog plate speed: 120 rev/mins (rpm)
Principal velocity: 120 rev/mins
Pressure: 6 pounds/square inch (psi)
Back-pressure: 0 pound/square inch
Temperature: 25 ℃
Slurry flow: the polishing of 150 ml/min was carried out 2 minutes.Measure of the change polishing speed by described wafer thickness.By means of TencorKLA type machine testing μ-cut.As a comparison, " SS-25 " slurry that Cabot is sold is as contrast.
The polishing ability of table 3 slurry
| Slurry | Particle size dispersion (nanometer) (on average) | Polishing performance | |
| Polishing speed (dust/minute) | The quantity of μ-cut | ||
| Embodiment 1 | 40～390(150) | 3550 | 0 |
| Embodiment 2 | 50～520(170) | 3570 | 12 |
| Embodiment 7 | 40～520(178) | 7210 | 50 |
| Embodiment 8 | 40～500(180) | 4830 | 42 |
| Comparative Examples 1 | 50～1200(456) | 3500 | 158 |
| Comparative Examples 10 | 70～1300(570) | 7210 | 290 |
| Comparative Examples 11 | 80～1550(680) | 6230 | 170 |
| SS-25 | 30～390(160) | 3430 | 123 |
As described above, with the CMP slurry of dispersing method of the present invention preparation than having advantage with the prepared slurry of traditional dispersing method.In the dispersing method of the present invention fluid carried out opposite direction collision and cavatition, and traditional dispersing method comprises and uses ball and only be that wall collides.Therefore, the particle of slurry of the present invention has narrower size distribution, and demonstrates the ultra-fine grain size of 30～500 nanometers.In addition, slurry of the present invention has little or no pollution in the whole process of its preparation, and does not show the tailing phenomenon, thereby has avoided μ-cut.Further, method of the present invention can be carried out under simple operations, and the degree of scatter of slurry depends on pressure and collision frequency, thereby slurry can be produced expeditiously again.The another one advantage of method of the present invention is that have can be with the ability of high productivity continuous production slurry.
Although by describing in detail with reference to some preferred embodiment, it should be understood that, the present invention can carry out various improvement within the spirit and scope of the present invention.Except that following claim, the present invention is unrestricted.
Claims (6)
1. preparation method who is applicable to the metal oxide CMP slurry of semiconducter device, wherein will contain the metal oxide of 1～50 heavy % and the water of 50～99 heavy % and in a premix tank, carry out the blended mixture, by means of a transmission pump by with high-pressure pump pressurization so that flow velocity is not less than 100 meter per seconds, mixture is transferred in the dispersing chamber, and in dispersing chamber, carry out the opposite direction collision and disperse by two apertures.
2. according to the process of claim 1 wherein that described metal oxide is selected from by silicon-dioxide (SiO
2), cerium dioxide (CeO
2), zirconium dioxide (ZrO
2) and composition thereof in the group formed.
3. according to the process of claim 1 wherein that described mixture is by pressurizeing so that flow velocity reaches 350 meter per seconds or higher with high-pressure pump.
4. according to the process of claim 1 wherein that the diameter range in described aperture is 0.05～0.5 millimeter.
5. according to the process of claim 1 wherein that the granulometric range of described slurry is 30～500 nanometers.
6. according to the process of claim 1 wherein that the exit diameter in described aperture is less than inlet diameter.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR39212/98 | 1998-09-22 | ||
| KR1019980039212A KR20000006595A (en) | 1998-09-22 | 1998-09-22 | Method for manufacturing metal dielectric slurry for cmp of semiconductor devices |
| KR39212/1998 | 1998-09-22 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1268967A CN1268967A (en) | 2000-10-04 |
| CN1113945C true CN1113945C (en) | 2003-07-09 |
Family
ID=19551460
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99800657A Expired - Lifetime CN1113945C (en) | 1998-09-22 | 1999-03-19 | Method for preparing metallic oxides sludge for chemical mechanical polishing for semiconductor |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1032615A1 (en) |
| JP (1) | JP2002526593A (en) |
| KR (1) | KR20000006595A (en) |
| CN (1) | CN1113945C (en) |
| TW (1) | TW440603B (en) |
| WO (1) | WO2000017282A1 (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20000055131A (en) * | 1999-02-03 | 2000-09-05 | 유현식 | Method for preparing metaloxide slurry for semiconductor element cmp |
| KR100310234B1 (en) * | 1999-08-20 | 2001-11-14 | 안복현 | Preparation method of metal oxide slurry for cmp of semiconductor |
| KR20020004425A (en) * | 2000-07-05 | 2002-01-16 | 안복현 | Cmp slurry and preparation method thereof |
| KR100341141B1 (en) * | 2000-07-26 | 2002-06-20 | 이종학 | Slurry for Polishing Inter Layer Dielectric of Semiconductor in Chemical Mechanical Polishing Process and Method for Preparing the Same |
| DE10054345A1 (en) * | 2000-11-02 | 2002-05-08 | Degussa | Aqueous dispersion, process for its preparation and use |
| DE10065027A1 (en) | 2000-12-23 | 2002-07-04 | Degussa | Aqueous dispersion, process for its preparation and use |
| EP1234800A1 (en) | 2001-02-22 | 2002-08-28 | Degussa Aktiengesellschaft | Aqueous dispersion, process for its production and use thereof |
| KR100781870B1 (en) * | 2001-05-14 | 2007-12-05 | 주식회사 하이닉스반도체 | Forming Method for Field Oxide of Semiconductor Device |
| DE10239144A1 (en) * | 2002-08-27 | 2004-03-18 | Degussa Ag | dispersion |
| KR100827591B1 (en) | 2006-11-27 | 2008-05-07 | 제일모직주식회사 | Chemical mechanical polishing slurry compositions and the precursor composition of the same |
| JP5360902B2 (en) * | 2009-11-12 | 2013-12-04 | 株式会社イズミフードマシナリ | Particle polishing method and particle polishing system |
| JP5906254B2 (en) * | 2010-12-28 | 2016-04-20 | サン−ゴバン セラミックス アンド プラスティクス，インコーポレイティド | Polishing slurry containing zirconia particles and method of using the polishing slurry |
| CN106450465A (en) * | 2016-11-21 | 2017-02-22 | 珠海光宇电池有限公司 | Preparation method of slurry of lithium-ion battery |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5575837A (en) * | 1993-04-28 | 1996-11-19 | Fujimi Incorporated | Polishing composition |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4057939A (en) * | 1975-12-05 | 1977-11-15 | International Business Machines Corporation | Silicon wafer polishing |
-
1998
- 1998-09-22 KR KR1019980039212A patent/KR20000006595A/en active Search and Examination
-
1999
- 1999-03-19 WO PCT/KR1999/000123 patent/WO2000017282A1/en not_active Application Discontinuation
- 1999-03-19 JP JP2000574185A patent/JP2002526593A/en active Pending
- 1999-03-19 EP EP99909365A patent/EP1032615A1/en not_active Withdrawn
- 1999-03-19 CN CN99800657A patent/CN1113945C/en not_active Expired - Lifetime
- 1999-09-07 TW TW088115383A patent/TW440603B/en not_active IP Right Cessation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5575837A (en) * | 1993-04-28 | 1996-11-19 | Fujimi Incorporated | Polishing composition |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1032615A1 (en) | 2000-09-06 |
| CN1268967A (en) | 2000-10-04 |
| JP2002526593A (en) | 2002-08-20 |
| TW440603B (en) | 2001-06-16 |
| KR20000006595A (en) | 2000-02-07 |
| WO2000017282A1 (en) | 2000-03-30 |
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