CN104726028A - Chemical mechanical polishing liquid and use method thereof - Google Patents
Chemical mechanical polishing liquid and use method thereof Download PDFInfo
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- CN104726028A CN104726028A CN201310697623.4A CN201310697623A CN104726028A CN 104726028 A CN104726028 A CN 104726028A CN 201310697623 A CN201310697623 A CN 201310697623A CN 104726028 A CN104726028 A CN 104726028A
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- polishing
- polishing fluid
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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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- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The present invention relates to a polishing liquid for a barrier layer. The polishing liquid comprises water, a cerium oxide abrasive, an organic dispersant, a complexing agent, and a corrosion inhibitor, and does not contain the oxidizing agent. According to the present invention, the polishing liquid of the present invention does not require the additional oxidizing agent addition, and provides high polishing rate on silicon dioxide (TEOS) and the barrier layer Ta or Ti, the corrosion of the oxidizing agent on the copper wire surface rate, and the generation of the dish-shaped concave groove and other defects during the polishing process are avoided, and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid, particularly relate to the polishing fluid that a kind of abrasive grains is cerium dioxide.
Background technology
Chemical-mechanical planarization (CMP) technology is that low cost manufactures the method for flat substrate surfaces the most reliably at present, it carries out usually in two steps: the first step removes copper fast by special formulation polishing fluid, after removal copper, second step removes the blocking layer below copper.
At present, the barrier polishing solution reported, generally needs to comprise oxygenant, to form metal oxide layer at blocking layer dielectric surface in polishing process, then by mechanical abrasive action, this zone of oxidation is removed to realize removing the continuous polishing on blocking layer.But the interpolation of oxygenant may produce multiple negative effect.As in acid condition, the interpolation of oxygenant easily causes the problems such as dish-shaped groove or corrosion to copper cash, patent CN1955249A discloses a kind of blocked acidic layer polishing fluid, it uses pH scope to be 2-4, with hydrogen peroxide, ammonium persulphate etc. for oxygenant, in polishing process, be very easy to the generation causing copper line surface corrosion default, therefore need in polishing fluid to add macro-corrosion inhibitor.And for example patent CN1696235A discloses the blocked acidic layer polishing fluid that a kind of pH is less than 7.0, and it exists the risk of oxygenant to etching of copper lines equally.The corrodibility of alkali barrier polishing fluid to copper reduces relatively, but conventional oxygenant is as H2O2, persulphates etc. in the basic conditions stability are not high, therefore oxygenant is separately packed by general requirement in packing of product transportation, being added by oxygenant is more in use mixed in polishing fluid, this obviously increases the transport management cost of product.
On the other hand, research for barrier polishing solution is reported mainly based on colloidal sol silica abrasive system, usually all need in such polishing fluid to add oxygenant to obtain higher blocking layer Ti, Ta polishing speed and adjustable Cu polishing speed, but the polishing speed of TEOS is relatively low, in order to obtain high TEOS polishing speed, also need higher solid content, this not only adds cost, also there is the risk of blocked pipeline.Take silicon-dioxide as the alkali barrier polishing fluid of abrasive material as patent CN101302405A discloses a kind of, in polishing fluid, silicon-dioxide solid content is under the condition of 14%, under the effect of guanidinesalt, the polishing speed of TaN can be greater than 1000A/min, but the polishing speed of TEOS is all less than 1500A/min.
Cerium oxide abrasives has high TEOS polishing speed, is subject to extensive concern in the industry.On the other hand, cerium oxide self has higher oxidation characteristic, and therefore it demonstrates the application characteristic of many uniquenesses to the polishing of metal medium.CN1872900 discloses a kind of chemical mechanical polishing liquid containing cerium oxide abrasive particles, but only relates to polishing cerium oxide polishing being applied to TEOS and SiN in this polishing fluid.Due to during to TEOS and SiN polishing, usually do not need to add oxygenant, therefore this section of patent does not discuss the impact of oxygenant on base material, and may corroding of how avoiding oxygenant to produce base material.And relate to the polishing of blocking layer and copper, usually need to add oxygenant, therefore the polishing composition jointly existed for cerium oxide abrasive particles and oxygenant is to polishing substrate, and what impact such as barrier material or copper etc. have, and not yet there are clear and definite theory or data instruction in this area.
Summary of the invention
The invention discloses a kind of take cerium oxide as the CMP polishing fluid of abrasive material, this polishing fluid does not need additionally to add oxygenant, to silicon-dioxide (TEOS), blocking layer Ta or Ti, there is high polishing speed simultaneously, to avoid in polishing process oxygenant to the generation of the defects such as the corrosion of copper line surface and dish-shaped groove, and reduce production cost.
The invention provides a kind of polishing fluid for blocking layer, comprise water, cerium oxide abrasives, organic dispersing agent, complexing agent, and corrosion inhibitor, and not containing oxygenant in this polishing fluid.
Wherein, the concentration of cerium oxide abrasives is mass percent 0.1%-5%, and the median size of cerium oxide abrasives is 60-160 nanometer, and average grain size is 10-60 nanometer.
Wherein, organic dispersing agent is selected from one or more in polyacrylic acid, polyoxyethylene glycol, Polyvinylpyrolidone (PVP).Optimization polypropylene acid.The molecular weight of polyacrylic molecular weight 3000-5000, described polyoxyethylene glycol is 3000-1000, the molecular weight of described Polyvinylpyrolidone (PVP) is 3000-10000.Wherein, the concentration of organic dispersing agent is mass percent 0.001%-0.5%.
Wherein, complexing agent is selected from one or more in L-arginine, Padil, citric acid and acetic acid.Preferred Padil.The concentration of complexing agent is mass percent 0.1%-1%.
Wherein, corrosion inhibitor is benzotriazole compounds.Corrosion inhibitor is preferably benzotriazole and/or amino-1,2, the 4-triazole of 3-.The concentration of corrosion inhibitor is mass percent 0.01-0.1%.
Wherein, water is deionized water, and the surplus of this polishing fluid is water.
Wherein, polishing fluid is also further containing pH adjusting agent, and concrete pH adjusting agent can be KOH or H
2sO
4.
Wherein, the pH value of polishing fluid is 7.5-12.0.
Positive progressive effect of the present invention is: CMP polishing fluid of the present invention take cerium dioxide as abrasive, do not need to add excess oxygen agent, higher polishing speed can be had to silicon-dioxide (TEOS), blocking layer Ta and Ti simultaneously, avoid the generation of oxygenant to defects such as copper cash dish grooves in the corrosion of copper line surface and polishing process, and reduce production cost.Meanwhile, this polishing fluid pH is within the scope of 7.5-12, relative acidic conditions, has higher polishing speed to silicon-dioxide and blocking layer Ta or Ti, and oxygenant can be avoided in polishing process the generation of the defects such as the corrosion of copper line surface and dish-shaped groove.
Embodiment
Set forth advantage of the present invention further below by specific embodiment, but protection scope of the present invention is not only confined to following embodiment.
Agents useful for same of the present invention and raw material are all commercially.The cerium oxide particle used in polishing fluid is first separated into the aqueous dispersions of original concentration 10wt% to 20wt% before product configuration through organic dispersing agent, the particle diameter of particle is on average to amount to diameter, and its median size is measured by the Nano-ZS90 laser particle size analyzer of Malvern company; The grain fineness number of the cerium oxide particle used in polishing fluid is measured by Japanese Shimadzu LabXXRD-6100 type X-ray diffractometer.First cerium oxide is added in setting concentration organic dispersing agent solution liquid and mix, again by the component except abrasive grains according to content listed in table, mix in deionized water, required pH value is adjusted to KOH, then the dispersion of abrasive particles of organic dispersing agent dispersion is added, if pH declines, be adjusted to required pH value with KOH, and supply percentage composition to 100wt% with deionized water, can chemical mechanical polishing liquid be obtained.
Table 1 gives chemical mechanical polishing liquid Example formulations of the present invention, and table 2 and 3 gives chemical mechanical polishing liquid comparative example of the present invention formula.The following stated percentage composition is mass percentage content.In formula, chemical reagent used is market buying.
Table 1 chemical mechanical polishing liquid Example formulations of the present invention
Table 2 chemical mechanical polishing liquid embodiment of the present invention comparative example
Table 3 chemical mechanical polishing liquid embodiment of the present invention comparative example
Effect example
With the chemical mechanical polishing slurry of polishing fluid 1-6 and comparative example 1-16 in above-described embodiment, polishing is carried out to blank Cu, TEOS, Ti and Ta wafer respectively, polishing condition is identical, burnishing parameters is as follows: Logitech polishing pad, downward pressure 3psi, rotary speed/rubbing head rotating speed=60/80rpm, polishing time 60s, chemical machinery throws flow rate of slurry 100mL/min.Polishing wafer coupons used forms by commercially available (such as U.S. SVTC company produces) 8 inches of plated film wafer coupons.The RT-7O/RG-7B tester that in Cu, Ti and Ta wafer coupons that polishing is used, Cu, Ti and Ta layer thickness is produced by NAPSON company records, and the NANO SPEC6100 tester that TEOS NANO Matrics company produces records.Namely obtain the removal speed of Cu, Ti and Ta divided by polishing consumes time by the thickness difference recorded before and after polishing.Polishing time is 1 minute.Concrete outcome as table 4, shown in 6.
Static corrosion is evaluated: under 40 DEG C of environment, fresh blank Cu wafer is put into corresponding polishing fluid dipping 15 minutes, measure Cu film thickness difference before and after dipping, thickness difference is excellent at 0-10A, thickness difference is good at 10-50A, thickness difference is general at 50-100A, and thickness difference is poor at >100A.Concrete outcome is as shown in table 7.
Saucerization is evaluated: adopt Semitech854 figure wafer to measure the saucerization of 80 micron metal block polishings after 1 minute, the blank Cu wafer of polishing condition copper, cup depth is by scanning electronic microscope S4800(Hitachi high technologies corp) measure.Concrete outcome is as shown in table 7.In table 4-7, the polishing effect of polishing fluid embodiment 1-6 of the present invention and comparative example 1-6 is compared and show, corresponding polishing fluid in embodiment 1-6, high polishing speed is shown to TEOS, higher polishing speed be also show to Ta and Ti simultaneously, and copper surface imperfection is less, without obviously corrosion, the graphical wafer saucerization degree of depth is more shallow.Comparative example 1-3 take cerium oxide as abrasive material, and with the addition of oxygenant, its polishing effect compares and shows, the interpolation of oxygenant improves obviously to the polishing speed of Cu, Ta and Ti, but produce significantly corrosion on copper surface, the graphical wafer saucerization degree of depth is also obviously deeper than embodiment result simultaneously; Comparative example 4-6 take silicon-dioxide as abrasive material, polish results shows, the polishing speed of TEOS is general lower, when adding oxygenant, the polishing speed of Cu, Ta and Ti is higher, but produce significantly corrosion on copper surface, the graphical wafer saucerization degree of depth is also obviously deeper than embodiment result simultaneously; When not adding oxygenant (comparative example 5,6), the polishing speed of Cu, Ta and Ti is very low, can not meet polishing requirement.
Table 4 chemical mechanical polishing liquid embodiment of the present invention polish results compares
Table 5 chemical mechanical polishing liquid embodiment of the present invention polish results compares
Table 6 chemical mechanical polishing liquid comparative example of the present invention polish results compares
Table 7 chemical mechanical polishing liquid comparative example of the present invention polish results compares
Should be understood that, wt% of the present invention all refers to mass percentage.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (15)
1. for the polishing fluid on blocking layer, comprise water, cerium oxide abrasives, organic dispersing agent, complexing agent, and corrosion inhibitor, it is characterized in that, not containing oxygenant in described polishing fluid.
2. polishing fluid as claimed in claim 1, it is characterized in that, the concentration of described cerium oxide abrasives is mass percent 0.1%-5%.
3. polishing fluid as claimed in claim 1, it is characterized in that, the median size of described cerium oxide abrasives is 60-160 nanometer, and average grain size is 10-60 nanometer.
4. polishing fluid as claimed in claim 1, is characterized in that, described organic dispersing agent be selected from polyacrylic acid, polyoxyethylene glycol, Polyvinylpyrolidone (PVP) one or more.
5. polishing fluid as claimed in claim 4, is characterized in that, the molecular weight of described polyacrylic molecular weight 3000-5000, described polyoxyethylene glycol is 3000-1000, the molecular weight of described Polyvinylpyrolidone (PVP) is 3000-10000.
6. polishing fluid as claimed in claim 1, it is characterized in that, the concentration of described organic dispersing agent is mass percent 0.001%-0.5%.
7. polishing fluid as claimed in claim 1, is characterized in that, described complexing agent be selected from L-arginine, Padil, citric acid and acetic acid one or more.
8. polishing fluid as claimed in claim 1, it is characterized in that, the concentration of described complexing agent is mass percent 0.1%-1%.
9. polishing fluid as claimed in claim 1, it is characterized in that, described corrosion inhibitor is benzotriazole compounds.
10. polishing fluid as claimed in claim 9, is characterized in that, described corrosion inhibitor is amino-1,2, the 4-triazole of benzotriazole and/or 3-.
11. polishing fluids as claimed in claim 1, is characterized in that, the concentration of described corrosion inhibitor is mass percent 0.01-0.1%.
12. polishing fluids as claimed in claim 1, it is characterized in that, described water is deionized water.
13. polishing fluids as claimed in claim 1, is characterized in that, described polishing fluid is also further containing pH adjusting agent.
14. polishing fluids as claimed in claim 13, it is characterized in that, described pH adjusting agent is KOH or H
2sO
4.
15. polishing fluids as claimed in claim 1, is characterized in that, the pH value of described polishing fluid is 7.5-12.0.
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| CN201310697623.4A CN104726028A (en) | 2013-12-18 | 2013-12-18 | Chemical mechanical polishing liquid and use method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740108A (en) * | 2017-10-16 | 2018-02-27 | 天津天鑫旺达金属热处理有限公司 | A kind of auto parts and components metal surface blast processing method |
| CN110358453A (en) * | 2018-04-10 | 2019-10-22 | 蓝思科技（长沙）有限公司 | A kind of glass polishing nano-cerium oxide polishing fluid and preparation method thereof |
| CN111718658A (en) * | 2020-07-29 | 2020-09-29 | 江西庞泰环保股份有限公司 | Semiconductor cerium dioxide grinding slurry |
| WO2023116867A1 (en) * | 2021-12-23 | 2023-06-29 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing slurry and usage method therefor |
| WO2024125476A1 (en) * | 2022-12-13 | 2024-06-20 | 安集微电子科技（上海）股份有限公司 | Polishing composition and use thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107740108A (en) * | 2017-10-16 | 2018-02-27 | 天津天鑫旺达金属热处理有限公司 | A kind of auto parts and components metal surface blast processing method |
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| CN111718658A (en) * | 2020-07-29 | 2020-09-29 | 江西庞泰环保股份有限公司 | Semiconductor cerium dioxide grinding slurry |
| WO2023116867A1 (en) * | 2021-12-23 | 2023-06-29 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing slurry and usage method therefor |
| WO2024125476A1 (en) * | 2022-12-13 | 2024-06-20 | 安集微电子科技（上海）股份有限公司 | Polishing composition and use thereof |
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Application publication date: 20150624 |