CN102051128A - Chemical mechanical polishing solution - Google Patents

Chemical mechanical polishing solution Download PDF

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CN102051128A
CN102051128A CN2009101983771A CN200910198377A CN102051128A CN 102051128 A CN102051128 A CN 102051128A CN 2009101983771 A CN2009101983771 A CN 2009101983771A CN 200910198377 A CN200910198377 A CN 200910198377A CN 102051128 A CN102051128 A CN 102051128A
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polishing fluid
polishing
silicon nitride
tbah
water surplus
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CN102051128B (en
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姚颖
宋伟红
孙展龙
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Anji microelectronic technology (Shanghai) Limited by Share Ltd
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Anji Microelectronics Shanghai Co Ltd
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Abstract

The invention discloses a chemical mechanical polishing solution which is used for polishing silicon nitride materials. The polishing solution comprises abrasive particles, quaternary ammonium compounds, a silicon nitride polishing accelerating agent and water, wherein the silicon nitride accelerating agent is selected from an anionic surfactant. The chemical mechanical polishing solution can effectively remove silicon nitride materials and provide the selectivity of the removal rate of silicon nitride materials toward the removal rate of silicon oxide materials.

Description

A kind of chemical mechanical polishing liquid
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid.
Background technology
In unicircuit is made, the standard of interconnection technique is improving, along with interconnection increase of the number of plies and dwindling of technology characteristics size, requirement to the silicon chip surface planeness is also more and more higher, if there is not the ability of planarization, create complicated on semiconductor crystal wafer and intensive structure is very limited, cmp method CMP is exactly the effective means that can realize the whole silicon wafer planarization.
CMP technology just is to use a kind of mixture and polishing pad polishing integrated circuit surface that contains abrasive material.In typical cmp method, substrate is directly contacted with rotating polishing pad, exert pressure at substrate back with a loads.During polishing, pad and operator's console rotation, the power that keeps down at substrate back is applied to abrasive material and chemically reactive solution (being commonly referred to polishing fluid or polishing slurries) on the pad simultaneously, and this polishing fluid begins to carry out polishing process with the film generation chemical reaction that is polishing.
As the method for each element of isolation of semiconductor devices, shallow trench isolation is the semiconductor processing technology of widespread use from (STI) technology, wherein forms silicon nitride layer on silicon base, form shallow slot by etching or photolithography, and dielectric layer is to fill this groove.Because the variation of the degree of depth of groove that forms or line by this way generally must deposit excessive dielectric materials and fill all grooves to guarantee safety on base top.
Generally remove excessive dielectric materials to expose silicon nitride layer by CMP (Chemical Mechanical Polishing) process.When silicon nitride layer exposed, the substrate that is exposed to the maximum area of chemical-mechanical polishing system comprised silicon nitride.Silicon nitride must be polished to obtain highly smooth and uniform surface then.Usually, the practice in past focuses on the selectivity that oxide cmp is had precedence over silicon nitride polishing.Therefore, total polishing speed descends when silicon nitride layer exposes, and silicon nitride layer is as stopping layer.Yet because the oxide compound line width becomes more and more littler in device of future generation, in some cases, expectation is used has the optionally polishing system of silicon nitride to oxide cmp, to reduce the defective of the oxide compound line that forms on substrate surface.China applies for a patent the removal speed that 200510116191.9 disclosed polishing fluid utilizations are selected from a kind of acid additive raising silicon nitride in hydrochloric acid, formic acid, acetate, oxalic acid, hexanodioic acid and the lactic acid, removes speed is removed speed to silicon oxide selectivity to improve silicon nitride.China applies for a patent 20078006548.5 and discloses the polishing fluid with pH value of 1 to 6 that is used for polish silicon nitride.It comprises abrasive and acidic components (for example, the combination of propanedioic acid and aminocarboxylic acid, stannate, uric acid, toluylic acid, or the combination of propanedioic acid, aminocarboxylic acid and vitriol).This polishing fluid can obtain the removal speed of higher silicon nitride, obtain silicon nitride and remove speed is removed speed to silicon oxide selectivity, China applies for a patent 200780026767.X and discloses a kind of polishing fluid, it contains colloid silica, at least a acidic components of 1 to 4.5 pKa, and aqueous carrier, pH value than little 0.5 the PH unit of pKa of these acidic components to scope than big 1.5 the PH units of this pKa.This polishing fluid can obtain higher silicon nitride and remove speed and lower silicon oxide removal speed.In this class patent, all be to utilize acidic components to improve the removal speed of silicon nitride.
In (STI) technology, the STI polishing fluid of current use has the removal speed to silica material faster (comparing with silicon nitride material) usually at shallow trench isolation.Therefore, total polishing speed descends when silicon nitride layer exposes, and silicon nitride layer is as stopping layer.Yet because the oxide compound line width becomes more and more littler in device of future generation, in some cases, expectation is used has the optionally polishing fluid of silicon nitride material to the silica material polishing, to reduce the defective of the oxide compound line that forms on substrate surface.
Summary of the invention
The purpose of this invention is to provide a kind of high relatively silicon nitride removal speed that has, the removal rate selection that can regulate silicon nitride and silicon oxide reduces the chemical mechanical polishing liquid of the defective of the oxide compound line that forms than the polishing requirement of satisfying technology on substrate surface.
Polishing fluid of the present invention comprises: abrasive grain, quaternary ammonium compound, silicon nitride polishing accelerator and water.Wherein, the silicon nitride polishing accelerator is an aniorfic surfactant, for example Witco 1298 Soft Acid, Sodium dodecylbenzene sulfonate, sodium methylene bis-naphthalene sulfonate, alkyl phosphate diethanolamine salt, alkyl phosphate triethanolamine salt, PAPE, glycerine polyoxypropylene ether phosphate triethanolamine salt, vinylformic acid-2-acrylamido-2-methyl propane sulfonic acid multipolymer, polyacrylic acid and anionic polyacrylamide etc.
Among the present invention, polyacrylic molecular weight is 2000～5000, and the molecular weight of anionic polyacrylamide is 5,000,000～12,000,000.
Among the present invention, the content of tensio-active agent is mass percent: 0.001～0.2%, and preferably be mass percent: 0.005～0.1%.
Among the present invention, abrasive grains is silicon-dioxide, aluminium sesquioxide, cerium dioxide or the silica dioxide granule of mixing aluminium.The abrasive grains particle diameter is 20～150nm, and content is mass percent: 1～20%.
Among the present invention, quaternary ammonium compound is Tetramethylammonium hydroxide and/or TBAH, and content is mass percent: 0.01～0.2%.
Among the present invention, the pH of polishing fluid is 2～7, preferably is 2～4.
Positively effect of the present invention is: remove silicon nitride material effectively; The selectivity of silicon nitride material to the removal speed of silica material is provided; The defective of the oxide compound line that minimizing forms on substrate surface.
Description of drawings
Fig. 1 is that the consumption of alkyl phosphate diethanolamine salt among the effect embodiment 2 is to Si 3N 4Removal speed comparison diagram with TEOS;
Fig. 2 is that the consumption of alkyl phosphate diethanolamine salt among the effect embodiment 2 is to Si 3N 4Removal rate selection ratio figure with TEOS;
Fig. 3 is that the different PH of polishing fluid among the effect embodiment 3 is to Si 3N 4Removal speed comparison diagram with TEOS;
Fig. 4 be among the effect embodiment 4 abrasive concentration to Si 3N 4Removal speed comparison diagram with TEOS.
Embodiment
Further set forth the present invention below by specific embodiment, therefore do not limit the present invention among the described scope of embodiments.
By listed prescription, with the simple uniform mixing of each composition, surplus is a water, adopts potassium hydroxide, ammoniacal liquor and nitric acid to be adjusted to suitable pH value afterwards, can make each embodiment polishing fluid.
Effect embodiment 1
Contrast polishing fluid 1 ' abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 2 ' abrasive silica (150nm) 4%, TMAH 0.2%, water surplus, pH=3;
Polishing fluid 1 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 2 abrasive silica (100nm) 4%, TBAH 0.05%, PAPE 0.02%, water surplus, pH=3;
Polishing fluid 3 abrasive silica (100nm) 4%, TBAH 0.05%, Witco 1298 Soft Acid 0.02%, water surplus, pH=3;
Polishing fluid 4 abrasive silica (100nm) 4%, TBAH 0.05%, vinylformic acid-2-acrylamido-2-methyl propane sulfonic acid multipolymer 0.02%, water surplus, pH=3;
Polishing fluid 5 abrasive silica (100nm) 4%, TBAH 0.05%, polyacrylic acid (molecular weight 3000) 0.02%, water surplus, pH=3;
Polishing fluid 6 abrasive silica (100nm) 4%, TBAH 0.05%, anionic polyacrylamide (molecular weight 8,000,000) 0.02%, water surplus, pH=3;
Polishing fluid 7 abrasive silica (100nm) 4%, TBAH 0.05%, sodium methylene bis-naphthalene sulfonate 0.02%, water surplus, pH=3;
Polishing fluid 8 abrasive silica (100nm) 4%, TBAH 0.05%, polyacrylic acid (molecular weight 2000) 0.02%, water surplus, pH=3;
Polishing fluid 9 abrasive silica (100nm) 4%, TBAH 0.05%, polyacrylic acid (molecular weight 5000) 0.02%, water surplus, pH=3;
Polishing fluid 10 abrasive silica (100nm) 4%, TBAH 0.05%, anionic polyacrylamide (molecular weight 5,000,000) 0.02%, water surplus, pH=3;
Polishing fluid 11 abrasive silica (100nm) 4%, TBAH 0.05%, anionic polyacrylamide (molecular weight 1,200 ten thousand) 0.02%, water surplus, pH=3;
Polishing fluid 12 abrasive silica (150nm) 4%, TMAH 0.05%, Sodium dodecylbenzene sulfonate 0.02%, water surplus, pH=3;
Polishing fluid 13 abrasive silica (150nm) 4%, TMAH 0.05%, alkyl phosphate triethanolamine salt 0.15%, water surplus, pH=3;
Polishing fluid 14 abrasive silica (150nm) 4%, TMAH 0.05%, glycerine polyoxypropylene ether phosphate triethanolamine salt 0.2%, water surplus, pH=3;
Polishing fluid 15 aluminium sesquioxide abrasive materials (20nm) 5%, Witco 1298 Soft Acid 0.15%, TBAH 0.15%, water surplus, pH=3;
Polishing fluid 16 cerium dioxide abrasive materials (150nm) 1%, methylene-bis are sodium sulfonate 0.02%, Tetramethylammonium hydroxide 0.01%%, water surplus, pH=4 how;
Polishing fluid 17 is mixed aluminium abrasive silica (45nm) 3%, polyacrylic acid (molecular weight 5000) 0.2%, Tetramethylammonium hydroxide 0.1%, water surplus, pH=3;
Polishing fluid 18 silicon-dioxide (80nm) 6%, alkyl phosphate diethanolamine salt 0.05%, TBAH 0.02%, water surplus, pH=2.
Polishing material: blank Si 3N 4Wafer, polishing condition: 4psi, polishing disk rotating speed 70rpm, polishing pad PPG, polishing fluid flow velocity 200ml/min, Logitech LP50 Polisher.Experimental result is as shown in table 1:
The different anion surfactant of table 1 is to Si 3N 4Remove the influence of speed
Figure B2009101983771D0000061
The result is as shown in table 1: polishing fluid of the present invention can effectively be removed Si 3N 4Wherein the anion surfactant of Tian Jiaing can improve Si significantly 3N 4Removal speed, especially, the interpolation of Witco 1298 Soft Acid makes Si 3N 4Removal speed reach
Figure B2009101983771D0000062
Effect embodiment 2
Contrast polishing fluid 19 ' abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=3;
Polishing fluid 19 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.001%, water surplus, pH=3;
Polishing fluid 20 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.005%, water surplus, pH=3;
Polishing fluid 21 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.01%, water surplus, pH=3;
Polishing fluid 22 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 23 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.03%, water surplus, pH=3;
Polishing fluid 24 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.05%, water surplus, pH=3;
Polishing fluid 25 abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.1%, water surplus, pH=3;
Polishing material: blank Si 3N 4Wafer, blank TEOS wafer; Polishing condition: 4psi, polishing disk rotating speed 70rpm, polishing pad PPG, polishing fluid flow velocity 200ml/min, Logitech LP50 Polisher.Experimental result such as table 2, illustrated in figures 1 and 2:
Table 2 alkyl phosphate diethanolamine salt consumption is to Si 3N 4Influence with TEOS removal speed
Figure B2009101983771D0000071
Result such as table 2 and shown in Figure 1: after adding anion surfactant in the polishing fluid of the present invention, can improve Si significantly 3N 4Removal speed and suppress the removal speed of TEOS.Along with the increase of anion surfactant consumption, polishing fluid of the present invention is to Si 3N 4The polishing promoter action strengthen gradually earlier, weaken gradually after reaching particular value.Illustrate and have only when the consumption of anion surfactant is a particular value, could be to Si 3N 4Removal speed promoter action is arranged.Otherwise excessive anion surfactant can suppress Si on the contrary 3N 4Polishing, even reduce Si 3N 4Removal speed.As table 2 and shown in Figure 2, can regulate Si by the concentration of regulating anion surfactant 3N 4With the selection ratio of the removal speed of TEOS, along with the increase of anion surfactant consumption, Si 3N 4With the selection of the removal speed of TEOS than also increasing gradually.
Effect embodiment 3
Contrast polishing fluid 26 ' (1) abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=2;
Contrast polishing fluid 26 ' (2) abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 26 ' (3) abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 26 ' (4) abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=5;
Contrast polishing fluid 26 ' (5) abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=7;
Polishing fluid 26 (1) abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=2;
Polishing fluid 26 (2) abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 26 (2) abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=4;
Polishing fluid 26 (3) abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=5;
Polishing fluid 26 (4) abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=7;
Polishing material: blank Si 3N 4Wafer, polishing condition: 4psi, polishing disk rotating speed 70rpm, polishing pad PPG, polishing fluid flow velocity 200ml/min, Logitech LP50Polisher.
The result is as shown in Figure 3: when the pH of polishing fluid was 2～4, with respect to the polishing fluid that does not contain anion surfactant, the polishing fluid that contains anion surfactant of the present invention can significantly increase Si 3N 4Polishing speed.
Effect embodiment 4
Contrast polishing fluid 27 ' (1) abrasive silica (100nm) 1%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 27 ' (2) abrasive silica (100nm) 2%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 27 ' (3) abrasive silica (100nm) 4%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 27 ' (4) abrasive silica (100nm) 8%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 27 ' (5) abrasive silica (100nm) 10%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 27 ' (6) abrasive silica (100nm) 15%, TBAH 0.05%, water surplus, pH=3;
Contrast polishing fluid 27 ' (7) abrasive silica (100nm) 20%, TBAH 0.05%, water surplus, pH=3;
Polishing fluid 27 (1) abrasive silica (100nm) 1%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 27 (2) abrasive silica (100nm) 2%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 27 (3) abrasive silica (100nm) 4%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 27 (4) abrasive silica (100nm) 8%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 27 (5) abrasive silica (100nm) 10%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 27 (6) abrasive silica (100nm) 15%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing fluid 27 (7) abrasive silica (100nm) 20%, TBAH 0.05%, alkyl phosphate diethanolamine salt 0.02%, water surplus, pH=3;
Polishing material: blank Si 3N 4Wafer, polishing condition: 4psi, polishing disk rotating speed 70rpm, polishing pad PPG, polishing fluid flow velocity 200ml/min, Logitech LP50 Polisher.
The result as shown in Figure 4, when the concentration of abrasive silica is between 1%～20% the time, with respect to the polishing fluid that does not contain anion surfactant, the polishing fluid that contains anion surfactant of the present invention can significantly increase Si 3N 4Polishing speed.

Claims (13)

1. chemical mechanical polishing liquid, it comprises: abrasive grain, quaternary ammonium compound, silicon nitride polishing accelerator and water.
2. polishing fluid as claimed in claim 1 is characterized in that: described silicon nitride polishing accelerator is an aniorfic surfactant.
3. polishing fluid as claimed in claim 2 is characterized in that: described aniorfic surfactant is selected from one or more of Witco 1298 Soft Acid, Sodium dodecylbenzene sulfonate, sodium methylene bis-naphthalene sulfonate, alkyl phosphate diethanolamine salt, alkyl phosphate triethanolamine salt, PAPE, glycerine polyoxypropylene ether phosphate triethanolamine salt, vinylformic acid-2-acrylamido-2-methyl propane sulfonic acid multipolymer, polyacrylic acid and anionic polyacrylamide.
4. polishing fluid as claimed in claim 3 is characterized in that: described polyacrylic molecular weight is 2000～5000, and the molecular weight of described anionic polyacrylamide is 5,000,000～12,000,000.
5. polishing fluid as claimed in claim 3 is characterized in that: the content of described tensio-active agent is mass percent: 0.001～0.2%.
6. polishing fluid as claimed in claim 5 is characterized in that: the content of described tensio-active agent is mass percent: 0.005～0.1%.
7. polishing fluid as claimed in claim 1 is characterized in that: described abrasive grains is selected from silicon-dioxide, aluminium sesquioxide, cerium dioxide and mixes in the silica dioxide granule of aluminium one or more.
8. polishing fluid as claimed in claim 1 is characterized in that: the particle diameter of described abrasive grains is 20～150nm.
9. polishing fluid as claimed in claim 8 is characterized in that: the content of described abrasive grains is mass percent: 1～20%.
10. polishing fluid as claimed in claim 1 is characterized in that: described quaternary ammonium compound is Tetramethylammonium hydroxide and/or TBAH.
11. polishing fluid as claimed in claim 10 is characterized in that: the content of described quaternary ammonium compound is mass percent: 0.01～0.2%.
12. polishing fluid as claimed in claim 1 is characterized in that: the pH of described polishing fluid is 2～7.
13. polishing fluid as claimed in claim 12 is characterized in that: the pH of described polishing fluid is 2～4.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102533116A (en) * 2010-12-10 2012-07-04 安集微电子（上海）有限公司 Chemical mechanical polishing solution
CN102559058A (en) * 2010-12-21 2012-07-11 安集微电子（上海）有限公司 Chemical-mechanical polishing liquid
CN103173127A (en) * 2011-12-23 2013-06-26 安集微电子（上海）有限公司 Chemical mechanical polishing liquid for flatting through silicon via blocking layers
WO2013189168A1 (en) * 2012-06-21 2013-12-27 安集微电子（上海）有限公司 Chemical mechanical polishing solution for silicon through-hole planarization
WO2014079144A1 (en) * 2012-11-22 2014-05-30 安集微电子（上海）有限公司 Chemical mechanical polishing solution
WO2016107414A1 (en) * 2014-12-29 2016-07-07 王晨 Application of composition in polishing of barrier layer
CN108117838A (en) * 2016-11-29 2018-06-05 安集微电子科技（上海）股份有限公司 A kind of silicon nitride chemical mechanical polishing liquid
CN108117840A (en) * 2016-11-29 2018-06-05 安集微电子科技（上海）股份有限公司 A kind of silicon nitride chemical mechanical polishing liquid
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CN101016440A (en) * 2006-02-08 2007-08-15 罗门哈斯电子材料Cmp控股股份有限公司 Multi-component barrier polishing solution

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CN101016440A (en) * 2006-02-08 2007-08-15 罗门哈斯电子材料Cmp控股股份有限公司 Multi-component barrier polishing solution

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CN108117838A (en) * 2016-11-29 2018-06-05 安集微电子科技（上海）股份有限公司 A kind of silicon nitride chemical mechanical polishing liquid
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WO2018099110A1 (en) * 2016-11-29 2018-06-07 安集微电子科技（上海）股份有限公司 Silicon nitride chemical-mechanical polishing solution
TWI732952B (en) * 2016-11-29 2021-07-11 大陸商安集微電子科技(上海)股份有限公司 A chemical mechanical polishing slurry for silicon nitride with a high selectivity
CN108117838B (en) * 2016-11-29 2021-09-17 安集微电子科技（上海）股份有限公司 Silicon nitride chemical mechanical polishing solution
CN108117840B (en) * 2016-11-29 2021-09-21 安集微电子科技（上海）股份有限公司 Silicon nitride chemical mechanical polishing solution
CN111378375A (en) * 2018-12-28 2020-07-07 安集微电子科技（上海）股份有限公司 Chemical mechanical polishing solution
CN111378375B (en) * 2018-12-28 2022-05-13 安集微电子科技（上海）股份有限公司 Chemical mechanical polishing solution

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