CN103897602A - Chemical mechanical polishing liquid and polishing method - Google Patents
Chemical mechanical polishing liquid and polishing method Download PDFInfo
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- CN103897602A CN103897602A CN201210568015.9A CN201210568015A CN103897602A CN 103897602 A CN103897602 A CN 103897602A CN 201210568015 A CN201210568015 A CN 201210568015A CN 103897602 A CN103897602 A CN 103897602A
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Abstract
The invention discloses a chemical mechanical polishing liquid for through-silicon via. The chemical mechanical polishing liquid contains abrasive particles, a complexing agent, a corrosion inhibitor, an oxidizing agent and carbonate. The chemical mechanical polishing liquid provided by the invention has high and stable silica removal rate, and adjustable copper removal rate, and can be used in different applications; and the polished copper surface has less defects.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid and finishing method.
Background technology
Along with the development of CMOS process exploitation, the characteristic dimension of device is dwindled gradually, becoming of current densities is more complicated, the Design and manufacture bringing thus becomes difficulty further, signal in interconnection process blocks up and further aggravates, integrated its physics limit of all the more approaching of miniaturization and superelevation, in order to continue Moore's Law, solve the delay issue of copper-connection, meet performance, the requirement of frequency range and power consumption, laminated chips encapsulation (3D encapsulation) technology grows up gradually, 3D encapsulates in the vertical direction by chip-stack, adopt directly and directly realize efficient interconnection through alive circuit, owing to greatly having shortened the length of interconnection line, not only improve circuit performance, also further reduce power consumption.3D encapsulation has the features such as size is little, silicon chip service efficiency is high, signal delay is short, and the special circuit design that some cannot be realized in conventional two-dimensional encapsulation becomes possibility.Be applied to as among the industrialized manufacturing technique of data storage, the digital chip of sensitization etc.
The silicon through hole (Through-silicon Via, TSV) producing at the back side of chip by operations such as etching, deposition and chemically machinery polisheds is realized three-dimensional stacked key between chip.Chemically machinery polished (Chemical Mechanical Polishing, CMP) is one requisite link in three-dimension packaging.Transistor size in size and the chip of silicon through hole has the difference of the order of magnitude, transistor size in main flow unicircuit is below micro to 100 nanometer at present, and the size of silicon through hole generally arrives tens of microns at several microns, therefore silicon through hole CMP (Chemical Mechanical Polishing) process has the requirement that is different from traditional chemical mechanical polishing process.For example: because the various medium layers in through-silicon via structure have larger thickness, thereby will have higher removal speed while requiring chemically machinery polished.On the other hand, through-silicon via structure is relatively loose for the requirement of planarization and surfaceness.
The processing procedure difference of silicon through hole, related material and CMP technique are also different.Shown in Fig. 1 and 2 is two kinds of more common processing procedures wherein.As seen from the figure, the material relating in through-silicon via structure is many, comprises metallic copper, blocking layer (tantalum or titanium), silicon-dioxide, the materials such as silicon nitride.Figure 1 shows that front end copper/barrier polishing technique, wherein the removal of copper is used TSV copper polishing fluid and is parked on blocking layer, then removes the saucerization of blocking layer, silicon-dioxide and adjusting copper with TSV barrier polishing solution.Figure 2 shows that rear end copper/insulation layer glossing, need to use to have higher silica, silicon nitride is removed speed, and the adjustable polishing fluid of speed of copper carrys out polishing.
Patent of invention US 2008/0276543A1 has introduced a kind of polishing fluid of alkalescence, and it contains oxygenant, silica abrasive, polyvinylpyrrolidone, imines blocking layer remover, carbonate, copper corrosion inhibitor, part and water.Imines blocking layer remover is wherein selected from a kind of or combination in carbonamidine, formamidine salt, carboxamidine derivatives, guanidine, guanidinesalt, guanidine derivative.SiO2(TEOS in cited embodiment in this invention) remove that speed is the highest to be only had
explain aobvious too low for TSV barrier polishing.
Patent of invention WO 2009/064365A2 has introduced a kind of polishing fluid of meta-alkalescence, and it contains water, oxygenant and borate ion.The cited SiO2(TEOS of embodiment in this patent) remove speed lower, only have an embodiment TEOS remove speed reached
all the other all exist
below.
Patent of invention US 6447563B1 has introduced a kind of polishing fluid of binary packing, wherein first part includes abrasive, stablizer and tensio-active agent, and another part includes at least two kinds in oxygenant, acid, amine (containing azanol), complexing agent, fluorochemicals, corrosion inhibitor, sterilant, tensio-active agent, buffer reagent.This patent has only been enumerated two embodiment that polishing is relevant, the removal speed of SiO2
also on the low side.
Patent of invention US 6638326B2 and US 7033409B2 have introduced the acid polishing slurry for blocking layer (tantalum Ta, tantalum nitride TaN) polishing, and it includes water, oxygenant, colloid silica abrasive.Oxygenant is wherein hydroxylamine nitriate, nitric acid, benzotriazole, ammonium nitrate, aluminum nitrate, hydrazine or its mixture aqueous solution.This polishing fluid have higher blocking layer (TaN) remove speed, but to SiO2(ILD) remove speed very low
Patent of invention US 7514363B2 has introduced a kind of polishing fluid that contains abrasive, Phenylsulfonic acid, superoxide and water.This polishing fluid have this polishing fluid have higher blocking layer (TaN) remove speed, but to SiO2(ILD) remove speed very low (under 2psi pressure,
).
In sum, in disclosed patent and document before this, do not have a kind of specially for TSV barrier polishing, the brilliant polishing fluid of carrying on the back the polishing of copper/dielectric layer, there is higher dielectric layer (SiO2), higher tantalum (Ta) and titanium (Ti), higher silicon nitride (SiN) is removed speed, and Cu removes the adjustable chemical mechanical polishing liquid of speed.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of polishing fluid and has the removal speed of higher silicon-dioxide, barrier metal, silicon nitride, metallic copper can be adjusted according to the concentration of oxygenant, and there is suitable susceptibility, and defective value (dish-like depression Dishing) to future has good correcting, surface contaminant level is lower.
In order to solve the problems of the technologies described above, the invention provides a kind of chemical mechanical polishing liquid, it contains abrasive grains, complexing agent, corrosion inhibitor and oxygenant.Polishing fluid of the present invention has the removal speed of higher silicon-dioxide, blocking layer, silicon nitride, and the removal speed of copper is adjustable, can be used for the polishing of silicon through hole copper barrier layer and brilliant back of the body copper/insulation layer, and surface of polished pattern is got well and had a lower surface contaminant.
Wherein, abrasive grains is one or more in the silicon-dioxide, cerium dioxide, titanium dioxide, polymer abrasive grains of silicon-dioxide, aluminum oxide, adulterated al or aluminium coating, is preferably silicon-dioxide.Content is 3～30wt%, is preferably 5～20wt%; Particle diameter is 20～250nm.
Wherein, complexing agent is ammonia carboxylation compound and salt, organic carboxyl acid and salt thereof, organic phospho acid and salt thereof, organic amine.Described ammonia carboxylation compound is one or more in glycine, L-Ala, α-amino-isovaleric acid, leucine, proline(Pro), phenylalanine, tyrosine, tryptophane, Methionin, arginine, Histidine, Serine, aspartic acid, L-glutamic acid, l-asparagine, glutamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), cyclohexanediaminetetraacetic acid, ethylenediamine disuccinic acid, diethylene triamine pentacetic acid (DTPA) and triethylenetetramine hexaacetic acid; Described organic carboxyl acid is one or more in acetic acid, oxalic acid, citric acid, tartrate, propanedioic acid, succinic acid, oxysuccinic acid, lactic acid, gallic acid and sulphosalicylic acid; Described organic phospho acid is 2-phosphonic acids butane-1,2, one or more in 4-tricarboxylic acid, Amino Trimethylene Phosphonic Acid, hydroxy ethylene diphosphonic acid, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene phosphonic acids, organic phosphine sulfonic and 2-HPAA, organic amine is one or more in quadrol, diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, triethylene tetramine and tetraethylene pentamine; The content of above-mentioned complexing agent is 0.01～5wt%.Be preferably 0.1～1wt%.
Wherein, corrosion inhibitor is the material that can form with copper insoluble compound, be preferably azole compounds, be selected from one or more in following: benzotriazole, 5-methyl benzotriazazole, 5-carboxy benzotriazole, 1-hydroxyl-benzotriazole, 1, 2, 4-triazole, 3-amino-1, 2, 4-triazole, 4-amino-1, 2, 4-triazole, 3, 5-diaminostilbene, 2, 4-triazole, 5-carboxyl-3-amino-1, 2, 4-triazole, 3-amino-5-sulfydryl-1, 2, 4-triazole, 5-acetic acid-1H-tetrazole, 5-methyl tetrazole, 5-phenyl tetrazole, 5-amino-1H-tetrazole and 1-phenyl-5-sulfydryl-tetrazole.
Wherein, the content of corrosion inhibitor is 0.005 ~ 1wt%.Be preferably 0.005～0.5wt%
Wherein, oxygenant is one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid, perchloric acid, high boric acid, potassium permanganate and iron nitrate.Be preferably hydrogen peroxide.The content of oxygenant is 0.05 ~ 5wt%.Be preferably 0.05～2wt%.
The pH of chemical mechanical polishing liquid of the present invention is 8～12, and it can contain carbonate, is preferably one or both in salt of wormwood, saleratus.The content of carbonate is 0.1～1wt%.
In chemical mechanical polishing liquid of the present invention, can also comprise that other typical additives are as tensio-active agent, pH adjusting agent, viscosity modifier, defoamers etc. reach polishing effect.The technique effect that these additives can play is that those skilled in the art can anticipate easily.
Above-mentioned chemical mechanical polishing slurry can be prepared into concentrating sample by other components except oxygenant, before using, is diluted to concentration range of the present invention and adds oxygenant with deionized water.
Positive progressive effect of the present invention is: polishing fluid of the present invention has the removal speed of higher silicon-dioxide, blocking layer, silicon nitride.The removal speed of copper is adjustable, can be used for the polishing of front silicon through hole copper barrier layer and brilliant back of the body copper/insulation layer.Copper few surface defects after polishing, the removal speed of silicon-dioxide is stable in storing and using.
Accompanying drawing explanation
Figure 1A is schematic diagram before the copper/barrier polishing technique polishing of front;
Figure 1B is schematic diagram after the copper/barrier polishing technique polishing of front;
Fig. 2 A is schematic diagram before the polishing of brilliant back of the body copper/insulation layer glossing;
Fig. 2 B is schematic diagram after the polishing of brilliant back of the body copper/insulation layer glossing;
Wherein, 1 is copper; 2 is blocking layer (tantalum or titanium); 3 is silicon-dioxide; 4 is silicon; 5 is silicon nitride.
Fig. 3 is the removal speed of polishing fluid 40 of the present invention to different substrate materials
Fig. 4 is polishing fluid 40 of the present invention and comparative example 2 polishing stable comparison in use
Fig. 5 is the polishing stable comparison in the shelf lives of polishing fluid 40 of the present invention and comparative example 2
Embodiment
Further set forth advantage of the present invention below by specific embodiment, but protection scope of the present invention is not only confined to following embodiment.
Table 1 has provided the embodiment 1 ~ 23 of chemical mechanical polishing liquid of the present invention, by the formula of giving in table, other components except oxygenant is mixed, and water is supplied mass percent to 100%.With KOH or HNO
3be adjusted to needed pH value.Oxidizer before using, mixes.
Table 1 embodiment 1 ~ 23
Table 2 has provided embodiment 24 ~ 40 and the comparative example 1～2 of chemical mechanical polishing liquid of the present invention, by the formula of giving in table, other components except oxygenant is mixed, and water is supplied mass percent to 100%.With KOH or HNO
3be adjusted to needed pH value.Oxidizer before using, mixes.
The embodiment 24 ~ 40 of table 2 chemical mechanical polishing liquid of the present invention and comparative example 1～2
Adopt contrast polishing fluid 1～2 and polishing fluid of the present invention 24 ~ 39, to empty sheet copper (Cu) wafer, empty sheet tantalum (Ta) wafer, empty sheet silicon-dioxide (Teos) wafer, empty sheet silicon nitride (SiN) wafer carries out polishing.The polishing speed of gained is in table 3.
Adopt polishing fluid 40 of the present invention, to empty sheet copper (Cu) wafer, empty sheet tantalum (Ta) wafer, empty sheet silicon-dioxide (Teos) wafer, empty sheet silicon nitride (SiN) wafer, empty sheet titanium (Ti) wafer, empty sheet titanium nitride (TiN) wafer, empty sheet silicon (Si) wafer carries out polishing.The polishing speed of gained is shown in Fig. 3.
Empty wafer polishing condition: overdraft 3psi; Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad IC1010, polishing fluid flow velocity 150ml/min, polishing time 1 minute, polishing machine platform is 8 " Mirra.
Table 3 embodiments of the invention 24 ~ 39 and comparative example's 1～2 removal speed
From table 3 and Fig. 3, polishing fluid of the present invention has the removal speed of higher silicon-dioxide, tantalum, titanium, titanium nitride, silicon nitride, silicon, and the removal speed of copper is adjustable, can adapt to different polishing requirements, make the surface topography of the silicon through hole after polishing meet the requirement of different processing procedures.
Stability in storage and online work-ing life are the indexs of evaluating polishing fluid stability, for the ease of producing and operation, require polishing fluid to have good stability in storing and using.In order further to investigate storage and the stability in use of such polishing fluid, the present invention adopts contrast polishing fluid 2 and the polishing fluid of the present invention 40 of different storage times and online duration of service to carry out polishing to silicon-dioxide (Teos) blank wafer.
Polishing condition is: overdraft 3psi; Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad IC1010, polishing fluid flow velocity 150ml/min, polishing time 1 minute, polishing machine platform is 8 " Mirra.
Result as shown in Figure 4 and Figure 5, known from Fig. 4 and Fig. 5, and compared with comparative example 2, polishing fluid of the present invention has higher silicon-dioxide and removes speed, and silicon-dioxide removal speed (pot life) in storing (shelf life) and using is more stable.
Claims (21)
1. a chemical mechanical polishing liquid, is characterized in that, comprises abrasive grains, complexing agent, corrosion inhibitor and oxygenant.
2. polishing fluid as claimed in claim 1, is characterized in that, described abrasive grains is selected from one or more in the silicon-dioxide, cerium dioxide, titanium dioxide, polymer abrasive grains of silicon-dioxide, aluminium sesquioxide, adulterated al or aluminium coating.
3. polishing fluid as claimed in claim 1, is characterized in that, the particle diameter of described abrasive grains is 20～250nm.
4. polishing fluid as claimed in claim 1, is characterized in that, described abrasive grains content is 3～30wt%.
5. polishing fluid as claimed in claim 4, is characterized in that, described abrasive grains content is 5～20wt%.
6. polishing fluid as claimed in claim 1, is characterized in that, described complexing agent is selected from one or more in ammonia carboxylation compound and salt, organic carboxyl acid and salt thereof, organic phospho acid and salt thereof, organic amine.
7. polishing fluid as claimed in claim 6, it is characterized in that, described ammonia carboxylation compound is selected from one or more in glycine, L-Ala, α-amino-isovaleric acid, leucine, proline(Pro), phenylalanine, tyrosine, tryptophane, Methionin, arginine, Histidine, Serine, aspartic acid, L-glutamic acid, l-asparagine, glutamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), cyclohexanediaminetetraacetic acid, ethylenediamine disuccinic acid, diethylene triamine pentacetic acid (DTPA) and triethylenetetramine hexaacetic acid; Described organic carboxyl acid is one or more in acetic acid, oxalic acid, citric acid, tartrate, propanedioic acid, succinic acid, oxysuccinic acid, lactic acid, gallic acid and sulphosalicylic acid; Described organic organic phospho acid is 2-phosphonic acids butane-1; 2; one or more in 4-tricarboxylic acid, Amino Trimethylene Phosphonic Acid, hydroxy ethylene diphosphonic acid, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene phosphonic acids, organic phosphine sulfonic and 2-HPAA, described organic amine is selected from one or more in quadrol, diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, triethylene tetramine and tetraethylene pentamine.
8. polishing fluid as claimed in claim 1, is characterized in that, the content of described complexing agent is 0.01～5wt%.
9. polishing fluid as claimed in claim 8, is characterized in that, the content of described complexing agent is 0.1～1wt%.
10. polishing fluid as claimed in claim 1, is characterized in that, described corrosion inhibitor is azole compounds.
11. polishing fluids as claimed in claim 10, it is characterized in that, described azole compounds is selected from benzotriazole, 5-methyl benzotriazazole, 5-carboxy benzotriazole, 1-hydroxyl-benzotriazole, 1, 2, 4-triazole, 3-amino-1, 2, 4-triazole, 4-amino-1, 2, 4-triazole, 3, 5-diaminostilbene, 2, 4-triazole, 5-carboxyl-3-amino-1, 2, 4-triazole, 3-amino-5-sulfydryl-1, 2, 4-triazole, 5-acetic acid-1H-tetrazole, 5-methyl tetrazole, 5-phenyl tetrazole, one or more in 5-amino-1H-tetrazole and 1-phenyl-5-sulfydryl-tetrazole.
12. polishing fluids as claimed in claim 1, is characterized in that, described corrosion inhibition agent content is 0.005 ~ 1wt%.
13. polishing fluids as claimed in claim 12, is characterized in that, described corrosion inhibition agent content is 0.005～0.5wt%.
14. polishing fluids as claimed in claim 1, it is characterized in that, described oxygenant is selected from one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid, perchloric acid, high boric acid, potassium permanganate and iron nitrate.
15. polishing fluids as claimed in claim 1, is characterized in that, described oxygenate content is 0.05 ~ 5wt%.
16. polishing fluids as claimed in claim 15, is characterized in that, described oxygenate content is 0.05 ~ 2wt%.
17. polishing fluids as claimed in claim 1, is characterized in that, the pH value of described polishing fluid is 8～12.
18. polishing fluids as claimed in claim 1, is characterized in that, described polishing fluid comprises carbonate.
19. polishing fluids as claimed in claim 1, is characterized in that, described carbonate is one or both in salt of wormwood, saleratus.
20. polishing fluids as claimed in claim 1, is characterized in that, described carbonate content is 0.1～1wt%.
The application in the polishing of silicon through hole of 21. 1 kinds of polishing fluids as claimed in claim 1.
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Cited By (6)
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|---|---|---|---|---|
| CN106835144A (en) * | 2016-12-16 | 2017-06-13 | 安徽宝恒新材料科技有限公司 | A kind of processing method of 8K mirror boards |
| CN108857860A (en) * | 2018-06-12 | 2018-11-23 | 宁波江丰电子材料股份有限公司 | Grinding method, wafer orientation ring and its application of wafer orientation ring and chemical mechanical polishing apparatus |
| CN112175525A (en) * | 2020-09-30 | 2021-01-05 | 常州时创新材料有限公司 | Polishing composition for IC copper barrier layer CMP and preparation method thereof |
| WO2022143719A1 (en) * | 2020-12-30 | 2022-07-07 | 安集微电子科技（上海）股份有限公司 | Chemical-mechanical polishing solution and use method therefor |
| CN115365996A (en) * | 2022-08-23 | 2022-11-22 | 福建省南安市宏炜新材料有限公司 | Chemical mechanical polishing process of N-Si substrate |
| WO2023178003A1 (en) * | 2022-03-14 | 2023-09-21 | Versum Materials Us, Llc | Stable chemical mechanical planarization polishing compositions and methods for high rate silicon oxide removal |
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| CN106835144A (en) * | 2016-12-16 | 2017-06-13 | 安徽宝恒新材料科技有限公司 | A kind of processing method of 8K mirror boards |
| CN108857860A (en) * | 2018-06-12 | 2018-11-23 | 宁波江丰电子材料股份有限公司 | Grinding method, wafer orientation ring and its application of wafer orientation ring and chemical mechanical polishing apparatus |
| CN112175525A (en) * | 2020-09-30 | 2021-01-05 | 常州时创新材料有限公司 | Polishing composition for IC copper barrier layer CMP and preparation method thereof |
| WO2022143719A1 (en) * | 2020-12-30 | 2022-07-07 | 安集微电子科技（上海）股份有限公司 | Chemical-mechanical polishing solution and use method therefor |
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| CN115365996A (en) * | 2022-08-23 | 2022-11-22 | 福建省南安市宏炜新材料有限公司 | Chemical mechanical polishing process of N-Si substrate |
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