CN103897600A - Chemical mechanical polishing liquid and application thereof - Google Patents
Chemical mechanical polishing liquid and application thereof Download PDFInfo
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- CN103897600A CN103897600A CN201210567934.4A CN201210567934A CN103897600A CN 103897600 A CN103897600 A CN 103897600A CN 201210567934 A CN201210567934 A CN 201210567934A CN 103897600 A CN103897600 A CN 103897600A
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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 and an oxidizing agent. 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 application thereof.
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 2008/0276543 A1 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 2009/064365 A2 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 6447563 B1 have 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 6638326 B2 and US 7033409 B2 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 7514363 B2 have 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
The invention provides the removal speed that a kind of polishing fluid has 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.
The invention provides a kind of chemical mechanical polishing liquid and finishing method thereof.This polishing fluid contains abrasive grains, complexing agent, corrosion inhibitor and oxygenant.Described abrasive grains is one or more in the silicon-dioxide, cerium dioxide, titanium dioxide, polymer abrasive grains of silicon-dioxide, aluminium sesquioxide, adulterated al or aluminium coating, is preferably silicon-dioxide.Content is mass percent 3～30%, is preferably mass percent 5～20%; Particle diameter is 20～250nm.
Wherein, complexing agent is ammonia carboxylation compound and salt, organic acid and salt thereof, organic phospho acid and salt thereof, organic amine.Be specially 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, described organic amine is one or more in quadrol, diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, triethylene tetramine and tetraethylene pentamine; The content of complexing agent is mass percent 0.01～5%.Be preferably 0.1～1%.
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.The content of corrosion inhibitor is mass percent 0.005 ~ 1%.Be preferably 0.005～0.5%
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 described oxygenant is mass percent 0.05 ~ 5%.Be preferably 0.05～2%.
The pH of chemical mechanical polishing liquid of the present invention is 8～12.
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.
Brief description of the drawings
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/dielectric 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 the surface scan electron microscope picture that uses the silicon via hole image wafer after polishing fluid 40 polishings of the present invention.
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.
preparation Example 1 ~ 23
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
Effect embodiment
Table 2 has provided embodiment 24 ~ 40 and the comparative example 1 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
Adopt contrast polishing fluid 1 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 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.
Adopt polishing fluid 40 of the present invention to carry out polishing to silicon via hole image wafer as shown in Figure 1.Polishing condition: overdraft 3psi; Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad IC1010, polishing fluid flow velocity 150ml/min, polishing machine platform is 8 " Mirra.The first step copper is removed and is used the commercially produced product TSV-A21 of An Ji company copper chemical mechanical polishing solution, the removal speed of copper is 24000 A/min of clocks, the removal of second step blocking layer and dielectric layer is used polishing fluid 40 of the present invention, polishing time 120 seconds, after polishing, the dish-like depression of silicon through hole is 950 dusts, can meet the requirement of silicon through hole processing procedure.The few (see figure 4) of wafer surface blemish after polishing.
Should be understood that, wt% of the present invention all refers to quality percentage composition.
Above specific embodiments of the invention be have been described in detail, 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 alternative also all among category of the present invention.Therefore, equalization conversion and the amendment done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (18)
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 silicon-dioxide, titanium dioxide and/or the polymer abrasive grains of silicon-dioxide, cerium dioxide, aluminium sesquioxide, adulterated al or aluminium coating.
3. polishing fluid as claimed in claim 1, is characterized in that, the concentration of described abrasive grains is mass percent 3～30%.
4. polishing fluid as claimed in claim 3, is characterized in that, the concentration of described abrasive grains is mass percent 5～20%.
5. polishing fluid as claimed in claim 1, is characterized in that, the particle diameter of described abrasive grains is 20～250nm.
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 acid and salt thereof, organic phospho acid and salt thereof, organic amine.
7. polishing fluid as claimed in claim 7, 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 phospho acid is selected from 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 mass percent 0.01～5%.
9. polishing fluid as claimed in claim 8, is characterized in that, the content of described complexing agent is mass percent 0.1～1%.
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 11, 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 mass percent 0.005 ~ 1%.
13. polishing fluids as claimed in claim 12, is characterized in that, described corrosion inhibition agent content is mass percent 0.005～0.5%.
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 mass percent 0.05 ~ 5%.
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.
The application in the polishing of silicon through hole of 18. 1 kinds of polishing fluids as described in claim 1-17 any one.
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| CN201210567934.4A CN103897600A (en) | 2012-12-24 | 2012-12-24 | Chemical mechanical polishing liquid and application thereof |
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| CN201210567934.4A CN103897600A (en) | 2012-12-24 | 2012-12-24 | Chemical mechanical polishing liquid and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106244023A (en) * | 2016-08-23 | 2016-12-21 | 广安恒昌源电子科技有限公司 | A kind of rare earth polishing and preparation method thereof |
| CN110690114A (en) * | 2019-10-11 | 2020-01-14 | 武汉新芯集成电路制造有限公司 | CMP polishing method |
| CN111378377A (en) * | 2018-12-29 | 2020-07-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution and application thereof |
| CN112301343A (en) * | 2020-11-04 | 2021-02-02 | 常州大学 | Novel water-soluble rust conversion agent and preparation method thereof |
| CN113122147A (en) * | 2019-12-31 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution and use method thereof |
| CN113122144A (en) * | 2019-12-31 | 2021-07-16 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN116144323A (en) * | 2022-12-15 | 2023-05-23 | 上海应用技术大学 | Composite microsphere with mesoporous core-shell structure for copper CMP, preparation method thereof, chemical mechanical polishing solution and application thereof |
-
2012
- 2012-12-24 CN CN201210567934.4A patent/CN103897600A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106244023A (en) * | 2016-08-23 | 2016-12-21 | 广安恒昌源电子科技有限公司 | A kind of rare earth polishing and preparation method thereof |
| CN111378377A (en) * | 2018-12-29 | 2020-07-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution and application thereof |
| CN110690114A (en) * | 2019-10-11 | 2020-01-14 | 武汉新芯集成电路制造有限公司 | CMP polishing method |
| CN113122147A (en) * | 2019-12-31 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution and use method thereof |
| CN113122144A (en) * | 2019-12-31 | 2021-07-16 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN113122147B (en) * | 2019-12-31 | 2024-03-12 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution and application method thereof |
| CN112301343A (en) * | 2020-11-04 | 2021-02-02 | 常州大学 | Novel water-soluble rust conversion agent and preparation method thereof |
| CN112301343B (en) * | 2020-11-04 | 2022-05-20 | 常州大学 | Novel water-soluble rust conversion agent and preparation method thereof |
| CN116144323A (en) * | 2022-12-15 | 2023-05-23 | 上海应用技术大学 | Composite microsphere with mesoporous core-shell structure for copper CMP, preparation method thereof, chemical mechanical polishing solution and application thereof |
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Application publication date: 20140702 |