CN103897602B - A kind of chemical mechanical polishing liquid and polishing method - Google Patents
A kind of chemical mechanical polishing liquid and polishing method Download PDFInfo
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- CN103897602B CN103897602B CN201210568015.9A CN201210568015A CN103897602B CN 103897602 B CN103897602 B CN 103897602B CN 201210568015 A CN201210568015 A CN 201210568015A CN 103897602 B CN103897602 B CN 103897602B
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Abstract
The invention discloses a kind of chemical mechanical polishing liquid for silicon hole, it contains abrasive grains, complexing agent, corrosion inhibitor and oxidant, and carbonate.The chemical mechanical polishing liquid of the present invention has the removal rate of higher and stable silica, and the removal rate of copper is adjustable.Go for copper few surface defects after different applications, polishing.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid and polishing method.
Background technology
The development developed with CMOS technology, the characteristic size of device is gradually reduced, and becoming for current densities is more complicated,
Thus the design and manufacture brought becomes further difficult, and the signal congestion in interconnection process is further exacerbated by, miniaturization and superelevation
It is integrated all the more to approach its physics limit, in order to continue Moore's Law, solve the delay issue of copper-connection, meet performance, frequency range and
The requirement of power consumption, Stacked Die Packaging（3D is encapsulated）Technology gradually grows up, and 3D is encapsulated chip-stack i.e. in vertical direction,
Efficient interconnections are directly realized by using directly through active circuit, due to substantially reducing the length of interconnection line, electricity are not only increased
Road performance, further reduces power consumption.3D encapsulation has the features such as size is small, silicon chip service efficiency is high, signal delay is short, and
And so that some special circuits that can not be realized in conventional two-dimensional encapsulation are designed to possibility.It has been applied to such as data storage
Among the industrialized manufacturing technique of device, photosensitive digital chip etc..
The silicon hole produced by processes such as etching, deposition and chemically mechanical polishings at the back side of chip（Through-
Silicon Via, TSV）It is to realize three-dimensional stacked key between the chips.Chemically mechanical polishing（Chemical Mechanical
Polishing, CMP）It is one of essential link in three-dimension packaging.Transistor size in the size and chip of silicon hole has
Micro is to less than 100 nanometers for transistor size in the difference of the order of magnitude, current mainstream integrated circuit, and the size of silicon hole
Some tens of pm typically is arrived at several microns, therefore silicon hole CMP process has different from conventional chemical-mechanical glossing
Requirement.For example：Because the various dielectric layers in through-silicon via structure have larger thickness, thus require to want during chemically mechanical polishing
There is higher removal rate.On the other hand, through-silicon via structure is then relatively loose for planarization and the requirement of surface roughness.
The processing procedure of silicon hole is different, and involved material and CMP is also different.Shown in Fig. 1 and 2 is two of which
Relatively common processing procedure.It can be seen that the material being related in through-silicon via structure is relatively more, including metallic copper, barrier layer（Tantalum or
Titanium）, silica, the material such as silicon nitride.Fig. 1 show front end copper/barrier polishing technique, and the removal of wherein copper uses TSV
Copper polishing fluid simultaneously stops over the barrier layer, and barrier layer, silica are then removed with TSV barrier polishing solutions and copper is adjusted
Saucerization.Fig. 2 show rear end copper/insulating barrier glossing, it is necessary to which using having higher silica, silicon nitride removes speed
Rate, the adjustable polishing fluid of speed of copper is polished.
Patent of invention US 2008/0276543A1 describe a kind of alkaline polishing fluid, and it contains oxidant, silica
Grinding agent, polyvinylpyrrolidone, imines barrier layer remover, carbonate, copper corrosion inhibitor, part and water.Imines resistance therein
The one kind or combination of barrier remover in carbonamidine, formamidine salt, carboxamidine derivatives, guanidine, guanidinesalt, guanidine derivatives.It is listed in the invention
For SiO2 in embodiment（TEOS）Removal rate highest only hasIt is substantially too low for TSV barrier polishings.
Patent of invention WO 2009/064365A2 describe a kind of polishing fluid of meta-alkalescence, and it contains water, oxidant and boron
Acid ion.The SiO2 cited by embodiment in the patent（TEOS）Removal rate is relatively low, only the TEOS of one embodiment
Removal rate reachesRemaining existsBelow.
Patent of invention US 6447563B1 describe a kind of polishing fluid of binary packing, and wherein Part I includes grinding
Agent, stabilizer and surfactant, another part include oxidant, acid, amine（Containing azanol）, complexing agent, fluorochemical, corruption
At least two in corrosion inhibitor, bactericide, surfactant, buffer reagent.The patent only lists two and polishes correlation
Embodiment, SiO2 removal rateAlso it is relatively low.
Patent of invention US 6638326B2 and US 7033409B2 are described for barrier layer（Tantalum Ta, tantalum nitride TaN）Throw
The acid polishing slurry of light, it includes water, oxidant, colloidal silica abrasive.Oxidant therein is HAN, nitre
Acid, BTA, ammonium nitrate, aluminum nitrate, hydrazine or its mixture aqueous solution.The polishing fluid has higher barrier layer（TaN）
Removal rate, but to SiO2（ILD）Removal rate is very low
Patent of invention US 7514363B2 describe a kind of polishing fluid containing grinding agent, benzene sulfonic acid, peroxide and water.
There is the polishing fluid polishing fluid to have higher barrier layer（TaN）Removal rate, but to SiO2（ILD）Removal rate is very low
（Under 2psi pressure,）.
In summary, in disclosed patent and document before this, there is not one kind specifically designed for TSV barrier polishings, crystalline substance
The polishing fluid of copper/dielectric layer polishing is carried on the back, i.e., with higher dielectric layer（SiO2）, higher tantalum（Ta）And titanium（Ti）, it is higher
Silicon nitride（SiN）Removal rate, and the adjustable chemical mechanical polishing liquid of Cu removal rates.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of polishing fluid with higher silica, barrier layer gold
Category, the removal rate of silicon nitride, metallic copper can be adjusted according to the concentration of oxidant, and have suitable susceptibility, and right
The defective value of future（Dish-like depression Dishing）With preferable correcting, surface contaminant level is relatively low.
In order to solve the above-mentioned technical problem, the invention provides a kind of chemical mechanical polishing liquid, it contains abrasive grains, network
Mixture, corrosion inhibitor and oxidant.The polishing fluid of the present invention has higher silica, barrier layer, the removal of silicon nitride
Speed, the removal rate of copper is adjustable, available for the polishing of silicon hole copper barrier layer and brilliant back of the body copper/insulating barrier, surface of polished shape
Looks are got well and have relatively low surface contaminant.
Wherein, abrasive grains are silica, ceria, the dioxy of silica, aluminum oxide, adulterated al or aluminium coating
Change the one or more in titanium, macromolecule abrasive grains, preferably silica.Content be 3~30wt%, preferably 5~
20wt%;Particle diameter is 20~250nm.
Wherein, complexing agent is ammonia carboxylation compound and its salt, organic carboxyl acid and its salt, organic phospho acid and its salt, organic amine.It is described
Ammonia carboxylation compound for glycine, alanine, valine, leucine, proline, phenylalanine, tyrosine, tryptophan, lysine,
Arginine, histidine, serine, aspartic acid, glutamic acid, asparagine, glutamine, nitrilotriacetic acid, ethylenediamine tetra-acetic acid, ring
One or more in hexamethylene tetraacetic acid, ethylenediamine disuccinic acid, diethylene triamine pentacetic acid (DTPA) and triethylenetetramine hexaacetic acid；Institute
The organic carboxyl acid stated is acetic acid, oxalic acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid, lactic acid, gallic acid and sulfo group
One or more in salicylic acid；Described organic phospho acid be 2- phosphonobutanes -1,2,4- tricarboxylic acids, ATMP,
Hydroxy ethylene diphosphonic acid, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine penta, organic phosphine sulfonic and 2- hydroxyl phosphines
One or more in acyl acetic acid, organic amine is ethylenediamine, diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, three
One or more in ethene tetramine and TEPA；The content of above-mentioned complexing agent is 0.01~5wt%.Preferably 0.1~1wt%.
Wherein, corrosion inhibitor is that the material of insoluble compound can be formed with copper, preferably azole compounds, is selected from down
One or more in row：BTA, 5- methyl benzotriazazoles, 5- carboxy benzotriazoles, 1- hydroxyls-benzo three
Nitrogen azoles, 1,2,4- triazoles, 3- amino -1,2,4- triazoles, 4- amino -1,2,4- triazoles, 3,5- diaminostilbenes, 2,4- tri-
Nitrogen azoles, 5- carboxyl -3- amino -1,2,4- triazoles, 3- amino -5- sulfydryls -1,2,4- triazoles, 5- acetic acid -1H- tetrazoles,
5- methyl tetrazoles, 5- phenyl tetrazole, 5- amino -1H- tetrazoles and 1- phenyl -5- sulfydryls-tetrazole.
Wherein, the content of corrosion inhibitor is 0.005 ~ 1wt%.Preferably 0.005~0.5wt%
Wherein, oxidant is hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic acid, persulfate, percarbonate, height
One or more in acid iodide, perchloric acid, high boric acid, potassium permanganate and ferric nitrate.Preferably hydrogen peroxide.The content of oxidant
For 0.05 ~ 5wt%.Preferably 0.05~2wt%.
The pH of the chemical mechanical polishing liquid of the present invention is 8~12, and it can contain carbonate, preferably potassium carbonate, bicarbonate
One or both of potassium.The content of carbonate is 0.1~1wt%.
Other typical additives such as surfactant, pH can also be included in the chemical mechanical polishing liquid of the present invention to adjust
Agent, viscosity modifier, defoamer etc. reaches polishing effect.The technique effect that these additives can be played, is this area skill
Art personnel are expected easily.
Other components in addition to oxidant can be prepared into concentrating sample by above-mentioned chemical mechanical polishing slurry, before use
The concentration range of the present invention is diluted to deionized water and oxidant is added.
The positive effect of the present invention is：The polishing fluid of the present invention has higher silica, barrier layer, nitridation
The removal rate of silicon.The removal rate of copper is adjustable, the polishing available for positive silicon hole copper barrier layer and brilliant back of the body copper/insulating barrier.
Copper few surface defects after polishing, the removal rate of silica is stable in storage and use.
Brief description of the drawings
Figure 1A is schematic diagram before front copper/barrier polishing technique polishing；
Figure 1B is schematic diagram after front copper/barrier polishing technique polishing；
Fig. 2A is schematic diagram before brilliant back of the body copper/insulating barrier glossing polishing；
Fig. 2 B are schematic diagram after brilliant back of the body copper/insulating barrier glossing polishing；
Wherein, 1 is copper；2 be barrier layer（Tantalum or titanium）；3 be silica；4 be silicon；5 be silicon nitride.
Fig. 3 is the removal rate of polishing fluid 40 of the invention to different substrate materials
Polishing stables of the Fig. 4 for polishing fluid 40 and comparative example 2 of the invention in use compares
Fig. 5 compares for the polishing fluid 40 and comparative example 2 of the present invention in the polishing stable of Storage period
Embodiment
Advantages of the present invention is expanded on further below by specific embodiment, but protection scope of the present invention is not only limited to
In following embodiments.
Embodiment 1 ~ 23
Table 1 gives the embodiment 1 ~ 23 of the chemical mechanical polishing liquid of the present invention, is formulated by given in table, will remove oxidant
Other components in addition are well mixed, and mass percent is supplied with water to 100%.With KOH or HNO3Adjust required pH
Value.Using preceding oxidizer, it is well mixed.
The embodiment 1 ~ 23 of table 1
Effect example 1
Table 2 gives the embodiment 24 ~ 40 and comparative example 1~2 of the chemical mechanical polishing liquid of the present invention, by institute in table
To formula, the other components in addition to oxidant are well mixed, mass percent is supplied with water to 100%.With KOH or HNO3
Adjust required pH value.Using preceding oxidizer, it is well mixed.
The embodiment 24 ~ 40 and comparative example 1~2 of the chemical mechanical polishing liquid of the present invention of table 2
Using contrast polishing fluid 1~2 and the polishing fluid 24 ~ 39 of the present invention, to empty piece copper（Cu）Chip, empty piece tantalum（Ta）It is brilliant
Piece, empty piece silica（Teos）Chip, empty piece silicon nitride（SiN）Chip is polished.The polishing speed of gained is shown in Table 3.
Using the polishing fluid 40 of the present invention, to empty piece copper（Cu）Chip, empty piece tantalum（Ta）Chip, empty piece silica
（Teos）Chip, empty piece silicon nitride（SiN）Chip, empty piece titanium（Ti）Chip, empty piece titanium nitride (TiN) chip, empty piece silicon（Si）
Chip is polished.The polishing speed of gained is shown in Fig. 3.
Empty wafer polishing condition：Lower pressure 3psi；Polishing disk and rubbing head rotating speed 93/87rpm, polishing pad IC1010,
Flow velocity 150ml/min is polished, polishing time 1 minute, polishing machine platform is 8 " Mirra.
The removal rate of the embodiments of the invention 24 ~ 39 of table 3 and comparative example 1~2
From table 3 and Fig. 3, polishing fluid of the invention have higher silica, tantalum, titanium, titanium nitride, silicon nitride,
The removal rate of silicon, and the removal rate of copper is adjustable, is adapted to different polishing requirements, makes the surface of the silicon hole after polishing
Pattern meets the requirement of different processing procedures.
Effect example 2
Storage stability and online service life are to evaluate the index of polishing fluid stability, for the ease of producing and operating,
It is required that polishing fluid has preferable stability in storage and use.In order to further investigate the storage of such polishing fluid and use
Stability, the present invention uses the contrast polishing fluid 2 and 40 pairs of the polishing fluid of the present invention of different storage times and online use time
Silica（Teos）Blank wafer is polished.
Polishing condition is：Lower pressure 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.
As a result as shown in Figure 4 and Figure 5, it was found from from Fig. 4 and Fig. 5, compared with comparative example 2, polishing fluid of the invention has
Higher silica removal rate, and silica removal rate is in storage（shelf life）In use（pot life）
It is more stable.
Claims (8)
1. a kind of chemical mechanical polishing liquid for silicon hole, it is characterised in that by abrasive grains, complexing agent, corrosion inhibitor,
Oxidant and potassium carbonate and/or saleratus composition, wherein, described abrasive grains are silica, and the complexing agent is selected from
One or more in ammonia carboxylation compound and its salt, organic carboxyl acid and its salt, organic phospho acid and its salt, organic amine, described corruption
Corrosion inhibitor is azole compounds, and described oxidant is selected from hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic acid, over cure
One or more in hydrochlorate, percarbonate, periodic acid, perchloric acid, high boric acid, potassium permanganate and ferric nitrate, described grinding
Granule content is 3~30wt%, and the content of described complexing agent is 0.01~5wt%, and described corrosion inhibitor content is
0.005~1wt%, described oxygenate content is 0.05~5wt%, potassium carbonate and/or the saleratus content is 0.1~
1wt%, the pH value of the polishing fluid is 8~12.
2. polishing fluid as claimed in claim 1, it is characterised in that the particle diameter of described abrasive grains is 20~250nm.
3. polishing fluid as claimed in claim 1, it is characterised in that described abrasive grains content is 5~20wt%.
4. polishing fluid as claimed in claim 1, it is characterised in that described ammonia carboxylation compound is selected from glycine, alanine, figured silk fabrics
Propylhomoserin, leucine, proline, phenylalanine, tyrosine, tryptophan, lysine, arginine, histidine, serine, asparagus fern ammonia
Acid, glutamic acid, asparagine, glutamine, nitrilotriacetic acid, ethylenediamine tetra-acetic acid, 1,2-diaminocyclohexane tetraacetic acid, the amber of ethylenediamine two
One or more in acid, diethylene triamine pentacetic acid (DTPA) and triethylenetetramine hexaacetic acid；Described organic carboxyl acid is acetic acid, grass
One kind or many in acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid, lactic acid, gallic acid and sulfosalicylic acid
Kind；Described organic phospho acid be 2- phosphonobutanes -1,2,4- tricarboxylic acids, ATMP, hydroxy ethylene diphosphonic acid,
One or more in ethylenediamine tetramethylene phosphonic acid, diethylenetriamine penta and 2- HPAAs, institute
State organic amine and be selected from ethylenediamine, diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, triethylene tetramine and four ethene
One or more in five amine.
5. polishing fluid as claimed in claim 1, it is characterised in that the content of described complexing agent is 0.1~1wt%.
6. polishing fluid as claimed in claim 1, it is characterised in that described azole compounds are selected from BTA, 5- first
Base BTA, 5- carboxy benzotriazoles, 1- hydroxyls-BTA, 1,2,4- triazoles, 3- amino -1,2,4- tri-
Nitrogen azoles, 4- amino -1,2,4- triazoles, 3,5- diaminostilbenes, 2,4- triazoles, 5- carboxyl -3- amino -1,2,4- triazoles,
3- amino -5- sulfydryls -1,2,4- triazoles, 5- acetic acid -1H- tetrazoles, 5- methyl tetrazoles, 5- phenyl tetrazole, 5- amino -
One or more in 1H- tetrazoles and 1- phenyl -5- sulfydryls-tetrazole.
7. polishing fluid as claimed in claim 1, it is characterised in that described corrosion inhibitor content is 0.005~
0.5wt%.
8. polishing fluid as claimed in claim 1, it is characterised in that described oxygenate content is 0.05~2wt%.
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| 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 |
| CN114686115A (en) * | 2020-12-30 | 2022-07-01 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution and use method thereof |
| 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 |
| 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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