CN102199400A - Copper polishing slurry for use in fine atomized CMP process - Google Patents
Copper polishing slurry for use in fine atomized CMP process Download PDFInfo
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- CN102199400A CN102199400A CN2011100735080A CN201110073508A CN102199400A CN 102199400 A CN102199400 A CN 102199400A CN 2011100735080 A CN2011100735080 A CN 2011100735080A CN 201110073508 A CN201110073508 A CN 201110073508A CN 102199400 A CN102199400 A CN 102199400A
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Abstract
The invention discloses a copper polishing slurry for use in a fine atomized chemical mechanical polishing (CMP) process, comprising 1-3wt% white carbon black, 2-8wt% hydrogen peroxide, 1wt% benzotriazol, 0.7wt% aminoacetic acid and the remainder consisting of deionized water, and the PH of the copper polishing slurry is 9.5-10.5. According to the invention, the components of the copper polishing slurry for the atomized polishing process are obtained by experimental research.
Description
Technical field
The present invention relates to polishing fluid, relate in particular to the copper polishing fluid.
Background technology
Chemically machinery polished (chemical mechanical polishing, CMP) be to utilize the slurry and the workpiece surface that mix by minute abrasive and chemical solution that the chemical bond that serial chemical reaction changes workpiece surface takes place, generate the low shearing resistance product of removing easily, pass through the mechanical effect of polymer polishing pad again, from workpiece surface removal layer of material as thin as a wafer, thereby obtain high precision low roughness not damaged smooth surface.The CMP technology can be taken into account the overall situation and the local planeness on surface effectively.Oneself becomes current ULSI the most widely used planarization of epoch the CMP technology.With present level, using chemical Mechanical Polishing Technique is the best approach that guarantees the planarization of substrate full wafer, it is irreplaceable interlayer flattening method in ULSI chip multilayer wiring not only, also is the final most effectual way that obtains nanometer grade super smooth not damaged surface of silicon chip processing
[1-4]The develop rapidly of CMP technology not only provides the overall market needs of CMP polissoir, also provides expendable material-polishing fluid (comprising dielectric layer polishing solution and metal-polishing liquid) boundless market
[5]
Polishing fluid is one of key element of CMP, and the performance of polishing slurries directly influences the quality of surface of polished.Polishing fluid mainly is made up of abrasive material, oxygenant, passivator or complexing agent, pH regulator agent, suspension agent, tensio-active agent and deionized water etc.Acid, its polishing mechanism difference of polishing fluid that alkalescence is different, polishing efficiency are also different.The side effect of acid slurry in polishing process is bigger.Generally comprise complexing agent, oxygenant, dispersion agent, pH modulator and mill section in the alkaline slurry.The chemical action of slurry plays a major role in CMP, the chemical constitution of slurry, and the kind of abrasive particle, granularity, shape and solid content, viscosity, pH value, flow velocity, flowpaths all have significant effects to the surface finish of removing speed and polished section
[6-10]
Yet, since the CMP technology begins to be applied to IC and makes, the blame of this technology had never been stopped.One of them is exactly that the cost of consumptive materials such as CMP slurry, polishing pad, correction-plate accounts for about 70% of CMP process total cost for the problem that the traditional C MP technology of generally acknowledging exists, the cost of polishing slurries just accounts for 60～80% of consumptive material, but the utilization ratio of polishing slurries can only reach about 20%; The management of polishing slurries and the processing of slug also quite bother, and are discharged into nature in a large number and cause environmental pollution.
From present stage, reducing production costs becomes the key that improves the IC product competitiveness, one of high most important reason of IC manufacturing cost is exactly the excessive use of polishing fluid, SpeedFam-IPEC studies show that, the expenditure of consumptive material accounts for 60～80% in the CMP technology, and the expenditure of polishing fluid (slurry) accounts for 60～80% of consumptive material.Ordinary copper polishing fluid price price $40/gallon, general 200 milliliters/min of every needs of CMP polishing machine; The discharging of a large amount of polishing waste liquids makes some deleterious chemical reagent enter nature in the traditional C MP process, is unfavorable for that the IC industry develops towards the direction of environmental protection.The technical barrier that these problems have become the following Ying Yong of traditional C MP Han to solve, overcoming these shortcomings of traditional C MP has become the important Practical Research direction of planarization techniques.
Ultrasonic finer atomization chemical Mechanical Polishing Technique is exactly that the component of extraordinary polishing fluid is controlled ultrasonic finer atomization frequently, forming the Suo Taier diameter is the even micron order liquid grain of 5～25 μ m, import polishing/polishing interface by particular form, through the high-performance evening chemical effect between strong absorption, strong activity and interface, be reacted into the lower even mulch film of shearing resistance at substrate surface, remove by mechanical effect, form the super smart nano level of smooth not damaged surface.Because the atomizing polishing technology proposes first for applicant place scientific research group, is in blank about the research that is applicable to the polishing fluid that atomizing is polished at present.
Summary of the invention
At the prior art above shortcomings, the applicant provides a kind of copper polishing fluid, is applicable to the atomizing glossing.
The present invention is directed to above-mentionedly in order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
The invention discloses a kind of finer atomization CMP copper polishing fluid that is applicable to, comprise white carbon black, hydrogen peroxide, benzotriazole, Padil, wherein the mass percent of white carbon black is 1% ~ 3%, the mass percent of hydrogen peroxide is 2% ~ 8%, the mass percent of benzotriazole is 1%, the mass percent of Padil is 0.7%, and remaining ingredient is a deionized water, and the pH value of described copper polishing fluid is 9.5-10.5.
Further, the mass percent of white carbon black is 3%, and the mass percent of hydrogen peroxide is 5%, and the mass percent of benzotriazole is 1%, and the mass percent of Padil is 0.7%.
Technique effect of the present invention is: study by experiment, obtained the copper polishing fluid component of suitable atomizing glossing.
Embodiment
Polishing fluid had both influenced CMP chemical action process, had influence on its mechanical effect process again.In order to form the soft and crisp oxide film of one deck at the copper glazed surface fast, so that machinery is removed, thereby improve the polishing clearance and reduce the copper surface finish, so the applicant adds the hydrogen peroxide of metal ion not as oxygenant in alkalescence polishing liquid.Selecting white carbon black for use is abrasive material, to avoid owing to Al
2O
3Surface damage that pellet hardness causes greatly and Al
3+The pollution problem that causes.Alkaline condition adds Padil down as complexing agent, forms copper amine complex ion, and the solubility of Reinforced Cu has improved the clearance of copper, and controls the pollution of metal ion, avoids solution to produce gelatin phenomenon.Add benzotriazole as promoting agent, under alkaline environment, BTA can guarantee that polishing fluid is dispersed preferably, and the formation that reduces the corrosion pit on copper surface.Use the pH regulator agent of borax in addition as polishing fluid, facile hydrolysis in the borax solution and show alkalescence, and can make the pH value stabilization about 9.5-10.5.
The making method of copper polishing fluid disclosed by the invention is as follows: at first add pH value conditioning agent (borax) and promoting agent (benzotriazole), and add a certain amount of deionized water and adjust solution to make pH value be 9.5-10.5, white carbon black is better dispersed in this pH scope, the white carbon black that under induction stirring, slowly adds particle diameter 12nm, add complexing agent (Padil) afterwards, add the oxygenant (hydrogen peroxide) of design flow again.Adopt the polishing fluid of aforesaid method preparation to have satisfactory stability.It is as follows that aforementioned electromagnetic stirs concrete operation method: the unit type of at first selecting for use German IKA to produce is the magnetic stirrer of C-MAG HS7; Connect attaching plug, switch placed " ON " shelves, stirrer is put into beaker, then beaker is placed on the magnetic stirrer, add pH value conditioning agent, go into promoting agent and deionized water, at this moment use the speed of the operation knob setting machine on the right, make rotating speed be 3r/s.
In the manufacturing processed of above-mentioned copper polishing fluid, the mass percent of white carbon black is 1% ~ 3%, the mass percent of hydrogen peroxide is 2% ~ 8%, the mass percent of benzotriazole is 1%, the mass percent of Padil is 0.7%, remaining ingredient is a deionized water, and wherein hydrogen peroxide is 30% superoxol.
The UNIPOL-1502 type polishing experiments machine that the present invention adopts Shenyang Kejing Automatic Equipment Co., Ltd to produce carries out the polishing effect test.Polishing disk rotating speed: 50 r/min, polish pressure: 5psi, envrionment temperature: room temperature; Tradition polishing time 5min, atomized liquid flow atomized liquid flow altogether is 800 ml; Atomizing polishing time 9min, the atomized liquid flow is 30 ml.Polishing finishes the back and throws 2min with deionized water; Test specimen: cutting of electrolysis copper rod line and thin slice that φ 25 * 1mm is thick through polishing; Material removing rate is with electronic balance (precision: 0.01 mg) measure, with the test specimen mean value calculation clearance of poor quality of replicate measurement before and after the polishing 4 times; Surface of polished roughness and pattern are measured with atomic force microscope (the CSPM5000 scanning probe microscope system that basis nanometer Instr Ltd. produces).
8 groups of embodiment that table 1 is chosen in aforementioned range for the applicant, and corresponding polishing effect value.Table 1
As can be seen from the table: under atomizing finishing method situation, the continuous increase of abrasive material content helps improving material removing rate, also can obtain the surface of good quality of finish simultaneously.But along with the continuous increase of oxygenant, the polishing clearance can descend.Wherein slurry 5 has obtained the relative higher removal of 188 nm/min, polishing efficiency that it is comprehensive and best results.
Table 2
From multiple test slurry, draw three kinds of polishing effects polishing fluid preferably, and their polishing effects are separately made comparisons.Slurry 1 and slurry 2 use traditional finishing method, and what slurry 3 used is the atomizing finishing method.
Atomizing polishing and tradition polishing difference aspect clearance are not very big as can be seen from Table 2, find that in experiment atomizing polishing polishing time needs the time a little long than the tradition polishing, and being beneficial to fog so fully spreads, and reaches comparatively ideal clearance.The composite order of different polishing fluids also is very big with the influence that each different set of dispense is compared polishing speed.Slurry 1 surface obviously produces corrosion pit, and slurry 2 surfaces produce cut.Copper corrosion hole and cut after slurry 3 polishing obviously reduce, and are slurry 1 and 2 1/tens times at the consumption of slurry 3 aspect the polishing fluid consumption.
No matter be the tradition polishing or the method for atomizing polishing fluid, can obtain the higher copper surface of planeness, but traditional finishing method cause the imbalance of chemical action and mechanical effect easily, such as the slice, thin piece surface contamination, cut and corrosion etc.Slurry 1 obviously reduces the copper sheet surfaceness, is reduced to 38.05nm by 50nm, and slurry 2 makes the copper sheet surfaceness be reduced to 15.22nm by 25nm.Surfaceness after the slurry 3 atomizing polishings is reduced to 7.61nm by 12nm, and the polishing fluid of visible atomizing not only can significantly reduce the polishing fluid consumption and can reach workpiece quality of finish preferably again.
Claims (2)
1. be applicable to the copper polishing fluid of finer atomization CMP, it is characterized in that comprising white carbon black, hydrogen peroxide, benzotriazole, Padil, wherein the mass percent of white carbon black is 1% ~ 3%, the mass percent of hydrogen peroxide is 2% ~ 8%, the mass percent of benzotriazole is 1%, the mass percent of Padil is 0.7%, and remaining ingredient is a deionized water, and the pH value of described copper polishing fluid is 9.5-10.5.
2. the finer atomization CMP copper polishing fluid that is applicable to according to claim 1, the mass percent that it is characterized in that white carbon black is 3%, and the mass percent of hydrogen peroxide is 5%, and the mass percent of benzotriazole is 1%, and the mass percent of Padil is 0.7%.
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| CN2011100735080A CN102199400A (en) | 2011-03-25 | 2011-03-25 | Copper polishing slurry for use in fine atomized CMP process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382576A (en) * | 2011-11-10 | 2012-03-21 | 江南大学 | Ultrasonic atomization alkaline polishing solution |
| CN104017501A (en) * | 2014-06-12 | 2014-09-03 | 江南大学 | Ultrasonic atomization-type polishing solution suitable for TFT-LCD (Thin Film Transistor-Liquid Crystal Display) glass substrate |
| CN111234708A (en) * | 2020-03-31 | 2020-06-05 | 河南联合精密材料股份有限公司 | Wet-type CMP mirror polishing solution for stainless steel mobile phone middle frame and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340583A (en) * | 2000-08-24 | 2002-03-20 | 不二见株式会社 | Polishing composition and polishing method for its use |
| CN101358108A (en) * | 2007-08-03 | 2009-02-04 | 罗门哈斯电子材料Cmp控股股份有限公司 | Selective barrier polishing slurry |
-
2011
- 2011-03-25 CN CN2011100735080A patent/CN102199400A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340583A (en) * | 2000-08-24 | 2002-03-20 | 不二见株式会社 | Polishing composition and polishing method for its use |
| CN101358108A (en) * | 2007-08-03 | 2009-02-04 | 罗门哈斯电子材料Cmp控股股份有限公司 | Selective barrier polishing slurry |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382576A (en) * | 2011-11-10 | 2012-03-21 | 江南大学 | Ultrasonic atomization alkaline polishing solution |
| CN104017501A (en) * | 2014-06-12 | 2014-09-03 | 江南大学 | Ultrasonic atomization-type polishing solution suitable for TFT-LCD (Thin Film Transistor-Liquid Crystal Display) glass substrate |
| CN111234708A (en) * | 2020-03-31 | 2020-06-05 | 河南联合精密材料股份有限公司 | Wet-type CMP mirror polishing solution for stainless steel mobile phone middle frame and preparation method thereof |
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Application publication date: 20110928 |