CN104559797B - Silicon wafer fine polishing combination and preparation method thereof - Google Patents
Silicon wafer fine polishing combination and preparation method thereof Download PDFInfo
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- CN104559797B CN104559797B CN201410811996.4A CN201410811996A CN104559797B CN 104559797 B CN104559797 B CN 104559797B CN 201410811996 A CN201410811996 A CN 201410811996A CN 104559797 B CN104559797 B CN 104559797B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention relates to a silicon wafer fine polishing combination and a preparation method thereof and belongs to the technical field of chemical-mechanical polishing (CMP). The combination comprises an acidic silica sol, a diol compound, a thiourea compound, an alkaline compound, salt, a surfactant and deionized water. According to the silicon wafer fine polishing combination provided by the invention, while the surface defect after rough polishing can be overcome, the stress generated in the rough polishing process is reduced, and the surface precision is improved; meanwhile, the polishing rate is close to that of silicon wafer rough polishing liquid.
Description
Technical field
The invention belongs to chemically mechanical polishing (cmp) technical field, particularly to a kind of silicon wafer fine polishing compositionss.
Background technology
Semiconductor materials based on silicon materials has been electronics and information industry most important basic function material, in state
Critically important status is occupied in people's economy and war industry.More than 95% is had to be to use silicon materials system in global semiconductor device
Become, wherein 85% integrated circuit is also to be fabricated from a silicon.At present, ic technology has been enter into the nanometer electricity that live width is less than 0.1 μm
In period of the day from 11 p.m. to 1 a.m generation, the suface processing quality requirement to silicon single-crystal polishing plate is more and more high, and traditional polishing fluid can not meet silicon single crystal flake
Polishing requires.In order to ensure higher machining accuracies such as silicon polished angularity, the partly flat degree in surface, surface roughnesses,
New polishing fluid and glossing must be developed.Obtaining the higher silicon wafer of surface processing accuracy is the weight manufacturing integrated circuit
Want link, be directly connected to the qualification rate of integrated circuit.
Simple chemical polishing, polishing speed is relatively slow, surface accuracy is higher, damage is low, integrity good, but it can not be revised
Surface surface precision, polishing concordance is also poor；Simple mechanical polishing concordance is good, and surface smoothness is high, and polishing speed is higher,
But damage layer depth, surface accuracy is relatively low；Chemically mechanical polishing both can obtain more perfect surface, can obtain higher throwing again
Optical speed, is that by the unique method of global planarizartion.Traditional cmp system is made up of following three parts: the silicon of rotation
Holder for x-ray film, the workbench carrying polishing pad, polishing fluid (slurry) supply system.During polishing, the workpiece of rotation is with certain
Pressure imposes on the polishing pad rotating with workbench, and polishing fluid flows between workpiece and polishing pad, and in surface of the work
Produce chemical reaction, the chemical reactant that surface of the work is formed is removed by the mechanical friction effect of abrasive material.In chemical membrane and machine
In the alternation procedure of tool striping, very thin layer of material is removed from surface of the work by the collective effect of chemistry and machinery, finally
Realize ultra-precision surface processing.Therefore, high efficiency to be realized, high-quality polishing are it is necessary to make chemical action process make with machinery
Realize good coupling with process.
At present, silicon wafer diameter has developed to more than 200mm, and the requirement to silicon wafer surface quality is higher, in order to ensure
The polishing precision of silicon wafer, reaches the technical specification of integrated circuits silicon wafers requirement, needs silicon chip is carried out with three step chemistry
Mechanical polishing (cmp) (rough polishing, fine polishing, finishing polish).
Polishing required precision due to polishing each step is different, and the requirement to polishing fluid is also different, then need to develop three kinds
Polishing fluid is targetedly polished to its each step, and to meet each step polishing requirement, (difference has: the chemical group of polishing fluid
Divide, polish wear particle size and distribution, polishing wear particle concentration and polishing fluid ph value etc.；The material of polishing cloth, porosity, hole size,
Surface groove structures and hardness etc.；Polish pressure, temperature, rotating speed, polishing flow quantity etc.), corresponding silicon chip respectively walks and will reach
To machining accuracy also different: first rough polishing is carried out to silicon chip it is therefore an objective to remove the damage that surface is stayed by front road manufacturing procedure
Hinder layer, and reach the physical dimension machining accuracy of requirement, typically require polishing speed to reach more than 1 micron, roughness is left in 1nm
Right；Then carry out fine polishing it is ensured that silicon chip surface eliminates removes at a high speed the stress causing reduction table further due to rough polishing
Surface roughness, in 0.5 microns, roughness is in 0.7nm for speed；Finally carry out " mist elimination " finishing polish it is ensured that silicon chip table
There is high surface nanotopology characteristic in face.
Similar with other silicon wafer polishing liquids, silicon wafer fine polishing liquid is mainly made up of three parts: abrasive material, chemical composition and
Water；In order to remove the target of the defects such as stress and the burn into residual of rough polishing introducing during realizing silicon wafer fine polishing, adopt both at home and abroad
Attempted with various ways, and achieved certain progress.
Abrasive material aspect, the abrasive material as polishing fluid is mostly oxide particle or organic granular, such as silicon dioxide, oxidation
Aluminum, cerium oxide, granules of polystyrene etc., wherein silicon dioxide are current using silicon wafer polishing liquid abrasive material the widest.Titanium dioxide
Silicon particle surface is rich in oh group, has stronger activity, can react with some chemical substances under certain condition.
Using this property of silicon dioxide granule, silica particle surface can be carried out with the transformation of chemical property.
In terms of integrated circuit wiring polishing, patent us6646348 discloses a kind of silane coupler as polishing fluid
Component, is formed oligomer after the hydrolysis of this silane coupler and is mixed with the abrasive material in polishing fluid and other chemical reagent phases, can obtain
Obtain the polishing speed of relatively low teos and ta, and obtain preferable polished surface.Patent us6656241 discloses a kind of dichloro two
The modified silica aggregate of methyl-monosilane, and it is applied to cu polishing fluid, silica aggregate can through modification
It is well dispersed in polishing fluid, and the polishing speed of cu and ta is affected by modification with selecting ratio.Patent
Ep0371147b1 discloses a kind of silicon wafer polishing compositionss of the coupling agent modified Ludox of trialkylsilane, in polishing process
Play the effect of stabilized colloidal silica, decrease the scuffing in polishing process；These are processed all only around improving polish abrasive
Stability, degree of scatter, obtain appropriateness reduction using the abrasive hardness after silylating reagent, polishing microcell inorganic abradant is to workpiece
" the hard impact " on surface is replaced by " Elastic Contact ", and silanization layer serves cushioning effect, for improving polishing defect.
Above improvement all achieves certain effect to defects controlling, but makes for being applied to minimizing silicon wafer surface rough polishing
The stress becoming and the monocrystal silicon fine polishing polishing fluid of defect, have lower surface roughness, higher surface accuracy, less corruption
The requirement of higher polishing speed aspect also will be had while erosion defect also to there is certain limitation.
Content of the invention
Instant invention overcomes silicon wafer surface defect control only focused in polishing process by traditional silicon wafer fine polishing polishing fluid
Problem, disclose a kind of silicon wafer fine polishing compositionss, while surface defect after rough polishing can not only be eliminated, reduce rough polishing mistake
The stress producing in journey, improves surface accuracy；Polishing speed is close to the polishing speed of silicon wafer rough polishing solution simultaneously.With general
Silicon wafer fine polishing liquid different, polishing composition of the present invention can achieve the polishing speed of general silicon wafer rough polishing liquid, simultaneously can be real
Now higher polishing precision, up to below 0.3nm, general rough polishing precision is in 0.6～0.9nm for polishing precision.
A kind of silicon wafer fine polishing compositionss of the present invention are it is characterised in that described compositionss include following components and contain
Amount:
The acid silicon dioxide sol of 10 weight % to 50 weight %；
One or more diol compound of 0.01 weight % to 1 weight %；
A kind of thiourea of 0.1 weight % to 1 weight %；
One or more alkali compounds of 0.5 weight % to 5 weight %；
A kind of salt of 0.01 weight % to 3 weight %；
A kind of surfactant of 0.001 weight % to 0.05 weight %；
Deionized water surplus.
The ph value of described compositionss is 9 to 12.
Described acid silicon dioxide sol is 10～100nm, the acidic silicasol that ph is less than 6.
Described diol compound is ethylene glycol (eg), propylene glycol (pg), butanediol (bg), hexanediol (hg), diethylene glycol
(deg), one or more of triethylene glycol (teg), Polyethylene Glycol (peg), polypropylene glycol (ppg).
Described thiourea is thiourea (tu), methylthiourea (mtu), dimethyl sulfourea (dmtu), tetramethyl thiourea
(tmtu), ethyl thiourea (etu), diethyl thiourea (detu), n-pro-pyl thiourea (ptu), di-isopropyl thiourea (dptu), allyl
One of base thiourea (atu), phenylthiourea (phtu), tolylthiourea (ttu) and chlorphenyl thiourea (cptu).
Described alkali compoundss are potassium hydroxide (koh), sodium hydroxide (naoh), Tetramethylammonium hydroxide (tmah), ammonia
(nh3), methyl amine (ma), dimethyl amine (dma), Trimethylamine (tma), ethylamine (ea), diethylamide (dea), triethyl group
Amine (tea), isopropanolamine (mipa), aminopropanol (ap), tetraethyl amine (teah), ethanolamine (mea), diethyl triamine
(dta), trientine (tta), hydroxyethylethylene diamine (aeea), hexamethylene diamine (hda), diethylenetriamines
(deta), one or more of trien (teta), Piperazine anhydrous (piz), anthalazine (pha).
Described salt is precipitation membranous type corrosion inhibiter, is the ammonium of carbonic acid, phosphoric acid, specially carbonic acid and its acid, potassium, sodium salt；Phosphorus
One of the ammonium of acid and its acid, potassium, sodium salt.
Described surfactant is in nonionic surfactant, anion surfactant or cationic surfactant
One kind.
Described nonionic surfactant is polydimethylsiloxane (pdms), fatty alcohol-polyoxyethylene ether (aeo), polyoxy
Propylene polyoxyethylene block copolymer (eo-po)；Anion surfactant is dodecylbenzene sodium sulfonate (sdbs), dodecane
Base sodium sulfonate (k-12), alpha-olefin sodium sulfonate (aos), diisooctyl succinate sodium sulfonate (aot), fatty alcohol-polyoxyethylene ether sulfur
Sour sodium (aes)；Cationic surfactant is myristyl benzyl dimethyl ammonium chloride, Dodecyl trimethyl ammonium chloride
(tdbac), guar hydroxypropyl trimonium chloride (c-162), bromination dodecyl trimethyl ammonium (dtab), bromination dodecane
One of base dimethyl benzyl ammonium (ddba).
A kind of preparation method of silicon wafer fine polishing compositionss of the present invention is it is characterised in that the method includes following step
Rapid:
1) weigh each component in described ratio, with agitator, acid silicon dioxide sol is scattered in deionized water；
2) add thiourea after under agitation, adding diol compound；
3) add surfactant, and add the mixture of alkali compoundss and salt, and by polishing composition ph value
Adjust to 9～12；
4) with the filter element that aperture is 0.5 μm, polishing composition is filtered, to remove the bulky grain in polishing composition
Impurity, that is, obtain finished product.The each group of the present invention is grouped into the chemistry effectively improving in polishing process and mechanism, raising
The precision of silicon wafer and also maintain high removal rate while surface quality after polishing.In the present invention, acidity silicon used is molten
Glue ph specifically controls in 3-5, and processes acidic silicasol with diol compound, improves polishing particles density of surface hydroxyl, promotes
Granule surface activity；The thiourea then adding will act on the high polishing particles surface of surface activity, improves polishing
While the mechanism of granule and protect silicon chip surface after polishing, the stress producing during eliminating rough polishing.
Match with the alkali compoundss in polishing fluid composition, alkali compoundss etching silicon layer, form soft layer, surface contains
The particle having thiourea can form adsorbed film on soft layer, plays the effect of protection silicon chip surface；Recycle precipitation
The increase protective effect further to silicon chip surface for the membranous type corrosion inhibiter, can avoid the damage because granule causes and chemistry to surface
Act on the corrosion causing, and keep higher removal rate.
In addition, being the surface accuracy of silicon wafer after improvement polishing further, also add in polishing fluid composition in the present invention
Enter appropriate surfactant, improved the hydrophilic on polishing fluid surface further, made the silicon wafer surface quality after polishing more
Good.
Brief description
Fig. 1 is the atomic force microscopy diagram using silicon chip after the polishing of the embodiment of the present invention 2 compositionss.
Fig. 2 is the atomic force microscopy diagram of the silicon chip after being polished using the embodiment of the present invention 6 compositionss.
Fig. 3 is the atomic force microscopy diagram of the silicon chip after being polished using comparative example 2 compositionss.
Fig. 4 is the atomic force microscopy diagram of the silicon chip after being polished using comparative example 3 compositionss.
Specific embodiment
Below by embodiment and comparative example, the invention will be further elaborated, certainly should not be construed as limit anyway
The scope of the present invention processed, such as no special mark, each component addition is all mass percent.
The above be only the preferred embodiment of the present invention it should be pointed out that be general technology for the art
For personnel, on the premise of without departing from the technology of the present invention principle, can also make corresponding adjust and improve, these adjustment and
Improve and also should be regarded as protection scope of the present invention.
Polishing composition after configuration is used for polishing experiments, polishing experiments parameter is as follows:
Buffing machine: single side polishing machine, it is furnished with 4 rubbing heads, each rubbing head can throw 4 silicon chips；
Polish pressure: 32kpa；
Polishing rotary speed: 90 turns/min；
Rubbing head rotating speed: 100 turns/min；
Polishing silicon single crystal flake specification: p-type<100>, diameter 100mm, resistivity: 0.1～100. ω cm；
Polishing time: 20min；
Polishing pad: polyurethane foam solidification polishing pad, rodel company sub 600 type polishing pad；
Polishing flow quantity: 230ml/min；
Polish temperature: 20 DEG C
Silicon chip surface quality testing after polishing:
For the attachment impact to testing result for the impurity avoiding silicon wafer surface to exist, before detection silicon wafer is existed respectively
It is cleaned by ultrasonic in acetone, dehydrated alcohol, deionized water.
Surface roughness using silicon wafer after afm detection polishing.Testing adopted afm is bruker dimension
Icon, probe radius is 10nm, and its vertical resolution is 0.01nm, and rate of scanning is 1.5hz, 50 × 50 μm 2 of sweep limitss.
Converge light source (tengsten lamp), converging beam spot diameter 20～40mm away from light source 100mm, range estimation inspection using high intensity
Test the defect (road plan) on whole polished silicon wafer surface, according to detection case by polished silicon wafer surface defect degree be divided into very well (◎ ◎),
Good (◎), preferably (zero), poor (☆), poor (☆ ☆).
Polishing Mean Speed: polish removal rate is obtained by the change calculations of silicon chip center portion thickness before and after polishing,
For the meansigma methodss of four silicon chip center thickness differences, its available calibrator records, when polishing speed is polishing clearance and polishing
Between ratio, polishing Mean Speed be polishing speed within the polishing pad service life time meansigma methodss.
Can be seen that from table 1 embodiment compared with conventional polishing compositions with the polishing experiments result of comparative example, the present invention
In polishing composition, while keeping high polishing clearance, silicon wafer surface precision is higher and surface defect is less.
As seen from the above-described embodiment, in the optimal polishing composition under polishing technological conditions of the present invention, each component contains
Measure and be: ph is 3, the acid silicon dioxide sol of mean diameter 30nm contains 40%；Diol compound pg0.2%；Thiourea chemical combination
Thing tu contains 0.1%；Alkali compoundss deta2%, koh1%；Potassium bicarbonate 0.3%, eo-po containing surfactant 0.05%
When, the silicon chip surface roughness low cause 0.173nm after polishing composition polishing, derate reaches 0.89 μm/min.
Above-described embodiment absolutely proves that the polishing composition of the present invention is a kind of cmp polishing material of function admirable, special
It is not suitable for silicon wafer fine polishing.
The preparation of table 1 embodiment and comparative example and test experiments result
Claims (9)
1. a kind of silicon wafer fine polishing compositionss are it is characterised in that the component of described compositionss and content are as follows:
The acid silicon dioxide sol of 10 weight % to 50 weight %；
One or more diol compound of 0.01 weight % to 1 weight %；
A kind of thiourea of 0.1 weight % to 1 weight %；
One or more alkali compounds of 0.5 weight % to 5 weight %；
A kind of salt of 0.01 weight % to 3 weight %；
A kind of surfactant of 0.001 weight % to 0.05 weight %；
Deionized water surplus；
The ph value of described compositionss is 9 to 12.
2. compositionss according to claim 1 are it is characterised in that described acid silicon dioxide sol is 10～100nm, ph
Acidic silicasol less than 6.
3. compositionss according to claim 1 it is characterised in that described diol compound be ethylene glycol eg, propylene glycol pg,
One of butanediol bg, hexanediol hg, diethylene glycol deg, triethylene glycol teg, Polyethylene Glycol peg, polypropylene glycol ppg or many
Kind.
4. compositionss according to claim 1 are it is characterised in that described thiourea is thiourea tu, methylthiourea
Mtu, dimethyl sulfourea dmtu, tetramethyl thiourea tmtu, ethyl thiourea etu, diethyl thiourea detu, n-pro-pyl thiourea ptu, two
In isopropylthiourea dptu, allylthiourea atu, phenylthiourea phtu, tolylthiourea ttu and chlorphenyl thiourea cptu one
Kind.
5. compositionss according to claim 1 are it is characterised in that described alkali compoundss are potassium hydroxide koh, hydroxide
Sodium naoh, Tetramethylammonium hydroxide tmah, ammonia nh3, methyl amine ma, dimethyl amine dma, Trimethylamine tma, ethylamine ea, two
Ethylamine dea, triethylamine tea, isopropanolamine mipa, aminopropanol ap, tetraethyl amine teah, ethanolamine mea, diethyl three
Amine dta, trientine tta, hydroxyethylethylene diamine aeea, hexamethylene diamine hda, diethylenetriamines deta, Sanya second
One or more of urotropine teta, Piperazine anhydrous piz, anthalazine pha.
6. it is characterised in that described salt is precipitation membranous type corrosion inhibiter, precipitation membranous type delays compositionss according to claim 1
Erosion agent is ammonium, potassium, sodium salt or one of the ammonium for phosphoric acid and its acid, potassium, sodium salt of carbonic acid and its acid.
7. compositionss according to claim 1 it is characterised in that described surfactant be nonionic surfactant,
One of anion surfactant or cationic surfactant.
8. compositionss according to claim 7 are it is characterised in that described nonionic surfactant is polydimethylsiloxanes
Alkane pdms, fatty alcohol-polyoxyethylene ether aeo, polyoxyethylene polyoxypropylene block copolymer eo-po；Anion surfactant is
Dodecylbenzene sodium sulfonate sdbs, dodecyl sodium sulfate k-12, alpha-olefin sodium sulfonate aos, diisooctyl succinate sodium sulfonate
Aot, polyoxyethylenated alcohol sodium sulfate aes；Cationic surfactant be myristyl benzyl dimethyl ammonium chloride, 12
Alkyl trimethyl ammonium chloride tdbac, guar hydroxypropyl trimonium chloride c-162, bromination dodecyl trimethyl ammonium dtab,
One of dodecyl dimethyl benzyl ammonium bromide ddba.
9. compositionss described in a kind of any one according to claim 1-8 preparation method it is characterised in that the method include following
Step:
1) weigh each component in described ratio, with agitator, acid silicon dioxide sol is scattered in deionized water；
2) add thiourea after under agitation, adding diol compound；
3) add surfactant, and add the mixture of alkali compoundss and salt, and polishing composition ph value is adjusted
To 9～12；
4) with the filter element that aperture is 0.5 μm, polishing composition is filtered, to remove the large granular impurity in polishing composition,
Obtain finished product.
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| CN105710760A (en) * | 2016-04-22 | 2016-06-29 | 衡阳市宏达威环保科技有限公司 | Aluminium alloy alkaline grinding fluid |
| CN108250973A (en) * | 2016-12-28 | 2018-07-06 | 安集微电子科技（上海）股份有限公司 | A kind of chemical mechanical polishing liquid for barrier layer planarization |
| CN109554119B (en) * | 2018-11-02 | 2020-11-20 | 山东天岳先进材料科技有限公司 | Silicon carbide chemical mechanical polishing solution with improved pH stability and application thereof |
| WO2020087721A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | Chemical-mechanical polishing solution for silicon carbide having increased ph stability, preparation method therefor, and use thereof |
| CN111098237A (en) * | 2019-12-24 | 2020-05-05 | 常州万博金属构件厂 | Preparation method of non-adhesive polished wafer |
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| CN102585706A (en) * | 2012-01-09 | 2012-07-18 | 清华大学 | Acidic chemical and mechanical polishing composition |
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