CN1861723A - Silicon mono crystal substrate material polishing fluid and preparation process thereof - Google Patents

Silicon mono crystal substrate material polishing fluid and preparation process thereof Download PDF

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Publication number
CN1861723A
CN1861723A CN 200610014297 CN200610014297A CN1861723A CN 1861723 A CN1861723 A CN 1861723A CN 200610014297 CN200610014297 CN 200610014297 CN 200610014297 A CN200610014297 A CN 200610014297A CN 1861723 A CN1861723 A CN 1861723A
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China
Prior art keywords
polishing fluid
agent
crystal substrate
substrate material
silicon
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CN 200610014297
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Chinese (zh)
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刘玉岭
檀柏梅
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Hebei University of Technology
Hebei Polytechnic University
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Hebei University of Technology
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Priority to CN 200610014297 priority Critical patent/CN1861723A/en
Publication of CN1861723A publication Critical patent/CN1861723A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a polishing fluid with the backing material of the silicon single crystal. The polishing fluid is made up of the grinding material 1-95%; FA/O pH modifier 0.5-10%; the activating agent of the ether alcohol 0.5-1%; the de-ionized water residuum. The polishing fluid uses the metasilicate which can generate the macromolecule in the condition of the CMP and the new amine which can generate the stable complex compound with the minim metal ions. Also it has the function of the pH modifier, the stabilizer of the silicon hydrosol, the buffering agent and the complexing agent. The pH is 9-13.5. The polishing fluid with the small particle, high activeness and the low surface tension can reach the low rough, damage and non uniformly corrosion pit, high speed, clear of the backing material.

Description

Silicon mono crystal substrate material polishing fluid and preparation method thereof
Technical field
The present invention relates to chemical mechanical polishing liquid and preparation method thereof, particularly relate to a kind of polishing fluid that is used for silicon crystal substrate material and preparation method thereof.
Background technology
Silicon single-crystal is the main substrate material of present IC, and along with the integrated level of IC improves constantly, characteristic dimension constantly reduces, and the perfection of silicon chip surface is required more and more higher, requires the silicon chip surface height smooth, low coarse, high clean.Because the particle on polished section surface and metallic impurity contamination can badly influence breakdown characteristics, interfacial state and minority carrier life time, particularly the MOS large-scale integrated circuit influence to surperficial effect type is bigger, so planeness, defective, roughness, metallic impurity contamination and the particle on polished section surface had extremely strict requirement and control.As to produce 64 megalines wide be the DRAM device of 0.35 μ m, requires the beavy metal impurity on polished silicon slice surface to stain all less than 5 * 10 10Atoms/cm 2, the polished silicon slice surface greater than the total number of particles of 0.2 μ m less than 20/sheet.
Silicon wafer polishing generally includes thick throwing, the smart throwing for two steps, and thick purpose of throwing is the affected layer that grinding is caused and the removal of distortion floor height efficient, and reaches certain planeness, is under the situation that guarantees planeness to the requirement of thick throwing, realizes high-level efficiency, two-forty; And smart main task of throwing is to remove the affected layer that thick throwing process exists, and realizes surperficial low roughness, and shines under the broadside directive in kicker light, and no mist occurs.The smart throwing is last link of silicon chip processing, and smart quality of throwing the result directly has influence on the electrical characteristic of device.
Polishing fluid is the key that obtains polishing effect, is applied to the thick polishing fluid of throwing at present and normally comes adjust pH with mineral alkali, as: sodium hydroxide, potassium hydroxide, ammoniacal liquor etc., polishing speed is not high enough, and occurs the orange peel shape defective easily.Because temperature is lower, and chemical reaction causes polishing speed slack-off slowly,, improves polishing speed with this, and then enhance productivity in smart the throwing so these companies adopt the mechanical effect in greater particle size abrasive material (50-70nm) the raising finishing polish process.But this method has also produced polishing mist defective, surface tear simultaneously, residual particles absorption is difficult to problems such as cleaning, metal ion contamination.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, solve substrate slice surfaceness height that silicon mono crystal substrate material polishing fluid exists in polishing process, easily scratch, problem such as the limit of easily collapsing, and disclose a kind of chemical action strong, remove that speed is fast, surfaceness is low, do not have and scratch, and the polishing fluid of the low silicon crystal substrate material of cost and preparation method thereof.
Implementation of the present invention is as follows for achieving the above object:
The present invention selects alkaline medium for use according to the chemical property of silicon crystal substrate material, self-control SiO 2The water-sol is as abrasive material, and particle diameter is 15-100nm, and the pH value is 9-13.5, and adding FA/O tensio-active agent prepares polishing fluid.And utilize under the different polishing technological conditions two step polishing methods to polish, can realize the low roughness on silicon crystal substrate material surface, and can satisfy industrial the precision machined requirement of silicon monocrystalline substrate sheet CMP.
A kind of silicon mono crystal substrate material polishing fluid is characterized in that described polishing fluid preparation composition and weight % are than composed as follows:
Abrasive material 1-95 FA/OpH conditioning agent 0.5-10
Ether alcohol class promoting agent 0.5-1.5 deionized water surplus.
Described abrasive material is the SiO of particle diameter 15-100nm 2Colloidal sol, its concentration 30%-50%.
The agent of described FA/O pH regulator is an amine alkali.
Described pH regulator agent is ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine); As the agent of polishing fluid pH regulator, can play the effect of buffer reagent, can generate macromole product and water-soluble again, simultaneously multiple metal ion be played sequestering action, make reaction product under little mechanical effect, can break away from finished surface, can also play complexing and sequestering action simultaneously.
Described ether alcohol class promoting agent is a tween, can select FA/O surfactivity, O II-7 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 7-H), O II-10 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 10-H), O-20 (C 12-18H 25-37-C 6H 4-O-CH 2CH 2O) 70-H), JFC one or more.Tensio-active agent can reduce surface tension, improves concavo-convex selection ratio, can play infiltration and lubrication again, can strengthen transport process, can reach high smooth, high bright and clean surface again.
A kind of preparation method of silicon mono crystal substrate material polishing fluid is prepared as thick throwing liquid and fine polishing liquid respectively, it is characterized in that may further comprise the steps:
(1) slightly throw liquid:
A. be the SiO of 30-50% with particle diameter 15-100nm, concentration 2Abrasive material, with the deionized water dilution,
B. regulate above-mentioned solution with the pH regulator agent and make the pH value in the 9-13.5 scope,
C. after having regulated pH, add the ether alcohol class promoting agent of 0.5-1.0% while stirring;
(2) fine polishing liquid
A. select the SiO of particle diameter 15-25nm, concentration 30-50% for use 2Abrasive material, with the deionized water dilution,
B. regulate the pH value in the 9-12 scope with the agent of FA/O pH regulator, must add while stirring at regulate process neutral and alkali auxiliary agent,
C. after having regulated pH, add the 0.5-1.0%FA/O tensio-active agent while stirring.
By discovering in the CMP dynamic process, chemical process is a control process, the chemical process raising can effectively reduce roughness, control scratches, raises the efficiency greatly, improves surface cleanliness, we at first develop under the CMP condition can and the pasc reaction product form macromolecular cpd soluble in water, and tens metal ion species are formed the complex compound of stabilizer pole, and greater than the FA/O novel agent that guaranteed abrasive material stability at 12.5 o'clock, the polishing fluid performance has been obtained the breakthrough of matter in the pH value.
The present invention can be made into thick throwing liquid and fine polishing liquid, is applicable to thick throwing and the smart technology of throwing respectively, adopts the thick liquid of throwing to realize the high speed of removing, and when removal amount during near institute's claimed range, realizes the control of low roughness again with fine polishing liquid under big flow, low temperature, low pressure.
The present invention has following beneficial effect:
1. select nanometer SiO for use 2Colloidal sol is as the polishing fluid abrasive material, and its particle diameter little (15-100nm), concentration height (>40%), hardness little (damaging little), good dispersion degree can reach two-forty, high smooth, low damage, pollution-free, efficiently solve existing Al 2O 3Many drawbacks such as big, the easy scuffing of abrasive hardness, easy precipitation.
2. this polishing fluid is an alkalescence polishing liquid, easily generates the compound of solubility, thereby easily breaks away from glazed surface, can equipment not had corrosion, the silicon sol good stability.
3. select tensio-active agent for use, increased and just selected ratio, greatly reduced surface tension, reduced affected layer, improved the homogeneity and the rate of exchange of silicon chip surface, strengthened transport process, the concave-convex surface difference reduces greatly simultaneously, thereby effectively improves the planeness on surface and reduce roughness.
4. select for use macromolecular amine alkali as the agent of polishing fluid pH regulator, can play the effect of buffer reagent, can generate macromole product and water-soluble again, make reaction product under little mechanical effect, can break away from finished surface, can also play complexing and sequestering action simultaneously.
5. prescription advantages of simple, preparation technology is simple and direct, and price reduces cost; The many usefulness of potion are widely used.
Embodiment
Below in conjunction with preferred embodiment, to details are as follows according to embodiment provided by the invention:
Embodiment 1:
(1) slightly throws liquid: get particle diameter 15-100nm SiO 2Colloidal sol 800g puts into the 2760g deionized water while stirring, gets 400g ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine) then, selects to add 40gFA/O, O II-7 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 7-H), O II-10 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 10-H), O-20 (C 12-18H 25-37-C 6H 4-O-CH 2CH 2O) 70-H) one or more tensio-active agents are poured aforesaid liquid while stirring into; Get 4000g silicon monocrystalline substrate polishing fluid after stirring.
(2) fine polishing liquid: get particle diameter 15-25nmSiO 2Colloidal sol 800g puts into the 2820g deionized water while stirring, gets 320g ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine) then, and the 60gFA/O promoting agent is poured aforesaid liquid while stirring into; Get 4000g silicon monocrystalline substrate polishing fluid after stirring.Tensio-active agent can select to add FA/O, O equally II-7 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 7-H), O II-10 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 10-H), O-20 (C 12-18H 25-37-C 6H 4-O-CH 2CH 2O) 70-H) one or more.
Embodiment 2:
(1) slightly throws liquid: get particle diameter 15-100nm SiO 2Colloidal sol 3600g puts into the 180g deionized water while stirring, gets 210g ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine) then, and the 10gFA/O promoting agent is poured aforesaid liquid while stirring into; Get 4000g silicon monocrystalline substrate polishing fluid after stirring.
(2) fine polishing liquid: get particle diameter 15-25nmSiO 2Colloidal sol 3600g puts into the 1200g deionized water while stirring, gets 160g ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine) then, and the 40gFA/O promoting agent is poured aforesaid liquid while stirring into; Get 5000g silicon monocrystalline substrate polishing fluid after stirring.
Above-mentioned detailed description of silicon mono crystal substrate material polishing fluid and preparation method thereof being carried out with reference to embodiment; be illustrative rather than determinate; can list several embodiment according to institute's limited range; therefore in the variation and the modification that do not break away under the general plotting of the present invention, should belong within protection scope of the present invention.

Claims (6)

1. silicon mono crystal substrate material polishing fluid is characterized in that described polishing fluid preparation composition and weight % are than composed as follows:
Abrasive material 1-95 FA/O pH regulator agent 0.5-10
Ether alcohol class promoting agent 0.5-1.5 deionized water surplus.
2. silicon mono crystal substrate material polishing fluid according to claim 1 is characterized in that described abrasive material is the SiO of particle diameter 15-25nm 2Colloidal sol, its concentration 30%-50%.
3. silicon mono crystal substrate material polishing fluid according to claim 1 is characterized in that described FA/OpH conditioning agent is an amine alkali.
4. silicon mono crystal substrate material polishing fluid according to claim 3 is characterized in that described amine alkali is ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine).
5. silicon mono crystal substrate material polishing fluid according to claim 1 is characterized in that described ether alcohol class promoting agent is FA/O tensio-active agent, O II-7 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 7-H), O II-10 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 10-H), O-20 (C 12-18H 25-37-C 6H 4-O-CH 2CH 2O) 70-H) one or more.
6. the preparation method according to the silicon mono crystal substrate material polishing fluid of claim 1 is prepared as thick throwing liquid and fine polishing liquid respectively, it is characterized in that may further comprise the steps:
(1) slightly throw liquid:
A. selecting particle diameter 15-100nm, concentration for use is the SiO of 30-50% 2Abrasive material, with the deionized water dilution,
B. regulate above-mentioned solution with the pH regulator agent and make the pH value in the 9-13.5 scope,
C. after having regulated pH, add the ether alcohol class promoting agent of 0.5-1.0% while stirring;
(2) fine polishing liquid
A. selecting particle diameter 15-25nm, concentration for use is the SiO of 30-50% 2Abrasive material, with the deionized water dilution,
B. regulate the pH value in the 9-12 scope with the agent of FA/O pH regulator, must add while stirring at regulate process neutral and alkali auxiliary agent,
C. after having regulated pH, add the 0.5-1.0%FA/O tensio-active agent while stirring.
CN 200610014297 2006-06-09 2006-06-09 Silicon mono crystal substrate material polishing fluid and preparation process thereof Pending CN1861723A (en)

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Application Number Priority Date Filing Date Title
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CN1861723A true CN1861723A (en) 2006-11-15

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101972753A (en) * 2010-07-21 2011-02-16 河北工业大学 Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing
CN102039283A (en) * 2010-07-21 2011-05-04 河北工业大学 Surface cleaning method for Ti barrier layer material subjected to chemically mechanical polishing
US20120315764A1 (en) * 2010-07-21 2012-12-13 Yuling Liu Method of polishing copper wiring surfaces in ultra large scale integrated circuits
US20120318293A1 (en) * 2010-07-21 2012-12-20 Yuling Liu Method of cleaning wafer surfaces after polishing aluminum wirings in ultra large scale integrated circuits
CN102952467A (en) * 2012-11-09 2013-03-06 中国电子科技集团公司第四十六研究所 Polishing solution and method for polishing cadmium sulfide (CdS) wafer by applying same
CN102990503A (en) * 2012-11-09 2013-03-27 中国电子科技集团公司第四十六研究所 Polishing method applied to CdS wafer
CN106118491A (en) * 2016-07-11 2016-11-16 河北工业大学 A kind of alkalescence polishing liquid for thin copper film barrier layer cobalt and preparation method thereof
CN107030583A (en) * 2017-03-21 2017-08-11 天津华海清科机电科技有限公司 Silicon substrate film polishing method and device
CN110885636A (en) * 2019-11-13 2020-03-17 河北工业大学 Sapphire substrate polishing solution
CN113150697A (en) * 2021-03-01 2021-07-23 广州凌玮科技股份有限公司 Polishing solution for polishing surface of monocrystalline silicon wafer and preparation method thereof
CN114591684A (en) * 2022-02-18 2022-06-07 浙江开化元通硅业有限公司 Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101972753A (en) * 2010-07-21 2011-02-16 河北工业大学 Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing
CN102039283A (en) * 2010-07-21 2011-05-04 河北工业大学 Surface cleaning method for Ti barrier layer material subjected to chemically mechanical polishing
US20120315764A1 (en) * 2010-07-21 2012-12-13 Yuling Liu Method of polishing copper wiring surfaces in ultra large scale integrated circuits
US20120318293A1 (en) * 2010-07-21 2012-12-20 Yuling Liu Method of cleaning wafer surfaces after polishing aluminum wirings in ultra large scale integrated circuits
US8921229B2 (en) * 2010-07-21 2014-12-30 Yuling Liu Method of polishing copper wiring surfaces in ultra large scale integrated circuits
CN102952467A (en) * 2012-11-09 2013-03-06 中国电子科技集团公司第四十六研究所 Polishing solution and method for polishing cadmium sulfide (CdS) wafer by applying same
CN102990503A (en) * 2012-11-09 2013-03-27 中国电子科技集团公司第四十六研究所 Polishing method applied to CdS wafer
CN102990503B (en) * 2012-11-09 2015-07-29 中国电子科技集团公司第四十六研究所 For the finishing method of CdS wafer
CN106118491A (en) * 2016-07-11 2016-11-16 河北工业大学 A kind of alkalescence polishing liquid for thin copper film barrier layer cobalt and preparation method thereof
CN106118491B (en) * 2016-07-11 2018-06-12 河北工业大学 It is a kind of for alkalescence polishing liquid of thin copper film barrier layer cobalt and preparation method thereof
CN107030583A (en) * 2017-03-21 2017-08-11 天津华海清科机电科技有限公司 Silicon substrate film polishing method and device
CN110885636A (en) * 2019-11-13 2020-03-17 河北工业大学 Sapphire substrate polishing solution
CN110885636B (en) * 2019-11-13 2023-02-28 河北工业大学 Sapphire substrate polishing solution
CN113150697A (en) * 2021-03-01 2021-07-23 广州凌玮科技股份有限公司 Polishing solution for polishing surface of monocrystalline silicon wafer and preparation method thereof
CN113150697B (en) * 2021-03-01 2023-08-22 广州凌玮科技股份有限公司 Polishing solution for monocrystalline silicon piece surface polishing and preparation method thereof
CN114591684A (en) * 2022-02-18 2022-06-07 浙江开化元通硅业有限公司 Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof
CN114591684B (en) * 2022-02-18 2024-01-30 浙江开化元通硅业有限公司 Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof

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