CN107400501B - A kind of chemical mechanical grinding agent, dispersed nano silicon oxide microsphere preparation method - Google Patents
A kind of chemical mechanical grinding agent, dispersed nano silicon oxide microsphere preparation method Download PDFInfo
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- CN107400501B CN107400501B CN201710775141.4A CN201710775141A CN107400501B CN 107400501 B CN107400501 B CN 107400501B CN 201710775141 A CN201710775141 A CN 201710775141A CN 107400501 B CN107400501 B CN 107400501B
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- silicon oxide
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The embodiment of the present application provides a kind of chemical mechanical grinding agent, is formulated by following substances in percentage by weight: dispersed nano silicon oxide microsphere abrasive material 0.01-30%, oxidant 0.01-20%, stabilizer 0.1-30%, surplus is water.In the chemical mechanical grinding agent, its abrasive material is dispersed nano silicon oxide microsphere, the shape of the dispersed nano silicon oxide microsphere is the spheroidal of rule, therefore its surface is smooth, there is no corner angle, so, when being ground using the chemical mechanical grinding agent to semiconductor chip, abrasive material therein will not scratch chip surface, defect is brought to chip surface, therefore, which can limit the scuffing defect for reducing chip surface in chemical mechanical planarization process, quality of finish is improved, there is good economic benefit.In addition, the embodiment of the present application also provides a kind of preparation methods of dispersed nano silicon oxide microsphere.
Description
Technical field
This application involves cmp technology fields more particularly to a kind of chemical mechanical grinding agent and monodisperse to receive
The preparation method of rice silicon oxide microsphere.
Background technique
As chip integration improves, line width constantly reduces in chip, the planarization quality requirement on semi-conductor silicon chip surface
It is higher and higher.Most widely used global planarization technology is chemical mechanical milling tech in semiconductor chip manufacture
(chemical mechanical polish, CMP) is risen and fallen chip surface height using chemical reaction and mechanical lapping
Profile carries out global planarization.The technology is widely used in the planarization of aluminium alloy, copper, tungsten, silica and silicon layer.
Chemical reaction and mechanical friction occur for grinding agent and grinding layer in chemical mechanical planarization process, grind to reach removing
Grind the purpose of layer.The physico-chemical property of abrasive material is the key factor for influencing surface roughness and surface defect in grinding agent.
In order to improve the grinding effect of grinding agent, domestic and foreign scholars have done a large amount of research work for abrasive material.For example, Europe
Using 5-50wt.% colloidal silica as abrasive material, 0.001-2.0wt.%'s has grinding agent disclosed in the patent EP1541653 A1 of continent
Machine object can significantly improve the quality of finish of chemical mechanical grinding as stabilizer.Chinese patent CN104059607A is " a kind of
Silicon chip grinding agent " it is open using hollow glass micro-ball as abrasive material, it is ground with additives compositions such as triethylamine, low density polyethylene (LDPE)s
Agent, the grinding agent have the damage and high removal rate of low chip surface.
The grinding agent of the above patent and research report has made very big improvement, but existing grinding in terms of grinding effect
Agent still remains following problem: during the grinding process, the polishing particles in grinding agent easily cause defect in chip surface.With core
Piece manufacture tends to smaller size, which will more protrude.
Summary of the invention
In view of this, this application provides a kind of chemical mechanical grinding agent and the preparations of dispersed nano silicon oxide microsphere
Method improves chip quality of finish to reduce the scuffing defect of chip surface in chemical mechanical planarization process.
In order to solve the above-mentioned technical problem, the application adopts the technical scheme that
A kind of preparation method of dispersed nano silicon oxide microsphere, comprising:
Ammonium hydroxide, second alcohol and water are mixedly configured into the first solution according to the first volume ratio；
Ethyl orthosilicate and ethyl alcohol are mixedly configured into the second solution by the second volume ratio；
Under agitation, the second solution is added gradually in the first solution, at least reacts 2 hours, obtains at room temperature
The reaction product arrived is dispersed nano silicon oxide microsphere.
Optionally, first volume ratio is 1.0-10:15-20:29-34.
Optionally, second volume ratio is 4-5:45-46.
A kind of chemical mechanical grinding agent, is formulated by following substances in percentage by weight: dispersed nano silica is micro-
Ball milling material 0.01-30%, oxidant 0.01-20%, stabilizer 0.1-30%, surplus is water, the dispersed nano silica
Microballoon is using the preparation of preparation method described in any of the above-described technical solution.
Optionally, the dispersed nano silicon oxide microsphere is the single dispersed nano silicon oxide microsphere of partial size.
Optionally, the particle size range of the dispersed nano silicon oxide microsphere is between 15nm-1000nm.
Optionally, the dispersed nano silicon oxide microsphere is the nano silicon oxide microballoon that can be dispersed with single microballoon.
Optionally, the oxidant is the mixture of pyrophosphate and hydrogen peroxide one or two.
Optionally, the stabilizer is that oleic acid diethyl amide and its salt, fat alcohol polyoxyethylene ether and potassium hydroxide are a kind of
Or a variety of mixture.
Compared to the prior art, the application has the advantages that
In chemical mechanical grinding agent provided by the present application, abrasive material is dispersed nano silicon oxide microsphere, which receives
The shape of rice silicon oxide microsphere is the spheroidal of rule, therefore its surface is smooth, and corner angle are not present, so, utilizing the chemistry
When double of the conductor chip grinding of mechanical grinding grinding agent, abrasive material therein will not scratch chip surface, bring defect to chip surface, because
This, which can limit the scuffing defect for reducing chip surface in chemical mechanical planarization process, improve polishing
Quality has good economic benefit.
Detailed description of the invention
In order to which the specific embodiment of the application is expressly understood, used when the application specific embodiment is described below
Attached drawing do a brief description.
Fig. 1 is chemical mechanical grinder reason figure；
Fig. 2 is the SEM picture of colloidal silica particles；
Fig. 3 is the SEM picture of dispersed nano silicon oxide microsphere.
Specific embodiment
Fig. 1 is combined to introduce chemical mechanical grinder reason first.
Simple chemical grinding, surface accuracy is higher, and damage is low, and integrality is good, it is not easy to surface/sub-surface damage occurs
Wound, but grinding rate is slower, material removal efficiency is lower, cannot correct surface type face precision, and grinding comparison of coherence is poor；It is single
Pure mechanical lapping, grinding consistency is good, and surface smoothness is high, and grinding efficiency is high, but is easy to appear superficial layer/sub-surface layer
Damage, surface roughness value are relatively low.Cmp technology combines the advantage of chemical grinding and mechanical lapping.Chemical machine
Tool grinding absorbs the respective advantage of the two, can obtain more perfect surface while guaranteeing material removal efficiency, obtain
Flatness than merely using both grinding than be higher by the 1-2 order of magnitude, and may be implemented nanoscale to atom level table
Surface roughness.
Cmp technology is carried out the profile that chip surface height rises and falls using chemical reaction and mechanical lapping complete
Face planarization.Fig. 1 is chemical mechanical grinder reason figure.Applying pressure to grinding pad 11, grinding agent 13 is contacted with 12 surface of chip,
Chemical machinery effect occurs for grinding agent 13 and 12 surface of chip, to grind away 12 surface particle of chip, reaches the mesh of planarization
's.
Because during the grinding process, the polishing particles in grinding agent 13 can be contacted with chip surface, and in the effect of pressure
Under, polishing particles can be pressed into chip interior, therefore, if the polishing particles in grinding agent 13 are in irregular shape or there are ribs on surface
If angle, then during the grinding process, which is easy to scratch chip surface, so that defect is caused in chip surface, with
Chip manufacturing tends to smaller size, which will more protrude.
For this purpose, the embodiment of the present application provides the scanning electron microscopic picture of traditional polishing particles colloidal silica particles i.e.
SEM (scanning electron microscope) picture, please refers to Fig. 2.From figure 2 it can be seen that colloidal silica
Grain it is in irregular shape, there are corner angle on surface, and therefore, during the grinding process, there are the colloids of corner angle in irregular shape or surface
Silicon oxide particle can scratch chip surface.
In view of this, the embodiment of the present application is received in configuration grinding agent using the smooth monodisperse in regular shape surface
Rice silicon oxide microsphere substitutes traditional colloidal silica particles as polishing particles, the shape of the dispersed nano silicon oxide microsphere
For the spheroidal of rule, therefore its surface is smooth, and corner angle are not present, so, using the chemical mechanical grinding agent to semiconductor
When chip is ground, abrasive material therein will not scratch chip surface, bring defect to chip surface, therefore, the chemical mechanical grinding
Agent can limit the scuffing defect for reducing chip surface in chemical mechanical planarization process, improve quality of finish, have warp well
Ji benefit.
As one embodiment of the application, chemical mechanical grinding agent provided by the present application, by following substance by weight hundred
Ratio is divided to be formulated: dispersed nano silicon oxide microsphere abrasive material 0.01-30%, oxidant 0.01-20%, stabilizer 0.1-
30%, surplus is water.
Wherein, the particle size range of dispersed nano silicon oxide microsphere is between 15nm-1000nm.Because grinding rate with grind
The partial size of abrasive grain is related, so, in order to preferably control grinding rate, as an alternative embodiment, dispersed nano
Silicon oxide microsphere is the silicon oxide microsphere with single particle size.For example, partial size is 400nm.
In addition, in order to reach better grinding polishing effect, as another alternative embodiment, the dispersed nano oxidation
Silicon microballoon can be the dispersed nano silicon oxide microsphere that can be dispersed with single microballoon.
As another alternative embodiment, dispersed nano silicon oxide microsphere can be synthesized using Stober method.The side stober
Method is a kind of physico-chemical process for synthesizing monodisperse silicon particle, by WernerEt al. find at first.It generally refers to lead to
It crosses and the method for generating silicon nanoparticle is added in ethyl alcohol and ammonium hydroxide in ethyl orthosilicate TEOS.
Specific preparation method can be such that
Ammonium hydroxide, second alcohol and water are mixedly configured into the first solution according to the first volume ratio；
Ethyl orthosilicate and ethyl alcohol are mixedly configured into the second solution by the second volume ratio；
Under agitation, the second solution is added gradually in the first solution, at least reacts 2 hours, obtains at room temperature
The reaction product arrived is dispersed nano silicon oxide microsphere.In the embodiment of the present application, room temperature range can be between -10 DEG C to 40
Between DEG C.
Optionally, first volume ratio can be 1.0-10:15-20:29-34.
Optionally, second volume ratio can be 4-5:45-46.
It is to be appreciated that microspherulite diameter can prolonging with the reaction time in dispersed nano silicon oxide microsphere preparation process
It grows and increases, and increase comparatively fast in initial reaction stage partial size, be reacted to after a certain period of time, partial size increasess slowly, the reaction later period has been arrived,
Partial size increases more slow.
As an example, dispersed nano silicon oxide microsphere provided by the embodiments of the present application can be prepared with the following method
Synthesis:
Ammonium hydroxide 64mL, ethyl alcohol 171.5mL and 264.5mL water are mixed and made into the first solution；Ethyl orthosilicate 45mL and ethyl alcohol
455mL is mixed and made into the second solution, the first solution is added in the second solution under stirring condition, after reaction 5 hours, obtaining partial size is
The dispersed nano silicon oxide microsphere of 400nm, Fig. 3 are the scanning electron microscopic picture of dispersed nano silicon oxide microsphere.
As an example, the embodiment of the present application also provides a kind of specific embodiments of chemical mechanical grinding agent configuration.
As an example, can by dispersed nano silicon oxide microsphere 20g, hydrogen peroxide 10g, the oleic acid diethyl amide 12g of 400nm,
Fat alcohol polyoxyethylene ether 10g, potassium hydroxide 3g, water 45g, be sufficiently mixed in container be configured to it is provided in an embodiment of the present invention
A kind of chemical mechanical grinding agent.
As another alternative embodiment, oxidant can be the mixture of pyrophosphate and hydrogen peroxide one or two.
As another alternative embodiment, stabilizer can for oleic acid diethyl amide and its salt, fat alcohol polyoxyethylene ether and
The one or more mixture of potassium hydroxide.
The above are the specific embodiments of chemical mechanical grinding agent provided by the embodiments of the present application.In the chemical mechanical grinding
In agent, abrasive material is dispersed nano silicon oxide microsphere, and the shape of the dispersed nano silicon oxide microsphere is the spheroidal of rule,
Therefore its surface is smooth, and corner angle are not present, so, when being ground using the chemical mechanical grinding agent to semiconductor chip, wherein
Abrasive material will not scratch chip surface, bring defect to chip surface, therefore, which can limit reductionization
The scuffing defect of chip surface in mechanical grinding process is learned, quality of finish is improved, there is good economic benefit.
The above is only embodiments herein, are not intended to limit this application.To those skilled in the art,
Various changes and changes are possible in this application.It is all within the spirit and principles of the present application made by any modification, equivalent replacement,
Improve etc., it should be included within the scope of the claims of this application.
Claims (4)
1. a kind of chemical mechanical grinding agent, which is characterized in that be formulated by following substances in percentage by weight: dispersed nano
Silicon oxide microsphere abrasive material 0.01-30%, oxidant 0.01-20%, stabilizer 0.1-30%, surplus is water, and the monodisperse is received
The preparation process of rice silicon oxide microsphere is as follows:
Ammonium hydroxide, second alcohol and water are mixedly configured into the first solution according to the first volume ratio；
Ethyl orthosilicate and ethyl alcohol are mixedly configured into the second solution by the second volume ratio；
Under agitation, the second solution is added gradually in the first solution, at least reacts 2 hours, obtains at room temperature
Reaction product is dispersed nano silicon oxide microsphere；
First volume ratio is 1.0-10:15-20:29-34；
Second volume ratio is 4-5:45-46；
The oxidant is the mixture of pyrophosphate and hydrogen peroxide one or two；
The stabilizer is oleic acid diethyl amide and its salt, fat alcohol polyoxyethylene ether and the one or more mixing of potassium hydroxide
Object.
2. chemical mechanical grinding agent according to claim 1, which is characterized in that the dispersed nano silicon oxide microsphere is
The single dispersed nano silicon oxide microsphere of partial size.
3. chemical mechanical grinding agent according to claim 1, which is characterized in that the dispersed nano silicon oxide microsphere
Particle size range is between 15nm-1000nm.
4. chemical mechanical grinding agent according to claim 1, which is characterized in that the dispersed nano silicon oxide microsphere is
The nano silicon oxide microballoon that can be dispersed with single microballoon.
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|---|---|---|---|---|
| CN1398938A (en) * | 2002-05-10 | 2003-02-26 | 河北工业大学 | Chemical and mechanical leveling polishing liquid for multilayer copper wire in large scale integrated circuit |
| CN101602508A (en) * | 2009-06-22 | 2009-12-16 | 浙江理工大学 | Method for preparing monodisperse nano silicon dioxide spherical particle hydrosol and uses thereof |
| CN101913612A (en) * | 2010-09-01 | 2010-12-15 | 中国石油大学(北京) | Method for preparing micron-sized monodisperse silica microspheres |
| CN103318899A (en) * | 2013-06-24 | 2013-09-25 | 哈尔滨工业大学 | Control method of grain sizes of monodisperse silicon dioxide pellets |
| CN103359745A (en) * | 2012-03-27 | 2013-10-23 | 浩华科技实业有限公司 | Method for batch preparation of monodisperse submicrometer silica powder |
| CN106744998A (en) * | 2017-01-17 | 2017-05-31 | 清华大学 | A kind of controllable amorphous monodisperse nano silicon dioxide raw powder's production technology of granularity |
-
2017
- 2017-08-31 CN CN201710775141.4A patent/CN107400501B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398938A (en) * | 2002-05-10 | 2003-02-26 | 河北工业大学 | Chemical and mechanical leveling polishing liquid for multilayer copper wire in large scale integrated circuit |
| CN101602508A (en) * | 2009-06-22 | 2009-12-16 | 浙江理工大学 | Method for preparing monodisperse nano silicon dioxide spherical particle hydrosol and uses thereof |
| CN101913612A (en) * | 2010-09-01 | 2010-12-15 | 中国石油大学(北京) | Method for preparing micron-sized monodisperse silica microspheres |
| CN103359745A (en) * | 2012-03-27 | 2013-10-23 | 浩华科技实业有限公司 | Method for batch preparation of monodisperse submicrometer silica powder |
| CN103318899A (en) * | 2013-06-24 | 2013-09-25 | 哈尔滨工业大学 | Control method of grain sizes of monodisperse silicon dioxide pellets |
| CN106744998A (en) * | 2017-01-17 | 2017-05-31 | 清华大学 | A kind of controllable amorphous monodisperse nano silicon dioxide raw powder's production technology of granularity |
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Inventor after: Yang Peng Inventor after: Xu Zongke Inventor after: Zhang Lei Inventor after: Zhou Wenbin Inventor before: Yang Peng Inventor before: Xu Zongke Inventor before: Zhang Lei Inventor before: Zhou Wenbin |