CN107400501A - A kind of cmp agent, the preparation method of dispersed nano silicon oxide microsphere - Google Patents
A kind of cmp agent, the preparation method of dispersed nano silicon oxide microsphere Download PDFInfo
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- CN107400501A CN107400501A CN201710775141.4A CN201710775141A CN107400501A CN 107400501 A CN107400501 A CN 107400501A CN 201710775141 A CN201710775141 A CN 201710775141A CN 107400501 A CN107400501 A CN 107400501A
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- silicon oxide
- nano silicon
- dispersed nano
- oxide microsphere
- cmp agent
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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
-
- 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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- Engineering & Computer Science (AREA)
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Materials Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The embodiment of the present application provides a kind of cmp agent, and it 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 cmp agent, its abrasive material is dispersed nano silicon oxide microsphere, the spheroidal for being shaped as rule of the dispersed nano silicon oxide microsphere, therefore its surface is smooth, in the absence of corner angle, so, when being ground using the cmp agent to semiconductor chip, abrasive material therein will not scratch chip surface, defect is brought to chip surface, therefore, the cmp agent can limit the scuffing defect for reducing chemical mechanical planarization process chips surface, quality of finish is improved, there is good economic benefit.In addition, the embodiment of the present application additionally provides a kind of preparation method of dispersed nano silicon oxide microsphere.
Description
Technical field
The application is related to cmp technology field, more particularly to a kind of cmp agent and single dispersing are received
The preparation method of rice silicon oxide microsphere.
Background technology
As chip integration improves, line width constantly reduces in chip, the planarization quality requirement on semi-conductor silicon chip surface
More and more higher.Most widely used global planarization technology is chemical mechanical milling tech in semiconductor chip manufacture
(chemical mechanical polish, CMP), it 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.
With grinding layer chemical reaction and mechanical friction occur for grinding agent in chemical mechanical planarization process, are ground so as to reach removing
Grind the purpose of layer.The physico-chemical property of abrasive material is the key factor for influenceing surface roughness and surface defect in grinding agent.
In order to improve the grinding effect of grinding agent, domestic and foreign scholars have done substantial amounts of research work for abrasive material.For example, Europe
Using 5-50wt.% colloidal silicas as abrasive material, 0.001-2.0wt.%'s has grinding agent disclosed in the patent EP1541653 A1 of continent
For machine thing as stabilizer, it can significantly improve the quality of finish of cmp.Chinese patent CN104059607A《It is a kind of
Silicon grinding agent》Disclosure is ground using hollow glass micro-ball as abrasive material with additive compositions such as triethylamine, low density polyethylene (LDPE)s
Agent, the grinding agent have the damage of low chip surface and high removal rate.
The grinding agent of above patent and research report has made very big improvement, but existing grinding in terms of grinding effect
Still there are the following problems for agent:In process of lapping, the polishing particles in grinding agent easily cause defect in chip surface.With core
Piece manufacture tends to smaller size, and the shortcoming will be protruded more.
The content of the invention
In view of this, this application provides a kind of cmp agent and the preparation of dispersed nano silicon oxide microsphere
Method, to reduce the scuffing defect on chemical mechanical planarization process chips surface, improve chip quality of finish.
In order to solve the above-mentioned technical problem, the application employs following technical scheme:
A kind of preparation method of dispersed nano silicon oxide microsphere, including:
Ammoniacal liquor, second alcohol and water are mixedly configured into the first solution according to the first volume ratio;
Tetraethyl orthosilicate and ethanol 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, obtain at room temperature
The reaction product arrived is dispersed nano silicon oxide microsphere.
Alternatively, first volume ratio is 1.0-10:15-20:29-34.
Alternatively, second volume ratio is 4-5:45-46.
A kind of cmp 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 prepared using the preparation method described in any of the above-described technical scheme.
Alternatively, the dispersed nano silicon oxide microsphere is the single dispersed nano silicon oxide microsphere of particle diameter.
Alternatively, the particle size range of the dispersed nano silicon oxide microsphere is between 15nm-1000nm.
Alternatively, the dispersed nano silicon oxide microsphere is the nano silicon oxide microballoon that can be disperseed with single microballoon.
Alternatively, the oxidant is pyrophosphate and the mixture of hydrogen peroxide one or two.
Alternatively, the stabilizer is oleic acid diethyl amide and its salt, fat alcohol APEO and potassium hydroxide one kind
Or a variety of mixture.
Compared to prior art, the application has the advantages that:
In the cmp agent that the application provides, its abrasive material is dispersed nano silicon oxide microsphere, and the single dispersing is received
The spheroidal for being shaped as rule of rice silicon oxide microsphere, therefore its surface is smooth, in the absence of corner angle, so, utilizing the chemistry
During double of the conductor chip grinding of mechanical grinding grinding agent, abrasive material therein will not scratch chip surface, and defect is brought to chip surface, because
This, the cmp agent can limit the scuffing defect for reducing chemical mechanical planarization process chips surface, improve polishing
Quality, there is good economic benefit.
Brief description of the drawings
In order to which the embodiment of the application is expressly understood, used when the application embodiment is described below
Accompanying drawing do a brief description.
Fig. 1 is chemical mechanical grinder reason figure;
Fig. 2 is the SEM pictures of colloidal silica particles;
Fig. 3 is the SEM pictures of dispersed nano silicon oxide microsphere.
Embodiment
First chemical mechanical grinder reason is introduced with reference to Fig. 1.
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 relatively low, it is impossible to corrects surface type face precision, grinding comparison of coherence is poor;It is single
Pure mechanical lapping, grinding uniformity is good, and surface smoothness is high, and grinding efficiency is high, but superficial layer/sub-surface layer easily occurs
Damage, surface roughness value is than relatively low.Cmp technology combines the advantage of chemical grinding and mechanical lapping.Chemical machine
The advantages of tool grinding absorbs both each, it can obtain more perfect surface while material removal efficiency is ensured, obtain
Flatness to be higher by the 1-2 order of magnitude using both grindings than merely, and nanoscale can be realized to the table of atom level
Surface roughness.
Cmp technology is carried out the profile that chip surface height rises and falls using chemical reaction and mechanical lapping complete
Face planarizes.Fig. 1 is chemical mechanical grinder reason figure.Applying pressure to grinding pad 11, grinding agent 13 contacts with the surface of chip 12,
With the surface of chip 12 chemical machinery effect occurs for grinding agent 13, so as to grind away the surface particle of chip 12, reaches the mesh of planarization
's.
Because in process of lapping, the polishing particles in grinding agent 13 can contact with chip surface, and in the effect of pressure
Under, polishing particles can be pressed into chip internal, therefore, if the polishing particles in grinding agent 13 are in irregular shape or surface has rib
If angle, then in process of lapping, the polishing particles easily scratch chip surface, so as to cause defect in chip surface, with
Chip manufacturing tends to smaller size, and the shortcoming will be protruded more.
Therefore, 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, refers to Fig. 2.From figure 2 it can be seen that colloidal silica
Grain it is in irregular shape, there are corner angle in surface, therefore, in process of lapping, in irregular shape or surface has the colloid of corner angle
Silicon oxide particle can scratch chip surface.
In view of this, the embodiment of the present application employs the smooth single dispersing in regular shape surface and received in grinding agent is configured
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, in the absence of corner angle, so, using the cmp agent to semiconductor
When chip is ground, abrasive material therein will not scratch chip surface, and defect is brought to chip surface, therefore, the cmp
Agent can limit the scuffing defect for reducing chemical mechanical planarization process chips surface, improve quality of finish, have warp well
Ji benefit.
The cmp agent provided as one embodiment of the application, the application, by following material 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 is with grinding
The particle diameter of abrasive particle is relevant, 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, particle diameter is 400nm.
In addition, in order to reach more preferable grinding polishing effect, as another alternative embodiment, the dispersed nano oxidation
Silicon microballoon can be the dispersed nano silicon oxide microsphere that can be disperseed with single microballoon.
As another alternative embodiment, dispersed nano silicon oxide microsphere can use Stober methods to synthesize.Stober side
Method is a kind of physico-chemical process for synthesizing single dispersing silicon grain, by WernerEt al. find at first.Generally refer to lead to
Cross the method that tetraethyl orthosilicate TEOS is added in ethanol and ammoniacal liquor and generates silicon nanoparticle.
Specific preparation method can be as follows:
Ammoniacal liquor, second alcohol and water are mixedly configured into the first solution according to the first volume ratio;
Tetraethyl orthosilicate and ethanol 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, obtain at room temperature
The reaction product arrived is dispersed nano silicon oxide microsphere.In the embodiment of the present application, room temperature scope can be between -10 DEG C to 40
Between DEG C.
Alternatively, first volume ratio can be 1.0-10:15-20:29-34.
Alternatively, second volume ratio can be 4-5:45-46.
It is to be appreciated that in dispersed nano silicon oxide microsphere preparation process, microspherulite diameter can prolonging with the reaction time
Grow and increase, and increase comparatively fast in initial reaction stage particle diameter, after being reacted to certain time, particle diameter increasess slowly, and has arrived the reaction later stage,
Particle diameter increases more slow.
As an example, the dispersed nano silicon oxide microsphere that the embodiment of the present application provides can be prepared with the following method
Synthesis:
Ammoniacal liquor 64mL, ethanol 171.5mL and 264.5mL water are mixed and made into the first solution;Tetraethyl orthosilicate 45mL and ethanol
455mL is mixed and made into the second solution, and the second solution added into the first solution under stirring condition, and after reaction 5 hours, obtaining particle diameter is
400nm dispersed nano silicon oxide microsphere, Fig. 3 are the scanning electron microscopic picture of dispersed nano silicon oxide microsphere.
As an example, the embodiment of the present application additionally provides a kind of embodiment of cmp agent configuration.
As an example, can by 400nm dispersed nano silicon oxide microsphere 20g, hydrogen peroxide 10g, oleic acid diethyl amide 12g,
Fat alcohol APEO 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 cmp agent.
As another alternative embodiment, oxidant can be pyrophosphate and the mixture of hydrogen peroxide one or two.
As another alternative embodiment, stabilizer can be oleic acid diethyl amide and its salt, fat alcohol APEO and
The one or more mixture of potassium hydroxide.
The embodiment of the cmp agent provided above for the embodiment of the present application.In the cmp
In agent, its abrasive material is dispersed nano silicon oxide microsphere, and the dispersed nano silicon oxide microsphere is shaped as regular spheroidal,
Therefore its surface is smooth, in the absence of corner angle, so, when being ground using the cmp agent to semiconductor chip, wherein
Abrasive material will not scratch chip surface, bring defect to chip surface, therefore, the cmp agent can limit reductionization
The scuffing defect on mechanical grinding process chips surface is learned, quality of finish is improved, there is good economic benefit.
Embodiments herein is these are only, is not limited to the application.To those skilled in the art,
The application can have various modifications and variations.All any modifications made within spirit herein and principle, equivalent substitution,
Improve etc., it should be included within the scope of claims hereof.
Claims (9)
- A kind of 1. preparation method of dispersed nano silicon oxide microsphere, it is characterised in that including:Ammoniacal liquor, second alcohol and water are mixedly configured into the first solution according to the first volume ratio;Tetraethyl orthosilicate and ethanol 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, obtain at room temperature Reaction product is dispersed nano silicon oxide microsphere.
- 2. preparation method according to claim 1, it is characterised in that first volume ratio is 1.0-10:15-20: 29-34。
- 3. preparation method according to claim 1, it is characterised in that second volume ratio is 4-5:45-46.
- 4. a kind of cmp agent, it is characterised 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 single dispersing is received Rice silicon oxide microsphere is prepared using the preparation method described in claim any one of 1-3.
- 5. cmp agent according to claim 4, it is characterised in that the dispersed nano silicon oxide microsphere is The single dispersed nano silicon oxide microsphere of particle diameter.
- 6. cmp agent according to claim 4, it is characterised in that the dispersed nano silicon oxide microsphere Particle size range is between 15nm-1000nm.
- 7. cmp agent according to claim 4, it is characterised in that the dispersed nano silicon oxide microsphere is The nano silicon oxide microballoon that can be disperseed with single microballoon.
- 8. according to the cmp agent described in claim any one of 4-7, it is characterised in that the oxidant is pyrophosphoric acid The mixture of salt and hydrogen peroxide one or two.
- 9. according to the cmp agent described in claim any one of 4-7, it is characterised in that the stabilizer is oleic acid two The one or more mixture of glycollic amide and its salt, fat alcohol APEO and potassium hydroxide.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111500258A (en) * | 2020-03-31 | 2020-08-07 | 长江存储科技有限责任公司 | Abrasive fine particles, method for producing same, and abrasive |
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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 |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111500258A (en) * | 2020-03-31 | 2020-08-07 | 长江存储科技有限责任公司 | Abrasive fine particles, method for producing same, and abrasive |
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