CN101475791A - Preparation and use of cerium oxide / silicon oxide compound abrasive - Google Patents
Preparation and use of cerium oxide / silicon oxide compound abrasive Download PDFInfo
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- CN101475791A CN101475791A CNA2009100281894A CN200910028189A CN101475791A CN 101475791 A CN101475791 A CN 101475791A CN A2009100281894 A CNA2009100281894 A CN A2009100281894A CN 200910028189 A CN200910028189 A CN 200910028189A CN 101475791 A CN101475791 A CN 101475791A
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Abstract
The invention relates to a method for preparing a ceria/monox compounded abrasive, and application of the compounded abrasive. The method uses monodisperse spherical monox as a kernel of a coating type compounded abrasive, hexamethylenetetramine (HMT) as a precipitator and cerium salt as a raw material, and adopts an even precipitation method process to synthesize the ceria/monox compounded abrasive. Through the optimization of process parameters, such as the use amount ratio of monox master particles to the cerium salt, the molar ratio of the HMT to the cerium salt, and reaction and calcination temperature, the method controls the covering amount, the shape and the distribution state of ceria particles on the surface of the monox, thereby preparing the ceria/monox compounded abrasive of which the nanometer-level ceria particles evenly cover on the surface of the monox and which has good monodispersity; the method does not need complex equipment; and the needed chemical materials have less varieties, cheap prices and good experiment repeatability. The ceria/monox compounded abrasive is prepared into polishing slurry for chemical mechanical polishing of a gallium arsenide chip so as to obtain the polishing surface with the roughness in sub-nanometer magnitude and further improve polishing speed, reduce polishing pass and improve efficiency.
Description
Technical field
The invention belongs to field of preparation of ultrafine compound powder, the preparation method of special monodisperse spherical cerium oxide/silicon oxide cladded type compounded abrasive, and the purposes in Ultraprecise polished.
Background technology
The raising with integrated level of reducing along with the super large-scale integration device feature size requires must reach nano level as the roughness of substrate material surface, and this just has higher requirement to the quality of finish of substrate material.(Chemical-mechanical polishing is a kind of important processing means that obtains super-smooth surface CMP), and almost is unique technology that can realize global planarization in chemically machinery polished.Gallium arsenide (GaAs) is a kind of important III-V group iii v compound semiconductor material, and GaAs material hardness low (Mohs' hardness is 4.5), fragility are big, easy cleavage, and what this made the GaAs wafer is processed into the main difficult problem of GaAs unicircuit in making.
CeO
2It is one of abrasive material that uses among the CMP, be widely used in the chemically machinery polished of precision glass polishing and ULSI silica dioxide medium layer, show that the glazed surface roughness is low, the polishing efficiency advantages of higher, but subject matter is to be difficult to form stable dispersion system, and the dispersiveness of slurry is stablized relatively poor.Abrasive material is brought into play important role as polishing medium in the Super-smooth Surface Polishing material removal process, the character of abrasive material self greatly influences the glazed surface quality.In order to overcome the shortcoming of single abrasive material, the research of compounded abrasive becomes the focus in the CMP field gradually.Compounded abrasive most typical application in CMP is that employing flame combustion process such as Wang Zhonglin prepare TiO
2Doping spherical CeO
2Powder, and be successfully applied to the chemically machinery polished of silicon wafer, by using this spherical TiO
2Doped Ce O
2Powder is as abrasive material, can be so that polishing speed improves 50%, surface imperfection reduces by 80% (Xiangdong Feng, Dean C.Sayle, Zhong Lin Wang, et al.Converting Ceria Polyhedral Nanoparticles into Single-Crystal Nanospheres[J] .Science, 2006,312:1504-1508.).
Lee is that precipitation agent adopts liquid-phase precipitation method at silicon oxide surface coating cerium oxide particle with ammoniacal liquor, find that this compounded abrasive is to the polishing performance of silica dioxide medium layer (the Seung-Ho Lee that is improved, Zhenyu Lu, S.V.Babu, et al.Chemical mechanical polishing of thermal oxide films using silicaparticles coatedwith ceria[J] .Materrials Research Society, 2002,17 (10): 2744-2749).Xiao Baoqi etc. are that precipitation agent adopts homogeneous precipitation method to prepare cerium oxide/silica abrasive to be used for the optical digital disk glass substrate with urea, obtained roughness and be 0.971nm glazed surface (Xiao Baoqi, Lei Hong. nanometer SiO
2/ CeO
2The preparation of Compostie abrasive particles and polishing characteristic research [J] thereof. the tribology journal, 2008 the 2nd phases), Lei Hong etc. and with regard to this art applications the patent (preparation method of alumina/silica Compostie abrasive particles, application number: 200610026974.2), in addition Lei Hong etc. also just with traditional abrasives such as ultra-fine alumina, silicon oxide and zirconium white be kernel, with the hydrophilic macromolecule chain segment compounds or to contain polarity organo-functional group compound be the preparation of the abrasive of shell, applied for patent (application number: 200510023377.X).Chai Mingxia etc. are raw material with cerous carbonate, basic zirconium chloride and ammoniacal liquor, adopt mechanical solid state reaction method to prepare submicron-grade superfine SiO
2-CeO
2Composite oxides, and (Feng Xiaoping waits .SiO for Chai Mingxia, Hu Jiandong to be used for the chemically machinery polished of opticglass
2-CeO
2The preparation of composite oxides and polishing performance [J]. Chinese Journal of Inorganic Chemistry, 2007 the 4th phases).Song also is that precipitation agent adopts liquid-phase precipitation method to prepare cladded type cerium oxide/silica powder with sodium hydroxide, studied the dispersiveness of coated powder, variation has taken place in the zeta current potential of this cladded type composite granule of presentation of results, dispersiveness (the Xiaolan Song that also is improved, Nan Jiang, Synthesis of CeO
2-coatedSiO
2Nanoparticle and dispersion stability of its suspension[J] .Materials Chemistry, 2008,110 (1): 128-135).But above-mentioned is the prepared cerium oxide/silica powder of precipitation agent with ammoniacal liquor or sodium hydroxide, and cerium oxide particle is even inadequately in the coating of silicon oxide surface, can not satisfy Ultraprecise polished requirement.
At present, generally using among the GaAs wafer CMP is SiO
2Abrasive material, but subject matter is SiO
2The polishing speed of abrasive material is low excessively, often adds oxygenant in actual applications and wait and improve polishing speed in the needs polishing slurries, therefore makes the complex chemical composition of polishing slurries; Perhaps adopt the method that increases the polishing passage, increases polishing time, therefore make polishing efficiency low.Chen Yang and Chen Zhigang etc. use ultra-fine CeO
2The abrasive polishing gallium arsenide wafer, obtained the glazed surface (Chen Yang of roughness Ra value for 0.740nm, Li Xiazhang, Chen Zhigang, etc. nanometer abrasive is to the polishing research [J] of GaAs wafer. Solid State Electronics research and progress, 2006 the 4th phases), and with regard to this art applications patent (application number: 200510041507.2), but what this technology was passed through is two step glossings, and total polishing time is 60 minutes, and polishing efficiency is on the low side.
Summary of the invention
The objective of the invention is the shortcoming for existing gallium arsenide polish abrasive, the preparation method and the purposes of a kind of monodisperse spherical cerium oxide/silicon oxide cladded type compounded abrasive is provided, the kernel of prepared compounded abrasive is a silicon oxide, and coating layer is a cerium oxide.This coated type cerium oxide can further improve polishing speed satisfying on the basis that obtains the glazed surface quality, reduces the polishing passage, raises the efficiency.
The present invention is with the kernel of monodisperse sphere conformal silicon oxide as the cladded type compounded abrasive, and is precipitation agent with vulkacit H (HMT), and cerium salt is raw material, adopts sluggish precipitation technology to synthesize.By optimizing the amount ratio of silicon oxide coatingparticles and cerium salt, the mol ratio of HMT and cerium salt, processing parameters such as reaction and calcining temperature come covering amount, pattern and the distribution of controlled oxidation cerium particle at silicon oxide surface, thereby have prepared the cerium oxide that nano level cerium oxide particle evenly coats at silicon oxide surface, monodispersity is good/silicon oxide compounded abrasive.And it is mixed with the chemically machinery polished that polishing slurries is used for gallium arsenide wafer, obtained the glazed surface of roughness in inferior nanometer scale.
Concrete preparation process of the present invention is: take by weighing a certain amount of particle diameter and be dispersed in the deionized water at single silicon oxide microsphere that disperses of 200～250nm, and the adding mass fraction is the dispersion agent (calculating with the quality of dispersion agent and the mass ratio of silicon oxide microsphere) of 10wt%, in silicon oxide suspension, add a certain amount of cerium salt again, stir with magnetic stirrer, wherein the mass concentration scope of silicon oxide suspension is 0.5～5wt%, and the concentration range of cerium ion is 0.01mol/l～0.5mol/l.Add a certain amount of vulkacit H again, stir, wherein the molar concentration rate of vulkacit H and cerium salt is between 2:1～20:1.Under the condition of induction stirring, place 70～90 ℃ water-bath to react 1～5h the reaction soln of preparation, with throw out centrifugation, washing (distilled water is given a baby a bath on the third day after its birth and is washed one time all over, dehydrated alcohol), place 70 ℃ of air dry oven oven dry again, grind, through 300～600 ℃ of calcining 0.5～4h, can obtain cerium oxide/silicon oxide cladded type compounded abrasive again.
Described cerium salt is cerous nitrate, and the mass concentration scope of silicon oxide suspension is 0.5～2wt%, and the concentration range of cerium ion is between 0.05mol/l～0.5mol/l, and calcining temperature is between 400～500 ℃, and calcination time effect between 1～2h is better.
Wherein, cerium salt can also be in cerous nitrate, cerous sulfate and the Cerium II Chloride any, and dispersion agent is any among Sodium dodecylbenzene sulfonate, Sodium hexametaphosphate 99 and the PEG400.
Prepared cerium oxide/silicon oxide compounded abrasive is mixed with polishing slurries, its mass concentration scope is at 0.5wt～5wt%, the mass concentration of oxygenant (hydrogen peroxide) is 5～15%, with ammoniacal liquor the pH value of polishing slurries is transferred to 8～10, use the high precision polishing machine under the processing condition (polish pressure is 25min as 5N, lower wall rotating speed as 200r/min, polishing time) of certain polishing, gallium arsenide wafer to be polished.
The prepared compounded abrasive of the present invention is spherical in shape, and its particle diameter is about 200～250nm, and monodispersity is good, and the kernel of this coated type cerium oxide is a silicon oxide, and coating layer is the cerium oxide particle of particle diameter at 10～20nm.By finishing and the surface modification of cerium oxide particle, thereby improved the zeta current potential absolute value of coated type cerium oxide in liquid phase water solution, and then improved its dispersiveness silicon oxide.In addition, the structure of the special coating of this cerium oxide/silicon oxide compounded abrasive also helps and reduces the polishing passage, improves polishing efficiency, improves the glazed surface quality.
The present invention adopts comparatively simple chemical technology to prepare and coats evenly, the coated type cerium oxide of good dispersity, need not complex apparatus, and required chemical feedstocks kind is few, low price, experiment favorable repeatability.While is because prepared compounded abrasive is spherical in shape, and surperficial clad nano level cerium oxide particle, and the Ultraprecise polished of gallium arsenide wafer had than obvious superiority, shows as high polishing clearance and the glazed surface roughness with inferior nanometer scale.
Description of drawings
Fig. 1 is the transmission electron microscope photo in the 500nm scale scope
Fig. 2 is the transmission electron microscope photo in the 200nm scale scope
Fig. 3 is the transmission electron microscope photo in the 100nm scale scope
Fig. 4 is the transmission electron microscope photo in the 100nm scale scope
Fig. 5 is the XRD spectra of coated type cerium oxide
Embodiment
The present invention is described in further detail below in conjunction with embodiment:
Embodiment 1: take by weighing silicon oxide microsphere 1g and be distributed in the 50ml deionized water, the Sodium dodecylbenzene sulfonate that adds 0.1g is again strengthened dispersion as dispersion agent by ultrasonic and mechanical stirring.Take by weighing the 1.263g cerous nitrate again and be dissolved in the 50ml deionized water, add the vulkacit H of 3g again, and electric mixer stirs.Two kinds of reaction solns are mixed, stir, and wherein the mass concentration of silicon oxide suspension is 1wt%, and cerium ion concentration is 0.02mol/l, and the molar concentration rate of vulkacit H and cerous nitrate is 10:1.Under the condition of induction stirring, place 80 ℃ water-bath to react 2h the reaction soln of preparation, with throw out centrifugation, washing (distilled water is given a baby a bath on the third day after its birth and is washed one time all over, dehydrated alcohol), place 70 ℃ of air dry oven oven dry again, grind, through 500 ℃ of calcining 1h, can obtain cerium oxide/silicon oxide cladded type compounded abrasive again.Characterize with the phase structure of XRD diffractometer, and prepare the particle diameter and the pattern of sample with transmission electron microscope (TEM) observation post the sample of gained.
The transmission electron microscope photo of pressing the prepared coated type cerium oxide sample of the processing parameter of embodiment 1 as shown in Figure 1, Figure 2, Figure 3 and Figure 4, wherein Fig. 1 is the transmission electron microscope photo in the 500nm scale scope, Fig. 2 is the transmission electron microscope photo in the 200nm scale scope, Fig. 3 is the transmission electron microscope photo in the 100nm scale scope, and Fig. 4 is the transmission electron microscope photo in the 50nm scale scope.Therefrom as can be seen, prepared coated type cerium oxide is spherical in shape, and its particle diameter is about 200～250nm, and monodispersity is fine, cerium oxide nanoparticles is even, complete is coated on silicon oxide core surface, the wherein about 5～10nm of the particle diameter of cerium oxide particle.The XRD of this coated type cerium oxide and pure silica and pure zirconia cerium compares collection of illustrative plates as shown in Figure 5.As can be seen, in the coating of preparation the characteristic diffraction peak of tangible cerium oxide has appearred in the XRD figure spectrum of silicon oxide of nano-cerium oxide, illustrate to have formed cerium oxide after reacting.The characteristic diffraction peak of simultaneous oxidation silicon is relatively very weak, may be because cerium oxide particle causes the complete coating of silicon oxide.
To be mixed with mass concentration with deionized water by the prepared cerium oxide of the processing parameter of embodiment 1/silicon oxide compounded abrasive is 2wt%, the mass concentration of oxygenant (hydrogen peroxide) is 10% polishing slurries, with ammoniacal liquor the pH value of polishing slurries is transferred to 9, use the high precision polishing machine that gallium arsenide wafer (100) is polished.Under certain polishing technological conditions (polish pressure is that 5N, lower wall rotating speed are that 200r/min, polishing time are 25min), test result shows that the surface roughness Ra value of polishing back gallium arsenide wafer is 0.591nm, with thickness difference (getting ten point measurement mean values) the exosyndrome material clearance of gallium arsenide wafer before and after the polishing, polishing speed reaches 1640nm/min after measured.
At present domestic document about the gallium arsenide wafer polishing is still rare, and documents (nanometer abrasive is to the polishing research [J] of GaAs wafer. Solid State Electronics research and progress, 2006 the 4th phases; Nano Ce O
2Particulate preparation and chemically machinery polished performance study [J] thereof. the tribology journal, the first phase in 2007) as can be known, Chen Yang, Li Xiazhang etc. use fine cerium oxide abrasive polishing gallium arsenide wafer, after two step polishings (total time of pre-polish(ing) and finishing polish is 60 minutes), the roughness Ra value of gallium arsenide wafer glazed surface is 0.740nm.And the prepared cerium oxide/silicon oxide compounded abrasive of processing parameter of use embodiment 1, just can directly the gallium arsenide abrasive sheet be thrown to minute surface through polishing (polishing time is 25 minutes) together, the surface roughness Ra value of polishing gallium arsenide wafer is 0.591nm, and polishing speed reaches 1640nm/min after measured.Show that more than the cerium oxide of this clad structure/silicon oxide compounded abrasive shows stronger polishing advantage, on the basis of satisfying the glazed surface quality, has improved polishing efficiency.
Embodiment 2: the step of present embodiment and the foregoing description 1 is basic identical, and difference is: the mass concentration of silicon oxide suspension is 0.5wt%, and cerium ion concentration is 0.01mol/l in the solution, and the molar concentration rate of vulkacit H and cerous nitrate is 5:1.Place 70 ℃ water-bath to react 1h the reaction soln of preparation, the presoma that institute's centrifugation is obtained is through 300 ℃ of calcining 0.5h again.
To be mixed with the polishing slurries that mass concentration is 0.5wt% by the prepared cerium oxide of the processing parameter of embodiment 2/silicon oxide compounded abrasive, the mass concentration of oxygenant (hydrogen peroxide) is 15%, with ammoniacal liquor the pH value of polishing slurries is transferred to 10, use the high precision polishing machine that gallium arsenide wafer (100) is polished, concrete glossing parameter is the same.
Embodiment 3: the step of present embodiment and the foregoing description 1 is basic identical, and difference is: the mass concentration of silicon oxide suspension is 5wt%, and cerium ion concentration is 0.5mol/l in the solution, and the molar concentration rate of vulkacit H and cerous nitrate is 20:1.Place 90 ℃ water-bath to react 5h the reaction soln of preparation, the presoma that institute's centrifugation is obtained is through 600 ℃ of calcining 4h again.
To be mixed with the polishing slurries that mass concentration is 5wt% by the prepared cerium oxide of the processing parameter of embodiment 3/silicon oxide compounded abrasive, the mass concentration of oxygenant (hydrogen peroxide) is 5%, with ammoniacal liquor the pH value of polishing slurries is transferred to 8, use the high precision polishing machine that gallium arsenide wafer (100) is polished, concrete glossing parameter is the same.
Embodiment 4: the step of present embodiment and the foregoing description 1 is basic identical, difference is: changing cerium salt is cerous sulfate, the change dispersion agent is a Sodium hexametaphosphate 99, the mass concentration of silicon oxide suspension is 2wt%, cerium ion concentration is 0.2mol/l in the solution, and the molar concentration rate of vulkacit H and cerous nitrate is 20:1.Place 80 ℃ water-bath to react 2h the reaction soln of preparation, the presoma that institute's centrifugation is obtained is through 400 ℃ of calcining 2h again.
To be mixed with the polishing slurries that mass concentration is 3wt% by the prepared cerium oxide of the processing parameter of embodiment 4/silicon oxide compounded abrasive, the mass concentration of oxygenant (hydrogen peroxide) is 12%, with ammoniacal liquor the pH value of polishing slurries is transferred to 9.5, use the high precision polishing machine that gallium arsenide wafer (100) is polished, concrete glossing parameter is the same.
Embodiment 5: the step of present embodiment and the foregoing description 1 is basic identical, difference is: changing cerium salt is that Cerium II Chloride change dispersion agent is PEG400, the mass concentration of silicon oxide suspension is 1wt%, cerium ion concentration is 0.2mol/l in the solution, and the molar concentration rate of vulkacit H and cerous nitrate is 15:1.Place 80 ℃ water-bath to react 2h the reaction soln of preparation, the presoma that institute's centrifugation is obtained is through 500 ℃ of calcining 2h again.
Polishing slurries composition and glossing parameter are with embodiment 1.
Claims (6)
1, the preparation method of a kind of cerium oxide/silicon oxide compounded abrasive, it is characterized in that, single the disperse silicon oxide microsphere of particle diameter at 200～250nm is dispersed in the deionized water, adding is the dispersion agent of 10wt% with the mass fraction that the mass ratio of the quality of dispersion agent and silicon oxide microsphere calculates, be to add cerium salt in the silicon oxide suspension of 0.5～5wt% to the mass concentration scope again, stir with magnetic stirrer, the concentration range of cerium ion is 0.01mol/l～0.5mol/l, the molar concentration rate that adds vulkacit H and cerium salt again is the vulkacit H of 2:1～20:1, stirs;
Under the condition of induction stirring, place 70～90 ℃ water-bath to react 1～5h the reaction soln of preparation, with throw out centrifugation, washing, place 70 ℃ of air dry oven oven dry again, grind, through 300～600 ℃ of calcining 0.5～4h, can obtain cerium oxide/silicon oxide cladded type compounded abrasive again.
2, the preparation method of cerium oxide according to claim 1/silicon oxide compounded abrasive is characterized in that, described throw out centrifugation, washing, and its washing process is that distilled water is given a baby a bath on the third day after its birth time, dehydrated alcohol is washed one time.
3, the preparation method of cerium oxide according to claim 1/silicon oxide compounded abrasive is characterized in that, cerium salt is any in cerous nitrate, cerous sulfate and the Cerium II Chloride.
4, the preparation method of cerium oxide according to claim 1/silicon oxide compounded abrasive is characterized in that, dispersion agent is any among Sodium dodecylbenzene sulfonate, Sodium hexametaphosphate 99 and the PEG400.
5, according to the preparation method of claim 1,2,3 or 4 described cerium oxide/silicon oxide compounded abrasives, it is characterized in that, the mass concentration scope of described silicon oxide suspension is 0.5～2wt%, the concentration range of described cerium ion is between 0.05mol/l～0.5mol/l, described calcining temperature is between 400～500 ℃, and described calcination time is between 1～2h.
6, a kind of purposes with claim 1 preparation cerium oxide/silicon oxide compounded abrasive, prepared cerium oxide/silicon oxide compounded abrasive is mixed with polishing slurries, its mass concentration scope is at 0.5wt～5wt%, oxygenant is a hydrogen peroxide, its mass concentration is 5～15%, with ammoniacal liquor the pH value of polishing slurries is transferred to 8～10, use the high precision polishing machine gallium arsenide wafer to be polished under as 5N, lower wall rotating speed as 200r/min, the processing condition of polishing time as the 25min polishing at polish pressure.
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