CN105800660A - Preparation method of cerium oxide and CMP polishing solution containing cerium oxide abrasive - Google Patents
Preparation method of cerium oxide and CMP polishing solution containing cerium oxide abrasive Download PDFInfo
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- CN105800660A CN105800660A CN201410840055.3A CN201410840055A CN105800660A CN 105800660 A CN105800660 A CN 105800660A CN 201410840055 A CN201410840055 A CN 201410840055A CN 105800660 A CN105800660 A CN 105800660A
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Abstract
The invention discloses a preparation method of cerium oxide. Reactants are preferably selected and preparation technology is optimally designed, cerium oxide particles have uniform particle dimensions, and mechanical forces are used for easily dispersing cerium oxide particles in a liquid phase; the CMP polishing solution which employs cerium oxide as an abrasive shows excellent planarizing and polishing efficiency in STI polishing applications.
Description
Technical field
The invention discloses a kind of cerium oxide preparation method and CMP planarization application thereof.
Background technology
Cerium oxide is a kind of chemically mechanical polishing abrasive material extensively concerned in recent years, and this is mainly due to its high polishing activity to silicon dioxide, and can reach high polishing effect under relatively low solid content.Therefore, the chemical mechanical polishing liquid being abrasive material with cerium oxide has bigger application prospect and the market advantage in performance and cost compared to traditional silicon oxide or alumina material.
At present, cerium oxide isolates the existing a large amount of reports of (STI) technique polishing research as abrasive applications in shallow trench, as patent 201310495424.5 reports a kind of chemically mechanical polishing (CMP) compositions isolating (STI) technique for shallow trench, compositions is with cerium oxide for abrasive material, and polishing requires that reaching high silicon oxide/silicon nitride polishing selects ratio；Patent 200510069987.3 reports a kind of chemical mechanical polishing slurry and the method for polishing substrate, involved polishing film is silicon oxide layer, require that silicon oxide is had high polishing speed and the generation of low defect, silicon nitride is shown low polishing speed, thus reaching high silicon oxide/silicon nitride polishing to select ratio.Patent reported above realizes the polishing requirement of polishing fluid each through choosing suitable chemical addition agent.But, when using cerium oxide as abrasive material, the particle characteristics of himself is most important on the impact of polishing effect.As, in STI polishing application, having bibliographical information cerium oxide particle size, shape characteristic to select the generation of defect in polishing process and polishing speed than equal important.At present, the cerium oxide abrasives Characteristics Control synthesis correlational study report based on STI polishing application demand is less.
Summary of the invention
For above-mentioned Problems existing, the invention discloses a kind of cerium oxide preparation method, by preferably designing with the optimization of preparation technology reactant, the cerium oxide particle of preparation has homogeneous particle size, is prone to cerium oxide particle is scattered in liquid phase by mechanical force；The CMP planarization liquid being abrasive material with this cerium oxide, demonstrates excellent planarization polishing efficiency in STI polishing application.
The preparation method that the invention discloses a kind of cerium oxide, it is characterised in that by preferably designing with the optimization of preparation technology reactant, the cerium oxide particle of preparation has homogeneous particle size, is prone to cerium oxide particle is scattered in liquid phase by mechanical force.
It is an aspect of the invention to the preparation method that a kind of cerium oxide nanoparticles is provided, including:
Step one: organic additive and cerium source aqueous solution are prepared the first compositions；
Step 2: by the first compositions and precipitant mix, and stir 0.5-10 hour, precipitation obtains cerous carbonate；
Step 3: described cerous carbonate high temperature is bakeed, and with prepared cerium oxide nanoparticles, and the particle diameter of this cerium oxide nanoparticles is 120-200 nanometer.
In abovementioned steps one, temperature is 80-150 DEG C, it is preferable that temperature range is 90-120 DEG C.
In abovementioned steps one, cerium source aqueous solution can be in cerous nitrate, cerium chloride, cerous acetate aqueous solution one or more, it is preferable that cerous nitrate.
In abovementioned steps one, organic additive can be in polyvinylpyrrolidone (PVP), Polyethylene Glycol (PEG) or polyvinyl alcohol (PVA) one or more, described organic additive mean molecule quantity is 1000-10000, it is preferred to polyvinylpyrrolidone (PVP).
In abovementioned steps two, precipitant can be in ammonium hydrogen carbonate or ammonium carbonate one or more.
In abovementioned steps one, two, in the aqueous solution of cerium source, cerium ion is 1:1.5～1:4.0 with the mol ratio of anion in precipitant, and in the aqueous solution of cerium source, cerium ion is 1.0:1.0～10.0:1.0 with the mol ratio of organic additive.Wherein, in the aqueous solution of cerium source, the molar concentration of cerium ion is 0.05M～1.0M, and in precipitant, the molar concentration of anion is 0.075M～4.0M, and the molar concentration of organic additive is 0.005M～1.0M.
In abovementioned steps two, the mixture particular determination of the first compositions and precipitant, it is preferable that be that the first compositions is added with certain flow rate in precipitant.
In abovementioned steps three, aforementioned cerous carbonate precipitate being carried out high temperature baking, sintering temperature is 400-900 DEG C, and roasting time is 0.5-10 hour, obtains cerium oxide nanoparticles.Preferably, before baking, cerous carbonate precipitate can through pure water 3 times.
And, preferably, after step 3 prepares cerium oxide nanoparticles, can be dispersed through further cerium oxide processing, described dispersion processing procedure is without particular determination, it is possible to be mechanical lapping such as ball milling, comminution by gas stream etc., can add organic dispersing agent in dispersive process, described organic dispersing agent is without particular determination, it is possible to for polyacrylic acid and its esters.
Another aspect of the present invention, is in that to provide a kind of STI polishing fluid, its cerium oxide nanoparticles including preceding method preparation and obtaining.Meanwhile, in this polishing fluid, may also include multiple well known in the art for polish STI can additive, as an example, it may include: high molecular polymer, oligosaccharide, water and pH adjusting agent.
In aforementioned polishing fluid, cerium oxide abrasives average particle size ranges for 120-200 nanometer, in polishing fluid, content is mass percent 0.2%-2.0%, described high molecular polymer content in polishing fluid is mass percent 0.01%-1.0%, described oligosaccharide content in polishing fluid is mass percent 0.1%-1.0%, and water is surplus.This polishing fluid pH ranges for 4.0-10.5.
The invention is characterised in that, described high molecular polymer can be one or more (mean molecule quantity is 1000-10000) in PAA, PVP or PEG, described oligosaccharide can be in alpha-cyclodextrin or beta-schardinger dextrin-one or more.
By the method synthesis cerium oxide nanoparticles that the application provides, it is distributed between 120-200 nanometer to its uniform particle sizes, and pattern rule, it can be applicable to CMP planarization liquid, has excellent STI and polishes characteristic.
Accompanying drawing explanation
Fig. 1 is that after the embodiment of the present invention 1 prepares the dispersion of gained cerium oxide, the SEM of granule schemes；
Fig. 2 is that after comparative example 1 of the present invention prepares the dispersion of gained cerium oxide, the SEM of granule schemes；
Fig. 3 is that after comparative example 2 of the present invention prepares the dispersion of gained cerium oxide, the SEM of granule schemes.
Detailed description of the invention
Advantages of the present invention is expanded on further below by specific embodiment, but protection scope of the present invention is not limited solely to following embodiment.
Agents useful for same of the present invention and raw material are all commercially.The polishing fluid of the present invention be can be prepared by by the simple Homogeneous phase mixing of mentioned component.
Embodiment 1
At ambient temperature, first PVP (mean molecule quantity is 10000) and cerous nitrate are dissolved and be mixed to get the first compositions, again precipitant ammonium carbonate is added in this first compositions, there is precipitation, in reaction system, the concentration of PVP is 0.05M, the concentration of cerous nitrate and ammonium carbonate respectively takes 0.05M and 0.075M, after precipitant interpolation terminates, reaction system is kept to stir 30 minutes, further by aggregate sample at 150 DEG C hydrothermal crystallizing react 0.5 hour, gained precipitate after pure water 3 times, be filtrated to get filter cake dry after obtain cerium carbonate powder；Gained cerium carbonate powder is roasting 10 hours in 400 DEG C of still airs further, obtain cerium oxide powder after cooling；By adding polyacrylic acid as dispersant, gained cerium oxide powder is carried out ball milling dispersion process, by controlling ball milling jitter time, the cerium oxide nanoparticles that grain diameter is distributed in 120-200 nanometer range can be obtained, result is as shown in Figure 1, as can be known from Fig. 1, less by reuniting between the preparation-obtained cerium oxide particle of the application method, particle size distribution is more uniform.
Embodiment 2
At ambient temperature, first PVA (mean molecule quantity is 1000) and cerous acetate are dissolved and be mixed to get the first compositions, again precipitant ammonium hydrogen carbonate is added in this first compositions, carry out precipitation, in reaction system, the concentration of PVA is 0.1M, the concentration of cerous acetate and ammonium hydrogen carbonate respectively takes 1.0M and 4.0M, after precipitant interpolation terminates, after keeping reaction system to stir 30 minutes, by aggregate sample at 80 DEG C hydrothermal crystallizing react 10 hours, gained precipitate after pure water 3 times, be filtrated to get filter cake dry after obtain cerium carbonate powder；Gained cerium carbonate powder is roasting 0.5 hour in 900 DEG C of still airs further, obtains cerium oxide powder after cooling；By adding polyacrylic acid as dispersant, gained cerium oxide powder is carried out ball milling dispersion process, by controlling ball milling jitter time, it is possible to obtain the cerium oxide nanoparticles that grain diameter is distributed in 120-200 nanometer range.
Embodiment 3
At ambient temperature, first PEG (mean molecule quantity is 3000) and cerous acetate are dissolved and be mixed to get the first compositions, again precipitant ammonium carbonate is added in this first compositions, carry out precipitation, in reaction system, the concentration of PEG is 0.25M, the concentration of cerous acetate and ammonium carbonate respectively takes 0.5M and 1.5M, after precipitant interpolation terminates, after keeping reaction system to stir 30 minutes, by aggregate sample at 120 DEG C hydrothermal crystallizing react 8 hours, gained precipitate after pure water 3 times, be filtrated to get filter cake dry after obtain cerium carbonate powder；Gained cerium carbonate powder is roasting 4 hours in 600 DEG C of still airs further, obtain cerium oxide powder after cooling；By adding polyacrylic acid as dispersant, gained cerium oxide powder is carried out ball milling dispersion process, by controlling ball milling jitter time, it is possible to obtain the cerium oxide nanoparticles that grain diameter is distributed in 120-200 nanometer range.
Embodiment 4
At ambient temperature, first PVP (mean molecule quantity is 4000) and cerium chloride are dissolved and be mixed to get the first compositions, again precipitant ammonium carbonate is added in the first compositions, carry out precipitation, in reaction system, the concentration of PVP is 0.25M, the concentration of cerium chloride and ammonium carbonate respectively takes 0.5M and 1.5M, after precipitant interpolation terminates, after keeping reaction system to stir 30 minutes, by aggregate sample at 90 DEG C hydrothermal crystallizing react 8 hours, gained precipitate after pure water 3 times, be filtrated to get filter cake dry after obtain cerium carbonate powder；Gained cerium carbonate powder is roasting 3 hours in 700 DEG C of still airs further, obtain cerium oxide powder after cooling；By adding polyacrylic acid as dispersant, gained cerium oxide powder is carried out ball milling dispersion process, by controlling ball milling jitter time, it is possible to obtain the cerium oxide nanoparticles that grain diameter is distributed in 120-200 nanometer range.
Comparative example 1
Comparative example 1 is without organic additive, and when reactant concentration proportioning is different, the embodiment of preparation cerium oxide nanoparticles.
At ambient temperature, first cerous nitrate is dissolved, again precipitant ammonium carbonate is added in cerous nitrate solution, there is precipitation, in reaction system, the concentration of cerous nitrate and ammonium carbonate respectively takes 0.05M and 0.05M, after precipitant interpolation terminates, keeps reaction system to stir 30 minutes, further by aggregate sample at 150 DEG C hydrothermal crystallizing react 0.5 hour, gained precipitate after pure water 3 times, be filtrated to get filter cake dry after obtain cerium carbonate powder；Gained cerium carbonate powder is roasting 10 hours in 400 DEG C of still airs further, obtain cerium oxide powder after cooling；By adding polyacrylic acid as dispersant, gained cerium oxide powder is carried out ball milling dispersion process, by controlling ball milling jitter time.As in figure 2 it is shown, as can be known from Fig. 2, when selecting improper such as reactant concentration proportioning and organic additive addition, then the cerium oxide nanoparticles pattern prepared is irregular to its result, reunites substantially between granule, and distribution of sizes is owed uniformly.
Comparative example 2
When comparative example 2 changes for precipitation temperature and reactant concentration proportioning is different, the embodiment of preparation cerium oxide nanoparticles.
At ambient temperature, first PVA (mean molecule quantity is 1000) and cerous acetate are dissolved mixing, again precipitant ammonium hydrogen carbonate is added in this mixed solution, carry out precipitation, in reaction system, the concentration of PVA is 0.1M, the concentration of cerous acetate and ammonium hydrogen carbonate respectively takes 2.0M and 3.0M, after precipitant interpolation terminates, after keeping reaction system to stir 30 minutes, by aggregate sample at 30 DEG C hydrothermal crystallizing react 10 hours, gained precipitate after pure water 3 times, be filtrated to get filter cake dry after obtain cerium carbonate powder；Gained cerium carbonate powder is roasting 0.5 hour in 900 DEG C of still airs further, obtains cerium oxide powder after cooling；By adding polyacrylic acid as dispersant, gained cerium oxide powder is carried out ball milling dispersion process, by controlling ball milling jitter time.As it is shown on figure 3, as can be known from Fig. 3, as the parameter such as temperature, reactant concentration selects improper, then the cerium oxide nanoparticles prepared is larger in size, and pattern is irregular, and particle size distribution is owed uniformly for its result.
Pattern irregular, will cause tremendous influence to final polishing effect, in following CMP planarization Application Example, it has been found that use the preparation-obtained cerium oxide nanoparticles of the application, has effect excellent especially in CMP field.
CMP planarization Application Example
With cerium oxide synthesized by the embodiment of the present invention and comparative example for abrasive material, corresponding to embodiment each in table 1 and comparative example, prepare CMP planarization liquid, mix homogeneously.It is further to note that
The aqueous dispersions that cerium oxide particle is original concentration 10wt% to 20wt% used in polishing fluid, the particle diameter of granule is on average to amount to diameter, and its mean diameter is measured by the Nano-ZS90 laser particle size analyzer of Malvern company；The grain size of the cerium oxide particle used in polishing fluid is by the test of XRD-6100 Shimadzu X-ray diffractometer.
In table 1, the concrete dispensing mode of polishing fluid is: described cerium oxide abrasive particles is both from the corresponding embodiment of above-mentioned cerium oxide preparation and comparative example, by the component except abrasive grains according to content listed in table, mix homogeneously in deionized water, it is adjusted to required pH value with KOH, it is subsequently adding dispersion of abrasive particles, if pH declines, it is adjusted to required pH value with KOH, and supplies percentage composition to 100wt% with deionized water, can be prepared by CMP chemical mechanical polishing liquid.
Table 1 cerium oxide synthetic example of the present invention and the chemical mechanical polishing liquid formula that comparative example is abrasive material
Effect example
It is polished by CMP planarization liquid 1-4 in above-described embodiment and 1,2 pairs of blank wafer of comparative example respectively, polishing condition is identical, burnishing parameters is as follows: Logitech polishing pad, downward pressure 3psi, rotary speed/rubbing head rotating speed=60/80rpm, polishing time 60s, chemical machinery throws flow rate of slurry 100mL/min.Polishing wafer coupons used forms by commercially available (such as U.S. SVTC company produces) 8 inches of plated film wafer coupons.The RT-7O/RG-7B tester that the used film thickness NANOMatrics company of polishing produces records.Namely obtaining metallic film removal rate by the thickness difference recorded before and after polishing divided by the polishing consumption time, polishing time is 1 minute.
The experimental technique of unreceipted actual conditions in embodiment, generally conventionally condition, or according to manufacturer it is proposed that condition.
Table 2 cerium oxide of the present invention synthetic example preparation corresponding to comparative example chemical mechanical polishing liquid polishing effect compares
As can be seen from Table 2, in embodiment 1-4, using the cerium oxide for preparing in the way of provided herein as abrasive material, polishing fluid can reach higher TEOS polishing speed and TEOS/SiN polishing selects ratio, but comparative example polishing fluid exists the significant problem of surface of polished cut, or polishing selects than phenomenon on the low side.Illustrate that the cerium oxide prepared by the present invention has good STI and polishes application characteristic.
It should be appreciated that wt% of the present invention refers to weight/mass percentage composition.
Above specific embodiments of the invention being described in detail, but it is intended only as example, the present invention is not restricted to particular embodiments described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and replacement are also all among scope of the invention.Therefore, the equalization made without departing from the spirit and scope of the invention converts and amendment, all should contain within the scope of the invention.
Claims (14)
1. the preparation method of a cerium oxide nanoparticles, it is characterised in that including:
Step one: organic additive and cerium source aqueous solution are prepared the first compositions；
Step 2: by described first compositions and precipitant mix, and stir 0.5-10 hour, precipitation obtains cerous carbonate；
Step 3: described cerous carbonate high temperature is bakeed, to prepare described cerium oxide nanoparticles, and the particle diameter of described cerium oxide nanoparticles is 120-200 nanometer.
2. preparation method as claimed in claim 1, wherein, in described step one, temperature is 80-150 DEG C.
3. preparation method as claimed in claim 1, wherein, in described step one, temperature is 90-120 DEG C.
4. preparation method as claimed in claim 1, wherein, in described step one, described cerium source aqueous solution be in cerous nitrate, cerium chloride, cerous acetate aqueous solution one or more.
5. preparation method as claimed in claim 1, wherein, in described step one, described machine additive be in polyvinylpyrrolidone, Polyethylene Glycol or polyvinyl alcohol one or more.
6. preparation method as claimed in claim 1, wherein, in described step one, described machine additive mean molecule quantity is 1000-10000.
7. preparation method as claimed in claim 1, wherein, in described step 2, described precipitant be in ammonium hydrogen carbonate or ammonium carbonate one or more.
8. preparation method as claimed in claim 1, wherein, in the aqueous solution of described cerium source, cerium ion is 1:1.5～1:4.0 with the mol ratio of anion in precipitant.
9. preparation method as claimed in claim 1, wherein, in the aqueous solution of described cerium source, cerium ion is 1.0:1.0～10.0:1.0 with the mol ratio of organic additive.
10. preparation method as claimed in claim 1, wherein, in the aqueous solution of described cerium source, the molar concentration of cerium ion is 0.05M～1.0M.
11. preparation method as claimed in claim 1, wherein, in described precipitant, the molar concentration of anion is 0.075M～4.0M.
12. preparation method as claimed in claim 1, wherein, the molar concentration of described organic additive is 0.005M～1.0M.
13. preparation method as claimed in claim 1, wherein, in described step 3, sintering temperature is 400-900 DEG C, and roasting time is 0.5-10 hour.
14. a STI polishing fluid, it includes the cerium oxide nanoparticles obtained just like preparation described in described any one of claim 1-13.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2019011251A1 (en) * | 2017-07-13 | 2019-01-17 | 安集微电子科技（上海）股份有限公司 | Chemical-mechanical polishing liquid |
| CN110589870A (en) * | 2019-09-16 | 2019-12-20 | 桂林电子科技大学 | Method for preparing monodisperse spherical nano rare earth oxide by uniform precipitation process |
| CN114045153A (en) * | 2021-12-21 | 2022-02-15 | 清华大学 | Method for preparing cerium dioxide suspension, cerium dioxide suspension and polishing solution |
| CN115595585A (en) * | 2022-11-10 | 2023-01-13 | 江西省科学院应用物理研究所（Cn） | Preparation method of special metallographic polishing agent for easily-oxidized metal |
| CN115974127A (en) * | 2022-11-25 | 2023-04-18 | 深圳市聚芯半导体材料有限公司 | Quasi-spherical nano cerium dioxide, suspension thereof, preparation method and application |
| TWI818699B (en) * | 2021-08-30 | 2023-10-11 | 韓商凱斯科技股份有限公司 | Cerium oxide abrasive particles and polishing slurry composition |
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2014
- 2014-12-29 CN CN201410840055.3A patent/CN105800660A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019011251A1 (en) * | 2017-07-13 | 2019-01-17 | 安集微电子科技（上海）股份有限公司 | Chemical-mechanical polishing liquid |
| CN110589870A (en) * | 2019-09-16 | 2019-12-20 | 桂林电子科技大学 | Method for preparing monodisperse spherical nano rare earth oxide by uniform precipitation process |
| TWI818699B (en) * | 2021-08-30 | 2023-10-11 | 韓商凱斯科技股份有限公司 | Cerium oxide abrasive particles and polishing slurry composition |
| CN114045153A (en) * | 2021-12-21 | 2022-02-15 | 清华大学 | Method for preparing cerium dioxide suspension, cerium dioxide suspension and polishing solution |
| CN115595585A (en) * | 2022-11-10 | 2023-01-13 | 江西省科学院应用物理研究所（Cn） | Preparation method of special metallographic polishing agent for easily-oxidized metal |
| CN115974127A (en) * | 2022-11-25 | 2023-04-18 | 深圳市聚芯半导体材料有限公司 | Quasi-spherical nano cerium dioxide, suspension thereof, preparation method and application |
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Application publication date: 20160727 |