CN101481640A - Aqueous cleaning composition - Google Patents
Aqueous cleaning composition Download PDFInfo
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- CN101481640A CN101481640A CNA2008100004295A CN200810000429A CN101481640A CN 101481640 A CN101481640 A CN 101481640A CN A2008100004295 A CNA2008100004295 A CN A2008100004295A CN 200810000429 A CN200810000429 A CN 200810000429A CN 101481640 A CN101481640 A CN 101481640A
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Abstract
An aqueous washing combination is used for integrated circuit copper wiring, chemical mechanical planarization processing procedure or the subsequent washing procedure, and contains 0.1wt%-20wt% of monoamino methane, 0.05wt%-20wt% of mono-quaternary ammonium compound and water; when being used in semiconductor planarization processing procedure or the subsequent washing procedure, the aqueous washing combination can effectively remove contamination, reduces the number of defects on the surface of wafer and maintain better surface roughness of the wafer.
Description
Technical field
The present invention relates to a kind of aqueous clean combination, particularly relate to a kind of aqueous clean combination that integrated circuit manufacture process chemical-mechanical planarization (CMP) is handled that is used for.
Background technology
About semiconductor element, now just towards littler live width, more the direction of high density of integration develops.When the unicircuit minimum feature was reduced to below 0.25 micron, resistance and the caused time lag of dielectric layer stray capacitance (RCdelay) by plain conductor itself had become the main key that influences the element arithmetic speed.Therefore, in order to improve the arithmetic speed of element, the dealer changes gradually in the high-order processing procedure below 0.13 micron and adopts the copper plain conductor and replace traditional aluminum-copper alloy lead at present, and this processing procedure is called " copper wiring " for short.
The technology of chemical-mechanical planarization (Chemical Mechanical Planarization) is applied in the copper plain conductor processing procedure, not only can overcome the problem that is difficult for being difficult to define pattern because of the copper metal etch, and grind the plane that the back forms a universe planarization (globalplanarity), help the carrying out of multi-layer conductor leads processing procedure.The principle of chemical-mechanical planarization is to borrow the abrasive grains in the lapping liquid to match with chemical assistant, make the crystal column surface material is produced abrasion, make the smooth higher position of air spots remove speed whereby because of pressurized produces height greatly, the lower that air spots is smooth, then have to remove speed more slowly, and reach the purpose of universe planarization because of pressurized is little.
In the process of lapping of chemical-mechanical planarization, a large amount of fine ground particles and chemical assistant in the lapping liquid, and the chip that the wafer abrasion are peeled off may be attached to crystal column surface.General wafer common pollutent after grinding is metal ion, organic compound or abrasive grains etc.If no effective wash procedure is removed above-mentioned pollutent, then will influence the carrying out of successive process and the yield and the reliability of reduction element.Therefore, in the CMP processing procedure or its follow-up wash procedure, become can successful Application CMP in the gordian technique of manufacture of semiconductor.
Copper wiring is with how using benzotriazole (benzotriazole is called for short BTA) or derivatives thereofs as corrosion inhibitor in the lapping liquid.In the produced pollution thing, be difficult to most remove with the BTA organic residue behind the copper wiring grinding wafer, major cause is that BTA is binding on the copper conductor in the chemisorption mode.Tradition only utilizes electrostatic repulsion, ultrasonic oscillation and polyvinyl alcohol (PVA) brush the mode of physical removal such as to scrub, and is difficult for that excellent cleaning effect is arranged.
Conventional metals interlayer dielectric layer (inter-metal dielectric layer) and tungsten plug (W plug) are behind chemical-mechanical planarization, often use ammonia soln, aqueous citric acid solution and/or fluorochemicals to clean, but above-mentioned solution and be not suitable for the wafer of copper plain conductor.Ammonia soln can corrode copper metallic face unevenly, and causes the phenomenon of roughening.Aqueous citric acid solution is too poor and the clearance of pollutent still had improve the space to copper dissolution power.Fluorochemicalss such as hydrofluoric acid then not only can make roughened copper surfaceization, and for avoiding its harmful to human and environment, need pay more costs in personnel safety guard and liquid waste disposal.
People's such as Small United States Patent (USP) the 6th, 498, disclose a kind of composition that is used to remove the CMP resistates No. 131, it comprises a pH value between 10 to 12.5 the aqueous solution, this aqueous solution comprises at least one non-ionic interfacial agent, at least one amine, at least one quaternary ammonium compound, and at least one surperficial setting-up agent that is selected from the group that constitutes by ethylene glycol, propylene glycol, polyoxyethylene, polyoxytrimethylene and composition thereof, this amine can be for example monoethanolamine (monoethanolamine is called for short MEA) etc.
People's such as Naghshineh United States Patent (USP) discloses a kind of scavenging solution that contains copper integrated circuit that is used to clean for the 6th, 492, No. 308, and it is by a C
1-C
10Tetraalkylammonium hydroxide (quaternary ammonium hydroxide), a polarity organic amine and a corrosion inhibitor form, this polarity organic amine can be selected from monoethanolamine etc.
People's such as Ward United States Patent (USP) the 5th, 988, No. 186 announcements are a kind of in order to remove the aqueous clean combination of organic or inorganic material, it comprises a mixture, this mixture is that corrosion inhibitor is formed by the alcohol ester of water, a water soluble polar solvent, an organic amine and a tool phenyl ring framework, and this organic amine that discloses in the specification sheets comprises tetraalkylammonium hydroxide, two amidos or monoamine base oxy-compound etc.
U.S.'s publication of people such as Chen No. 2007/0066508 (No. the 200641121st, TaiWan, China publication) discloses a kind of aqueous clean combination that contains the copper conductor wafer that is used for cleaning behind the integrated circuit manufacture process chemical-mechanical planarization, and it is made up of a nitrogen heterocyclic ring organic bases, a hydramine and water.
U.S.'s publication of people such as Walker No. 2006/0229221 (No. the 200706647th, TaiWan, China publication) discloses a kind of cleaning combination that is used for the cleaning microelectronic substrate, it is by a hydroxide level Four ammonium, one alkanolamine (alkanolamine) and water are formed, this hydroxide level Four ammonium is preferably and is selected from tetramethyl ammonium hydroxide (tetramethylammonium hydroxide, abbreviate TMAH as), tetrabutylammonium or these mixture, and this alkanolamine is preferably and is selected from monoethanolamine, 1-amido-2-propyl alcohol, 2-(methylamino) ethanol, trolamine or these mixture.
Progress along with the semiconductor crystal wafer processing procedure, the plain conductor width has narrowed down to 32 nanometers, the problem that new planarization processing procedure still has many need to overcome, for example the crystal column surface of nano-scale linewidth is through fabrication process rear surface roughness possible deviation, and live width is dwindled the testing electrical property (open/short test) of back copper conductor wafer and reliability test (reliabilitytest) variation as a result.Industrial community still needs one more can effectively remove the cleaning combination that residues in the pollutent on the copper conductor crystal column surface and reduce the number of defects of crystal column surface than prior art to copper conductor wafer manufacturing process for cleaning.
Summary of the invention
The applicant considers, though ammonia or amido have stronger etching for copper, but how suitably controlling amine is a difficult problem to the etching of copper, therefore if can adjust and avoid corroding unevenly copper by the existence of other substituting groups or component, should address the above problem.Though aforementioned partial monopoly case has utilized the hydramine (such as monoethanolamine (MEA)) that has amido and hydroxyl concurrently to be used as cleaning component, but the applicant finds after the reality test, when using this type of hydramine to clean pollutent on the copper conductor crystal column surface, have obviously higher problem of strong corrosion copper wafer and surfaceness.
The applicant is surprised to find in the process that addresses the above problem, when using the another kind of amido methane that has amido and hydroxyl simultaneously (is dihydroxymethyl amido methane (2-amino-1,3-propanediol) and/or tri methylol amino methane (2-amino-2-(hydroxymethyl)-1,3-propanediol) and collocation when using the quaternary ammonium compound that conventional clean uses, as long as with the two relation with contents regulation and control in a specific scope, can reach strange good pollutants removal rate, and can not damage to some extent for surfaceness, and be the clean-out system that is better than in the past yet the dissolving power of copper.
The purpose of this invention is to provide a kind of aqueous clean combination, it is specially adapted to chemical-mechanical planarization or its follow-up wash procedure in the copper wiring, said composition comprises the amido methane of 0.1wt%-20wt%, the quaternary ammonium compound of 0.05wt%-20wt%, and water; This amido methane is to be selected from dihydroxymethyl amido methane, tri methylol amino methane or its combination.
Aqueous clean combination according to purpose of the present invention is characterized in that, this amido methane is tri methylol amino methane.
Aqueous clean combination according to purpose of the present invention is characterized in that, this quaternary ammonium compound is a tetraalkylammonium hydroxide.
Aqueous clean combination according to purpose of the present invention is characterized in that, this quaternary ammonium compound is selected from tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide or its combination.
Aqueous clean combination according to purpose of the present invention is characterized in that, this quaternary ammonium compound is a tetramethyl ammonium hydroxide.
Aqueous clean combination according to purpose of the present invention is characterized in that, the content of this amido methane is 0.1wt%-15wt%.
Aqueous clean combination according to purpose of the present invention is characterized in that, the content of this amido methane is 0.1wt%-10wt%.
Aqueous clean combination according to purpose of the present invention is characterized in that, the content of this quaternary ammonium compound is 0.05wt%-15wt%.
Aqueous clean combination according to purpose of the present invention is characterized in that, the content of this quaternary ammonium compound is 0.05wt%-10wt%.
Aqueous clean combination according to purpose of the present invention is characterized in that, also comprises a nitrogen heterocyclic ring organic bases.
Aqueous clean combination according to purpose of the present invention is characterized in that, this nitrogen heterocyclic ring organic bases is a piperazine.
Beneficial effect of the present invention is: contact one period working lipe with aqueous clean combination of the present invention with cupric semiconductor crystal wafer after chemical-mechanical planarization grinds, can remove the pollutent that residues in after the grinding on the crystal column surface effectively, keep the preferable surfaceness of copper conductor simultaneously.Another beneficial effect of the present invention is: need not use interfacial agent and be used for the corrosion inhibitor (as BTA and/or its derivative and anti-vitamin C deficiency acid etc.) that cleaning process is protected copper metallic face; can remove the pollutent that residues in after the grinding on the crystal column surface effectively, can avoid interfacial agent and corrosion inhibitor to residue in problem on the wafer.
Embodiment
Preferably, this amido methane is tri methylol amino methane.
Preferably, this quaternary ammonium compound is a tetraalkylammonium hydroxide, more preferably is tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide or its combination.In concrete example of the present invention, this quaternary ammonium compound is a tetramethyl ammonium hydroxide.
Optionally, this aqueous clean combination can further comprise a nitrogen heterocyclic ring organic bases.Preferably, this nitrogen heterocyclic ring organic bases is piperazine (piperazine).
Relevant amido methane and the concentration of quaternary ammonium compound in aqueous clean combination of the present invention are generally and save production, transportation and warehouse cost, and the producer can provide the composition of higher concentration usually, doubly use the back with the about 1-60 of ultrapure water dilution at use side again.Under the specific demand situation, as saving the treatment time, cleaning combination stoste that can concentration is higher is directly in order to cleaning wafer.
Can use under the cleaning combination normal temperature of the present invention, this cleaning combination is contacted one period working lipe with the cupric semiconductor crystal wafer, can remove the pollutent that residues on the crystal column surface effectively, keep the preferable surfaceness of copper conductor simultaneously.Generally speaking, when working concentration is low, need long duration of contact (for example, 1-3 minute), when working concentration is higher, only need short duration of contact (for example, being shorter than 1 minute).When reality was used, the user can be by the processing procedure optimization (process optimization) of seeking cleaning combination concentration and duration of contact according to need.
Under every factor of taking all factors into consideration manufacturing, transport and using, with the total restatement of composition, the amido methane content in the said composition is 0.1wt%-20wt%, more preferably is 0.1wt%-15wt%, more preferably is again 0.1wt%-10wt%.
Considering under the above-mentioned factor that equally with the total restatement of composition, the quaternary ammonium compound content in the said composition is 0.05wt%-20wt%, more preferably is 0.05wt%-15wt%, more preferably is again 0.05wt%-10wt%.
Illustrative in each concrete example of the present invention is that concentration is rarer but can reach the concentration of purpose, those skilled in the art should understand, and when using the higher cleaning combination of absolute concentration, it still can reach purpose of the present invention, and ageing will be better, but raw materials cost is higher.
As previously mentioned, crystal column surface after employed corrosion inhibitor in the lapping liquid that the copper wiring chemical-mechanical planarization is used (as the BTA or derivatives thereof) can residue in grinding, and the physical method that described organic residue is difficult to only depend on general using electrostatic repulsion, ultrasonic oscillation and polyvinyl alcohol (PVA) brush to scrub is removed.Amido methane and quaternary ammonium compound that cleaning combination of the present invention contained can promote the saturation solubility of cleaning combination to organic residue (as BTA), thereby can provide bigger motivating force with dissolving BTA particulate.Therefore, the mode that above-mentioned conventional physical is removed is used under the disclosed cleaning combination in collocation, can reach better wash result.
Cleaning combination of the present invention can be used for cleaning on the board of chemical-mechanical planarization the crystal column surface through planarization, also can be at a crystal column surface that independently cleans on the cleaning machine through planarization.
Embodiment
The present invention will be described further with regard to following examples, but will be appreciated that, described embodiment only is used to illustrate, and should not be interpreted as restriction of the invention process.
The effect test
The same test that each aqueous clean combination carried out that makes at following each embodiment and comparative example is as shown in following:
I. the test of copper dissolution ability
One bronze medal blank wafer is cut into each wafer of 1.5 centimeters of length and width, this wafer is carried out acid dissolving pre-treatment to remove the top layer cupric oxide, then this wafer is soaked in 50 milliliters the aqueous clean combination, takes out wafer after one minute, and measure copper ion concentration in the solution with ICP-MS.
The test of II.BTA saturation solubility
Aqueous clean combination under the environment of 25 ℃ of constant temperature, is inserted excessive BTA stirring and dissolving in addition, and the insolubles after 4 hours in the filtering cleaning combination is with the BTA concentration in high-performance liquid chromatograph (HPLC) analytical solution.
III. the measurement of surfaceness
Aqueous clean combination is cleaned the copper blank wafer that ground on cleaning machine Ontrak, and scavenging period is 2 minutes, and the cleaning combination flow is 600 milliliters of per minutes.After finishing, cleaning measures the surfaceness (average roughness Ra and r.m.s. roughness Rq) of copper wafer with atomic force microscope (AFM).
IV. the removal efficiency test of surface particle pollutent
The copper blank wafer is soaked in contain corrosion inhibitor BTA copper wiring with lasting 1 minute in the lapping liquid to pollute.After the pollution, at the Rotary drying in addition after 18 seconds of flushing on the cleaning machine Ontrak, measure the particle number A that pollutes on the wafer of back with TOPCON WM-1700 wafer measuring fine particles instrument again with ultrapure water.The known wafer that pollutes the back particle number was scrubbed on cleaning machine Ontrak 2 minutes with different cleaning combinations, last and with ultrapure water flushing Rotary drying in addition after 18 seconds, measure to clean particle number B on the wafer of back with TOPCONWM-1700 wafer measuring fine particles instrument once more, so calculate each cleaning combination to clearance (clearance=((A-B)/A) * 100%) of crystal column surface particulate pollutant.
＜embodiment 1-5 and comparative example 1-3 〉
The cleaning combination that makes original composition earlier according to component and the usage ratio (all in wt%) of each embodiment in the table 1, then 30 times of cleaning combinations that become test usefulness of redilution, and with table 1 in the cleaning combination that contains diethanolamine, trolamine and piperazine (comparative example 1) that uses of prior art; Citric acid clean-out system (comparative example 2) commonly used; And water (comparative example 3) compares, and comply with above-mentioned each test mode and assess the copper dissolution ability of the cleaning combination of each embodiment and comparative example, BTA saturation solubility, clean the back wafer surface roughness, and the clearance of surface particle pollutent, these results all list in the table 1.
Result and discussion
As shown in Table 1, tri methylol amino methane has the ability of etching dissolve copper metal, can increase the etching dissolution rate of copper metal; By the result of embodiment 5 as can be known, the interpolation of (nitrogen heterocyclic ring organic bases) can promote the saturation solubility of cleaning combination to BTA.And by the result of comparative example 2 and 3 as can be known, citric acid and water there is no the ability of dissolve copper metal.Copper dissolving metal ability that the cleaning combination tool is healed strong and the BTA saturation solubility of healing high, representative has the good cleaning performance of healing to organic pollutants such as pollutent on the copper metal and BTA, but copper metal etch dissolving power (too fast and/or inhomogeneous) then need be careful the negative impact that roughness causes improperly.
By the cleaning combination of embodiment 1 to 5 and comparative example 1 to 3 more as can be known, though the amine of more amount can make surfaceness increase, but still keep than prior art (comparative example 1,2) near or preferable surfaceness level.But show cleaning combination of the present invention not only etching dissolve copper metal in broad concentration range, and can keep good copper metallic face roughness.Moreover, use the hydramine of citric acid (comparative example 2) or prior art to add nitrogen heterocyclic ring organic bases composition (comparative example 1) separately, though can remove most pollutent, but when tri methylol amino methane and tetramethyl ammonium hydroxide use (embodiment 1～4) jointly, more can significantly promote cleaning performance.
In sum; the amido methane of the employed particular types of the present composition is except that having amido; also has hydroxyl; and the existence of hydroxyl can reduce the etch capabilities of amido for copper; therefore simultaneously can also protect the copper surface; form etching and protect the mechanism of carrying out simultaneously, the unlikely roughened copper surface degree variation that allows so behind the collocation quaternary ammonium compound, can corrode the copper surface equably, the pollutants removal rate that shows simultaneously is superior more many than cleaning combination in the past.
Claims (11)
1. an aqueous clean combination is characterized in that, comprises the amido methane of 0.1wt%-20wt%, a quaternary ammonium compound and the water of 0.05wt%-20wt%; This amido methane is to be selected from dihydroxymethyl amido methane, tri methylol amino methane or its combination.
2. aqueous clean combination according to claim 1 is characterized in that, this amido methane is tri methylol amino methane.
3. aqueous clean combination according to claim 1 is characterized in that this quaternary ammonium compound is a tetraalkylammonium hydroxide.
4. aqueous clean combination according to claim 3 is characterized in that, this quaternary ammonium compound is selected from tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide or its combination.
5. aqueous clean combination according to claim 4 is characterized in that this quaternary ammonium compound is a tetramethyl ammonium hydroxide.
6. aqueous clean combination according to claim 1 is characterized in that, the content of this amido methane is 0.1wt%-15wt%.
7. aqueous clean combination according to claim 6 is characterized in that, the content of this amido methane is 0.1wt%-10wt%.
8. aqueous clean combination according to claim 1 is characterized in that, the content of this quaternary ammonium compound is 0.05wt%-15wt%.
9. aqueous clean combination according to claim 8 is characterized in that, the content of this quaternary ammonium compound is 0.05wt%-10wt%.
10. aqueous clean combination according to claim 1 is characterized in that, also comprises a nitrogen heterocyclic ring organic bases.
11. aqueous clean combination according to claim 10 is characterized in that, this nitrogen heterocyclic ring organic bases is a piperazine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100004295A CN101481640B (en) | 2008-01-10 | 2008-01-10 | Aqueous cleaning composition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100004295A CN101481640B (en) | 2008-01-10 | 2008-01-10 | Aqueous cleaning composition |
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| CN101481640A true CN101481640A (en) | 2009-07-15 |
| CN101481640B CN101481640B (en) | 2011-05-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI228538B (en) * | 2000-10-23 | 2005-03-01 | Kao Corp | Polishing composition |
| MY143399A (en) * | 2001-07-09 | 2011-05-13 | Avantor Performance Mat Inc | Microelectronic cleaning compositons containing ammonia-free fluoride salts for selective photoresist stripping and plasma ash residue cleaning |
| JP2004023009A (en) * | 2002-06-20 | 2004-01-22 | Nikon Corp | Polishing body, polishing device, semiconductor device, and method of manufacturing the same |
| EP1562225A4 (en) * | 2002-11-08 | 2007-04-18 | Wako Pure Chem Ind Ltd | Cleaning composition and method of cleaning therewith |
| US8338087B2 (en) * | 2004-03-03 | 2012-12-25 | Advanced Technology Materials, Inc | Composition and process for post-etch removal of photoresist and/or sacrificial anti-reflective material deposited on a substrate |
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Address after: Kaohsiung City, Taiwan, China Patentee after: Xinming Materials Co.,Ltd. Address before: Taiwan County, Kaohsiung, China Patentee before: Changxing Development Technology Co.,Ltd. |
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Effective date of registration: 20230926 Address after: Delaware Patentee after: Integ Ltd. Address before: Taiwan, Kaohsiung, China Patentee before: Xinming Materials Co.,Ltd. |
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