TW516989B - Polishing method using a reconstituted dry particulate polishing composition - Google Patents

Abstract

A polishing method uses a dry particulate solids composition that is reconstituted into an aqueous composition for delivery to a polishing apparatus. In one aspect of the invention, the dry particulate solids composition is provided in a package size that is just substantially sufficient to make a reconstituted slurry for completing the polishing of a predetermined number of work pieces. The quantity of dry particulate solids delivered to a reconstitution apparatus can be an amount appropriate for polishing one work piece or a small number of work pieces, or the system can operate in larger batches or a continuous flow mode. The reconstituted aqueous polishing solution can be monitored for physical or chemical properties, filtered, blended with other chemical mixtures, or modified in other ways prior to being used in the polishing apparatus.

Description

516989 A7 B7 V. Description of the Invention (1) Field of the Invention The present invention relates generally to a polishing slurry and its use for polishing, and particularly to a method for polishing a work piece using a reconstituted dry particle polishing composition. Background Polishing preparations for chemical mechanical polishing (CMP) of integrated circuit wafers and polishing preparations for high-tech optical components or other ultra-fine surface finishing applications are generally composed of a solid (abrasive) and various chemical components. Consisting of an aqueous dispersion. This commercially available material can be a single mixture of solids or divided into several parts, one part containing a concentrated type of abrasive and the other part containing a concentrated type of chemical ingredients. Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the notes on the back before filling out this page). As CMP technology of chemical mechanical polishing becomes more and more important, complex chemical and polishing systems have been developed. These aqueous formulations need to have a long-term pot life and good stability so that the material does not change during storage. Uncontrolled or excessive physical changes during storage can make these formulations unusable for their use. For example, when a mixture of solids is stored, the solids settle in the storage container to form a hard deposit, and the consumer can no longer easily use the mixture. Moreover, if the concentration of the reactive substance in the chemical system changes significantly, the polishing slurry cannot be used for its intended purpose. The main cause of physical and chemical instability is often that the polishing slurry is generally sold in the form of an aqueous dispersion. Recently, a chemical mechanical polishing CMP system has been developed in which an abrasive is contained in a polishing pad and is not contained in a liquid polishing composition provided on the polishing interface. However, the liquid polishing composition used for these types of polishing pads often has a water content that is compatible with the conventional moisture content -4- this paper size applies to China National Standard (CNS) A4 specifications (210X 297 mm). Imprint 516989 V. Description of the invention (2) Chemical instability of the same type of loose polishing slurry. Preparation of a solid particle abrasive composition and drying of the combination f. The stability of the chemistry and the miller = the hunter eliminates the "water content" in the system, which is partially and minimized. The reason is to prepare the dry particles that actually compose the end-user's disposal Water ^ from «Polishing slurry composition, the throwing money can be used after the gas preparation to dry the polishing slurry." Time rolls off two fruit mouths, so it can take the end user's heart complaint, up to six months or more Long. The edge-polishing composition is disclosed in the patent application serial number 009/413, 〇83, which was filed on October 6, 2009. According to the disclosed formula 3, the dry particle polishing slurry combination was simply reorganized before the exhibition. Although the method of preparing dry polishing slurry has significantly improved the ability to store polishing slurry composition for a long time, the method 重组 method using recombinant polishing slurry has been developed. In order to summarize the polishing invention for further improvement, the present invention proposes a polishing method using a dry particulate solid composition. =: It includes a chemical mechanical polishing composition, which contains a chemical composition that can be used for chemical processing: polishing CMP and substantially completely Chemicals removed by water can be immediately reconstituted into chemical mechanical polishing compositions. This composition is taken through, and & to become an aqueous polishing solution. The granular solid composition may include abrasive particles, oxidants, complexes :: purification agents, surfactants, dispersants, or used in chemical mechanical polishing Start with any type of compound in the table. The solid amount of dry particles delivered to the reorganization device can be suitable for polishing a worksheet paper size (CNS) Α4 specification (pack-(Please read the precautions on the back before filling this page) Order 4 -5 V. Description of the invention (Crystals printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs, the first film and I, or the system can be used in large quantities or under the construction ~ flow mode; ^. 4, reconstituted aqueous polishing solution It can be used to test its physical or chemical properties, filtration, blending with other :::, or other modification before being used in polishing. For example, the method of the present invention includes providing a dry granular solid group 5 items, and dried fine solids, L, and L, dry granular solid composition to form a number of water-containing composition. The amount of y ^ ^ θ water composition is sufficient to complete the quality. Polishing of a predetermined number of working pieces. ^ ㈣ ^ 中 'The method of the present invention includes deciding to fix the pattern and preparing a dry granular solid composition, which is just enough in shape and can be polished in a fixed number of working pieces. The amount of reorganized polishing slurry. Single description FIG. 1 is a schematic diagram of a typical spray dryer used to perform the method of the present invention; FIG. 2 is a schematic diagram illustrating a method of the present invention after drying; FIG. Is a schematic diagram of a typical polishing slurry reorganization device that can be used to perform the method of the present invention And FIG. 4 is a step-by-step frequency distribution diagram of three types of coin thrown distribution in Example 1. The preferred specific examples are detailed in this April k to maintain the abrasive to chemical ratio of the polishing composition without water. Dispersion effect is unstable and the method of aging. The abrasive and chemicals are mixed for the immediate use of the end user, or the ratio of the components that can be prepared into the concentrate is in a common multiple relationship. Immediately after spraying, dehydration by spray drying, cold to dry, or any number of current drying or dehydration methods. The dried granular solid composition is usually (please read the precautions on the back before filling this page) Φ item and then fill in Equipment ·, 11 -6-This paper size is applicable to Chinese National Standard (CNS) A4 (210X 297 mm) 4 4 Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 516989 V. Invention Note (For flowable, powder, can be packed in custom bags or other non-reactive containers, and stored indefinitely without degradation. ☆ Another advantage of Ben Maoming is that the weight of the product is reduced. It reaches about 70% to 100 knife ratio. Considering the worldwide transportation of liquid and water-containing polishing slurry, it saves considerable costs. When it is good to use, the end user can use an appropriate amount of water for official use. The knife-shaped knife is dispersed stately to reconstitute the dry granular solid composition. Other chemicals can be added as needed without sacrificing the use of the present invention. The resulting polishing slurry can be filtered and used in chemical mechanical polishing cMp operations .You can also check the pH and other properties before use, which can be adjusted appropriately. When a single serving of polishing slurry is provided (for polishing a specific number of work pieces or a polishing cycle), subsequent batches of polishing slurry can be mixed, while the current batch of polishing slurry is used for polishing. The preferred mixing unit is one that cleans itself between different batches. Because of the connection of the polishing water, the... Batches may have different compositions. Preferred mixing units include materials that do not contaminate the polishing slurry. As I expected, the formation of a polishing slurry does not produce unnecessary agglomerates. It is inferred that the polishing slurry was adjusted to a completely fully dispersed state just before drying. When the colloidal dispersion mixture of component i is dried, the abrasive particles are surrounded by the dry salt which is uniformly present, which effectively protects the abrasive particles from agglomeration. When the salt dissolves during the recombination process, the abrasive particles are released essentially in the same state as they existed before drying. Typical sub-micron abrasives used in chemical mechanical polishing slurries are oxides such as oxide oxide, stone dioxide, oxide brocade, oxide drink, oxidation error, and oxidation. This paper is suitable for towels and household products (CNS) A4 size TITO · Shy one

--------- 0 ^ ------ 1T ----- IMW, (Please read the notes on the back before filling in this V3C 516989 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs Description of the Invention (5) Zirconium Temple. Abrasive particles are usually used in CMP slurry, with a concentration of about 1 weight eight hundred to f about 30 weight percent. Preferred are oxide oxide, dioxide, oxide: titanium oxide, or Its mixture has a concentration of about 3% by weight to 0% by weight. The types of chemicals that can be used in the operation of rhenium are oxidants, chemical and silver engraving agents, dispersants, surfactants, complexing agents, and dioxygen cutting rates: , Purifying agent, dioxin protecting agent, buffering agent and inhibitor, all the shellfish are present in the dry pulp of the present invention.-General hydroxides, such as hydroxide, ammonium hydroxide, and sodium hydroxide 'and Various amines are used as dispersants for CMP honing agents. It has been found that compounds of the type known as amino alcohols can also be used. Oxidation Jiantong is a component of chemical mechanical polishing slurry, which is used to oxidize the metal layer to its corresponding Oxides, such as oxidizing cranes to oxidized cranes. This layer is mechanically polished to Oxidation removal. Although a wide range of oxidation components can be used, the preferred components include metal oxide salts, metal oxide complexes, iron salts such as nitrate, sulfate, EDTA, citrate, ferric cyanide Aluminum, sodium, potassium, ammonium, quaternary ammonium, scaly, peroxide, chlorate, perchlorate, permanganate, persulfate, iodate, etc. The content of the oxidation component in the polishing slurry is generally sufficient to determine the rapid oxidation of the metal layer, so that the mechanical and chemical polishing components of the polishing slurry are balanced. The content of the oxidizing agent in the chemical-mechanical polishing slurry is generally about 0.5 weight percent to about 15 weight percent, preferably from about 丨 weight percent to about 7 weight percent. The dry granular solid composition of the present invention may additionally be included as applicable for the size of this paper as the Chinese National Standard (CNS) A4 specification (210X 297 Gongchu) (Please read the notes on the back before filling this page)

4 items are filled with A, 11 516989 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Description of Invention () 6

Sio2 is used as a complexing or clamping compound. The complexing agent and the doughing agent are described in U.S. Patent No. 5,391,258 and U.S. Patent No. 5,476,606 which are incorporated by reference into the present invention. These compounds need to have at least two acid groups present in the structure, affecting the dioxin incorporation. Acid species are defined as functional groups with dissociable protons. This fluorene includes, but is not limited to, sulfenyl, fluorenyl, sulfo, and dioxo. The carboxyl group and the hydroxyl group are preferred because they have the most effective species. Particularly effective structures have two or more carboxyl groups, and the hydroxyl group is at the alpha position, such as linear mono- and di-carboxylic acids and salts, including, for example, rhylic acid and malate, tartaric acid and tartrate, and glucose Acids and gluconates. Tri- and polycarboxylic acids and salts, such as citric acid and citric acid, having secondary or tertiary hydroxyl groups at the α position relative to the carboxyl group can also be used. Compounds containing benzene rings can also be used, such as o-di- and polyhydroxyarsanoic acid and acid salts, phthalic acid and acid salts, pyrocatechol, pyrogallol, gallic acid and gallate, and tannic acid and dan Ningrate. The amount of these complexing agents in the chemical mechanical polishing CMP slurry may be from about 0.1% by weight to about 7% by weight. A more preferred range is from about 2 weight percent to about 4 weight percent. In addition, the polishing slurry composition may include a chemical etchant that is substantially free of metal ions. Typical etchant systems include persulfate, nitrate, sulfate, phosphate, citrate, oxalate, mixtures thereof, and the like. The etchant is preferably a non-metallic persulfate, such as ammonium persulfate. The etchant facilitates the dissolution of the metal subjected to chemical mechanical polishing, thereby making the metal soluble in the aqueous dispersion. The amount of these chemicals usually in the chemical mechanical polishing slurry ranges from about 1 weight percent to about 10 weight percent. Preferably it is in the range of about 2 weight percent to about 7 weight percent.

If HBl — · ϋ · 1 ΙΒ ^ Ιϋ fl_ ^ i_l— mi — · Ι · 1_ϋ ^ n ··· ^ ϋϋ ··· ^ — ^ ϋ · t (Please read the precautions on the back before filling this page)- 9-Group 5% 3% 4% 8 8% V. Description of the invention (Chemical mechanical polishing slurry often contains its preparations. Submerged apricots and fu 0 soils do not contain metal ion corrosion inhibitors, fields (corrosion inhibitors include ^ And repair BT), and other-general disk-/ (BTA), thiothiobenzene house 丨 is 丨 々. "The edge is like copper-the corrosion inhibition table used in the polishing operation and subsequent material exposure Metal :: Negative effect. The proportion of typical rotten preparations in chemical mechanical polishing slurry is less than about 1% by weight of the summer series. The flatter simmers range from about 0.05% by weight to 40.6% by weight. Preparation of dry granular solids Renbi 7 persons @ 口 口 < 罘 One step is to determine the actual proportion of all components in the polishing slurry when used. For example, it includes about 5 percent solid II abrasive and about 7 percent chemical composition and has two For a polishing slurry with a chemical composition, the total weight composition of the formulations that can be used can be: η solid Abrasive Chemical A Chemical B After the water is removed, the solid and dissolved solids maintain a ratio of 5/3/4. When spray-dried, it is usually preferred to make the pre-dried polishing slurry concentrate as high as possible. Solid content to reduce the amount of water that needs to be evaporated, thereby reducing costs and increasing flux. Therefore, when manufacturing concentrates for drying, use a 5/3/4 ratio multiplied by a factor. The factor is generally determined by one It is determined by the solubility limit or maximum solid loading limit of the component. For example, when chemical A has high solubility or unlimited solubility and chemical B can only be dissolved to a maximum concentration of about 10%, in order to dissolve all chemical components Completely uniform ^ -10- This paper size applies to China National Standard (CNS) A4 specification (210X 297 mm) --------- ϋ 丨 装 ------ 1T ----- Awm (Please read the notes on the back before filling out this page) Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 516989 A7 B7 V. Description of the Invention 01〇 / 〇〇4 2 5. Therefore, the concentration of the components of the pre-drying polishing slurry is determined by multiplying by each component, and the water system at different locations is multiplied by a factor of 2.5. The final concentration of the drying polishing slurry is: 2.5x5 = 12.5% 2.5x3 = 7.5% 2.5x4 = 10.0 〇 / 0 balance 70.0 〇 /. This wither produces a dry granular solid composition when dried, contains three active ingredients, and has 5/3/4 as a ready-to-use polishing slurry Proportional, but concentrated, the spray drying operation is more effective when spraying the starting material of the dryer. This drying technology can be used in Ma Xi species, including spray drying, cold; east drying, flash drying, direct air drying, heating plate or conveyor drying. In a preferred technique, spray-drying is used because it provides the most product that is easier to control particle size,%, and reproducibility of the product. The schematic diagram of a typical σ lean dryer is shown in Fig. I. The mouth dryer 10 is a composition of hot air 12 which is used in the big 2; 14; among them, the rotary atomizer 18 or pressure suction is used to spray the radon / liquid polishing paddle 16 into the heated air, here ^ Except for almost all water content, solid particles 20 that are free of water are formed. The pellets are further advanced by the air to the exit point of our tank 14 and captured by a cyclone or a collection container, as shown in "Element M. Many coarser materials are collected in the collection container, and Smaller or more: (, two (fine)) are collected in the cyclone separator. In the present invention, both types of harvesters are satisfactory, because the size of the dried particles is not the point. After drying by this ignorance The processing system is shown in Figure 2. After collection, the solid abrasive chemical A chemical B water m scale: mi nn m · — IB ^ m nn Ha (Please read the precautions on the back before filling this page)

、 1T 镛 -11-516989 V. Description of the invention (Dry powder printed and delivered by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs is sent to produce large quantities. Dry at the end pt. Collect the dry powder here, similar to the device in the dry collection Large double-circle cone blender 26 or mixed with dry materials, individually changed two "powder f batches are uniform. By force >. The amount of material can be much greater than the liquid equivalent 'because the weight of water is 75%; ^ The main π, a ... and the limbs have been removed from the concentrate. Uniform high-volume is particularly important for the semiconductor industry. A-^, .. must be tested or quality measured before use of a batch of new materials. : The preparation of the dried granular solid composition is completed. The dried granules are packed in any suitable type of container, such as a barrel lined with plastic fibers, a seven-day-old girl, and塑料 A paper bag with plastic. It is expected that the container size is equal to the amount of the dry particulate solid composition 'easy to reconstitute for various polishing effects. According to the present invention, the dry particulate solid composition can be packed in various packaging sizes The package size depends on the dry granular solid composition. For example, the dry granular solid composition can be packaged in a single use in terms of the amount of polishing slurry used to polish a single work piece or a few work pieces at a time. In package 27. For the polishing of larger batches of work pieces, batch package 28 can be used to store the dry granular solid composition, while in several batches, the dry granular solid composition is filled in the evening batch package 29. Borrow Packing the dried granular solid composition in a package size for polishing a specific amount of work 'can be polished under the optimal amount of polishing slurry. It is' the quality of the polishing method can be improved, and the total cost of the polishing method can be reduced The dry granular solid composition can be carried out in the illustrated mixing unit 30 ~ group 'as shown in the flow chart of Figure 3. The equipment includes the introduction of the measured amount to remove the most loaded component and the re-detachment --- -φά ------ IT ----- MW, (Please read the notes on the back before filling out this page) 12- This paper size applies to China National Standard (CNS) A4 specification (2 丨 〇X 297) Chu) 516989 Α7 Β7 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (10) The water 32 and powder polishing slurry 34 are mixed in the mixing tank 36. The mixing unit 30 includes a high-speed rotor stator placed vertically in the mixing tank 36 38. High-speed rotor stator 38 can provide extremely high shear. After proper mixing of the reconstituted polishing slurry (usually determined by how much energy is consumed per product added), the reorganized polishing slurry is pumped from the reorganization equipment through a sub-micron filter The system 40, and then reach the polishing system or enter the sun trough (not without). The reconstituted polishing slurry can be circulated from this sun trough and used by the end user in the polishing method. Heat is known to those skilled in the art. The polishing slurry system performs several modifications. For example, the capacity of the mixing tank 36 may be from about liters to about 10 liters. In addition, the mixing unit 30 can be a stand-alone system or a system component of a polishing device. In addition-in the alternative, the mouthpiece unit 30 can be constructed to convey a stable amount of reconstituted polishing slurry, the rate of which is the same as the consumption rate of the combined polishing device, and the polishing rate is about, for example, about each work piece. 5 liters to about 15 liters. In another alternative, the dry granular solid composition may be fed directly into the mixing tank 36 in the form of pellets or mirrors, or the pellets may be ground or used as a powder polishing slurry 34. Therefore, the mixing unit 30 is the only example of various equipment structures that can reconstitute the dry granular solid composition of the present invention. w 入 '月 （In the reorganization method carried out with the conventional example, the mixing tank 36 is filled with deionized water 32, off _42 and on _. It is intended to be used for a single charge. // (,, .. heart water Or, water can be used to recombine the cycle time and slowly add a trick. Mountain and soil, a small part of the water is introduced into the mix, then the reorganization is started to start the rotor stator 38. At the dry rate Into the water, a certain amount! ... Under the speed sheep, hunted by the powder feeder, 'Carcass composition 34 leads into the circulation line 47. Polish the side and combine the pulp --------- -------, 玎 ----- (Please read the notes on the back before filling out this page) W scale applies -13- Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs ^ 16989 A7 —___ B7 5 , ^^ --- 11 The circulation system through the circulation line 47 is continued until the required polishing slurry concentration and viscosity are obtained. The detection system 50 continuously analyzes the physical properties and chemical properties of the polishing slurry, such as the percentage of solid I, and ρΗ, etc. Although the detection system shown is not connected to the mixing tank 36, the detection function can also be performed at a certain point of the circulation line 47. The polishing slurry of the product is closed by the rotor stator 38 and the valve 4 2 is opened to convey a predetermined amount of the reorganized polishing slurry through the filter system 40. Depending on the specific application, the reorganized polishing slurry is delivered to the sun trough, or directly To the mouthpiece of the polishing device. In another alternative embodiment, the tank can be used as a mixing and dispersing state. During the polishing slurry transport, the recombination pump 46 can be kept active, for example, by preventing the solids in the mixing tank 36 from settling, In order to maintain the consistency of the polishing slurry. After polishing the slurry, the valve 42 is closed, and water is washed through the mixing tank 36 and the circulation & line 47. After that, the drain valve 52 is opened, and the contents of the mixing tank 36 and the circulation pipeline are flushed. To the drain. Using the current method of aqueous polishing slurry, if the polishing slurry is a dual-group wound system, the components containing solids generally need to be mixed in advance, so that the solids are dispersed in In the container. If this action is not performed, the weight percentage of solids in the final mixture is incorrect. Similarly, the second component of Sun should be pre-mixed in order to transport it to the day tank or polishing system. First homogenize the solution. In addition to metering water in a partially concentrated system, these two components usually require some type of metering, or by weight or by bones. This composition needs to be processed to do so. Remove any contaminants. In the present invention, 軚 Jia series does not need to be mixed in advance, because it does not involve sedimentation or stability issues. It is better to introduce pre-packaged dry via powder feed 48-14. This paper size applies to China Standard (CNS) M specifications (210X297 public envy) -------- 0 · ^ ------ 1T ----- (Please read the precautions on the back before filling this page) 516989 A7 B7 V. Description of the invention (12 Dry granular solid composition. Or envy Fei S dry I granule solid composition weight (or Chu Sheng "go to w 14 ,," work% for the next day and weighed in advance for each size) or poured or isolated to this --- ------ 0 · ^! (Please read the precautions on the back before filling this page) Have the correct amount of water in the mixing tank 36 and mix. In addition, other chemicals such as hydrogen peroxide and organic compounds can be added during the mixing process. : Organic compounds can include surfactants, clamps, weak acids, biocides, etc. It is true that those skilled in the art can use this technique before / / π Jin "and then describes the invention without taking any points. Therefore, the following cases of "7 gold and more than gold", and Α 丨 仲 ΠΟ Fu Maobei's crimes are only used to illustrate rather than limit the disclosure of the present invention. Example 1 is used to prepare a polishing slurry prepared for polishing copper in integrated circuit applications. The polishing slurry generally has a very short pot life under a single-component polishing slurry, while it has only a short pot life (several weeks) under a two-component polishing slurry because several components react with each other. The other component is photosensitive in liquid form. The drying of this polishing slurry is more complicated because several salts are ammonium salts and are easily decomposed by heat. The polishing slurry can be prepared into a "2x concentrate to facilitate spray-drying operations." "2x concentrates are solids and dissolved solids are each concentrated to twice the amount of polishing polymer typically used for polishing. The pre-dried polishing slurry has the following composition: • Phosphoric acid is printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs: 11.2 0/0 Scale 8 5% Persulfur Fe Record · 8 5% Organic Rotten Rice Inhibitor: 0.3% Dioxide鈇 9.9% DI water balance -15- This paper size applies to Chinese National Standard (CNS) A4 specification (210X297 mm) 516989 A7 B7 V. Description of the invention (u) I 〇 This component is mixed, using Hill rotor stator mixer The temperature dispersed into the tank increased by about 10 ° C. Within about three days, part of the mixture was spray-dried in an APV laboratory spray dryer with an electric air heater, a rotary atomizer, and a screw feed pump with a variable speed motor. Collect the dried powder from the bottom of the dryer and cyclone. The atomizer is adjusted to prevent the product from sticking to the side wall of the dryer. The inlet air temperature and feed rate are adjusted to obtain an outlet air temperature of about 80 ° C to about 85 ° C. The powder is sealed in a plastic bag for further processing. The rest of the polishing slurry is stored in liquid form in sealed containers for further processing. The detailed series of spray-drying tests are shown in Table 1 below. The test was performed using different dryer conditions. Table 1 Test inlet temperature (.o outlet temperature (.o) feed rate (ml / min) atomizer speed (rpm) I 250-260 80-85 130 49000 II 180-185 80-85 65 41000 Central standard of the Ministry of Economic Affairs Printed by the Bureau's Consumer Cooperative (please read the precautions on the back before filling out this page). The two tests indicate that the two different inlet temperatures of the dryer are operated to determine whether the inlet temperature has any effect on the decomposition of volatile or thermosensitive components. It is found that there is no statistically significant difference between the powder physical properties of two inlet temperatures or the polishing performance of the reconstituted polishing slurry. The results of the physical properties of the polishing slurry are also shown in Table 2 below. The following examples use reorganization test I and Test II Polishing test of powder. The method for detecting usability of the present invention is the analysis and determination of the main active ingredient-ammonium persulfate-in the polishing slurry. This component is sensitive to heat and light at the same time in a water-containing state. The two types of dry polishing slurry and their analyzed concentrates were analyzed one week after spray drying. The series of results are shown in Table 2 below. So-16- This paper size applies to Chinese national standards (CNS) A4 size (210X 297 mm)

~~~ Τ ~~ 7 ~~~~; -— The data listed in Table 2 shows that spray-drying is the least retained ^ 516989 V. Description of the invention (the concentrations are all concentrations that are immediately available— " Liquid Concentrate for 10 Days — Calculate / make * 1 Do not 疋 效果 the effect of chemical components 0 P so that within 10 days, a single part of polishing slurry should be oxidized components, peroxic acid, pour sulfuric acid The strength of the ammonium foot is still reduced. From the data in Table 2, it can be seen that the persulfate concentrate does not change with the increase of the mouth temperature, but actually maintains the state it needs in the original composition. The particle sizes of the two dry particles are actually Return to its state before the drying operation. A comparison of the particle size distributions of the pre-dried concentrate and two reconstituted test polishing slurries is shown in Figure 4. These three materials are very close, so the three distributions appear to be the same TT week after spray-drying, the polishing test and copper polishing slurry dry polishing slurry sample test were performed on the pre-dried polishing slurry concentrate. The final concentration of the three polishing slurry was adjusted to the following levels: .----- -ίτ ----- ^ w, (Please read the notes on the back before filling in this ) Phosphoric acid printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs: Ammonium phosphate persulfate according to: Organic rot silver inhibits titanium dioxide deionized water agent 5.6% 4.3% 4.3% 0.15% 4.9% balance-17 This paper is in accordance with Chinese national standards ( CNS) A4 specification (210X297 mm) 516989 A7 B7 V. Description of the invention (u) 15 Measure out the sprayed polishing slurry to obtain the aforementioned concentration and disperse it in the Hill rotor stator mixer until d T is 10 ° C The remaining six-week-long concentration polishing slurry was diluted with about 1 part of concentrate to 1 part of water to obtain the actual concentration mentioned above, and mixed using a propeller mixer. All polishing slurry was filtered through a 1 micron bag filter. Six inches in diameter Copper film wafers were polished using the Strasbaugh 6EC wafer polisher (Strasbaugh, San Luis Obispo, CA) with each of the three polishing slurries under the same polishing parameters. The SiO2 film wafers were also polished for copper and silicon dioxide A relative polishing rate known as oxide selectivity was established. The results of these tests are shown in Table 3. The polishing rate is shown in Angstroms per minute (A / min): _ Table 3 ---- i -1--- --- Order (please read the precautions on the back before filling this page) Polishing slurry source Pre-dried concentrate diluted to use the reconstituted polishing slurry sprayed with concentration # 1 Copper removal rate 2200 A / min 7049 A / min for oxidation Choice of materials Ί 26: 1 Cu: oxide rate 63: 1 Cu: oxide rate-The typical removal rate of copper polishing pastes printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs is 6000 to 7000 A / min . The six-week long concentrate was significantly damaged in the case of a single component mixture. The spray-dried material retains the characteristics of a commercially available two-part polishing slurry. Example 2 The second single spray-dried material of thistle test II was tested in a copper crystal round polishing control at nine weeks after drying. This test was used as a comparison between the reorganized test π material and the freshly mixed copper polishing slurry. This polishing is performed in substantially the same manner as the foregoing. The concentration of the two polishing slurries was adjusted to the aforementioned concentration. The series of results of the polishing test are shown in Table 4 below: f -18- This paper is based on the national standard (CNS) A4 specification (516989 A7 B7 of the paper) 5. Description of the invention (16

New = dry reorganized polishing slurry Table 4 Copper removal rate 6100 A / min 6600 A / min Sex ratio 3 ratio 6: 1 Cu: Oxygen 6: 1 Cu: Oxide rate is also studied for these wafers Surface gloss. The surface scraping between the two polishing slurries is obviously different. Example 3 This test was performed using a Niro Mobile Minor (R) -type spray dryer. This operation is performed in the same manner as in the previous embodiment. The polish used in this test was used to polish tungsten. The polishing slurry used in this test is a ready-to-use formulation with the following ingredients: 3% tribasic acid, 0.3% oxidizing component, 6% abrasive, 9% deionized water, and a concentrate of this polishing slurry for preparation. Spray dry, and; Chen degree has doubled. The concentrate was spray-dried at several temperatures that allowed the chemical and abrasive components to exit, to measure the degree of degradation of the carboxylic acid component, if any. The outlet temperature was changed by changing the feed rate of the concentrate and keeping all other parameters constant. Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs This dry flowable powder is reconstituted into the aforementioned even-throwable polishing slurry composition for polishing wafers and thermal oxide film wafers. Part of the original concentrate used to make the powder is also diluted to a ready-to-use concentration, and as a baseline -19- This paper size applies the Chinese National Standard (CNS) Α4 specification (2ί0 × 297 mm) 516989 Staff Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs Printing A7 V. Description of Invention () 17. The following Table 6 shows the results of spray drying and polishing tests: Table 5 Crane speed vs. oxide depletion; M: Concentrate diluted 2344 A / min 416: 1 diluted from spray drying process " " " " " ^ Freshly prepared polishing slurry 2177 A / min 3 86ΤΪ ~ ^ ---- ^ Reconstituted spray-dried powder 2328 A / min ~ 3ΐ ^ ΤΓ ~ Microscope inspection of the surface of a oxide film wafer after polishing shows any There was no difference in scraping between test wafers. Example 4 Several tests were performed using a standard mixing process and the same polishing composition prepared by the present invention to compare the polishing activity of a conventionally prepared Yan polishing composition (called w 2000 "). The polished wafers were measured for Film removal rate, selectivity, surface roughness, and defect formation. A set of 200 mm test wafers, each with 5000 angstroms, covering the surface of the wafer with a sufficient thermal oxide base layer, and 500 angstroms of titanium nitride were known. The layer is 8000 angstrom tungsten layer isolated from thermal oxide. When preparing wafers for the test group, the polishing pad IC-1400 K of Rodel, Inc. (Newark, DE) was equipped with Rare Eanh Sciences,

Inc. (from Newark, DE, Newark, DE). Strasbaugh 6DS_sp polishing system for four-inch processing grid < platen. To process the pad, rinse with deionized DI water for ten times before processing, and then process two simulated oxide wafers into two simulated tungsten wafers. After the pad was initially processed, a set of 13 200 mm test wafers was polished. 3 4 The inspection system uses a conventional preparation of polishing slurry to polish a set of four control test wafers, and then uses a polishing slurry reconstituted according to the present invention to polish a set of five pieces. -20-This paper size applies to Chinese National Standard (CNS) A4 Specifications (21〇xl ^ i ^ --------- 0 · ^ —----- IT ----- (Please read the precautions on the back before filling this page) 516989 A7 B7 18 5 The invention is carried out on test wafers. Finally, a second set of four control test wafers is polished using a conventionally prepared polishing slurry. To help determine that the polishing slurry on the surface of the polishing pad will not be carried from one group to the next, Two simulated oxides were processed between the successive groups. The following polishing pad treatment and polishing conditions were used in each test: Polishing: downward force: 7 pieces per square inch 忖 back pressure: 0 pounds per square inch platen Speed: 60 rpm Carrier speed: 60 rpm Temperature: 100 F The test results are listed in Table 6 below. Tox film removal rate (please read the precautions on the back before filling this page). Polishing pad treatment: down Force: 14 碡 Cleaning: 2 (after DI water) Platen speed: 70 rpm Disk speed: 75 rpm RR It is tungsten (W), titanium (Ti), and oxygen expressed in Angstroms per minute. The removal rate of the thin film layer is measured using a SM-300 thin film measurement tool (KLA_Tencor, Frem nt 'CA). Brother' a The average removal rate series of the second, second, and second test wafers are shown in the columns labeled Avg.W, Avg Ti, and Avg Tox. The test wafers marked with "-Recon" are reconstituted using the present invention The polishing slurry was polished, while the remaining test wafers were polished using conventional polishing slurry. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economy Table 6 Polishing slurry RRW Avg W RR Ti Avg Ti RR Tox Avg Tox MSW2000 2108 110 MSW2000 2312 109 MSW2000 2212 275 112 MSW2000 2338 2243 277 276 102 108 MSW2000 -Recon 2176 102 MSW2000 -Recon 2183 115 21-This paper size is applicable to Chinese National Standard (CNS) A4 (210X297 mm) 516989 7 Β V. Description of the invention (19) MSW2000-Recon 2193 120 MSW2000 -Recon 2201 334 120 MSW2000 -Recon 2286 2208 361 348 114 MSW2000 2266 119 MSW2000 2280 118 MSW2000 2306 297 119 MSW2000 233 1 2296 305 301 123 120 To determine any differences in surface roughness characteristics between conventional and reconstituted polishing slurries, six test wafers were coated with silicon dioxide using tetraethylorthosilane (TEOS) deposition and then polished. This test method is the same as the foregoing. After each test, an atomic force microscope (Model 5000, Digital Instruments, Inc., Sant a Barbara, CA) was used to perform the surface sugar test. Table 7 below lists the roughness 値, where “Rms” is the root mean square 値 of the surface, measured in nanometers: ----------- (Please read the precautions on the back before filling This page) Order Table 7 Polishing paste Rms (nm) MSW2000 0.530 MSW2000 0.542 MSW2000-Recon 0.537 MSW2000-Recon 0.600 MSW2000 0.526 MSW2000 0.558 The removal rate data listed in Table 6 and the surface roughness data listed in Table 7 are displayed. There is no significant difference in the polishing performance between the reorganized polishing slurry printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs and the conventional polishing slurry. Therefore, it has been apparent that a polishing method using a reconstituted dry particle polishing composition which completely provides the aforementioned advantages has been disclosed. Although the foregoing embodiment records the application of the chemical mechanical polishing slurry of the present invention to integrated circuits, the present invention can still be applied to other types of formulations. For example, many papers containing abrasives and chemicals-22- This paper is sized to the Chinese National Standard (CNS) A4 specification (210 × 297 mm) 516989 A7 B7 V. Description of the invention (2) Product 1 is used to provide a higher removal rate Or a specific surface condition-the polishing preparation can be dried in the same way and reconstituted when used. Grinding slurries are used for polishing special optical instruments, polishing semiconductor substrates such as sec and gallium arsenide, plastic lenses and contact lenses, and other similar technologies. Therefore, all such changes and modifications are included in the scope of patent applications and their equivalents. -------- Awl 1T (Please read the notes on the back before filling out this page) Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs-23- This paper size applies to China National Standard (CNS) A4 specifications ( 210X297 mm)

Claims (1)

A polishing method, which includes the following steps: (Please read the precautions on the back before filling out this page) Provide a predetermined number of work pieces: k dry solid composition for granules; and dry granules with a weight of 1 The solid composition is formed to form an aqueous composition in an amount substantially sufficient to polish the predetermined number of working pieces. Mouth • The polishing method as described in the first patent application scope, which further includes analyzing at least one physical property and chemical property of the water-containing composition. For example, the polishing method of item 1 in the scope of patent application, wherein providing a dry polishing composition includes a package providing a dry granular solid composition, which has a dry granular solid combination containing substantially enough to complete the polishing of the predetermined number of work pieces. Thing. 4. The polishing method according to item 1 of the application, wherein providing a predetermined number of work pieces includes providing a work piece. 5. The polishing method according to item 1 of the patent application scope, further comprising polishing a predetermined number of work pieces using an aqueous composition. 6. The polishing method according to item 5 of the patent application scope, further comprising storing the aqueous composition in a storage device before polishing the pre-filled number of work pieces. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs7. For the polishing method in the scope of patent application item 5, wherein polishing the predetermined number of work pieces additionally includes providing a batch polishing device and placing a batch of work pieces in the Polishing device. 8. The polishing method according to item 7 of the patent application, wherein providing a predetermined number of work pieces includes providing a batch of work pieces. -24- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 516989 2. Application for patent scope The polishing method as described in item 8 of the patent application scope, wherein the reorganization of a specific amount of dry granular solid composition includes reorganization of a dry granular solid composition in an amount sufficient to polish a batch of working pieces. Lishen calls the polishing method of item 1 of the patent, wherein providing a predetermined number of working pieces includes providing a predetermined number of semiconductor substrates. 'Such as the polishing method of item 1 of the patent scope, which further includes providing a polishing device having a consumption rate of polishing slurry per work piece, wherein the content is exactly 1 疋 to complete the drying of the predetermined number of work pieces. Reconstituting a particulate solid limb composition into an aqueous composition includes reconstituting a quantity of dry particulate I solid composition into an aqueous composition at a rate substantially equal to the rate of polishing slurry consumption of each work piece. 12. A polishing method comprising the steps of: drying a granular solid composition for use in a polishing method; determining a fixed number of work pieces to be polished; and preparing a quantity of dried granular solid composition in an amount A reconstituted polishing slurry in an amount sufficient to form a polished amount of the work piece. Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 13. The polishing method of item 12 in the scope of patent application, wherein the step of preparing a quantity of dry granular solid composition includes providing a volume sufficient to hold dry particles sufficient to polish a work piece A package of a solid composition, and the package is filled with a dry granular solid composition. • The polishing method according to item 12 of the patent application scope, which further includes providing a polishing device having several positions on the reduction device workstation, and providing step-by-step quantities of the dry granular solid composition, including providing a volume sufficient to hold -25-516989 A8 B8 C8 D8 sufficient to polish-batch the dry granular solid composition Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, patent application package, and filling the package with the dry granular solid composition. is. The polishing method according to item 12 of the patent application scope, which further comprises recombining the dry granular solid composition to form a water-containing composition, and polishing a fixed number of working pieces using the present water composition. 16. The polishing method of item 15 in the patent, which further includes filtering the aqueous composition before polishing a sufficient number of work pieces. 17. A polishing method comprising the steps of: supplying a dry particulate solid composition; reconstituting a dry particulate solid composition in an amount sufficient to form an amount of an aqueous composition; adding a material selected from the group consisting of hydrogen peroxide and volatile organic acids A group of chemicals in the aqueous composition; and the aqueous composition is transferred to a workstation of a polishing apparatus. 18. The polishing method according to item 17 of the scope of patent application, wherein the step of providing a dry solid composition comprises the following steps: forming a dry powder of the granular solid composition; collecting the dry powder in a storage hopper to obtain Large batches; blending the dry powder to homogenize the powder; and packaging the dry powder. 19. The polishing method according to item 18 of the patent application scope, wherein the step of packaging the dried powder includes providing a package of a volume sufficient to hold a polished dry granular solid composition sufficient to complete a predetermined number of pieces, and in the package Fill with dry powder. 20. The polishing method according to item 17 of the scope of patent application, in which the aqueous composition is used in granular powder (please read the precautions on the back before filling this page) r-pack -------- order ---- -# 26- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 516989 The steps of applying for a patent to be rotated to the workstation of the polishing device include providing a polishing device having a consumption rate of polishing slurry for each film foot, at a speed that is substantially equal to the consumption rate of polishing slurry for each work piece ... Work station of the polishing device. Suyangxia 'Transporting Water-containing Group Outline (please read the phonetic notes on the back before filling this page) i Binding ------- Wisdom Discussion of the Ministry of Economic Affairs: 一 ί, Γ -27- This paper size applies to China Standard (CNS) A4 size (210 x 妁 7 mm)