CN101451045B - Process for preparing chemico-mechanical polishing liquid - Google Patents

Abstract

The present invention discloses a process for preparing chemical and mechanical polishing liquid, which comprises the following steps: grouping the components of the chemical and mechanical polishing liquid according to working mechanisms, functions and chemical or physical properties; respectively mixing the components of each group in parallel so as to obtain each intermediate premixing product; carrying out quality control tests on the intermediate premixing products; and mixing the intermediate premixing products after all the intermediate premixing products are tested to be qualified, and obtaining the chemical and mechanical polishing liquid. The preparing process has the advantages for shortening the process flow time of large-scale production, greatly improving productivity, reducing production cost, increasing the quality control point of the process flow, improving quality control level, greatly improving product quality guarantee and reducing the risk of production quality accidents, so that the preparing process has obvious economic values.

Description

A kind of preparation technology of chemical mechanical polishing liquid

Technical field

The present invention relates to a kind of preparation technology of chemical mechanical polishing liquid.

Background technology

Along with the development of microelectric technique, the integrated level of very large scale integration chip has reached tens components and parts, and characteristic size has entered nanoscale.This just requires hundreds of procedure, especially multilayer wiring, substrate, medium in microelectronic technique must pass through chemical-mechanical planarization (CMP).Chemical mechanical polishing liquid can optionally promote the removal of particular semiconductor surfacing, conventional chemical mechanical polishing liquid comprises abrasive grains and various chemical additive, for example grinding rate elevator, corrosion inhibitor, oxidant, acidity-basicity regulator and carrier.

At present, what the preparation of chemical mechanical polishing liquid was mainly adopted is on a small scale, the reinforced preparation method of inefficient sequence type, and its flow process is: in a reaction vessel, by feeding tube (mouth), required component is added in order successively.All finish and mix the sampling and measuring that qualifying point is carried out at the rear reinforced, as pH, concentration, LPC and ICP etc.Need in this technical process to use: 1) multiple measuring equipment, on-ground weigher as gentle in the sky; 2) complicated pipeline pipeline valve and control system thereof; 3) various delivery pumps.Usually, the measuring accuracy of these industrial equipments is lower, and applied load is larger, so easily make a mistake or use error.And the chemical mechanical polishing liquid that uses as semicon industry is often to the concentration of component, quality etc. require very high, and raw material is usually more expensive, and institute thinks and avoids occuring quality accident, usually adopts the reinforced mixing preparation method of safer sequence type to avoid the generation of this type of accident.

This preparation technology's shortcoming is also apparent: 1) process time is long: the whole production cycle is the cumulative of all operations flow time, and efficient is lower, can cause the production line production capacity low; 2) control of product quality has a big risk: do not insert clear and definite effectively quality control method in the technological process process, if any one walk out of existing error or the misoperation meeting causes whole subsequent technique flow process to become idle work in technical process.Whether qualified product, except controlling all one pack system material qualities, relies on the detection of final stage fully, is the entirely passive type operation.Therefore, from cost and efficient aspect, overcome this problem in the urgent need to a kind of new preparation technology.

Summary of the invention

Technical problem to be solved by this invention be for the preparation technology's production cycle that overcomes existing chemical mechanical polishing liquid long, efficient is low, the defective that control of product quality has a big risk, and a kind of preparation technology of new chemical mechanical polishing liquid is provided.

The preparation technology of chemical mechanical polishing liquid of the present invention is: each composition of chemical mechanical polishing liquid is divided into groups by its working mechanism, function, chemistry or physical property, the parallel composition with every group mixes respectively, obtain each middle pre-composition, middle pre-composition is carried out the quality control test, after all middle pre-composition detection is qualified, mix, make chemical mechanical polishing liquid.

Wherein, described quality control test can be the quality control test to pH, concentration, solid content, total number of particles detection and trace metal ion content detection.

Wherein, described grouping better for being divided into 2～5 groups, better for being divided into 3 or 4 groups.

Chemical mechanical polishing liquid generally includes component: abrasive grains, fluid mechanics controlling agent, surfactant, complexing agent, bactericide, pH adjusting agent and corrosion inhibiter etc.Wherein, abrasive grains is the main mechanical abrasive action that rises in CMP (Chemical Mechanical Polishing) process, is generally the aqueous solution of higher concentration.Can dilute the stability that its concentration keeps abrasive grains colloidal solution by deionized water.The fluid mechanics controlling agent is for controlling polishing fluid fluid mechanics state in CMP (Chemical Mechanical Polishing) process, being generally the aqueous solution.Surfactant is to increase the cleaning effect of polishing fluid for CMP (Chemical Mechanical Polishing) process, is generally macromolecular compound solution.Complexing agent is to grind for complexing the metal ion that gets off, is generally macromolecular compound solution.Corrosion inhibiter is be used to preventing excessive electrochemical corrosion, as the aqueous solution of BTA (BTA).PH adjusting agent be for the pH value of regulating chemical mechanical polishing liquid to the optimum scope, the aqueous solution of acid or alkali normally.Bactericide is for preventing that thereby chemical mechanical polishing liquid from generating bacterium and affecting its quality and performance, is generally macromolecular compound solution.

In preferred embodiments of the present invention, divide into groups by following scheme:

Middle pre-composition 1: abrasive grains and water.Middle pre-composition 1 needs use after total number of particles detection (LPC), pH and solid content detection are qualified.

Middle pre-composition 2: fluid mechanics controlling agent and water.Middle pre-composition 2 needs to use after concentration, total number of particles detection and trace metal ion content detection are qualified.Also abrasive grains, water and fluid mechanics controlling agent can be mixed as a middle pre-composition.

Middle pre-composition 3: one or more in surfactant, complexing agent, corrosion inhibiter and bactericide, and water and pH value conditioning agent.Due to the mentioned component chemistry, physical property is all gentleer, not conflict mutually, and the content of these components in chemical mechanical polishing liquid is few, concentration is low, causes operate miss for avoiding these low content components to add separately, so these components are mixed separately as middle pre-composition 3.Middle pre-composition needs to use after concentration, pH, total number of particles detection and trace metal ion content detection are qualified.Also corrosion inhibiter can be proposed separately as one independently in the middle of pre-composition, the operation when this is particularly useful for using mixed inhibitor.

Middle pre-composition 4:pH value conditioning agent.Particularity due to chemical-mechanical grinding liquid, its pH value requires comparatively accurate usually, excursion is less, may be consuming time longer in practical adjustments, so better is divided into two parts with pH value conditioning agent, in the middle of a part is added to, in pre-composition 3, remainder is directly used in final polishing fluid pH to be worth regulating, this two-part mass ratio normally 60～80%: 20～40%.Also all pH adjusting agents can be mixed with surfactant, complexing agent, corrosion inhibiter and bactericide, not get separately the part pH adjusting agent as a middle pre-composition.

In the present invention, described water is deionized water.

Positive progressive effect of the present invention is:

1. adopt the parallelization technological process to substitute sequence type technological process far away, greatly the shortened process time, enhance productivity and production capacity, reduce production costs, improve product competitiveness.

2. each the middle pre-composition for preparation after grouping increases qualifying point, as pH, and concentration, LPC and ICP etc.Pre-compositions can be used for the mixing of final chemical mechanical polishing liquid finished product in qualified rear after testing in the middle of all, greatly increase the technological process qualifying point and improved quality control level, the product quality guarantee is greatly improved, and reduces quality of production accident risk.

Description of drawings

Fig. 1 is the production equipment schematic diagram that the present invention prepares polishing fluid.

Embodiment

Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.

The preparation technology of 1 one kinds of copper barrier layer chemical mechanical polishing liquids of embodiment

1. instrument and equipment list:

Production line pipeline equipment: comprise the finished product blending tank, middle pre-composition blending tank, material solution preparation tank, raw material process pipeline, delivery pump, blender, pure water supply line, metering (weighing), control instrument and corresponding electrical apparatus control system etc.

Quality analysis checkout equipment: total number of particles checkout equipment: PSS780, Rion KF-28B; Trace metal ion content detection equipment: Perkin Elmer ICP2100DV; Concentration detection device: Waters 1525HPLC; PH meter: Mettler Toledo SevenMulti pH meter.

2. preparation technology:

1) confirm that all raw materials are qualified after testing, put in place; Check and proofread and correct measuring equipment, production equipment, pure water supply system guarantees that it meets operating specification and requirement;

2) pre-composition 1 in the middle of: add 1470 kilograms of silicon dioxide abrasive grains and 1445 kilograms of pure water through feeding system in the finished product blending tank, and be opened into and mix, detect (LPC), pH and solid content through total number of particles and detect after qualified stand-by;

Middle pre-composition 2: add 210 kilograms of glycerine (glycerol) in mix and blend tank 1, and add 210 kg of water, be stirred to and mix, through concentration, total number of particles detect and the trace metal ion content detection stand-by after qualified;

middle pre-composition 3: add 832 kilograms of pure water in mix and blend tank 2, be under the mixing speed of 120 rev/mins at rotating speed, add 8.4 kilograms of BTAs (BTA) to dissolving fully, and then add successively 8.4 kilograms of surfactant polyacrylic acid, 8.4 kilogram complexing agent 2-phosphonic acids butane-1, 2, 4-tricarboxylic acids (PBTC), 0.84 kilogram hundred kills to get solution (manufacturer: three rich biochemical technology (Shanghai) Co., Ltd.) and 7.56 kilograms of 20wt% salpeter solutions, be stirred to and mix, record the pH value, through concentration, total number of particles detection and trace metal ion content detection are qualified rear stand-by,

Middle pre-composition 4:1.9 kilogram 20wt% salpeter solution is stand-by.

3) in the situation that stirring is got 420 kilograms of glycerites (middle pre-composition 2) to the finished product blending tank by pump in mix and blend tank 1; In the middle of getting 864.8 kilograms by pump in mix and blend tank 2, pre-composition 3 is to the finished product blending tank.Mentioned component is pH value determination after stirring 3 hours, and is adjusted to the pH value stabilization in 3.0 ± 0.1 by about 1.9 kilograms of salpeter solutions;

4) stop stirring, upper from the finished product blending tank respectively, in, lower 3 sampling points sampling, pH value determination guarantees that system mixes, and send quality department to detect;

5) above-mentioned chemical mechanical polishing liquid finished product after each concentration of component, pH, total number of particles detection and trace metal ion content detection are qualified, is packed discharging under clean environment.

The preparation technology of 2 one kinds of copper barrier layer chemical mechanical polishing liquids of embodiment

1. instrument and equipment list:

Production line pipeline equipment: comprise the finished product blending tank, middle pre-composition blending tank, material solution preparation tank, raw material process pipeline, delivery pump, blender, pure water supply line, metering (weighing), control instrument and corresponding electrical apparatus control system etc.

Quality analysis checkout equipment: total number of particles checkout equipment: PSS780, Rion KF-28B; Trace metal ion content detection equipment: Perkin Elmer ICP2100DV; Concentration detection device: Waters 1525HPLC; PH meter: Mettler Toledo SevenMulti pH meter.

2. preparation technology:

1) confirm that all raw materials are qualified after testing, put in place; Check and proofread and correct measuring equipment, production equipment, pure water supply system guarantees that it meets operating specification and requirement;

2) pre-composition 1 in the middle of: add 210 kilograms of glycerine, 1470 kilograms of silicon dioxide abrasive grains and 1655 kilograms of pure water through feeding system in the finished product blending tank, and be opened into and mix, through concentration of component, total number of particles detects (LPC), pH and solid content and detects qualified rear stand-by;

middle pre-composition 2: add 832 kilograms of pure water in mix and blend tank 2, be under the mixing speed of 120 rev/mins at rotating speed, add 8.4 kilograms of BTAs (BTA) to dissolving fully, and then add successively 8.4 kilograms of surfactant polyacrylic acid, 8.4 kilogram 2-phosphonic acids butane-1, 2, 4-tricarboxylic acids (PBTC), 0.84 kilogram hundred kills to get solution (manufacturer: three rich biochemical technology (Shanghai) Co., Ltd.) and 5.46 kilograms of 20wt% salpeter solutions, be stirred to and mix, record the pH value, through each concentration of component, total number of particles detection and trace metal ion content detection are qualified rear stand-by,

Middle pre-composition 3:4 kilogram 20wt% salpeter solution is stand-by.

3) in the situation that stirring is got 864.8 kilograms of middle pre-compositions 2 to the finished product blending tank by pump in mix and blend tank 2.Mentioned component is pH value determination after stirring 3 hours, and is adjusted to the pH value stabilization in 3.0 ± 0.1 by about 1.9 kilograms of acid-base modifiers;

4) stop stirring, upper from the finished product blending tank respectively, in, lower 3 sampling points sampling, pH value determination guarantees that system mixes, and send quality department to detect;

5) above-mentioned chemical mechanical polishing liquid finished product after each concentration of component, pH, total number of particles detection and trace metal ion content detection are qualified, is packed discharging under clean environment.

The preparation technology of 3 one kinds of barrier layer chemical mechanical polishing liquids of embodiment

1. instrument and equipment list:

Production line pipeline equipment: comprise the finished product blending tank, middle pre-composition blending tank, material solution preparation tank, raw material process pipeline, delivery pump, blender, pure water supply line, metering (weighing), control instrument and corresponding electrical apparatus control system etc.

Quality analysis checkout equipment: total number of particles checkout equipment: PSS780, Rion KF-28B; Trace metal ion content detection equipment: Perkin Elmer ICP2100DV; Concentration detection device: Waters 1525HPLC; PH meter: Mettler Toledo SevenMulti pH meter.

2. preparation technology:

1) confirm that all raw materials are qualified after testing, put in place; Check and proofread and correct measuring equipment, production equipment, pure water supply system guarantees that it meets operating specification and requirement;

2) pre-composition 1 in the middle of: add 1610 kilograms of silicon dioxide abrasive grains and 840 kilograms of pure water through feeding system in the finished product blending tank, and be opened into and mix, detect (LPC), pH and solid content through total number of particles and detect after qualified stand-by;

Middle pre-composition 2: add 420 kilograms of glycerine (glycerol) in mix and blend tank 1, and add 420 kg of water, be stirred to and mix, through concentration, total number of particles detect and the trace metal ion content detection stand-by after qualified;

Middle pre-composition 3: add 850 kilograms of pure water in mix and blend tank 2, be under the mixing speed of 120 rev/mins at rotating speed, add 2.1 kilograms of BTAs (BTA) and 4.2 kilograms of 5-amino-tetrazoles (ATA), being stirred to fully, dissolving mixes, record the pH value, stand-by after each concentration of component, total number of particles detection and trace metal ion content detection are qualified;

Middle pre-composition 4: prepare 8.4 kilograms of surfactant polyacrylic acid, 25.2 kilogram 2-phosphonic acids butane-1,2,4-tricarboxylic acids (PBTC), 0.84 kilogram hundred kills to get solution (manufacturer: three rich biochemical technology (Shanghai) Co., Ltd.) and 0.684 kilogram of 10wt% potassium hydroxide solution, be stirred to and mix, record the pH value, through each concentration of component, total number of particles detect and the trace metal ion content detection stand-by after qualified;

Middle pre-composition 5:0.456 kilogram 20wt% salpeter solution is stand-by.

3) in the situation that stirring is got 840 kilograms of glycerites (middle pre-composition 2) to the finished product blending tank by pump in mix and blend tank 1; Middle pre-composition 4 is added in mix and blend tank 2, and after stirring, in the middle of pump is got 891.6 kilograms, the mixed solution of pre-composition 3 and middle pre-composition 4 is to the finished product blending tank.Mentioned component is pH value determination after stirring 3 hours, and is adjusted to the pH value stabilization in 2.95 ± 0.1 by about 0.34 kilogram of salpeter solution;

4) stop stirring, upper from the finished product blending tank respectively, in, lower 3 sampling points sampling, pH value determination guarantees that system mixes, and send quality department to detect;

5) above-mentioned chemical mechanical polishing liquid finished product after each concentration of component, pH, total number of particles detection and trace metal ion content detection are qualified, is packed discharging under clean environment.

The preparation technology of 4 one kinds of barrier layer chemical mechanical polishing liquids of embodiment

1. instrument and equipment list:

Production line pipeline equipment: comprise the finished product blending tank, middle pre-composition blending tank, material solution preparation tank, raw material process pipeline, delivery pump, blender, pure water supply line, metering (weighing), control instrument and corresponding electrical apparatus control system etc.

Quality analysis checkout equipment: total number of particles checkout equipment: PSS780, Rion KF-28B; Trace metal ion content detection equipment: Perkin Elmer ICP2100DV; Concentration detection device: Waters 1525HPLC; PH meter: Mettler Toledo SevenMulti pH meter.

2. preparation technology:

1) confirm that all raw materials are qualified after testing, put in place; Check and proofread and correct measuring equipment, production equipment, pure water supply system guarantees that it meets operating specification and requirement;

2) pre-composition 1 in the middle of: add 420 kilograms of glycerine, 1610 kilograms of silicon dioxide abrasive grains and 1260 kilograms of pure water through feeding system in the finished product blending tank, and be opened into and mix, through concentration, total number of particles detect, trace metal ion content and solid content detect after qualified stand-by;

middle pre-composition 2: add 850 kilograms of pure water in mix and blend tank 2, be under the mixing speed of 120 rev/mins at rotating speed, add 2.1 kilograms of BTAs (BTA) and 4.2 kilograms of 5-amino-tetrazoles (ATA) to dissolving fully, and then add successively 8.4 kilograms of surfactant polyacrylic acid, 25.2 kilogram 2-phosphonic acids butane-1, 2, 4-tricarboxylic acids (PBTC), 0.84 kilogram hundred kills to get solution (manufacturer: three rich biochemical technology (Shanghai) Co., Ltd.) and 0.3 kilogram of 10wt% potassium hydroxide solution, be stirred to and mix, record the pH value, through each concentration of component, total number of particles detection and trace metal ion content detection are qualified rear stand-by,

3) in the situation that stirring is got 891.0 kilograms of middle pre-compositions 2 to the finished product blending tank by pump in mix and blend tank 2.Mentioned component is pH value determination after stirring 3 hours, and the pH value can be stable at 2.95 ± 0.1;

4) stop stirring, upper from the finished product blending tank respectively, in, lower 3 sampling points sampling, pH value determination guarantees that system mixes, and send quality department to detect;

5) above-mentioned chemical mechanical polishing liquid finished product after each concentration of component, pH, total number of particles detection and trace metal ion content detection are qualified, is packed discharging under clean environment.

Claims (3)

1. the preparation technology of a chemical mechanical polishing liquid, it is characterized in that comprising the steps: that each composition with chemical mechanical polishing liquid divides into groups by its working mechanism, function, chemistry or physical property, the parallel composition with every group mixes respectively, obtain each middle pre-composition, middle pre-composition is carried out the quality control test, after all middle pre-composition detection is qualified, mix, make chemical mechanical polishing liquid, wherein said each composition with chemical mechanical polishing liquid is undertaken by following scheme by its working mechanism, function, chemistry or physical property grouping:

Middle pre-composition 1A: abrasive grains and water;

Middle pre-composition 2A: fluid mechanics controlling agent and water;

Middle pre-composition 3A: one or more in surfactant, complexing agent, corrosion inhibiter and bactericide, and water and pH value conditioning agent;

Middle pre-composition 4A:pH value conditioning agent; Or

Middle pre-composition 1B: fluid mechanics controlling agent, abrasive grains and water;

Middle pre-composition 2B: one or more in surfactant, complexing agent, corrosion inhibiter and bactericide, and water and pH value conditioning agent;

Middle pre-composition 3B:pH value conditioning agent; Or

Middle pre-composition 1C: abrasive grains and water;

Middle pre-composition 2C: fluid mechanics controlling agent and water;

Middle pre-composition 3C: corrosion inhibiter and water;

Middle pre-composition 4C: one or more in surfactant, complexing agent and bactericide, and water and pH value conditioning agent;

Middle pre-composition 5C:pH value conditioning agent; Or

Middle pre-composition 1D: fluid mechanics controlling agent, abrasive grains and water;

Middle pre-composition 2D: one or more in surfactant, complexing agent, corrosion inhibiter and bactericide, and water and pH value conditioning agent.

2. preparation technology as claimed in claim 1, it is characterized in that: the ratio of pH value conditioning agent in pH value conditioning agent and middle pre-composition 4A in middle pre-composition 3A, the ratio of pH value conditioning agent in pH value conditioning agent and middle pre-composition 3B in pre-composition 2B perhaps, perhaps in the pre-composition 4C of centre in pH value conditioning agent and middle pre-composition 5C the mass ratio of pH value conditioning agent be 60～80%:20～40%.

3. preparation technology as claimed in claim 1 is characterized in that: described quality control test is for detecting pH, concentration, solid content, total number of particles and the quality control test of trace metal ion content detection.

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