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CN-122006615-A - Low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system

CN122006615ACN 122006615 ACN122006615 ACN 122006615ACN-122006615-A

Abstract

The invention provides a low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system, which relates to the technical field of iminodiacetic acid preparation, integrates in-situ induction complexing, supergravity sedimentation, nano gradient screening units and a developing line cleaning coupling module, peels off a nickel ion solvation layer through a high-frequency cavitation generator, generates a nickel complexing precursor by matching with a functional filler layer, utilizes a horizontal asymmetric rotary drum to generate a supergravity field of not less than 3000g to realize liquid-solid forced separation, adopts a multilayer ceramic composite membrane with the aperture of decreasing from 1 mu m to 5nm to match with a self-assembled monomolecular membrane to carry out physical interception and chemical adsorption double refining, and is matched with on-line quality monitoring and self-adaptive reflux logic to ensure that the concentration of nickel ions in a produced liquid is stably maintained at an extremely low level of not more than 10ppb, effectively solves the problems of low nickel reactivity in extremely dilute solution, difficult separation of colloid impurities, metal precipitation of equipment and the like, and provides purity for a semi-conductive advanced process.

Inventors

  • YAN CHAO
  • LI JUAN

Assignees

  • 湖北倍思电子材料有限公司

Dates

Publication Date
20260512
Application Date
20260129

Claims (9)

  1. 1. The low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system is characterized in that: the refining system comprises an in-situ induction complexing unit, a supergravity settling unit, a nano gradient screening unit and a developing line cleaning coupling module, wherein: The in-situ complexing reaction unit is internally provided with a high-frequency cavitation generator and a functionalized filler layer with molecular recognition characteristics, and is used for injecting a complexing agent into an iminodiacetic acid system and inducing to generate an insoluble nickel complexing center; The feeding end of the supergravity sedimentation unit is communicated with the in-situ complexing reaction unit, the supergravity sedimentation unit adopts a horizontal asymmetric rotary drum structure, and the forced sedimentation and liquid phase separation of the nickel complexing center are realized by utilizing a generated centrifugal force field; the nanoscale gradient screening unit is connected with the liquid phase output end of the supergravity sedimentation unit through a pipeline, and the inside of the nanoscale gradient screening unit is provided with a pore diameter meter Decreasing to Is a multi-layer ceramic composite film layer; And the feed end of the developing line cleaning module receives the produced liquid of the nanoscale gradient screening unit and is used for conveying the refined iminodiacetic acid to a semiconductor developing cleaning line.
  2. 2. The low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system of claim 1, wherein the ultrasonic frequency of the high-frequency cavitation generator is 4kHz to 120kHz, and the high-frequency cavitation generator is used for generating micro-turbulence cavitation nuclei in iminodiacetic acid solution and improving the collision frequency of nickel ions and complexing agents.
  3. 3. The low nickel system in situ complexing electronic grade iminodiacetic acid refining system of claim 1, wherein the substrate of the functionalized filler layer is a perfluoropolymer particle, and the surface is grafted with a polyamine carboxylic acid type functional molecule with high selectivity to nickel ions.
  4. 4. The low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system of claim 1, wherein the inner wall of the rotary drum of the supergravity settling unit is lined with a high-density polytetrafluoroethylene layer, and the rotating speed of the rotary drum is adjustable to form centrifugal acceleration not lower than 3000 g.
  5. 5. The system for refining low-nickel system in-situ complexing electronic grade iminodiacetic acid of claim 1, wherein a self-assembled monomolecular film is arranged on the surface of the film layer of the nanoscale gradient screening unit, and the terminal group of the monomolecular film and the insoluble nickel complexing center have space complementary structures.
  6. 6. The low nickel system in situ complexing electronic grade iminodiacetic acid refining system of claim 1, further comprising an on-line mass monitoring unit comprising a high sensitivity inductively coupled plasma mass spectrometer interface and a laser particle counter.
  7. 7. The low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system of claim 1, wherein all pipelines, pump bodies and valve linings in contact with materials in the refining system are made of perfluoroalkoxy resin.
  8. 8. The refining process of the low nickel system in-situ complexing electronic grade iminodiacetic acid refining system as set forth in any one of claims 1 to 7, wherein the refining process comprises the following steps: sp1, pumping the iminodiacetic acid solution to be refined into an in-situ complexing reaction unit, starting a high-frequency cavitation generator, and continuously injecting an organic sulfur complexing agent according to a stoichiometric ratio of 1.5 to 3 times of the content of nickel impurities; Sp2, carrying out preliminary heterogeneous complexation reaction on the material when the material passes through the functionalized filler layer to form a submicron-level nickel complexation precursor; sp3, delivering the mixed solution into a hypergravity settling unit, and realizing centrifugal settling of solid phase particles and continuous deslagging under the high-speed rotation condition; sp4, separating clear liquid, and grading and intercepting the clear liquid with a interception diameter larger than that of the nano-grade gradient screening unit through a multilayer ceramic composite membrane Residual complexing molecular clusters of (2); Sp5, the nickel ion concentration is detected to be qualified And (3) conveying the refined liquid with the concentration of 10ppb to a developing line cleaning module for cleaning operation, and triggering a reflux logic to return to Sp1 if the concentration of nickel ions is higher than 10 ppb.
  9. 9. The refining process of the low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system of claim 8, wherein in Sp4, when the inlet-outlet pressure difference of the nano gradient screening unit exceeds 0.2MPa, the system automatically starts a high-pressure pulse back flushing program.

Description

Low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system Technical Field The invention relates to the technical field of iminodiacetic acid preparation, in particular to a low-nickel system in-situ complexing electronic-grade iminodiacetic acid refining system. Background In the manufacturing process of semiconductor integrated circuits, electronic grade iminodiacetic acid (IDA) is used as a key high-purity chemical product, is widely applied to wafer surface cleaning operation after development, the purity level of the electronic grade iminodiacetic acid is directly related to the microcosmic cleanliness of the wafer surface and the electrical property of a final chip, and as the semiconductor industry enters the era of nano-scale process, the limit requirement of the process on key metal impurities, especially nickel (Ni) ions, is severe to below 10ppb, and because iminodiacetic acid molecules have extremely strong coordination capability, the iminodiacetic acid molecules are extremely easy to combine with trace nickel in equipment or environment in the actual production and reflow cycle process to form a complex system which is extremely difficult to remove, so that extremely high technical challenges are presented to the refining process. The traditional refining scheme usually adopts ion exchange resin, chemical precipitation or conventional precise filtration technology, however, the prior art has obvious problems in practical application that trace nickel ions are surrounded by a stable solvation water layer under the order of 10ppb, so that the effective collision probability with a complexing agent is extremely low, the reaction kinetics is extremely slow, meanwhile, nickel complexes generated under extremely low concentration often exist in a sol or micro-nano cluster form, conventional filter media are extremely easy to penetrate or intercept failure caused by surface tension, thorough separation is difficult to realize, and in addition, due to extremely easy trace precipitation of metal parts of the filter equipment in an IDA (integrated digital assistant) which is a strong coordination system, a pollution cycle of 'edge removal and edge dyeing' is formed, and the prior art system mostly adopts an open-circuit mode, lacks self-adaptive adjustment capability for the fluctuation of a back flow load of a development line, and is difficult to maintain stable limit purity output. Disclosure of Invention Technical problem to be solved Aiming at the defects of the prior art, the invention provides a low-nickel system in-situ complexing electronic grade iminodiacetic acid refining system, which solves the technical problems existing in the prior art. Technical proposal The invention is realized by the following technical scheme that the low nickel system in-situ complexing electronic grade iminodiacetic acid refining system comprises an in-situ induction complexing unit, a supergravity settling unit, a nano gradient screening unit and a developing line cleaning coupling module, wherein: The in-situ complexing reaction unit is internally provided with a high-frequency cavitation generator and a functionalized filler layer with molecular recognition characteristics, and is used for injecting a complexing agent into an iminodiacetic acid system and inducing to generate an insoluble nickel complexing center; The feeding end of the supergravity sedimentation unit is communicated with the in-situ complexing reaction unit, the supergravity sedimentation unit adopts a horizontal asymmetric rotary drum structure, and the forced sedimentation and liquid phase separation of the nickel complexing center are realized by utilizing a generated centrifugal force field; the nanoscale gradient screening unit is connected with the liquid phase output end of the supergravity sedimentation unit through a pipeline, and the inside of the nanoscale gradient screening unit is provided with a pore diameter meter Decreasing toIs a multi-layer ceramic composite film layer; And the feed end of the developing line cleaning module receives the produced liquid of the nanoscale gradient screening unit and is used for conveying the refined iminodiacetic acid to a semiconductor developing cleaning line. Preferably, the ultrasonic frequency of the high-frequency cavitation generator is 4kHz to 120kHz, and the high-frequency cavitation generator is used for generating micro-turbulence cavitation nuclei in iminodiacetic acid solution and improving the collision frequency of nickel ions and complexing agents. Preferably, the substrate of the functionalized filler layer is a perfluoropolymer particle, and the surface is grafted with a polyamine carboxylic acid type functional molecule having high selectivity to nickel ions. Preferably, the inner wall of the rotary drum of the supergravity sedimentation unit is lined with a high-density polytetrafluoroethylene layer, and the rotating speed of the rotary drum is