CN110938378B - Polishing solution for polishing oxygen surface of zinc oxide crystal and preparation method thereof - Google Patents
Polishing solution for polishing oxygen surface of zinc oxide crystal and preparation method thereof Download PDFInfo
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- CN110938378B CN110938378B CN201911012859.3A CN201911012859A CN110938378B CN 110938378 B CN110938378 B CN 110938378B CN 201911012859 A CN201911012859 A CN 201911012859A CN 110938378 B CN110938378 B CN 110938378B
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- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
The invention discloses a polishing solution for polishing an oxygen surface of a zinc oxide crystal, which comprises the following raw materials: abrasive, electrolyte, surfactant and deionized water; and adjusting the pH value of the polishing solution to 2.5-6.0 by adopting a pH regulator. The polishing solution disclosed by the invention solves the technical problems that the oxygen-containing crystal face of a zinc oxide crystal is low in polishing efficiency and an orange peel phenomenon is easy to occur on the surface; meanwhile, the polished surface has no pits and scratches, and completely meets the production requirements of the subsequent electronic components. The invention also discloses a preparation method of the polishing solution for polishing the oxygen surface of the zinc oxide crystal.
Description
Technical Field
The invention relates to the technical field of polishing materials for an oxygen surface of a zinc oxide crystal, and particularly relates to a polishing solution for polishing the oxygen surface of the zinc oxide crystal and a preparation method thereof.
Background
The development goal of modern manufacturing industry is industrial 4.0 intelligent manufacturing, the intelligent manufactured crown is ultra-precise manufacturing, and the bright bead of the ultra-precise surface crown is ultra-precise nondestructive surface processing. For example, the fabrication of very large integrated circuit chips has entered 7 nm node fabrication, and in such ultra-precise fabrication processes, the features of the devices are all at the nanometer level, approaching the human neuronal system. Without the assurance of ultra-precise surface machining, the most advanced fabrication of very large scale integrated circuit chips cannot be accomplished. At present, the polishing of the ultra-large integrated circuit chip forms a complete system from equipment, process and polishing solution, and ensures that the manufacturing technology of the ultra-large integrated circuit chip can be smoothly extended and developed.
The development of the third generation compound semiconductor material, along with 5G, clean energy, photoelectric high-efficiency conversion chips, intelligent equipment and terminal equipment industries is in the way of the different military, and the third generation compound semiconductor material will become the latest power for the development of the future industries. The zinc oxide single crystal semiconductor material is a new material with wide application scenes, wherein the new third generation compound semiconductor material has high energy band, photoelectric effect and cost advantage. However, the oxygen-containing crystal face of the zinc oxide crystal has a lower polishing efficiency than the zinc-containing crystal face, and orange peel tends to occur on the surface.
Therefore, it is urgently needed to develop a polishing solution for polishing the oxygen-containing crystal face of the third-generation semiconductor zinc oxide crystal so as to improve the polishing efficiency and the surface quality of the oxygen-containing crystal face of the zinc oxide crystal, thereby completely meeting the production requirements of the subsequent electronic components.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide the polishing solution for polishing the oxygen-containing crystal face of the zinc oxide crystal and the preparation method thereof, so as to solve the technical problems that the oxygen-containing crystal face of the zinc oxide crystal is low in polishing efficiency and the orange peel phenomenon is easy to occur on the surface; meanwhile, the polished surface has no pits and scratches, and completely meets the production requirements of the subsequent electronic components.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
the polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following raw materials: abrasive, electrolyte, surfactant and deionized water; and adjusting the pH value of the polishing solution to 2.5-6.0 by adopting a pH regulator.
Preferably, the raw materials comprise the following components in percentage by mass in the polishing solution: 0.1 wt% -40 wt% of abrasive, 0.05 wt% -5 wt% of electrolyte, 1 wt% -35 wt% of surfactant and the balance of deionized water.
Preferably, the abrasive is at least one of silicon oxide, aluminum oxide, cerium oxide and titanium oxide.
The grinding material is core-shell structured nano composite particles, the core of the core-shell structured nano composite particles is at least one of silicon oxide, aluminum oxide, cerium oxide and titanium oxide, and the shell of the core-shell structured nano composite particles is ionized acrylic acid derivative resin.
Preferably, the electrolyte is an organic salt electrolyte, and the organic salt electrolyte is at least one of organic carboxylate, amino acid salt, organic sulfonate, organic phosphate and organic ammonium salt; more preferably, the organic salt electrolyte is an organic carboxylate and/or an organic sulfonate.
Preferably, the surfactant is a silicon-containing surfactant and/or a fluorine-containing surfactant.
Preferably, the silicon-containing surfactant is an anionic silicone surfactant; the fluorine-containing surfactant is a sulfonate fluorocarbon surfactant and/or a non-ionic fluorocarbon surfactant.
Preferably, the pH regulator is at least one of citric acid, tartaric acid, oxalic acid, hydrochloric acid, sulfuric acid, benzoic acid, and salicylic acid.
The preparation method of the polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following steps:
s1: weighing a fixed content of abrasive, adding the abrasive into a fixed content of deionized water, uniformly stirring, adding a fixed content of electrolyte and surfactant, and further uniformly stirring;
s2: and finally, adding a pH regulator, regulating the pH value to 2.5-6.0, and fully and uniformly stirring to obtain the polishing solution for polishing the oxygen surface of the zinc oxide crystal.
The invention has the beneficial effects that:
according to the polishing solution disclosed by the invention, the oxygen-containing surface of the zinc oxide crystal is modified by introducing the surface active substance, so that the polishing efficiency is greatly improved, and meanwhile, a proper electrolyte is introduced to balance the acting force between chemical polishing and mechanical polishing, so that the problem of surface orange peel is solved, and the defect-free ultra-precise surface required by the subsequent epitaxial process is realized.
The electrolyte is suitable for promoting the removal of the oxygen-containing crystal face of the zinc oxide crystal, thereby further improving the polishing efficiency.
The polishing solution is used for polishing the oxygen-containing crystal face of the third-generation semiconductor zinc oxide crystal, and the polished surface has no pits and scratches, so that the surface quality of the zinc oxide crystal is improved, and the production requirements of subsequent electronic components are completely met.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following raw materials: abrasive, electrolyte, surfactant and deionized water; and adjusting the pH value of the polishing solution to 2.5-6.0 by adopting a pH regulator.
In the polishing solution, the oxygen-containing crystal face of the zinc oxide crystal is more beneficial to polishing operation under an acidic condition, and the polishing surface quality is high.
Preferably, the raw materials comprise the following components in percentage by mass in the polishing solution: 0.1 wt% -40 wt% of abrasive, 0.05 wt% -5 wt% of electrolyte, 1 wt% -35 wt% of surfactant and the balance of deionized water.
Preferably, the abrasive is at least one of silicon oxide, aluminum oxide, cerium oxide and titanium oxide.
The grinding material is core-shell structured nano composite particles, the core of the core-shell structured nano composite particles is at least one of silicon oxide, aluminum oxide, cerium oxide and titanium oxide, and the shell of the core-shell structured nano composite particles is ionized acrylic acid derivative resin.
The nano composite particles with the core-shell structure take methyl acrylate as a reaction medium, abrasive materials are added according to the proportion that the abrasive materials account for 1-20% of the mass of the methyl acrylate, and the nano composite particles are uniformly dispersed by ultrasonic-assisted mechanical stirring; and then, mixing the monomer N, N, N-trimethyl ammonium acrylate and the monomer 1, 4-butanediol diacrylate according to the mass ratio of 1: 1-5, adding the mixture into the reaction medium, and reacting in a solution polymerization reaction mode to obtain the core-shell structured nano composite particles, wherein the shell of the nano composite particles is ionized acrylic acid derivative resin with the glass transition temperature of 70-110 ℃. The total monomer accounts for 3-6% of the total weight of the ionized acrylic acid derivative resin.
Preferably, the electrolyte is an organic salt electrolyte, and the organic salt electrolyte is at least one of organic carboxylate, amino acid salt, organic sulfonate, organic phosphate and organic ammonium salt; more preferably, the organic salt electrolyte is an organic carboxylate and/or an organic sulfonate.
Preferably, the surfactant is a silicon-containing surfactant and/or a fluorine-containing surfactant.
Preferably, the silicon-containing surfactant is an anionic silicone surfactant; the fluorine-containing surfactant is a sulfonate fluorocarbon surfactant and/or a non-ionic fluorocarbon surfactant.
The sulfonate fluorocarbon surfactant has better oxidation resistance and small sensitivity to strong acid and electrolyte; the nonionic fluorocarbon surfactant is not ionized in water solution, so that the nonionic fluorocarbon surfactant has high stability on pH value and is less influenced by electrolyte and inorganic salt.
Preferably, the pH regulator is at least one of citric acid, tartaric acid, oxalic acid, hydrochloric acid, sulfuric acid, benzoic acid, and salicylic acid.
The preparation method of the polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following steps:
s1: weighing a fixed content of abrasive, adding the abrasive into a fixed content of deionized water, uniformly stirring, adding a fixed content of electrolyte and surfactant, and further uniformly stirring;
s2: and finally, adding a pH regulator, regulating the pH value to 2.5-6.0, and fully and uniformly stirring to obtain the polishing solution for polishing the oxygen surface of the zinc oxide crystal.
The abrasive material of the present invention is preferably a nanocomposite particle having a core-shell structure; the ionized acrylic acid derivative resin shell has good hydrophilic and lipophilic balance, is beneficial to the environmental stability of charge quantity, is easy to form an electric double layer on the surface of abrasive particles, and increases the electrostatic repulsion among the particles, thereby weakening the sedimentation tendency of the particles, improving the suspension property and the fluidity of the abrasive in the polishing solution, and further improving the polishing efficiency of the polishing solution on the oxygen surface of zinc oxide crystals under the synergistic action of a surfactant; the abrasive is easy to use and long in storage time, and the service life of the abrasive in recycling is prolonged.
According to the polishing solution disclosed by the invention, the oxygen-containing surface of the zinc oxide crystal is modified by introducing the surface active substance, so that the polishing efficiency is greatly improved, and meanwhile, a proper electrolyte is introduced to balance the acting force between chemical polishing and mechanical polishing, so that the problem of surface orange peel is solved, and the defect-free ultra-precise surface required by the subsequent epitaxial process is realized. The surfactant and the electrolyte in the polishing solution have good stability under an acidic condition, so that the polishing efficiency of the polishing solution is improved, and the service life of the polishing solution is prolonged.
The polishing solution is used for polishing the oxygen-containing crystal face of the third-generation semiconductor zinc oxide crystal, so that the polishing efficiency is greatly improved, the polished surface has no pits or scratches, the surface quality of the zinc oxide crystal is high, and the production requirements of subsequent electronic components are completely met.
For further understanding of the present invention, the following embodiments are provided to illustrate the technical solutions of the present invention in detail, and the scope of the present invention is not limited by the following embodiments.
Example 1
The polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following raw materials: abrasive, electrolyte, surfactant and deionized water; and adjusting the pH value of the polishing solution to 4.8 by adopting a pH regulator.
The polishing solution comprises the following components in percentage by mass: 26% of abrasive, 3% of electrolyte, 26% of surfactant and the balance of deionized water.
The grinding material is core-shell structured nano composite particles, the inner cores of the core-shell structured nano composite particles are respectively silicon oxide and cerium oxide, the shells of the core-shell structured nano composite particles are respectively ionized acrylic acid derivative resin, and the mass ratio of the silicon oxide to the cerium oxide is 5: 1.
the electrolyte is prepared from the following components in a mass ratio of 1: 1, and organic sulfonates.
The surfactant is prepared from the following components in a mass ratio of 3: 2 and sulfonate fluorocarbon surfactant.
The pH regulator is prepared from the following components in a mass ratio of 3.2: 1 of citric acid and hydrochloric acid.
Example 2
The polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following raw materials: abrasive, electrolyte, surfactant and deionized water; and adjusting the pH value of the polishing solution to 2.5 by adopting a pH regulator.
The polishing solution comprises the following components in percentage by mass: 12 wt% of abrasive, 5 wt% of electrolyte, 18 wt% of surfactant and the balance of deionized water.
The grinding material is core-shell structured nano composite particles, the inner cores of the core-shell structured nano composite particles are respectively silicon oxide and titanium oxide, the shells of the core-shell structured nano composite particles are respectively ionized acrylic acid derivative resin, and the mass ratio of the silicon oxide to the cerium oxide is 3: 1.
the electrolyte is prepared from the following components in percentage by mass of 2: 3 and organic carboxylic acid salts and organic sulfonic acid salts.
The surfactant is prepared from the following components in a mass ratio of 1: 1 and a nonionic fluorocarbon surfactant.
The pH regulator is prepared from the following components in a mass ratio of 1: 2.9 tartaric acid and sulfuric acid.
Example 3
The polishing solution for polishing the oxygen surface of the zinc oxide crystal comprises the following raw materials: abrasive, electrolyte, surfactant and deionized water; and adjusting the pH value of the polishing solution to 6 by adopting a pH regulator.
The polishing solution comprises the following components in percentage by mass: 30% of abrasive, 1% of electrolyte, 30% of surfactant and the balance of deionized water.
The grinding material is core-shell structured nano composite particles, the inner cores of the core-shell structured nano composite particles are respectively silicon oxide and aluminum oxide, the shells of the core-shell structured nano composite particles are respectively ionized acrylic acid derivative resin, and the mass ratio of the silicon oxide to the cerium oxide is 2: 1.
the electrolyte is prepared from the following components in a mass ratio of 1: 1.2 with organic carboxylic acid salts and organic sulfonic acid salts.
The surfactant is prepared from the following components in a mass ratio of 3: 1 and sulfonate fluorocarbon surfactant.
The pH regulator is prepared from the following components in a mass ratio of 4.6: 1 oxalic acid and hydrochloric acid.
Example 4
The formula of the polishing solution for polishing the oxygen surface of the zinc oxide crystal in the embodiment is basically similar to that of the polishing solution in the embodiment 1, and the main difference is that the components in the raw materials in the polishing solution are as follows by mass percent: 16 wt% of abrasive, 5 wt% of electrolyte, 28 wt% of surfactant and the balance of deionized water. And adjusting the pH value of the polishing solution to 3.7 by using a pH regulator.
The electrolyte is an organic salt electrolyte, and the organic salt electrolyte is prepared from the following components in a mass ratio of 2: 1, an amino acid salt.
Example 5
The formula of the polishing solution for polishing the oxygen surface of the zinc oxide crystal in the embodiment is basically similar to that of the polishing solution in the embodiment 1, and the main difference is that the components in the raw materials in the polishing solution are as follows by mass percent: 36 wt% of abrasive, 1.5 wt% of electrolyte, 18 wt% of surfactant and the balance of deionized water. And adjusting the pH value of the polishing solution to 5.3 by using a pH regulator.
The electrolyte is an organic salt electrolyte, and the organic salt electrolyte is prepared from the following components in a mass ratio of 2: 3 organic sulfonate and organic phosphorus salt.
Comparative example 1
The polishing solution for polishing the oxygen surface of zinc oxide crystal of this comparative example had a formulation substantially similar to that of example 1, except that the abrasive was added to the polishing solution in the form of a conventional silica sol.
Comparative example 2
The polishing solution for the oxygen-side polishing of zinc oxide crystal of this comparative example had a formulation substantially similar to that of example 1, except that the polishing solution contained no electrolyte.
Comparative example 3
The polishing solution for polishing the oxygen surface of zinc oxide crystals of this comparative example had a formulation substantially similar to that of example 1, except that the surfactant was a quaternary ammonium salt cationic surfactant.
Comparative example 4
The polishing solution for polishing the oxygen surface of zinc oxide crystals of the comparative example has a formulation substantially similar to that of example 1, and is mainly different in that the surfactant is only an anionic silicone surfactant.
Comparative example 5
The formulation of the polishing slurry for polishing the oxygen surface of zinc oxide crystal of this comparative example is substantially similar to that of example 1, and the main difference is that the surfactant is only a sulfonate fluorocarbon surfactant.
Comparative example 6
The polishing solution for polishing the oxygen surface of the zinc oxide crystal of the comparative example has a formula basically similar to that of example 1, and mainly differs in that the surfactant is only a nonionic fluorocarbon surfactant.
The polishing liquids prepared in examples 1 to 5 and comparative examples 1 to 6 were subjected to performance tests, and the results are shown in table 1:
and (3) appearance observation: judging the flaw condition of the surface appearance and whether the orange peel phenomenon appears or not in a visual observation mode; and testing the glossiness of the surface of each workpiece by adopting a gloss meter.
And (3) testing the polishing efficiency: the prepared samples were polished on a san gao single-side polisher. The test conditions were as follows: pressing: 10 psi, lower disc and carrier disc rotation speed 80 RPM, slurry flow rate: 100 ml/min, polishing pad material: black damping cloth; the polishing time was 30 minutes. The zinc oxide thin sheet was used for polishing test. And judging the polishing efficiency according to the cutting rate of the polishing solution on the metal surface.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed.
Claims (4)
1. The polishing solution for polishing the oxygen surface of the zinc oxide crystal is characterized by comprising the following raw materials: abrasive, electrolyte, surfactant and deionized water; adjusting the pH value of the polishing solution to 2.5-6.0 by adopting a pH regulator; the grinding material is core-shell structured nano composite particles, the core of the core-shell structured nano composite particles is at least one of silicon oxide, aluminum oxide, cerium oxide and titanium oxide, and the shell of the core-shell structured nano composite particles is ionized acrylic acid derivative resin; the electrolyte is an organic salt electrolyte which is organic carboxylate and organic sulfonate; the surfactant is a silicon-containing surfactant and a fluorine-containing surfactant; the silicon-containing surfactant is an anionic organic silicon surfactant; the fluorine-containing surfactant is a sulfonate fluorocarbon surfactant or a nonionic fluorocarbon surfactant; the nano composite particles with the core-shell structure take methyl acrylate as a reaction medium, abrasive materials are added according to the proportion that the abrasive materials account for 1-20% of the mass of the methyl acrylate, and the nano composite particles are uniformly dispersed by ultrasonic-assisted mechanical stirring; and then, mixing the monomer N, N, N-trimethyl ammonium acrylate and the monomer 1, 4-butanediol diacrylate according to the mass ratio of 1: 1-5, adding the mixture into the reaction medium, and reacting in a solution polymerization reaction mode to obtain the core-shell structured nano composite particles, wherein the shell of the nano composite particles is ionized acrylic acid derivative resin with the glass transition temperature of 70-110 ℃.
2. The polishing solution for polishing the oxygen surface of a zinc oxide crystal according to claim 1, wherein the raw materials comprise the following components in percentage by mass in the polishing solution: 0.1 wt% -40 wt% of abrasive, 0.05 wt% -5 wt% of electrolyte, 1 wt% -35 wt% of surfactant and the balance of deionized water.
3. The polishing solution for oxygen-face polishing of zinc oxide crystals as claimed in claim 1, wherein the pH adjusting agent is at least one of citric acid, tartaric acid, oxalic acid, hydrochloric acid, sulfuric acid, benzoic acid, salicylic acid.
4. The method for preparing a polishing liquid for polishing an oxygen face of a zinc oxide crystal according to any one of claims 1 to 3, comprising the steps of:
s1: weighing a fixed content of abrasive, adding the abrasive into a fixed content of deionized water, uniformly stirring, adding a fixed content of electrolyte and surfactant, and further uniformly stirring;
s2: and finally, adding a pH regulator, regulating the pH value to 2.5-6.0, and fully and uniformly stirring to obtain the polishing solution for polishing the oxygen surface of the zinc oxide crystal.
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Citations (3)
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|---|---|---|---|---|
| CN101125416A (en) * | 2007-09-14 | 2008-02-20 | 中国科学院上海光学精密机械研究所 | Polishing method for zinc oxide single crystal substrate level substrate |
| CN102212316A (en) * | 2011-05-10 | 2011-10-12 | 天津理工大学 | Acidic nano polishing solution for chemical mechanical planarization of zinc oxide and application thereof |
| CN102220088A (en) * | 2011-05-10 | 2011-10-19 | 天津理工大学 | Alkaline nanometer polishing slurry for chemical mechanical planarization of zinc oxide, and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101974297A (en) * | 2010-11-12 | 2011-02-16 | 大连三达奥克化学股份有限公司 | Core/shell type composite nano-abrasive copper chemical-mechanical polishing liquid |
| CN101974296A (en) * | 2010-11-12 | 2011-02-16 | 大连三达奥克化学股份有限公司 | Core/shell type composite nano abrasive silicon slice polishing liquid |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125416A (en) * | 2007-09-14 | 2008-02-20 | 中国科学院上海光学精密机械研究所 | Polishing method for zinc oxide single crystal substrate level substrate |
| CN102212316A (en) * | 2011-05-10 | 2011-10-12 | 天津理工大学 | Acidic nano polishing solution for chemical mechanical planarization of zinc oxide and application thereof |
| CN102220088A (en) * | 2011-05-10 | 2011-10-19 | 天津理工大学 | Alkaline nanometer polishing slurry for chemical mechanical planarization of zinc oxide, and application thereof |
Non-Patent Citations (1)
| Title |
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| "Investigation of chemical mechanical polishing of zinc oxide thin films";Sushant Gupta等;《Applied Surface Science》;20110202(第257期);5837-5843 * |
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