CN113717691A - Preparation method and application of polyethylene polyamine modified diamond composite abrasive particles - Google Patents
Preparation method and application of polyethylene polyamine modified diamond composite abrasive particles Download PDFInfo
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- CN113717691A CN113717691A CN202111008632.9A CN202111008632A CN113717691A CN 113717691 A CN113717691 A CN 113717691A CN 202111008632 A CN202111008632 A CN 202111008632A CN 113717691 A CN113717691 A CN 113717691A
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- polyethylene polyamine
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention discloses a preparation method of polyethylene polyamine modified diamond composite abrasive particles and application thereof in precision polishing. Compared with the diamond abrasive particles before modification, the polishing solution prepared from the composite abrasive particles has good dispersion stability, and is used for polishing ceramic cover plates of mobile phones and the like.
Description
Technical Field
The invention relates to superfine diamond composite abrasive particles for polishing a ceramic cover plate of a mobile phone and a preparation method thereof, in particular to polyethylene polyamine modified diamond composite abrasive particles and a preparation method thereof, belonging to the technical field of surface grinding and polishing.
Background
With the application of wireless charging and the coming of 5G communication technology, the ceramic has the excellent characteristics of high hardness (2 times of glass), scratch resistance, wear resistance, strong electromagnetic signal penetration capacity, attractive appearance and the like, becomes an ideal material for the rear cover plate of the next-generation smart phone, and has huge market and wide application prospect. The method is applied to high-end models of millets, Android, Hua P7, Apple Watch and other brands at present. An ultra-smooth and flat ceramic surface is not only required for beautifying products and obtaining good hand feeling, but also is an important influence factor for ensuring the product quality and prolonging the service life of workpieces.
Surface polishing is one of the key processes in the manufacture of the ceramic cover plate of the mobile phone. However, ceramics have high melting point, high hardness, high brittleness, high crack sensitivity, and the like, and thus are difficult to process. Compared with metal materials, the ceramic polishing efficiency is low and the defect level is high. At present, low processing efficiency and high surface defect level cause low yield, which is one of the main obstacles of the industrialization of the ceramic cover plate of the mobile phone.
The polishing solution is used as a main polishing carrier in polishing process and has been the research focus of all researchers. The polishing liquid is mainly composed of abrasive grains and chemical agents (surfactants, catalysts, oxidizing agents, etc.). The abrasive particles are the basis and key components of the polishing solution, and the polishing performance of the polishing solution is obviously influenced by the physicochemical indexes of the type, structure, hardness, granularity, morphology and the like of the abrasive particles.
The diamond is an inorganic abrasive particle frequently adopted in polishing processing, the polishing efficiency is high, but because the diamond hardness is high, particles are agglomerated to generate large particles, serious polishing damage is often caused, the generated surface defects are more, the surface precision requirements of ceramic cover plates of mobile phones and the like cannot be met, and the industrial mass production requirement of the ceramic cover plates is difficult to meet.
Disclosure of Invention
The invention aims to solve the problem of insufficient polishing precision of the existing diamond abrasive particles, and provides the polyethylene polyamine modified diamond composite abrasive particles, which can effectively reduce particle agglomeration, reduce polishing damage and improve the surface precision after polishing.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the polyethylene polyamine modified diamond composite abrasive particle comprises a diamond abrasive particle, and the surface of the diamond abrasive particle is modified by adopting an organic matter with a polyethylene polyamine structure to obtain the polyethylene polyamine modified diamond composite abrasive particle.
A preparation method of polyethylene polyamine modified diamond composite abrasive particles comprises the following steps:
s01: mixing concentrated sulfuric acid and concentrated nitric acid in a weight ratio of 1:2 in a three-neck flask with a reflux device, adding diamond abrasive particles, heating to 90-110 ℃, and reacting for 12 hours under continuous stirring; cooling the mixed solution to room temperature, performing centrifugal separation and deionized water washing, repeating for M times, washing the precipitate with ethanol for N times, filtering, and vacuum drying the precipitate at room temperature to obtain diamond abrasive particle powder with carboxyl functional groups; wherein M and N are integers greater than or equal to 1;
s02: adding a toluene solvent into a three-neck flask with a reflux device and an oil-water separator, adding a certain amount of diamond abrasive particle powder with carboxyl functional groups prepared in the step S01 under the stirring condition, uniformly stirring, adding an organic matter with a polyethylene polyamine structure, heating to 90-100 ℃, stirring for reaction for 2-4 hours, cooling to room temperature, performing centrifugal separation, washing the precipitate with ethanol for P times, performing suction filtration, and performing vacuum drying on the precipitate at room temperature to obtain polyethylene polyamine modified diamond composite abrasive particle powder; wherein, P is an integer greater than or equal to 1; .
Further, in step S01: the mass ratio of the mixed solution of concentrated sulfuric acid and concentrated nitric acid to the diamond abrasive particles is 100: 2.
further, in step S01: the grain diameter of the diamond abrasive grain is 10 nm-1000 nm.
Further, in step S02: the mass ratio of the toluene solvent, the carboxylated diamond abrasive powder, the organic matter with the polyethylene polyamine structure and the like is 100: 1: 5.
further, in step S02: the organic matter with the structure of the polyethylene polyamine is one of diethylenetriamine, triethylene tetramine, tetraethylene pentamine, pentaethylene hexamine and polyethylene polyamine.
The invention has the following beneficial effects: the method utilizes the polyethylene polyamine organic matter to modify the superfine diamond abrasive particles, can effectively reduce the agglomeration phenomenon of the diamond particles, prevents the generation of large particles, is applied to the polishing of ceramic cover plates of mobile phones and the like, can effectively reduce the surface roughness after polishing, and reduces the polishing damage of the diamond abrasive particles.
Detailed description of the preferred embodiments
The technical solutions of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides polyethylene polyamine modified diamond composite abrasive particles, which are superfine modified diamond composite abrasive particles; the inner core of the composite abrasive grain is 10-1000 nm diamond abrasive grain, and organic matter with a polyethylene polyamine structure is adopted to modify the surface of the diamond abrasive grain.
The polyethylene polyamine modified superfine diamond composite abrasive grain provided by the invention is prepared by the processes of surface carboxylation of diamond abrasive grains, condensation reaction with polyethylene polyamine and the like, and the method comprises the following steps:
s01: mixing concentrated sulfuric acid and concentrated nitric acid in a weight ratio of 1:2 in a three-neck flask with a reflux device, adding a certain amount of diamond abrasive particles, heating to about 100 ℃, and reacting for 12 hours under continuous stirring. Cooling the mixed solution to room temperature, performing centrifugal separation and deionized water washing, repeating for 3 times, washing the precipitate for 3 times by using ethanol, filtering, and performing vacuum drying on the precipitate at room temperature to obtain diamond abrasive particle powder with carboxyl functional groups; in the step, the mass ratio of the mixed solution of concentrated sulfuric acid and concentrated nitric acid to the diamond abrasive particles is 100: 2; the grain diameter of the diamond abrasive grain is 10 nm-1000 nm.
S02: adding a toluene solvent into a three-neck flask with a reflux device and an oil-water separator, adding a certain amount of the diamond abrasive grain powder with the carboxyl functional group prepared in S01 under the stirring condition, uniformly stirring, adding a certain amount of organic matter with a polyethylene polyamine structure, heating to about 95 ℃, stirring to react for 2-4 hours, centrifugally separating, washing the precipitate with ethanol for 3 times, filtering, precipitating, and performing vacuum drying at room temperature to obtain the polyethylene polyamine modified diamond abrasive grain powder. In this step: the mass ratio of the toluene solvent, the carboxylated diamond abrasive powder, the organic matter with the polyethylene polyamine structure and the like is 100: 1: 5; the organic matter with polyethylene polyamine structure can be diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, polyethylene polyamine, etc.
The prepared abrasive particles are prepared into polishing solution by the following method: adding 2 g of polyethylene polyamine modified diamond abrasive particle powder prepared in the step S02 into 100 g of deionized water, performing ultrasonic dispersion for 0.5 hour, sequentially adding 0.2% of polyether surfactant and 0.3% of commercial PM polishing accelerator while stirring, and uniformly stirring to obtain the polishing solution of polyethylene polyamine modified superfine diamond composite abrasive particles with the concentration of 2.0 wt.%.
The polishing solution of the polyethylene polyamine modified superfine diamond composite abrasive particles is used for polishing a ceramic cover plate of a mobile phone, the surface roughness after polishing can reach below 6 nanometers, and the defects and damages under a fluorescent lamp are light.
The invention is further illustrated by the following specific examples and comparative examples:
example 1
The embodiment provides a preparation method of polyethylene polyamine modified superfine diamond composite abrasive particles, which is prepared through the processes of surface carboxylation of diamond abrasive particles, condensation reaction with polyethylene polyamine and the like, and comprises the following steps:
s01: mixing concentrated sulfuric acid and concentrated nitric acid in a weight ratio of 1:2 in a three-neck flask with a reflux device, adding a certain amount of diamond abrasive particles, heating to about 100 ℃, and reacting for 12 hours under continuous stirring. Cooling the mixed solution to room temperature, performing centrifugal separation and deionized water washing, repeating for 3 times, washing the precipitate for 3 times by using ethanol, filtering, and performing vacuum drying on the precipitate at room temperature to obtain diamond abrasive particle powder with carboxyl functional groups; in the step, the mass ratio of the mixed solution of concentrated sulfuric acid and concentrated nitric acid to the diamond abrasive particles is 100: 2; the grain diameter of the superfine diamond abrasive grains is 15 nanometers.
S02: adding a toluene solvent into a three-neck flask with a reflux device and an oil-water separator, adding a certain amount of the diamond abrasive grain powder with the carboxyl functional group prepared in S01 under the stirring condition, uniformly stirring, adding a certain amount of organic matter with a polyethylene polyamine structure, heating to about 95 ℃, stirring to react for 2-4 hours, centrifugally separating, washing the precipitate with ethanol for 3 times, filtering, precipitating, and performing vacuum drying at room temperature to obtain the polyethylene polyamine modified diamond abrasive grain powder. In this step: the mass ratio of the toluene solvent, the carboxylated diamond abrasive powder, the organic matter with the polyethylene polyamine structure and the like is 100: 1: 5. the organic matter of the polyethylene polyamine structure adopted in the step is tetraethylenepentamine.
S03: and preparing the polishing solution of the polyethylene polyamine modified superfine diamond composite abrasive particles. Adding 2 g of tetraethylenepentamine modified diamond abrasive particle powder prepared in the step S02 into 100 g of deionized water, ultrasonically dispersing for 0.5 hour, sequentially adding 0.2% of polyether surfactant and 0.3% of commercial PM polishing accelerator while stirring, and uniformly stirring to obtain the polishing solution of tetraethylenepentamine modified superfine diamond composite abrasive particles with the concentration of 2.0 wt.%.
Example 2
The same as example 1 except that the grain size of the ultra fine diamond abrasive grain used in step S01 was 100 nm.
Example 3
The same as example 1 except that the ultra fine diamond abrasive grains used in step S01 had a grain size of 1000 nm.
Example 4
The same as example 1, except that the organic material having a polyethylene polyamine structure used in step S02 was diethylenetriamine.
Example 5
The same as example 1, except that triethylene tetramine was used as the organic material having a polyethylene polyamine structure in step S02.
Example 6
The same as example 1 except that the organic substance having a polyethylene polyamine structure used in step S02 is pentaethylenehexamine.
Comparative example 1
A preparation method of a 15 nanometer superfine diamond composite abrasive grain polishing solution comprises the following steps:
adding 2 g of 15 nanometer ultrafine diamond abrasive particle powder into 100 g of deionized water, performing ultrasonic dispersion for 0.5 hour, sequentially adding 0.2% of polyether surfactant and 0.3% of commodity PM polishing accelerator while stirring, and uniformly stirring to obtain the polishing solution with the concentration of 2.0 wt.% of 15 nanometer ultrafine diamond composite abrasive particles. .
Comparative example 2
A preparation method of a polishing solution with ultra-fine diamond abrasive particles with the particle size of 100 nanometers is the same as that of comparative example 1, except that the ultra-fine diamond abrasive particles with the particle size of 100 nanometers are adopted.
Comparative example 3
A method for preparing a polishing solution with ultra-fine diamond abrasive particles having a particle size of 1000nm is the same as that of comparative example 1 except that the ultra-fine diamond abrasive particles having a particle size of 1000nm are used.
The polishing liquids of examples 1 to 6 and comparative examples 1 to 3 were used to perform polishing tests on a ceramic cover plate of a mobile phone and a sapphire wafer under certain polishing conditions. The polishing conditions were as follows:
polishing machine: UNIPOL-1000S automatic pressure grinding polisher;
polishing the workpiece: zirconia mobile phone ceramic plates with side length of 80.0mm multiplied by 80.0 mm;
polishing the pad: SUBA-800 polishing pads;
polishing pressure: 5 kg;
rotating speed of a lower disc: 70 rpm;
polishing time: 2 h;
after the polishing was completed, the zirconia ceramic cover plate of the cell phone was washed and dried, and the surface average roughness (Ra) of the workpiece was measured by a 3D optical profiler (Sneox090v2) in a test range of 1000 μm × 1000 μm. And observing the polished surface defects and damages under a fluorescent lamp.
The polishing solutions of the examples and the comparative examples and the polishing effects thereof on the zirconia mobile phone ceramic sheets are summarized in table 1. As can be seen from Table 1, the pure diamond abrasive grains with different particle sizes in comparative examples 1-3 are used for polishing the ceramic cover plate of the mobile phone, and have many polishing defects and large roughness after polishing; all of the examples show low surface roughness after polishing and less polishing damage.
TABLE 1 polishing effect of ultra fine diamond abrasive grains of examples and comparative examples of the present invention on ceramic cover plate of cellular phone
In a word, compared with the conventional diamond commercial abrasive particles, the polyethylene polyamine modified superfine diamond composite abrasive particles are used for polishing the ceramic cover plate of the mobile phone, the surface roughness can reach below 6 nanometers, the microscopic defects are light, and the polishing effect of high speed and high precision is achieved.
Claims (6)
1. The polyethylene polyamine modified diamond composite abrasive grain is characterized by comprising diamond abrasive grains, wherein the surface of the diamond abrasive grains is modified by adopting an organic matter with a polyethylene polyamine structure, so that the polyethylene polyamine modified diamond composite abrasive grain is obtained.
2. The preparation method of the polyethylene polyamine modified diamond composite abrasive particle is characterized by comprising the following steps:
s01: mixing concentrated sulfuric acid and concentrated nitric acid in a weight ratio of 1:2 in a three-neck flask with a reflux device, adding diamond abrasive particles, heating to 90-110 ℃, and reacting for 12 hours under continuous stirring; cooling the mixed solution to room temperature, performing centrifugal separation and deionized water washing, repeating for M times, washing the precipitate with ethanol for N times, filtering, and vacuum drying the precipitate at room temperature to obtain diamond abrasive particle powder with carboxyl functional groups; wherein M and N are integers greater than or equal to 1;
s02: adding a toluene solvent into a three-neck flask with a reflux device and an oil-water separator, adding a certain amount of diamond abrasive particle powder with carboxyl functional groups prepared in the step S01 under the stirring condition, uniformly stirring, adding an organic matter with a polyethylene polyamine structure, heating to 90-100 ℃, stirring for reaction for 2-4 hours, cooling to room temperature, performing centrifugal separation, washing the precipitate with ethanol for P times, performing suction filtration, and performing vacuum drying on the precipitate at room temperature to obtain polyethylene polyamine modified diamond composite abrasive particle powder; wherein, P is an integer greater than or equal to 1; .
3. The method of manufacturing polyethylene polyamine-modified diamond composite abrasive grains according to claim 2, wherein in step S01: the mass ratio of the mixed solution of concentrated sulfuric acid and concentrated nitric acid to the diamond abrasive particles is 100: 2.
4. the method for producing polyethylene polyamine-modified ultrafine diamond composite abrasive grains according to claim 2, wherein in step S01: the grain diameter of the diamond abrasive grain is 10 nm-1000 nm.
5. The method for producing polyethylene polyamine-modified ultrafine diamond composite abrasive grains according to claim 2, wherein in step S02: the mass ratio of the toluene solvent, the carboxylated diamond abrasive powder, the organic matter with the polyethylene polyamine structure and the like is 100: 1: 5.
6. the method for producing polyethylene polyamine-modified ultrafine diamond composite abrasive grains according to claim 2, wherein in step S02: the organic matter with the structure of the polyethylene polyamine is one of diethylenetriamine, triethylene tetramine, tetraethylene pentamine, pentaethylene hexamine and polyethylene polyamine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115651608A (en) * | 2022-10-31 | 2023-01-31 | 太仓硅源纳米材料有限公司 | Preparation method and application of nano-alumina composite abrasive particles |
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Application publication date: 20211130 |