CN116589928A - Super-dispersed diamond suspension and preparation method thereof - Google Patents

Super-dispersed diamond suspension and preparation method thereof Download PDF

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Publication number
CN116589928A
CN116589928A CN202310554194.9A CN202310554194A CN116589928A CN 116589928 A CN116589928 A CN 116589928A CN 202310554194 A CN202310554194 A CN 202310554194A CN 116589928 A CN116589928 A CN 116589928A
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China
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diamond
suspension
dispersed
nano
ultra
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章洋
章敏
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Nebo Testing Technology Wuhan Co ltd
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Nebo Testing Technology Wuhan Co ltd
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Priority to CN202310554194.9A priority Critical patent/CN116589928A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions

Abstract

The invention relates to the technical field of precision grinding and polishing, in particular to a super-dispersion diamond suspension and a preparation method thereof.

Description

Super-dispersed diamond suspension and preparation method thereof
Technical Field
The invention relates to the technical field of precision grinding and polishing, in particular to a super-dispersed diamond suspension and a preparation method thereof.
Background
Diamond is an excellent 21 st century material. Because diamond has the characteristics of excellent thermal conductivity, high hardness, low friction, good optical property, biocompatibility coefficient and the like, the nano diamond not only inherits the advantages of large-scale diamond particles, but also has the characteristics of nano materials. Diamond powder as the hardest superfine abrasive has been widely used in industrial departments of machinery, aerospace, optical instruments, glass, ceramics, petroleum, electronics, photoelectricity, semiconductors, war industry and the like, is an ideal material for grinding and polishing various hard and brittle materials such as artificial crystals, precious stones, hard alloy, optical crystals, ceramics, super hard alloy and the like, and can be prepared into grinding and polishing products of paste, aerosol, membranous, oily or aqueous liquid, but diamond paste and aerosol have the defects of easy crust deposition, difficult dispersion, serious waste and the like, and the application of the aqueous grinding and polishing liquid has the advantages of environmental protection, no corrosion, low cost, high polishing efficiency and the like, and is increasingly widely applied in various fields. However, when the nano-level particles are dispersed in a solution for treatment, the smaller the particles are, the more easily aggregation between the particles occurs, and in addition, since the aggregated particles are settled, it is very difficult to obtain a stable dispersion, and the surface quality of the abrasive is affected; how to invent a super-dispersed diamond suspension is a technical problem to be solved.
Disclosure of Invention
In order to overcome the defects of the technology, the invention provides the super-dispersed diamond suspension with excellent dispersion stability even with high concentration and the preparation method thereof, and the precipitation and delamination of diamond powder in the suspension are effectively prevented.
In one aspect, the present invention provides a super-dispersed diamond suspension, which is characterized in that: a diamond suspension of 6-12% wt by mass of diamond particles having a particle size of 2-200 nm dispersed in a solvent.
The diamond is synthesized by an air-cooled detonation method, and in a preferred scheme, the particle size is 2-100nm, in a more preferred scheme, the particle size is 2-50nm, and further preferred particle size is 2-20nm.
Preferably, the suspension has a pH of 4-6 and a conductivity of < 40. Mu.S/cm. In a more preferable embodiment, the pH of the suspension is 4 to 5.5, and further preferably, the pH of the suspension is 5 to 5.5, from the viewpoint of dispersion stability; in addition, the conductivity is < 40. Mu.S/cm, preferably < 30. Mu.S/cm, more preferably < 20. Mu.S/cm, particularly preferably < 20. Mu.S/cm.
Preferably, the suspension has a pH of 8-10 and a conductivity of < 200. Mu.S/cm. In a more preferable embodiment, the pH of the suspension is 9 to 10, and further preferably, the pH of the suspension is 9.5 to 10, from the viewpoint of dispersion stability; in addition, the electrical conductivity is < 200. Mu.S/cm, preferably 150 to 190. Mu.S/cm, more preferably 160 to 180. Mu.S/cm, particularly preferably 165 to 175. Mu.S/cm.
Preferably, the mass fraction of the diamond suspension is 10-12% wt.
On the other hand, the invention provides a preparation method of the super-dispersed diamond suspension, which is characterized by comprising the following steps:
s1, putting nano diamond, deionized water and a modifier into a container, and mixing, dispersing and stirring for 20-30 minutes under the action of ultrasound to obtain a nano diamond solution;
s2, stirring the nano-diamond solution prepared in the step S1, adding a suspending agent, and adjusting the pH value to obtain a diamond pretreatment solution;
s3, adding the diamond pretreatment liquid prepared in the step S2 into a bead mill with a screen for grinding, and collecting grinding liquid;
s4, performing ultrasonic dispersion on the grinding liquid, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
Preferably, the nanodiamond is derived from diamond synthesized by an air-cooled detonation method.
Preferably, the modifier is one or more of fatty alcohol polyoxyethylene ether ammonium sulfate and linear alkyl benzene sodium sulfonate, and the mass fraction of the modifier in the nano-diamond solution is 0.5-1.0%.
Preferably, the suspending agent is one or more of isoamyl nitrite and fatty acid polyethylene glycol ester, and the mass fraction of the suspending agent in the diamond pretreatment liquid is 0.8-1.2%.
Preferably, in S3, the rotation speed of the bead mill is 4000-5000 min -1 The bead grinding time is 3-6 hours.
Preferably, in S4, the ultrasonic dispersion time is 0.5-1 h, and the power is 500-700W.
The invention has the beneficial effects that: according to the invention, the modifier and the suspending agent are added into the aqueous solution in which the nano diamond particles are dispersed, so that the surface of the nano diamond is modified, the dispersibility of the nano diamond in the aqueous solution is improved, and the diamond pretreatment liquid is regulated to a specific pH value and specific conductivity and then subjected to graded dispersion treatment, so that the diamond suspension with excellent high-concentration dispersion stability, which is difficult to generate aggregation under the condition of long-time storage, can be obtained.
Detailed Description
The present invention will be described in detail with reference to specific embodiments thereof, so that those skilled in the art can better understand the technical solutions of the present invention. The experimental procedures, which do not address the specific conditions in the examples below, are generally carried out under conventional conditions or under conditions recommended by the manufacturer. The test materials used in the examples described below, unless otherwise specified, were purchased from conventional biochemical reagent stores. Percentages and parts are by weight unless otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present invention. The preferred methods and materials described herein are presented for illustrative purposes only.
EXAMPLE 1 preparation of ultra-dispersed diamond suspension
The nano-diamond with the grain diameter of 15-20nm synthesized by an air cooling detonation method, deionized water and fatty alcohol polyoxyethylene ether ammonium sulfate are placed into a container, and mixed, dispersed and stirred for 20-30 minutes under the action of ultrasound, so that a nano-diamond solution can be obtained, wherein the adding amount of the fatty alcohol polyoxyethylene ether ammonium sulfate is 0.5-0.7% wt of the mass of the nano-diamond solution, and the nano-diamond is from diamond synthesized by the air cooling detonation method; stirring and adding isoamyl nitrite into the prepared nano diamond solution, and adjusting the pH value, wherein the adding amount of the isoamyl nitrite is 0.8-1.0 wt% of the mass of the diamond pretreatment liquid to obtain the diamond pretreatment liquid, wherein the solid content concentration of the diamond pretreatment liquid is 6%, the conductivity is 38 mu S/cm, and the pH value is 4.3; adding the obtained diamond pretreatment solution into a bead mill with a screen for grinding, wherein the rotating speed of the bead mill is 4000min -1 The bead grinding time is 5-6 hours, and the grinding liquid is collected; and (3) performing ultrasonic dispersion on the grinding liquid for 0.5-0.8 h with the power of 500W, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
EXAMPLE 2 preparation of ultra-dispersed diamond suspension
The nano-diamond with the grain diameter of 2-5nm synthesized by an air cooling detonation method, deionized water and linear sodium alkylbenzenesulfonate are placed into a container, and mixed, dispersed and stirred for 20-30 minutes under the action of ultrasound, so that a nano-diamond solution can be obtained, wherein the addition amount of the fatty alcohol polyoxyethylene ether ammonium sulfate is 0.8-1.0 wt% of the mass of the nano-diamond solution; stirring and adding fatty acid polyethylene glycol ester into the prepared nano diamond solution, and adjusting the pH value, wherein the adding amount of the fatty acid polyethylene glycol ester is 1.0-1.2 wt% of the mass of the diamond pretreatment solution to obtain the diamond pretreatment solution, wherein the solid component concentration of the diamond pretreatment solution is 8%, the conductivity is 30 mu S/cm, and the pH value is 5.5; adding the obtained diamond pretreatment solution into a bead mill with a screen for grinding, wherein the rotation speed of the bead mill is 5000min -1 The bead grinding time is 5-6 hours, and the grinding liquid is collected; and (3) performing ultrasonic dispersion on the grinding liquid for 0.5-0.8 h with power of 700W, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
EXAMPLE 3 preparation of ultra-dispersed diamond suspension
The nano diamond with the grain diameter of 5-10nm synthesized by an air cooling detonation method, deionized water and fatty alcohol polyoxyethylene ether ammonium sulfate are placed into a container, and mixed, dispersed and stirred for 20-30 minutes under the action of ultrasound, so that a nano diamond solution can be obtained, wherein the adding amount of the fatty alcohol polyoxyethylene ether ammonium sulfate is 0.6-0.8 wt% of the mass of the nano diamond solution; stirring and adding isoamyl nitrite into the prepared nano diamond solution, and adjusting the pH value, wherein the adding amount of the isoamyl nitrite is 0.9-1.1 wt% of the mass of the diamond pretreatment liquid, so as to obtain the diamond pretreatment liquid, wherein the solid component concentration of the diamond pretreatment liquid is 10%, the conductivity is 13 mu S/cm, and the pH value is 4.8; adding the obtained diamond pretreatment solution into a bead mill with a screen for grinding, wherein the rotation speed of the bead mill is 4500min -1 The bead grinding time is 5-6 hours, and the grinding liquid is collected; and (3) performing ultrasonic dispersion on the grinding liquid for 0.5-0.8 h with the power of 600W, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
EXAMPLE 4 preparation of ultra-dispersed diamond suspension
The nano-diamond with the grain diameter of 12-18nm synthesized by an air cooling detonation method, deionized water and linear sodium alkylbenzenesulfonate are placed into a container, and mixed, dispersed and stirred for 20-30 minutes under the action of ultrasound, so that a nano-diamond solution can be obtained, wherein the adding amount of the linear sodium alkylbenzenesulfonate is 0.6-0.7% wt of the mass of the nano-diamond solution; stirring and adding isoamyl nitrite into the prepared nano diamond solution, and adjusting the pH value, wherein the adding amount of the isoamyl nitrite is 0.8-1.0 wt% of the mass of the diamond pretreatment liquid to obtain the diamond pretreatment liquid, wherein the solid content concentration of the diamond pretreatment liquid is 7%, the conductivity is 168 mu S/cm, and the pH value is 8.5; adding the obtained diamond pretreatment solution into a bead mill with a screen for grinding, wherein the rotating speed of the bead mill is 4000min -1 The bead grinding time is 5-6 hours, and the grinding liquid is collected; and (3) performing ultrasonic dispersion on the grinding liquid for 0.5-0.8 h with the power of 500W, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
EXAMPLE 5 preparation of ultra-dispersed diamond suspension
The nano-diamond with the grain diameter of 8-15nm synthesized by an air cooling detonation method, deionized water and fatty alcohol polyoxyethylene ether ammonium sulfate are placed into a container, and mixed, dispersed and stirred for 20-30 minutes under the action of ultrasound, so that a nano-diamond solution can be obtained, wherein the adding amount of the fatty alcohol polyoxyethylene ether ammonium sulfate is 0.9-1.0 wt% of the mass of the nano-diamond solution, and the nano-diamond is from diamond synthesized by the air cooling detonation method; stirring and adding fatty acid polyethylene glycol ester into the prepared nano diamond solution, and adjusting the pH value, wherein the adding amount of the fatty acid polyethylene glycol ester is 0.9-1.1 wt% of the mass of the diamond pretreatment solution to obtain the diamond pretreatment solution, wherein the solid component concentration of the diamond pretreatment solution is 12%, the conductivity is 190 mu S/cm, and the pH value is 10; adding the obtained diamond pretreatment solution into a bead mill with a screen for grinding, wherein the rotation speed of the bead mill is 5000min -1 The bead grinding time is 5-6 hours, and the grinding liquid is collected; and (3) performing ultrasonic dispersion on the grinding liquid for 0.5-0.8 h with power of 700W, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
EXAMPLE 6 preparation of ultra-dispersed diamond suspension
The nano-diamond with the grain diameter of 6-10nm synthesized by an air cooling detonation method, deionized water and fatty alcohol polyoxyethylene ether ammonium sulfate are placed into a container, and mixed, dispersed and stirred for 20-30 minutes under the action of ultrasound, so that a nano-diamond solution can be obtained, wherein the adding amount of the fatty alcohol polyoxyethylene ether ammonium sulfate is 0.7-0.9 wt% of the mass of the nano-diamond solution, and the nano-diamond is from diamond synthesized by the air cooling detonation method; stirring and adding isoamyl nitrite into the prepared nano diamond solution, and adjusting the pH value, wherein the adding amount of the isoamyl nitrite is 1.0-1.2 wt% of the mass of the diamond pretreatment liquid to obtain the diamond pretreatment liquid, wherein the solid content concentration of the diamond pretreatment liquid is 11%, the conductivity is 170 mu S/cm, and the pH value is 9.5; adding the obtained diamond pretreatment solution into a bead mill with a screen for grinding, wherein the rotation speed of the bead mill is 5000min -1 The bead grinding time is 5-6 hours, and the grinding liquid is collected; and (3) performing ultrasonic dispersion on the grinding liquid for 0.5-0.8 h with power of 700W, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
Comparative example 1
Unlike example 3, the diamond pretreatment solution had a conductivity of 50. Mu.S/cm and a pH of 3.
Comparative example 2
Unlike example 6, the diamond pretreatment solution had a conductivity of 340. Mu.S/cm and a pH of 10.5.
Comparative example 3
The difference from example 2 is that no modifier is added.
Comparative example 4
Unlike example 4, no suspending agent was added.
The dispersion stability of the dispersions obtained in examples and comparative examples was evaluated, and after one month from the day of preparation of the dispersions, the particle diameters of the nanodiamond particles were measured, and the test results are shown in the following table.
The results show that the ultra-dispersed diamond suspension prepared by the invention has excellent dispersion stability even at high concentration, the diamond particle size is basically unchanged, and the dispersion liquid of the comparative example is coagulated to form a precipitate, so that the stability is obviously poor.
Finally, it should be noted that the above description is only a preferred embodiment of the present invention, and that many similar changes can be made by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The ultra-dispersed diamond suspension is characterized in that: a diamond suspension of 6-12% wt by mass of diamond particles having a particle size of 2-200 nm dispersed in a solvent.
2. The ultra-dispersed diamond suspension according to claim 1, wherein: the pH value of the suspension is 4-6, and the conductivity is less than 40 mu S/cm.
3. The ultra-dispersed diamond suspension according to claim 1, wherein: the pH value of the suspension is 8-10, and the conductivity is less than 200 mu S/cm.
4. The ultra-dispersed diamond suspension according to claim 1, wherein: the mass fraction of the diamond suspension is 10-12%wt.
5. A method of preparing the ultra-dispersed diamond suspension according to claims 1-4, comprising the steps of:
s1, putting nano diamond, deionized water and a modifier into a container, and mixing, dispersing and stirring for 20-30 minutes under the action of ultrasound to obtain a nano diamond solution;
s2, stirring the nano-diamond solution prepared in the step S1, adding a suspending agent, and adjusting the pH value to obtain a diamond pretreatment solution;
s3, adding the diamond pretreatment liquid prepared in the step S2 into a bead mill with a screen for grinding, and collecting grinding liquid;
s4, performing ultrasonic dispersion on the grinding liquid, and centrifugally collecting supernatant to obtain the ultra-dispersed nano-diamond suspension.
6. The method of manufacturing according to claim 5, wherein: the nanodiamond is derived from diamond synthesized by an air-cooled detonation method.
7. The method of manufacturing according to claim 5, wherein: the modifier is one or more of fatty alcohol polyoxyethylene ether ammonium sulfate and linear alkyl benzene sodium sulfonate, and the mass fraction of the modifier in the nano diamond solution is 0.5-1.0%.
8. The method of manufacturing according to claim 5, wherein: the suspending agent is one or more of isoamyl nitrite and fatty acid polyethylene glycol ester, and the mass fraction of the suspending agent in the diamond pretreatment liquid is 0.8-1.2%.
9. The process according to claim 5, wherein in S3, the rotation speed of the bead mill is 4000 to 5000min -1 The bead grinding time is 3-6 hours.
10. The method according to claim 5, wherein in S4, the ultrasonic dispersion time is 0.5-1 h and the power is 500-700W.
CN202310554194.9A 2023-05-17 2023-05-17 Super-dispersed diamond suspension and preparation method thereof Pending CN116589928A (en)

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