CN104449400B - Corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder and preparation method - Google Patents
Corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder and preparation method Download PDFInfo
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- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The invention discloses a kind of corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder and preparation method thereof, after industrial carbonic acid lanthanum cerium is dissolved in diluted acid, add appropriate graphene oxide, urea and cationic surfactant cetyl trimethylammonium bromide, using microwave stirring hydrothermal chemistry method In-situ reaction to prepare nano lanthanum oxide cerium/graphene composite material, in cerium lanthanum oxide/graphene composite material, Graphene content is 0.3-1.5%.Nano lanthanum oxide cerium of the present invention/graphene composite material outward appearance main body pattern is corn shape, the iblet structure of body surfaces is nano-scale particle, preparation method uses heating using microwave, stirring, technique is advanced, and the reaction time is short, low cost, glass being thrown erosion amount high, glass surface, without scratching, is particularly suitable for the precise polished of the goods such as smart mobile phone display screen, optical glass.
Description
Technical field
The present invention relates to field of nano material preparation, particularly to a kind of corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder and preparation method.
Background technology
Polishing powder from rare earth is with the physics of its uniqueness, chemical characteristic and excellent polishing performance and be widely used in display screen glass, optical glass, the glass devices such as Crystal ornaments and precision instrument precise polished, use at present more abrasive polishing materials to be cerium oxide in the world or cerium lanthanum oxide is the rare earth oxide of main component, these polishing powder from rare earth are many with water as dispersant, use after reconciling into slurry, but polishing powder from rare earth the most often occurs that suspension is poor, grinding efficiency is low, glass surface is easily scratched and blocks owing to particle precipitation is solidified into hard material the problems such as the technological parameter of circulating line or destruction setting, thus have impact on quality and the grinding efficiency of product.And generally solve the two problem and usually add suitable suspending agent and prepare special appearance and the polishing powder having particular particle size to be distributed, harsh to material preparation process and equipment requirement complexity, using effect but can not reach promising result.
Graphene, as the nano-carbon material of a kind of New Two Dimensional structure, is to be found first in 2004 by Novoselov et al., and rapidly becomes study hotspot.Graphene is the thinnest, the material of maximum intensity known today, has excellent conduction and the capacity of heat transmission, and has high rigidity and good ductility simultaneously, and these premium properties of Graphene make it have potential application prospect in a lot of fields.
The present invention is the disadvantages mentioned above during overcoming existing rare earth lanthanum oxide cerium polishing powder to use, it is breach from the nature of change polishing powder from rare earth cerium lanthanum oxide material, uses a kind of microwave hydrothermal chemical method quickly synthesizing nano level cerium lanthanum oxide/Graphene composite polishing material.
Summary of the invention
The technical problem to be solved is easily to scratch the defect of glass for glass polishing powder in prior art, a kind of corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder and preparation method are provided, graphene uniform is wrapped in cerium lanthanum oxide particle by the nano lanthanum oxide cerium/graphene composite material obtained, glass is thrown erosion amount high, the fragility of polishing powder can be relaxed in real time, thus avoiding the scuffing to glass, polishing performance is excellent.
For solve above-mentioned technical problem, the present invention by the following technical solutions:
A kind of corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder, in described nano lanthanum oxide cerium/graphene composite material, principal phase is lanthana and cerium oxide, and Graphene content is 0.3 ~ 1.5%.
Described corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder outward appearance main body pattern is that corn is bar-shaped.
The preparation method of the corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder of the present invention, step is as follows:
(1) being dissolved in deionized water by lanthanum carbonate cerium, obtain lanthanum carbonate cerium solution, in lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium is 0.1 ~ 0.5g/mL, is 6.5 ~ 7.0 by the pH value of diluted acid regulation lanthanum carbonate cerium solution, obtains solution A；
(2) graphene oxide solution and urea, cetyl trimethylammonium bromide that concentration is 0.5 ~ 1.5g/L being mixed, obtain solution B, wherein the mass ratio of graphene oxide solution, urea and cetyl trimethylammonium bromide is 1:300 ~ 600:20 ~ 80；
(3) 40 ~ 60mL solution A and 25 ~ 50mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 20 ~ 30min, after being further continued for being warmed up to 170 DEG C ~ 200 DEG C insulation 30 ~ 60min, naturally cooling is precipitated thing, and sediment is scrubbed, be dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
In described step (1), the concentration of diluted acid is 0.5 ~ 2.0 mol/L.
One or more mixtures that diluted acid is dust technology, watery hydrochloric acid or dilute sulfuric acid in described step (1).
Lanthanum in lanthanum carbonate cerium in described step (1), cerium atom number than for 1:2 ~ 1:10.
Washing in described step (3) uses centrifugal, filtering and washing or press filtration washing.
Graphene oxide solution used in the present invention is the graphene oxide solution using the Hummers method improved to prepare.(preparation method sees M.
Inagaki, Y. A. Kim and M. Endo, Graphene:preparation and
Structural perfection, J. Mater. Chem.,
2011,21,3280 ~ 3294)
Described corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder for smart mobile phone display screen, optical glass precise polished.
Beneficial effects of the present invention: the corn shape nano lanthanum oxide cerium of (1) present invention/Graphene compound rare-earth polishing powder outward appearance main body pattern is unique, bar-shaped in corn, the iblet structure of body surfaces is nano-scale particle, glass is thrown erosion amount high, glass surface is without scratching, being particularly suitable for the precise polished of the goods such as smart mobile phone display screen, optical glass, polishing performance is excellent.(2) the apparent grain size of polishing powder needed for the corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder of the present invention does not only reach polished glass, nanostructured (small-size effect of nano particle) and the relaxation layer (Graphene has excellent heat conduction and ductility) of Graphene that its corn is granular in turn ensure that glass surface is not scratched, graphene uniform is wrapped in particle, based on rare earth oxide, during polishing powder from rare earth polished glass, composite is constantly abraded, Graphene engenders, relax the fragility of polishing powder in real time, thus avoid the scuffing to polishing object (glass).(3) present invention uses liquid phase environment, and omnidistance stirring in microwave process, it is ensured that the mixing of each material, the uniformity of reaction, technique is advanced, and the reaction time is short, low cost.(4) use the graphene oxide solution of excellent performance well prepared in advance, it is ensured that the purity of Graphene in product composite, thus improve the purity of end product.
Accompanying drawing explanation
Fig. 1 is the SEM figure of corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder of the present invention；
Fig. 2 is the XRD of corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder of the present invention；
Fig. 3 is heating curve and corresponding pressure, microwave output power figure in the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is elaborated.
Embodiment 1
Weigh 8.9305 g industrial carbonic acid lanthanum cerium (atomic ratio La:Ce=1:2) to be dissolved in 50.00 ml deionized waters, it is slowly added to dust technology, stop when solution ph is 6.5 ~ 7.0 adding, again 13.5112g urea and 1.0g CTAB being added 25.0mL concentration is the graphene oxide solution of 1.0mg/mL, above two solution is slowly mixed together, add deionized water to mix and constant volume makes whole liquor capacity reach 120mL, proceed in microwave hydrothermal retort, under constant agitation, from room temperature to 85 DEG C and after being incubated 20 min in 5 min, in 15min, it is warmed up to 180 DEG C and is incubated 60 min, obtain linen cerium lanthanum oxide/Graphene compound rare-earth polishing powder.As shown in Figure 1a, as shown in fig. 1b and fig. lc, the body contours of gained composite is corn club shaped structure to partial enlarged drawing to the shape appearance figure of resulting materials, a length of 5 ~ 8 m, and the iblet structure of the bar-shaped body surfaces of corn is nano-scale particle；Its XRD spectra is as in figure 2 it is shown, comparison PDF card 34 ~ 0394 and 22 ~ 0369 understands, and gained material principal phase is CeO2And La2O3Mixture, its powder is grey, and pure zirconia cerium and lanthanum oxide powder are the most white, may determine that product is corn shape nano lanthanum oxide cerium/graphene composite material in conjunction with preparation technology.Fig. 3 is the present embodiment heating curve and corresponding pressure, microwave output power figure, and its preferred equipment is new instrument MWAVE ~ 5000, Shanghai multifunction microwave chemical reaction instrument.
Embodiment 2
Weigh 7.6860 g industrial carbonic acid lanthanum cerium (atomic ratio La:Ce=1:2) to be dissolved in 50.00 mL deionized waters, it is slowly added to watery hydrochloric acid, stop when solution ph is 6.5 ~ 7.0 adding, again 10.8876g urea and 2.5g CTAB being added 40.0mL concentration is the graphene oxide solution of 1.0mg/mL, above two solution is slowly mixed together, add deionized water to mix and constant volume makes whole liquor capacity reach 120mL, proceed in microwave hydrothermal retort, under constant agitation, from room temperature to 85 DEG C and after being incubated 25 min in 5 min, in 15min, it is warmed up to 200 DEG C and is incubated 30 min, obtain linen cerium lanthanum oxide/Graphene compound rare-earth polishing powder.
Embodiment 3
Weigh 10.2784 g industrial carbonic acid lanthanum cerium (atomic ratio La:Ce=1:2) to be dissolved in 50.00 mL deionized waters, it is slowly added to dilute sulfuric acid, stop when solution ph is 6.5 ~ 7.0 adding, again 15.6840g urea and 2.02 CTAB being added 20.0mL concentration is the graphene oxide solution of 1.0mg/mL, above two solution is slowly mixed together, add deionized water to mix and constant volume makes whole liquor capacity reach 120mL, proceed in microwave hydrothermal retort, under constant agitation, from room temperature to 85 DEG C and after being incubated 30 min in 5 min, in 15min, it is warmed up to 170 DEG C and is incubated 45 min, obtain linen cerium lanthanum oxide/Graphene compound rare-earth polishing powder.
Embodiment 4
The preparation method of the nano lanthanum oxide cerium of the present embodiment/Graphene compound rare-earth polishing powder, step is as follows:
(1) by lanthanum carbonate cerium (lanthanum, cerium atom number than for 1:10) be dissolved in deionized water, obtain lanthanum carbonate cerium solution, in lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium is 0.1g/mL, is 6.5 by the pH value that concentration is 0.5mol/L dust technology regulation lanthanum carbonate cerium solution, obtains solution A；
(2) graphene oxide solution 1g and urea 300g, cetyl trimethylammonium bromide 20g that concentration is 0.5g/L are mixed, obtain solution B；
(3) 40mL solution A and 25mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 20min, after being further continued for being warmed up to 170 DEG C of insulation 60min, naturally cooling is precipitated thing, sediment by centrifugation, filtering and washing, be dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
Embodiment 5
The preparation method of the nano lanthanum oxide cerium of the present embodiment/Graphene compound rare-earth polishing powder, step is as follows:
(1) by lanthanum carbonate cerium (lanthanum, cerium atom number than for 1:5) be dissolved in deionized water, obtain lanthanum carbonate cerium solution, in lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium is 0.5g/mL, is 7.0 by the pH value that concentration is 2.0 mol/L watery hydrochloric acid regulation lanthanum carbonate cerium solution, obtains solution A；
(2) graphene oxide solution and 600g urea, 80g cetyl trimethylammonium bromide that 1 g concentration is 1.5g/L are mixed, obtain solution B；
(3) 60mL solution A and 50mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 30min, after being further continued for being warmed up to 200 DEG C of insulation 30min, naturally cooling is precipitated thing, scrubbed centrifugal, the press filtration washing of sediment, is dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
Embodiment 6
The preparation method of the nano lanthanum oxide cerium of the present embodiment/Graphene compound rare-earth polishing powder, step is as follows:
(1) by lanthanum carbonate cerium (lanthanum, cerium atom number than for 1:4) be dissolved in deionized water, obtain lanthanum carbonate cerium solution, in lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium is 0.1g/mL, is 6.8 by the pH value that concentration is 1.0mol/L dilute sulfuric acid regulation lanthanum carbonate cerium solution, obtains solution A；
(2) graphene oxide solution and 400 g urea, 50 g cetyl trimethylammonium bromides that 1 g concentration is 1.0g/L are mixed, obtain solution B；
(3) 50mL solution A and 40mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 25min, after being further continued for being warmed up to 180 DEG C of insulation 50min, naturally cooling is precipitated thing, sediment by centrifugation, filtering and washing, be dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
Embodiment 7
The preparation method of the nano lanthanum oxide cerium of the present embodiment/Graphene compound rare-earth polishing powder, step is as follows:
(1) by lanthanum carbonate cerium (lanthanum, cerium atom number than for 1:6) be dissolved in deionized water, obtain lanthanum carbonate cerium solution, in lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium is 0.2g/mL, it is 6.5 by the pH value of the mixed solution regulation lanthanum carbonate cerium solution that concentration is 1.5mol/L dust technology and watery hydrochloric acid, obtains solution A；
(2) graphene oxide solution and 500 g urea, 60 g cetyl trimethylammonium bromides that 1 g concentration is 1.2g/L are mixed, obtain solution B；
(3) 45mL solution A and 30mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 28min, after being further continued for being warmed up to 190 DEG C of insulation 40min, naturally cooling be precipitated thing, sediment by centrifugation, press filtration washing, be dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
Embodiment 8
The preparation method of the nano lanthanum oxide cerium of the present embodiment/Graphene compound rare-earth polishing powder, step is as follows:
(1) by lanthanum carbonate cerium (lanthanum, cerium atom number than for 1:8) be dissolved in deionized water, obtain lanthanum carbonate cerium solution, in lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium is 0.3g/mL, is 7.0 by the pH value that concentration is 0.5mol/L dust technology regulation lanthanum carbonate cerium solution, obtains solution A；
(2) graphene oxide solution and 450 g urea, 30 g cetyl trimethylammonium bromides that 1g concentration is 0.8g/L are mixed, obtain solution B；
(3) 55mL solution A and 35mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 22min, after being further continued for being warmed up to 175 DEG C of insulation 50min, naturally cooling is precipitated thing, sediment by centrifugation, filtering and washing, be dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
Nano lanthanum oxide cerium/Graphene polishing powder for smart mobile phone display screen, optical glass precise polished:
Embodiment 1 ~ 8 gained cerium lanthanum oxide/graphene composite material is made into the polishing fluid slurries that concentration is 100g/L.Use YM015.1
(Nanjing profit the third contact of a total solar or lunar eclipse scholar Machinery Co., Ltd.) precise grinding polisher is to 39
K9 glass is polished, and automatic stirring is pulled an oar, and polishing arbor rotating speed is 100r/min, pressure is 1Kg, and polished leather is KSP90 ~ 0.8, and polishing time is 1.0 hours, every 20min record wash dried glass quality, polishing terminate after in darkroom sight glass scratch situation.According to weighed polished glass quality before and after polished divided by polishing time and transparency area, (unit is: mg/min.cm to calculate throwing erosion amount2, it is designated as S20min, S40min, S60min) and average throwing erosion amount (SAveragely), comparative example is industrial oxidation lanthanum cerium mischmetal polishing powder material.Its result of implementation is as shown in table 1.
Table 1 implementation result contrast table
| S20min | S40min | S60min | SAveragely | Surface tear situation | |
| Embodiment 1 | 0.036 | 0.038 | 0.040 | 0.038 | Nothing |
| Embodiment 2 | 0.035 | 0.039 | 0.042 | 0.039 | Nothing |
| Embodiment 3 | 0.034 | 0.038 | 0.040 | 0.037 | Nothing |
| Embodiment 4 | 0.037 | 0.038 | 0.042 | 0.039 | Nothing |
| Embodiment 5 | 0.038 | 0.037 | 0.042 | 0.039 | Nothing |
| Embodiment 6 | 0.036 | 0.038 | 0.040 | 0.038 | Nothing |
| Embodiment 7 | 0.039 | 0.037 | 0.040 | 0.039 | Nothing |
| Embodiment 8 | 0.035 | 0.038 | 0.042 | 0.038 | Nothing |
| Comparative example | 0.024 | 0.026 | 0.025 | 0.025 | There is scuffing |
Result shows, the composite of preparation is thrown erosion amount and is greatly improved than general industry cerium lanthanum oxide, and glass surface is without scratching.
The present invention is compared with prior art, have the advantage that nano lanthanum oxide cerium/Graphene rare earth composite material pattern prepared by the present invention is unique, high to the throwing erosion amount of glass, glass, without scratching, is suitable for the precise polished of smart mobile phone display screen, optical instrument precision camera lens etc..Preparation method uses heating using microwave, is aided with stirring, and technique is advanced, and the reaction time is short, low cost.
The general principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and specification; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within scope of the claimed invention.
Claims (7)
1. corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder, it is characterised in that: in described nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder, principal phase is lanthana and cerium oxide, and Graphene content is 0.3 ~ 1.5%；The preparation method of described corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder, it is characterised in that step is as follows:
(1) lanthanum carbonate cerium is dissolved in deionized water, obtains lanthanum carbonate cerium solution, the concentration of lanthanum carbonate cerium in lanthanum carbonate cerium solution
It is 0.1 ~ 0.5g/mL, is 6.5 ~ 7.0 by the pH value of diluted acid regulation lanthanum carbonate cerium solution, obtains solution A；
(2) graphene oxide solution and urea, cetyl trimethylammonium bromide that concentration is 0.5 ~ 1.5g/L are mixed
Uniformly, obtaining solution B, wherein the mass ratio of graphene oxide solution, urea and cetyl trimethylammonium bromide is 1:300 ~ 600: 20 ~ 80；
(3) 40 ~ 60mL solution A and 25 ~ 50mL solution B are added microwave hydrothermal reaction kettle to be sufficiently mixed, stirring is warmed up to 85 DEG C of insulation 20 ~ 30min, after being further continued for being warmed up to 170 DEG C ~ 200 DEG C insulation 30 ~ 60min, naturally cooling is precipitated thing, and sediment is scrubbed, be dried to obtain nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder.
2. according to the corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder described in claim 1, it is characterised in that: described nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder outward appearance main body pattern is that corn is bar-shaped.
Corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder the most according to claim 1, it is characterised in that: in described step (1), the concentration of diluted acid is 0.5 ~ 2.0 mol/L.
Corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder the most according to claim 1, it is characterised in that: one or more mixtures that diluted acid is dust technology, watery hydrochloric acid or dilute sulfuric acid in described step (1).
Corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder the most according to claim 1, it is characterised in that: in described step (1), in lanthanum carbonate cerium, lanthanum, the atom number ratio of cerium are 1: 2 ~ 1: 10.
Corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder the most according to claim 1, it is characterised in that: the washing in described step (3) uses centrifugal, filtering and washing or press filtration washing.
7. in claim 1 ~ 6 corn shape nano lanthanum oxide cerium/Graphene compound rare-earth polishing powder described in any one for smart mobile phone display screen, optical glass precise polished.
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