CN101007252B - Apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond and its producing method - Google Patents
Apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond and its producing method Download PDFInfo
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Abstract
The invention involves a nano-diamond powder and its production methods, particularly relates to nanometer, sub-micron ultra-fine and super scattering diamond powder which apparent granularity peak value can be controlled and production methods. The ultra-fine and super scattering diamond powder in the invention which apparent granularity peak value can be controlled has a series of product with granularity peak value from 50 nm to 500 nm, it has higher ZETA electric potential value when scatters in water and can scatters steadily in water media or straight-chain paraffin media and maintain long-term stability scattering status. The production method in the invention of ultra-fine and super scattering diamond powder which apparent granularity peak value can be controlled uses the nano-diamond which synthesized by negative-oxygen-balanced explosive detonation as raw material, purifies chemically and surface modifies, uses gravitional settling or centrifugal separation, classifies through adjusti the depositing time or the rotary speed of centrifugal machine to gain wet powder with different granularities, then washes the powder in organic solvent and prepares the product after low temperature normal atmosphere dried or vacuum dried under the condition of temperature<=80DEG C.
Description
One, technical field: the present invention relates to a kind of Nano diamond micro mist and production method thereof, particularly relate to the controllable nanoscale of a kind of apparent particle size peak value, submicron-grade superfine, ultra-dispersed diamond micro mist and production method thereof.
Two, technical background: adopt the synthetic Nano diamond of oxygen negative explosive detonation, has the superpower hardness of diamond, the nano-meter characteristic that has the excellence of nano material simultaneously, under electron microscope, observe, the synthetic Nano diamond of detonation has perfectly round profile, does not have tangible crystal face and sharp-pointed corner angle to exist.When nanoscale that surpasses flatness and Subnano-class polishing attrition process, can obtain fabulous surface roughness.When using as lubricating additive, the friction condition of friction pair has greatly been improved on perfectly round surface, has reduced friction loss, therefore is excellent grinding-material and lubriation material.
Because the complex chemical reaction of detonation process, actual product is the mixture of Nano diamond and nano-graphite micro mist.Nano diamond wherein is the aggregate that is formed in the effect by physics and chemistry of the diamond particles of 5～10nm by elementary particle, its particle diameter distributes from tens nanometers to tens micron continuous distributed, and general process for dispersing can not open it to the nano particle size level fully and keep the stable dispersion state.The Nano diamond of reporting in the document is not classified product mostly at present, though have the basic granules of nanometer, actual acquisition product is submicron order even micron-sized aggregate, can't bring into play the nano-meter characteristic of Nano diamond in actual applications.Permitted to wait the people to describe in the aqueous medium on the sunny side and modification processing method (30～34 pages of Chinese powder technology 2003 the 9th the 4th phases of volume of Nano diamond in the white oil medium, mining metallurgical engineering was rolled up 61～64 pages of the 4th phases in 2004 the 24th), but the not description of Nano diamond that obtains required granularity handled for how carrying out classification.Patent CN1560161A has described the method that the Nano diamond modification is handled, and how product is not carried out classification to obtain the product of desired particle size value but have to solve.Though the method that patent CN1203915C has proposed to adopt film to separate realizes carrying out classification according to granularity; but operating system complexity and can not control change of size easily; the output of product is lower; and can not adapt in the real work for the requirement that obtains multiple apparent particle size distribution of products, not possess actual large-scale production ability.How to control particle diameter effectively and distribute, realize that scale, the suitability for industrialized production of product is the technical problem that needs to be resolved hurrily.
Three, summary of the invention:
Purpose of the present invention: solve the deficiency that prior art exists, a kind of novel controlled nanoscale, submicron-grade superfine oversubscription of apparent particle size peak value synthetic Nano diamond micro mist of detonation that looses is provided, and production method that can scale.
Technical scheme of the present invention: a kind of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond be the apparent particle size peak value at 50nm to the series of products between the 500nm, ZETA current potential absolute value 〉=35mv when in aqueous medium, disperseing, through mixing in aqueous medium or the linear paraffin medium in can stable dispersion, can keep the stable dispersion state at 10～20 days, this ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond is to make with following method: the Nano diamond that detonation is synthetic is through the wet chemistry purified treatment, remove graphite and other impurity, it is 2～10% suspension that Nano diamond after purifying is mixed with concentration, add surface modifier, after ultrasonic being uniformly dispersed, use gravitational settling or centrifugal separation to carry out grain size grading, with the varigrained wet Nano diamond powder that obtains, behind organic solvent washing, low-temperature atmosphere-pressure drying or vacuum drying obtain product under≤80 ℃ condition.。
These ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond series of products comprise that apparent particle size is the diadust of 50 nanometers, apparent particle size is the diadust of 80 nanometers, apparent particle size is the diadust of 100 nanometers, apparent particle size is the diadust of 200 nanometers, apparent particle size is the diadust of 300 nanometers, and apparent particle size is the diadust of 500 nanometers.
A kind of production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond, adopting the synthetic Nano diamond of oxygen negative explosive detonation is raw material, the Nano diamond that detonation is synthetic is through the wet chemistry purified treatment, remove wherein graphite and other impurity, it is 2～10% suspension that Nano diamond after purifying is mixed with concentration, add surface modifier, after ultrasonic being uniformly dispersed, use gravitational settling or centrifugal separation to carry out grain size grading, with the varigrained wet Nano diamond powder that obtains, behind organic solvent washing, low-temperature atmosphere-pressure drying or vacuum drying obtain product under≤80 ℃ condition; It is the mixed acid that adopts red fuming nitric acid (RFNA), sulfuric acid and perchloric acid that described chemical cleaning method is handled, under 180～220 ℃ temperature conditions, the Nano diamond reaction that itself and detonation is synthetic, described red fuming nitric acid (RFNA), sulfuric acid and perchloric acid are analyzes pure or guaranteed reagent, nitric acid, sulfuric acid, perchloric acid volume ratio are 1～2: 1～2: 1～5, and the Nano diamond weight of material ratio 〉=4 that the total amount of the mixed acid of used red fuming nitric acid (RFNA), sulfuric acid and perchloric acid is synthetic with detonation.。
Described ultrasonic dispersion, supersonic frequency 20～40kHz, power 300～800W, ultrasonic time 20～40 minutes.
Described surface modifier be in anionic surfactant, non-ionic surface active agent, the stabilizing polymer dispersant one or both and more than.
Described surface modifier consumption is 0.1～1% of the back Nano diamond consumption of purifying; Described anionic surfactant is neopelex, sodium stearyl sulfate, enuatrol, triethanolamine oleate, glyceryl monolaurate sulfate, ethoxylated dodecyl alcohol sodium sulphate, lauramide SES; Described non-ionic surface active agent is alkylphenol-polyethenoxy base ether, lauroyl diethanolamine, sorbitan mono-laurate, anhydrous sorbitol monopalmitate polyoxyethylene (20), sorbitan monostearate, polyglycereol poly monoricinolein; Described macromolecular dispersion stabilizer is polyglycerol fatty acid propylene alcohol ester sodium sulfonate, polyacrylamide, Sodium Polyacrylate, polyvinyl alcohol, polyethylene glycol.
The production method of described apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond, settling methods classification are to carry out grain size grading, sedimentation time 〉=120h by the regulation and control sedimentation time.
The production method of described apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond, centrifugal separation classification are to carry out grain size grading, centrifuge speed 3000～8000rpm, 30～60 minutes centrifugation time by the regulation and control centrifuge speed.
The production method of described apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond, organic solvent are absolute ethyl alcohol, or are acetone.
Positive beneficial effect of the present invention:
1. apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond of the present invention, its apparent particle size peak value is from 50nm to 500nm, can satisfy the needs of different grain size requirement, metals content impurity is low, below 50 μ g/g, and product has good dispersive property, can the stable for extended periods of time dispersity when disperseing in aqueous medium or in other medium, can keep the stability of its performance.
2. apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond production method of the present invention by chemical cleaning method processing and surface modification treatment, can guarantee that product has high purity and good dispersive property.
3. apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond production method of the present invention, adopt gravitational settling or centrifugal separation to carry out grading, can obtain the Nano diamond powder of different grain size requirement by regulation and control sedimentation time or centrifugation rotating speed, and it is simple that gravitational settling or centrifugal separation are carried out grading, easy to operate.
4. apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond production method of the present invention, step is simple, and is easy to operate, and cost is low, can large-scale industrial production.
Four, Figure of description:
Fig. 1: 100nm ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond granularity Detection report
Fig. 2: 200nm ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond granularity Detection report
Five, the specific embodiment:
Embodiment one: the column TNT/RDX composite explosives (TNT+RDX=1+1) of 500g are placed 4m
3The steel high-pressure closed vessel in, use electric cap to ignite, carry out the detonation synthetic reaction.The repetition aforesaid operations is repeatedly opened a jar collection detonation product, removes the residual foreign material of blast, drying, the mixed black powder of acquisition Nano diamond and graphite.Get 200g mixed black powder, place the corrosion-resistant and high-temperature resistant container, add 2000ml mixed acid, (mixed acid is: nitric acid+hydrofluoric acid+perchloric acid=1+1+5), be heated to 220 ℃, kept about 4 hours, and become light gray to the mixing material color, stop heating.Be cooled to room temperature, use washed with de-ionized water to neutral, obtain the pure nano diamond, adopt atomic absorption spectrophotometer or high-frequency inductor coupled plasma emission spectrometer to measure the metal impurities of surface absorption, total impurities content is lower than 50 μ g/g.
The pure Nano diamond that obtains is mixed with the suspension of concentration 3%, places the classification of sedimentation bottle standing sedimentation, set the extraction time, from 1/3 extraction upper strata suspension highly.Change time parameter, repeat the suspension that aforesaid operations obtains the different grain size value.Ratio according to 0.5% adds anionic surfactant sodium dodecylbenzene sulfonate, or triethanolamine oleate, or ethoxylated dodecyl alcohol sodium sulphate, stir ultrasonic dispersion 40 minutes, concentrated suspension liquid, obtain moisture wet powder, with absolute ethanol washing 1～2 time, place vacuum drying chamber in 75 ℃ of vacuum drying, obtain the super-dispersed nano diamond powder that different grain size requires.The varigrained Nano diamond micro mist with fine dispersion effect of table 1 for obtaining by the regulation and control sedimentation time.
Table 1 gravitational settling grading result
| Sequence number | Sedimentation time (h) | Granularity (nm) |
| 1 | 120 | 500 |
| 2 | 200 | 300 |
| 3 | 280 | 200 |
| 4 | 360 | 100 |
| 5 | 480 | 80 |
Adopt varigrained each 1g of Nano diamond powder of above-mentioned acquisition, add the 100ml deionized water, under 1000rpm, mixed 1 hour with electric blender, adopt the HORIBALA920 laser particle analyzer to test, the Nano diamond product test result of 100nm, 200nm is shown in accompanying drawing 1,2, and its granularity peak value is consistent with the numerical value of product indicia.It is carried out the ξDian Wei test, and its potential value shows that it has good dispersiveness more than 35mv; Carry out the dispersing and settling test, product can keep the stable suspersion more than 10～20 days to disperse.The Zeta potential and the dispersing and settling result of 1% suspension that table 2 is prepared for varigrained Nano diamond powder.
The Zeta potential of table 2 Nano diamond 1% suspension and dispersing and settling result
| Sequence number | Granularity peak value (nm) | Zeta potential (mv) | The dispersing and settling test | |
| Observation in 24 hours | Observation in 480 |
|||
| 1 | 500 | 35 | No layering | No layering, the bottom small amount of |
| 2 | 300 | 37 | No layering | No layering, nothing |
| 3 | 200 | 35 | No layering | No layering, nothing |
| 4 | 100 | 38 | No layering | No layering, nothing |
| 5 | 80 | 40 | No layering | No layering, nothing precipitation |
Embodiment two: the basic operation of detonation method synthesizing nano diamond and method of purification thereof are with embodiment one, no longer describe in detail, difference is that it is 9% suspension that the pure Nano diamond powder that will obtain is mixed with concentration, ratio according to 0.9% adds the non-ionic surface active agent sorbitan monostearate, or alkylphenol-polyethenoxy base ether, or lauroyl diethanolamine, or polyglycereol poly monoricinolein, stir, ultrasonic dispersion placed the Centrifuge Cup of supercentrifuge after 20 minutes, set different rotating speeds and centrifugation time, collect supernatant liquid, concentrate, obtain wet powder, add acetone washing 1～3 time, in electrically heated drying cabinet, in 65 ℃ of dry down, that the acquisition different grain size requires super-dispersed nano diamond powders.The varigrained Nano diamond micro mist with fine dispersion effect of table 3 for obtaining by the regulation and control centrifuge speed.
Table 3 centrifugation grading result
| Sequence number | Centrifuge speed, rpm | Time, min | Granularity, |
| 1 | 3000 | 40 | 500 |
| 2 | 4000 | 40 | 300 |
| 3 | 4500 | 40 | 200 |
| 4 | 5000 | 40 | 100 |
| 5 | 6000 | 60 | 80 |
| 6 | 8000 | 60 | 50 |
Adopt varigrained each 1g of Nano diamond powder of above-mentioned acquisition, add the 100ml deionized water, under 1000rpm, mixed 1 hour with electric blender, it is carried out the ξDian Wei test, its potential value is between 35～43mv, show that it has good dispersiveness, carry out the dispersing and settling test, the stable suspersion that sample can keep 10～20 days disperses.The Zeta potential and the dispersing and settling result of the test of 1% suspension that table 4 is prepared for varigrained Nano diamond powder.
The Zeta potential of table 41% suspension and dispersing and settling result of the test
| Sequence number | The granularity peak value, nm | Zeta potential, mv | The dispersing and settling test | |
| Observation in 24 hours | Observation in 480 |
|||
| 1 | 500 | 38 | No layering | No layering, nothing |
| 2 | 300 | 41 | No layering | No layering, nothing |
| 3 | 200 | 40 | No layering | No layering, nothing |
| 4 | 100 | 43 | No layering | No layering, nothing |
| 5 | 80 | 41 | No layering | No layering, nothing |
| 6 | 50 | 41 | No layering | No layering, nothing precipitation |
Embodiment three: the basic operation of detonation method synthesizing nano diamond and method of purification thereof are with embodiment one, no longer describe in detail, difference is that it is 5% suspension that the pure Nano diamond powder that will obtain is mixed with concentration, ratio according to 0.1% adds macromolecular dispersion stabilizer polyglycerol fatty acid propylene alcohol ester sodium sulfonate, or polyacrylamide, or polyethylene glycol, stir, ultrasonic dispersion is after 30 minutes, place the Centrifuge Cup of supercentrifuge, set different rotating speeds and centrifugation time, collect supernatant liquid, concentrate, obtain wet powder, add acetone washing 1～3 time, in electrically heated drying cabinet, in 65 ℃ of dry down, that the acquisition different grain size requires super-dispersed nano diamond powders.The varigrained Nano diamond micro mist with fine dispersion effect of table 5 for obtaining by the regulation and control centrifuge speed.
Table 5 centrifugation grading result
| Sequence number | Centrifuge speed, rpm | Time, min | Granularity, |
| 1 | 3000 | 40 | 500 |
| 2 | 4000 | 40 | 300 |
| 3 | 4500 | 40 | 200 |
| 4 | 5000 | 40 | 100 |
| Sequence number | Centrifuge speed, rpm | Time, min | Granularity, |
| 5 | 6000 | 60 | 80 |
| 6 | 8000 | 60 | 50 |
Claims (7)
1. the production method of an apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond, adopting the synthetic Nano diamond of oxygen negative explosive detonation is raw material, it is characterized in that: the Nano diamond that detonation is synthetic is through the wet chemistry purified treatment, remove wherein graphite and other impurity, it is 2～10% suspension that Nano diamond after purifying is mixed with concentration, add surface modifier, after ultrasonic being uniformly dispersed, use gravitational settling or centrifugal separation to carry out grain size grading, with the varigrained wet Nano diamond powder that obtains, behind organic solvent washing, low-temperature atmosphere-pressure drying or vacuum drying obtain product under≤80 ℃ condition; It is the mixed acid that adopts red fuming nitric acid (RFNA), sulfuric acid and perchloric acid that described chemical cleaning method is handled, under 180～220 ℃ temperature conditions, the Nano diamond reaction that itself and detonation is synthetic, described red fuming nitric acid (RFNA), sulfuric acid and perchloric acid are analyzes pure or guaranteed reagent, nitric acid, sulfuric acid, perchloric acid volume ratio are 1～2: 1～2: 1～5, and the Nano diamond weight of material ratio 〉=4 that the total amount of the mixed acid of used red fuming nitric acid (RFNA), sulfuric acid and perchloric acid is synthetic with detonation.
2. the production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond according to claim 1 is characterized in that: described ultrasonic dispersion, supersonic frequency 20～40kHz, power 300～800W, ultrasonic time 20～40 minutes.
3. the production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond according to claim 1 is characterized in that: described surface modifier be in anionic surfactant, non-ionic surface active agent, the stabilizing polymer dispersant one or both and more than.
4. the production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond according to claim 3 is characterized in that: described surface modifier consumption is 0.1～1% of the back Nano diamond consumption of purifying; Described anionic surfactant is neopelex, sodium stearyl sulfate, enuatrol, triethanolamine oleate, glyceryl monolaurate sulfate, ethoxylated dodecyl alcohol sodium sulphate, lauramide SES; Described non-ionic surface active agent is alkylphenol-polyethenoxy base ether, lauroyl diethanolamine, sorbitan mono-laurate, anhydrous sorbitol monopalmitate polyoxyethylene (20), sorbitan monostearate, polyglycereol poly monoricinolein; Described macromolecular dispersion stabilizer is polyglycerol fatty acid propylene alcohol ester sodium sulfonate, polyacrylamide, Sodium Polyacrylate, polyvinyl alcohol, polyethylene glycol.
5. the production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond according to claim 1 is characterized in that: described settling methods classification is to carry out grain size grading, sedimentation time 〉=120h by the regulation and control sedimentation time.
6. the production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond according to claim 1, it is characterized in that: described centrifugal separation classification is to carry out grain size grading by the regulation and control centrifuge speed, centrifuge speed 3000～8000rpm, 30～60 minutes centrifugation time.
7. the production method of apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond according to claim 1 is characterized in that: described organic solvent is an absolute ethyl alcohol, or is acetone.
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