CN104229853A - Preparation method of self-lubrication material nanometer calcium fluoride for ceramic cutting tool - Google Patents
Preparation method of self-lubrication material nanometer calcium fluoride for ceramic cutting tool Download PDFInfo
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- CN104229853A CN104229853A CN201410441908.6A CN201410441908A CN104229853A CN 104229853 A CN104229853 A CN 104229853A CN 201410441908 A CN201410441908 A CN 201410441908A CN 104229853 A CN104229853 A CN 104229853A
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Abstract
The invention relates to a preparation method of a self-lubrication material nanometer calcium fluoride for a ceramic cutting tool. The preparation method comprises the following steps: (1) weighing calcium nitrate and ammonium fluoride, respectively placing in a beaker, adding distilled water and anhydrous ethanol, to obtain a calcium nitrate liquid with content of calcium nitrate being 1mol/l, and an ammonium fluoride liquid with content of ammonium fluoride being 2.2-3.2mol/l; (2) weighing a certain amount of polyethylene glycol (PEG6000) dispersing agent with molecular weight of 6000, adding the ammonium fluoride liquid so that the mass fraction of the polyethylene glycol in the liquid is 1-2%; performing ultrasonic dispersion for 10-15min, thoroughly dissolving, to obtain a polyethylene glycol-ammonium fluoride complex liquid; and (3) placing the polyethylene glycol-ammonium fluoride complex liquid into a magnetic stirrer, setting the reaction temperature of 15-50DEG C, dropping the calcium nitrate liquid in the polyethylene glycol-ammonium fluoride complex liquid through a separating funnel, appropriately adjusting the speed to be close to flow-in speed (drop-in speed is 1-30ml/min), wherein the stirring frequency under which no liquid is splashed is the best. The prepared nanometer calcium fluoride powder is high in purity, complete in crystal form, high in crystal degree, uniform in size distribution, and good in dispersity.
Description
Technical field
The invention belongs to chemical field, relate to a kind of preparation method of sintex self-lubricating material nano calcium fluoride.
Background technology
Self-lubricating knife tool refers to that cutter material itself has antifriction, wear-resistant and lubricating function, can realize self-lubricating machining under the condition without additional lubricating fluid or lubricant, significantly can improve the friction, lubrication state of dry cutting process.Solid lubricant is directly added in cutter material, is prepared into the compound tool containing solid lubricant.During dry cutting, the solid lubricant of cutter rake face is owing to being subject to the effect of high temperature, friction and cutting force, be " squeezed. " out tool surface, under cutting temperature effect, solid lubricant is in plastic state and is dragged and spreads on tool surface, form solid profit film, thus give the self-lubricating property of cutter.Improve the aspects such as surfaceness and also play effective effect.
Calcium Fluoride (Fluorspan) (CaF
2) be that one commonly uses solid lubricant when preparing self-lubrication ceramic compound tool.Adding solid lubricant is the compound tool preparing self-lubricating material.The frictional coefficient of they and metallic substance can be reduced to 0.11 ~ 0.12, is only 1/4 ~ 1/2 of universal cutter material.Solid lubricant has the features such as utmost carrying ability is high, stability at elevated temperature good, physical property change is little, under a particular job condition, have good lubricity.But there are some researches show, at A1
20
3solid lubricant CaF is added in/TiC sintex matrix
2improve its tribological property, prepare A1
2o
3/ TiC/CaF
2self-lubrication ceramic cutter, under identical machining condition, adds the A1 of solid lubricant
2o
3/ TiC/CaF
2the rubbing factor of self-lubricating knife tool is than the A1 not adding solid lubricant
2o
3/ TiC sintex significantly reduces, and the mechanical property of self-lubrication ceramic cutter material significantly reduces (being about 20%), and the range of application seriously limiting cutter (can see Deng Jianxin, Cao Tongkun, Ai Xing .A1
20
3/ TiC/CaF
2mechanism of Friction Reduction [J] in self-lubrication ceramic tool cutting process, mechanical engineering journal, 2006,7 (42): 109-112).
With micron and the nanometer Al of component
2o
3the relative density of/TiC cutter material is similar, but the bending strength of nano combined cutter material improves 23.5% and 74.5% than corresponding micron order complex cutter material respectively with fracture is hot, and hardness does not have large change (can see Song Shixue, Ai Xing, Zhao Jun .Al
2o
3the preparation of/TiC Nano-scale Ceramic Tool Material and Study on Cutting Performance [J]. China Mechanical Engineering, 2002 (17): 1523-1525).It can thus be appreciated that nano particle not only has good toughness, its intensity and hardness ratio common micro material also significantly improve.There is no commercial nano solid lubricant both at home and abroad for selecting, can limit the applied research of nano particle in tribological field at present.Zhou Yuxin etc. adopt percussion flow liquid-liquid reactions method to prepare CaF
2nano particle, see Zhou Yuxin, Zhu Huajuan.Impinging stream reaction-precipitator method prepare the light industry of nano calcium fluoride Guangxi, and 2010,26 (3): 17-19.Hua Ruinian etc. propose to adopt microemulsion method to prepare CaF2 nano particle, see Hua Ruinian, Lei Ping Fu, and the shed people. microemulsion method prepares CaF2 nano particle SCI .2003, and 24 (10): 1756-1757.Lv Yanfei, Wu Xijun, Wu great Xiong.The precipitation of nanophase CaF 2 and sign [J] in ethanol/water double solvents.Functional materials, 2006,7 (37): 1108-1111.
Chinese patent document CN101885505A provides a kind of preparation method of calcium fluoride hollow nanospheres, comprise: the first extracts composition formed with di-(2-ethylhexyl)phosphoric acid and organic solvent extracts the Ca2+ in the first feed liquid, obtain the first extraction liquid, described first feed liquid is ca nitrate soln or calcium chloride solution; The second extracts composition formed with secondary carbon primary amine and organic solvent extracts the F-in the second feed liquid, and obtain the second extraction liquid, described second feed liquid is hydrofluoric acid solution; By described first extraction liquid and described second extraction liquid mixing, reaction 0.1h ~ 24h, centrifugal, washing, obtains calcium fluoride hollow nanospheres after drying.Though the Calcium Fluoride (Fluorspan) that this invention obtains is nano level, it is hollow, can not for the preparation of self-lubricating knife tool material.
Summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides that a kind of crystal formation is complete, degree of crystallinity is high, the preparation method of the sintex self-lubricating material nano calcium fluoride of even size distribution.
the present invention is achieved through the following technical solutions:
The preparation method of sintex self-lubricating material nano calcium fluoride of the present invention, is characterized in that: comprise the following steps:
(1) according to mol ratio 1: the ratio of (2.2-3.2) takes nitrocalcite and Neutral ammonium fluoride, put into beaker separately, add distilled water and dehydrated alcohol, distilled water and dehydrated alcohol are with distilled water: the volume ratio mixing and stirring of dehydrated alcohol≤1, obtained nitrocalcite content is the ca nitrate soln of 1mol/l, and ammonium fluoride content is the ammonium fluoride solution of 2.2-3.2mol/l;
(2) polyoxyethylene glycol (PEG6000) dispersion agent that a certain amount of molecular weight is 6000 is taken, add ammonium fluoride solution, make the massfraction of polyoxyethylene glycol in solution be 1-2%, ultrasonic disperse 10-30min, dissolve completely, obtain polyoxyethylene glycol-Neutral ammonium fluoride composite solution;
(3) polyoxyethylene glycol-Neutral ammonium fluoride composite solution is put into magnetic stirring apparatus, temperature of reaction setting 15-50 DEG C, ca nitrate soln instills polyoxyethylene glycol-Neutral ammonium fluoride composite solution by separating funnel, conservative control instillation speed (instillation speed 1-30ml/min), stirring frequency is spattered for good so that solution is not outer;
(4) ca nitrate soln reacts 5-15min after dripping off under the condition of magnetic agitation, temperature of reaction 15-50 DEG C, takes out and puts into the ultrasonic 5-25min of ultrasonic stirrer; Then ageing 24-72h is placed;
(5) under 3000-4000r/min condition, centrifugation 10-20min is carried out, with washes of absolute alcohol 4-6 time, vacuum-drying 24-48h under 20-35 DEG C of condition; (state of the calcium fluoride melt solution before centrifugal is a kind of light blue suspension liquid of emulsus, forms white precipitate after centrifugation)
(6) nano calcium fluoride powder is obtained through mechanical mill.
Experiment concrete operation step and optimized choice::
1., in preferred step (1), the mol ratio of nitrocalcite and ammonium fluoride is 1: 3.0; The nitrocalcite content of ca nitrate soln is 1mol/l, and the ammonium fluoride content of ammonium fluoride solution is 3mol/l, and the volume ratio 1: 1 of distilled water and dehydrated alcohol mixes.The raw materials used nitrocalcite of the present invention and Neutral ammonium fluoride are commercially available prod, analytical pure.
2., in preferred step (2), in composite solution, the massfraction of polyoxyethylene glycol is 1.5%, and the ultrasonic disperse time is 15min.
3. in preferred step (3), polyoxyethylene glycol-Neutral ammonium fluoride composite solution is put into magnetic stirring apparatus, and temperature of reaction sets 35 DEG C, and ca nitrate soln instills polyoxyethylene glycol-Neutral ammonium fluoride composite solution by separating funnel, instillation speed is 10ml/min, and stirring frequency is spattered for good so that solution is not outer.
?4. in preferred step (4), temperature of reaction 35 DEG C, the reaction times is 5min; Ultrasonic time is 5min, places ageing 48h.
5., in preferred step (5), centrifuge speed is 3500r/min, disengaging time 15min, with washes of absolute alcohol 5 times, and vacuum-drying 24h under 35 DEG C of conditions.
Preparation method of the present invention adopts ultrasonic reduction method, with nitrocalcite and Neutral ammonium fluoride for raw material, is that the polyoxyethylene glycol (PEG6000) of 6000 prepares nano calcium fluoride by the precipitator method for dispersion agent with molecular weight.In self-lubrication ceramic complex cutter material field, nanoscale solids lubricant becomes the key factor affecting cutter mechanical property.But the preparation of nano level Calcium Fluoride (Fluorspan) is a difficult problem, and the present invention successfully prepares the grain diameter of nano calcium fluoride between 13-22nm always.Technical characterstic of the present invention is in Raw material processing and synthetic reaction process, adopt ultrasonic disperse and magnetic agitation dual function to ensure that building-up reactions is under the favourable condition of nanoprecipitation colloidal dispersions all the time, add PEG6000 and sterically hindered mechanism can improve the dispersiveness of nanometer powder, and introduce magnetic agitation can promote react quick, fully carry out, ensure the homogeneity of nanometer powder and small scale, simultaneous reactions fully to carry out also can eliminating in raw material calcium ion and nitrate ion to the impact of product purity.The present invention is based on the synergies such as ultrasonic disperse principle, sterically hindered mechanism and magnetic agitation, ensure that excellent results of the present invention.
the invention has the beneficial effects as follows, find through scanning electronic microscope (SEM) observation and X ray diffraction (XRD) analysis, energy spectrum analysis, the particle size of the preparation-obtained nano calcium fluoride of the present invention is between 13-22nm, and the particle size of the nano calcium fluoride obtained under the condition of embodiment 1 is about about 15nm.Purity is high, crystal formation is complete, degree of crystallinity is high, even size distribution, good dispersity, preparation process inclusion-free element is introduced, and technological process is simple, easy to operate, equipment requirements is low, the dehydrated alcohol consumption used is few, preparation process time is short, and what meet self-lubricating knife tool material completely prepares needs.
Accompanying drawing explanation
fig. 1 is scanning electronic microscope (SEM) photo of the nano calcium fluoride powder obtained by the embodiment of the present invention 1.
Embodiment
Embodiment 1
Take nitrocalcite 12.8g and Neutral ammonium fluoride 5.05g respectively according to the ratio of mol ratio 1:3.0, put into beaker separately, respectively add 25ml distilled water and 25ml dehydrated alcohol respectively, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solutions; Take the PEG6000 of 0.75g, add pre-assigned ammonium fluoride solutions, ultrasonic disperse 15min, make it dissolve completely, obtain the double solvents of polyoxyethylene glycol and ammonium fluoride solutions, wherein, the weight concentration of polyoxyethylene glycol PEG6000 is 1.5%.
Magnetic agitation temperature is set as 35 DEG C, under magnetic agitation condition, instills in (instillation speed is 10ml/min) scattered ammonium fluoride solution by ca nitrate soln fast by separating funnel, reaction 5min.Take out reacted solution and carry out ultrasonic disperse 5min, place ageing 48h.Under 3500r/min condition, carry out centrifugation 15min, with washes of absolute alcohol 5 times, vacuum-drying 24h under 25 DEG C of conditions, can obtain nano calcium fluoride powder through mechanical mill.
Observe according to XRD interpretation of result, calculating and SEM, the average particle size particle size of obtained nano calcium fluoride is 14.7nm, and crystal formation is complete, degree of crystallinity is high, even size distribution, good dispersity, and purity is more than 96.7%.
Embodiment 2
Take nitrocalcite 6.4g and Neutral ammonium fluoride 2.525g respectively according to the ratio of mol ratio 1:3.0, put into beaker separately, respectively add 12.5ml distilled water and 12.5ml dehydrated alcohol respectively, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solutions; Take the PEG6000 of 0.5g, add pre-assigned ammonium fluoride solutions, ultrasonic disperse 15min, make it dissolve completely, obtain the double solvents of polyoxyethylene glycol and ammonium fluoride solutions, wherein, the weight concentration of polyoxyethylene glycol PEG6000 is 2%.
Magnetic agitation temperature is set as 20 DEG C, under magnetic agitation condition, instills in (instillation speed is 1ml/min) scattered ammonium fluoride solution, reaction 5min by ca nitrate soln by separating funnel.Take out reacted solution and carry out ultrasonic disperse 5min, place ageing 48h.Under 3500r/min condition, carry out centrifugation 15min, with washes of absolute alcohol 5 times, vacuum-drying 24h under 25 DEG C of conditions, can obtain nano calcium fluoride powder through mechanical mill.
Observe according to XRD interpretation of result, calculating and SEM, the average particle size particle size of obtained nano calcium fluoride is 16.7nm, and crystal formation is complete, degree of crystallinity is high, even size distribution, good dispersity, and particle is ellipse, and purity is more than 97.9%.
Embodiment 3
Take nitrocalcite 12.8g and Neutral ammonium fluoride 5.05g respectively according to the ratio of mol ratio 1:3.0, put into beaker separately, respectively add 25ml distilled water and 25ml dehydrated alcohol respectively, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solutions; Take the PEG6000 of 0.5g, add pre-assigned ammonium fluoride solutions, ultrasonic disperse 15min, make it dissolve completely, obtain the double solvents of polyoxyethylene glycol and ammonium fluoride solutions, wherein, the weight concentration of polyoxyethylene glycol PEG6000 is 1%.
Magnetic agitation temperature is set as 35 DEG C, under magnetic agitation condition, instills in (instillation speed is 30ml/min) scattered ammonium fluoride solution, reaction 5min by ca nitrate soln by separating funnel.Take out reacted solution and carry out ultrasonic disperse 5min, place ageing 48h.Under 3500r/min condition, carry out centrifugation 15min, with washes of absolute alcohol 5 times, vacuum-drying 24h under 25 DEG C of conditions, can obtain nano calcium fluoride powder through mechanical mill.
Observe according to XRD interpretation of result, calculating and SEM, the average particle size particle size of obtained nano calcium fluoride is 13.3nm, and crystal formation is complete, degree of crystallinity is high, even size distribution, good dispersity, and purity is more than 96.26%.
?embodiment 4
?take nitrocalcite 12.8g and Neutral ammonium fluoride 4.62g respectively according to the ratio of mol ratio 1:2.5, put into beaker separately, respectively add 25ml distilled water and 25ml dehydrated alcohol respectively, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solutions; Take the PEG6000 of 0.75g, add pre-assigned ammonium fluoride solutions, ultrasonic disperse 30min, make it dissolve completely, obtain the double solvents of polyoxyethylene glycol and ammonium fluoride solutions, wherein, the weight concentration of polyoxyethylene glycol PEG6000 is 1.5%.
Magnetic agitation temperature is set as 50 DEG C, under magnetic agitation condition, instills in (instillation speed is 1ml/min) scattered ammonium fluoride solution by ca nitrate soln fast by separating funnel, reaction 15min.Take out reacted solution and do not carry out ultrasonic disperse, directly place ageing 48h.Under 3500r/min condition, carry out centrifugation 15min, with washes of absolute alcohol 5 times, vacuum-drying 24h under 25 DEG C of conditions, can obtain nano calcium fluoride powder through mechanical mill.
Observe according to XRD interpretation of result, calculating and SEM, the average particle size particle size of obtained nano calcium fluoride is 17.1nm, and crystal formation is complete, degree of crystallinity is high, even size distribution, good dispersity, and purity is more than 96.3%.
?embodiment 5
?take nitrocalcite 12.8g and Neutral ammonium fluoride 5.92g respectively according to the ratio of mol ratio 1:3.2, put into beaker separately, respectively add 25ml distilled water and 25ml dehydrated alcohol respectively, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solutions; Take the PEG6000 of 0.5g, add pre-assigned ammonium fluoride solutions, ultrasonic disperse 30min, make it dissolve completely, obtain the double solvents of polyoxyethylene glycol and ammonium fluoride solutions, wherein, the weight concentration of polyoxyethylene glycol PEG6000 is 1%.
?magnetic agitation temperature is set as 15 DEG C, under magnetic agitation condition, instills in (instillation speed is 3ml/min) scattered ammonium fluoride solution, reaction 25min by ca nitrate soln by separating funnel.Take out reacted solution and carry out ultrasonic disperse 25min, place ageing 48h.Under 3500r/min condition, carry out centrifugation 15min, with washes of absolute alcohol 5 times, vacuum-drying 24h under 25 DEG C of conditions, can obtain nano calcium fluoride powder through mechanical mill.
Observe according to XRD interpretation of result, calculating and SEM, the average particle size particle size of obtained nano calcium fluoride is 16.4nm, and crystal formation is complete, degree of crystallinity is high, even size distribution, good dispersity, and purity is more than 96%.
Claims (6)
1. a sintex preparation method for self-lubricating material nano calcium fluoride, is characterized in that: comprise the following steps:
(1) according to mol ratio 1: the ratio of (2.2-3.2) takes nitrocalcite and Neutral ammonium fluoride, put into beaker separately, add distilled water and dehydrated alcohol, distilled water and dehydrated alcohol are with distilled water: the volume ratio mixing and stirring of dehydrated alcohol≤1, obtained nitrocalcite content is the ca nitrate soln of 1mol/l, and ammonium fluoride content is the ammonium fluoride solution of 2.2-3.2mol/l;
(2) polyoxyethylene glycol (PEG6000) dispersion agent that a certain amount of molecular weight is 6000 is taken, add ammonium fluoride solution, make the massfraction of polyoxyethylene glycol in solution be 1-2%, ultrasonic disperse 10-30min, dissolve completely, obtain polyoxyethylene glycol-Neutral ammonium fluoride composite solution;
(3) polyoxyethylene glycol-Neutral ammonium fluoride composite solution is put into magnetic stirring apparatus, temperature of reaction setting 15-50 DEG C, ca nitrate soln instills polyoxyethylene glycol-Neutral ammonium fluoride composite solution by separating funnel, instillation speed 1-30ml/min, and stirring frequency is spattered for good so that solution is not outer;
(4) ca nitrate soln reacts 5-15min after dripping off under the condition of magnetic agitation, temperature of reaction 15-50 DEG C, takes out and puts into the ultrasonic 5-25min of ultrasonic stirrer; Then ageing 24-72h is placed;
(5) under 3000-4000r/min condition, centrifugation 10-20min is carried out, with washes of absolute alcohol 4-6 time, vacuum-drying 24-48h under 20-35 DEG C of condition;
(6) nano calcium fluoride powder is obtained through mechanical mill.
2. the preparation method of sintex self-lubricating material nano calcium fluoride according to claim 1, is characterized in that:
In step (1), the mol ratio of nitrocalcite and ammonium fluoride is 1: 3.0; The nitrocalcite content of ca nitrate soln is 1mol/l, and the ammonium fluoride content of ammonium fluoride solution is 3mol/l, and the volume ratio 1: 1 of distilled water and dehydrated alcohol mixes.
3. the preparation method of sintex self-lubricating material nano calcium fluoride according to claim 1, it is characterized in that: in step (2), in composite solution, the massfraction of polyoxyethylene glycol is 1.5%, and the ultrasonic disperse time is 15min.
4. the preparation method of sintex self-lubricating material nano calcium fluoride according to claim 1, it is characterized in that: in step (3), polyoxyethylene glycol-Neutral ammonium fluoride composite solution is put into magnetic stirring apparatus, temperature of reaction sets 35 DEG C, ca nitrate soln instills polyoxyethylene glycol-Neutral ammonium fluoride composite solution by separating funnel, instillation speed is 10ml/min, and stirring frequency is spattered for good so that solution is not outer.
5. the preparation method of sintex self-lubricating material nano calcium fluoride according to claim 1, it is characterized in that: in step (4), temperature of reaction 35 DEG C, the reaction times is 5min; Ultrasonic time is 5min, places ageing 48h.
6. the preparation method of sintex self-lubricating material nano calcium fluoride according to claim 1, it is characterized in that: in step (5), centrifuge speed is 3500r/min, disengaging time 15min, with washes of absolute alcohol 5 times, vacuum-drying 24h under 35 DEG C of conditions.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107697941A (en) * | 2017-10-17 | 2018-02-16 | 齐鲁工业大学 | A kind of nano calcium fluoride particle of size tunable and preparation method thereof |
| CN110372025A (en) * | 2019-08-28 | 2019-10-25 | 齐鲁工业大学 | A kind of flake nano calcirm-fluoride raw powder's production technology |
| CN116332216A (en) * | 2023-02-28 | 2023-06-27 | 武汉理工大学 | Synthesis method of high-purity calcium fluoride raw material |
| CN117264451A (en) * | 2023-10-08 | 2023-12-22 | 东莞市霖晨纳米科技有限公司 | Nano lubricating ceramic coating material and preparation method thereof |
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| CN102583486A (en) * | 2012-03-09 | 2012-07-18 | 山东轻工业学院 | Preparation method of nano calcium fluoride for self-lubricating tool material |
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| CN102583486A (en) * | 2012-03-09 | 2012-07-18 | 山东轻工业学院 | Preparation method of nano calcium fluoride for self-lubricating tool material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107697941A (en) * | 2017-10-17 | 2018-02-16 | 齐鲁工业大学 | A kind of nano calcium fluoride particle of size tunable and preparation method thereof |
| CN110372025A (en) * | 2019-08-28 | 2019-10-25 | 齐鲁工业大学 | A kind of flake nano calcirm-fluoride raw powder's production technology |
| CN116332216A (en) * | 2023-02-28 | 2023-06-27 | 武汉理工大学 | Synthesis method of high-purity calcium fluoride raw material |
| CN117264451A (en) * | 2023-10-08 | 2023-12-22 | 东莞市霖晨纳米科技有限公司 | Nano lubricating ceramic coating material and preparation method thereof |
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Application publication date: 20141224 |