CN103922374A - Aluminium fluoride nano material as well as preparation method and application thereof - Google Patents
Aluminium fluoride nano material as well as preparation method and application thereof Download PDFInfo
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- CN103922374A CN103922374A CN201410176450.6A CN201410176450A CN103922374A CN 103922374 A CN103922374 A CN 103922374A CN 201410176450 A CN201410176450 A CN 201410176450A CN 103922374 A CN103922374 A CN 103922374A
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- powder
- nano material
- aluminum fluoride
- fluoride nano
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Abstract
The invention relates to an antifriction additive and in particular relates to an aluminium fluoride nano material as well as a preparation method and application thereof. The preparation method of the aluminium fluoride nano material comprises the following steps: adding Ti3AlC2 powder and hydrofluoric acid solution into a reaction kettle, carrying out reaction for a certain time at high temperature, precipitating with distilled water and ethanol, carrying out suction filtration, and drying, so that a cubic aluminium fluoride nano material is obtained, wherein the high temperature is 180-200 DEG C, and the certain time is 24-48 hours. Preparation technical parameters in the preparation method of the aluminium fluoride nano material can be easily controlled; the prepared aluminium fluoride nano material has excellent antifriction, antiwear and lubricating properties and can be taken as an antifriction additive for lubricating oil and grease.
Description
Technical field
The present invention relates to antifriction additive, be specifically related to a kind of aluminum fluoride nano material and preparation method and purposes.
Background technology
Inoganic solids fluorochemical energy gap is large, from ultraviolet to mid infrared region, have that good light transmission phonon energy is low, electronic cloud expansion effect is little, compared with oxide compound, fluorochemical specific refractory power is little, easily and matrix matching, can avoid serious scattering of light, reduce the transmission loss of light, therefore be easy to luminous energy storage, transmission and conversion; Inoganic solids fluorochemical, because of its structure and characteristic advantage, receives much attention as functional materials, and it electrically, magnetic and photosensitiveness obtained extensive utilization.Aluminum fluoride, as a kind of fluorochemical of simple structure, has the common feature of other fluorochemical, as high and low in fusing point under melt temperature fluorion lattice be half flow state, good electroconductibility etc., be often used as aluminium electrolyte adjusting agent.
The preparation of aluminum fluoride is subject to investigator's extensive concern always, patent of invention CN201210157654 discloses a kind of preparation method of fine hair shape aluminum fluoride, taking Neutral ammonium fluoride or ammonium aluminum fluoride and aluminium salt or aluminium hydroxide as raw material, prepare burden and make solution by stoichiometric ratio, in reaction vessel, there is the mixing solutions that chemical reaction generates aluminum fluoride etc., mixed solution is put into process furnace, the protective gas such as logical nitrogen or helium enter stove, in 2-3 hour, be warmed up to 400 DEG C from room temperature, in 400 DEG C of insulation 3-5 hour; Water in mixed solution is about 100 DEG C evaporations, and along with the rising of temperature, the material of its pyrolytic resolves into gas and is removed within the scope of 100-400 DEG C, thereby makes fine hair shape aluminum fluoride crystal; Patent CN201010208661.5 discloses a kind of preparation method of β-aluminum fluoride of high-specific surface area.Taking gama-alumina, charcoal source, HF gas as raw material, adopt the method for incipient impregnation that the aqueous solution in charcoal source is impregnated in gama-alumina, gama-alumina behind impregnated carbon source obtains the gama-alumina containing charcoal by after dry, charing, again the gama-alumina containing charcoal and HF gas reaction are obtained to the aluminum fluoride containing charcoal, the β-aluminum fluoride that remove charcoal, acid treatment, washing finally by crossing, be dried, calcining obtains high-specific surface area; Patent CN200810049583.1 " a kind of production technique of aluminum fluoride by dry process " also discloses a kind of production technique of aluminum fluoride by dry process.Described technique comprises that preparation, HF and the aluminium hydroxide of HF gas prepares aluminum fluoride, wherein the preparation method of HF gas is: the vitriol oil and nicotinic acid normal temperature are added to fuming acid reactor, and the mixing acid obtaining after mixing directly fully reacts and obtains HF gas with fluorite again in Reaktionsofen.
The report of preparing for aluminum fluoride in prior art, complex technical process; There is not yet report about the preparation of cubic aluminum fluoride nano particle and as the application of antifriction additive simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cube aluminum fluoride nano material as antifriction additive of excellent property; The present invention is the nanocubes of length of side 90-220nm as the aluminum fluoride nano material of antifriction additive.
To achieve the above object of the invention, the preparation method of cube aluminum fluoride nano material that the present invention proposes, its step is as follows:
Step (1), employing planetary high-energy ball mill mix titanium valve, aluminium powder, Graphite Powder 99 and glass putty ball milling under the speed of 200 rpm;
Step (2), the powder after ball milling is placed in to crucible, puts it in tubular react furnace, pass into Ar gas, be incubated 20 minutes after being heated to 1400 DEG C, cool to room temperature with the furnace, take out powder in crucible and make Ti
3alC
2powder.
Step (3), by the Ti making
3alC
2powder and hydrofluoric acid solution add in reactor, at high temperature react certain hour, after through distilled water and ethanol precipitation, suction filtration, the dry cube aluminum fluoride nano material that obtains.
The ratio of the amount of substance of wherein said Ti powder, Al powder, Graphite Powder 99, glass putty is 3:1:2:0.2.
In described step (1), the ball mill mixing time is 5-10 hour.
Hydrofluoric acid solution concentration 40wt% in described step (3).
In described step (3), every ml hydrofluoric acid solution adds 0.05 gTi
3alC
2powder.
In described step (3), high temperature is 180-200 DEG C.
In described step (3), certain hour refers to 24-48 hour.
By controlling temperature of reaction and time, can obtain aluminum fluoride nanocubes.
The aluminum fluoride nanocubes making is joined in base oil; the lubricating oil configuring is in friction process; because contained additive aluminum fluoride nano material can form the protective membrane with certain supporting capacity, lubrication in friction process; provide effectively lubricated; the all right filling and repairing friction surface of aluminum fluoride nano particle simultaneously; play the repair of wear surface, can improve wear resistance, antifriction quality and the extreme pressure property of lubricating base oils, the work-ing life of prolonged mechanical part.
Brief description of the drawings
Fig. 1 is the X ray collection of illustrative plates (XRD) of the prepared solid lubrication oil additive of the present invention cube aluminum fluoride nano particle.
Fig. 2 is the microscopic appearance picture (1 under the prepared solid lubrication oil additive of the present invention cube aluminum fluoride nano particle low power field emission scanning electron microscope (SEM)
).
Fig. 3 is the microscopic appearance picture (100nm) under the prepared solid lubrication oil additive of the present invention cube aluminum fluoride nano particle high power field emission scanning electron microscope (SEM).
Embodiment
Embodiment 1
Titanium valve, aluminium powder, Graphite Powder 99 and glass putty are weighed to 7.181 grams, Ti powder in the ratio of the ratio 3:1:2:0.2 of amount of substance, 1.349 grams, Al powder, 1.2 grams of Graphite Powder 99s, 1.187 grams, Sn powder, take Stainless Steel Ball in the ratio of ratio of grinding media to material 10:1, put into the stainless cylinder of steel of clean ball mill together with question response powder, seal, and extract the air in tank out, ball milling 5 h(ball mill speed 200rpm on planetary ball mill); Take out powder in ball grinder and be placed in crucible, put it in tubular react furnace, pass into Ar gas, be incubated 20min after being heated to 1400 DEG C, cool to room temperature with the furnace, take out powder in crucible and make Ti
3alC
2powder; By the Ti making
3alC
2powder and 40% hydrofluoric acid solution add in reactor, 200 DEG C of reactions 24 hours, after through distilled water and ethanol precipitation, suction filtration, the dry aluminum fluoride nano material that to obtain.
Fig. 1 is the XRD figure spectrum of the prepared product of embodiment 1, and product is pure AlF
3cubic system.Fig. 2, Fig. 3 is the SEM photo of the prepared product of embodiment 1, can obviously see the nanocubes of a large amount of homogeneous, it is of a size of 90-220 nm.
Embodiment 2
The ratio that is 3:1:2:0.2 in the ratio of amount of substance by titanium valve, aluminium powder, Graphite Powder 99 and glass putty weighs 7.181 grams, Ti powder, 1.349 grams, Al powder, 1.2 grams of Graphite Powder 99s, 1.187 grams, Sn powder, take Stainless Steel Ball in the ratio of ratio of grinding media to material 10:1, put into the stainless cylinder of steel of clean ball mill together with question response powder, seal, and extract the air in tank out, ball milling 8h(ball mill speed 200rpm on planetary ball mill); Take out powder in ball grinder and be placed in crucible, put it in tubular react furnace, pass into Ar gas, be incubated 20min after being heated to 1400 DEG C, cool to room temperature with the furnace, take out powder in crucible and make Ti
3alC
2powder; By the Ti making
3alC
2powder and 40% hydrofluoric acid solution add in reactor, 180 DEG C of reactions 48 hours, after through distilled water and ethanol precipitation, suction filtration, the dry aluminum fluoride nano material that to obtain.
Embodiment 3
The ratio that is 3:1:2:0.2 in the ratio of amount of substance by titanium valve, aluminium powder, Graphite Powder 99 and glass putty weighs 7.181 grams, Ti powder, 1.349 grams, Al powder, 1.2 grams of Graphite Powder 99s, 1.187 grams, Sn powder, take Stainless Steel Ball in the ratio of ratio of grinding media to material 10:1, put into the stainless cylinder of steel of clean ball mill together with question response powder, seal, and extract the air in tank out, ball milling 10h(ball mill speed 200rpm on planetary ball mill); Take out powder in ball grinder and be placed in crucible, put it in tubular react furnace, pass into Ar gas, be incubated 20min after being heated to 1400 DEG C, cool to room temperature with the furnace, take out powder in crucible and make Ti
3alC
2powder; By the Ti making
3alC
2powder and 40% hydrofluoric acid solution add in reactor, 190 DEG C of reactions 36 hours, after through distilled water and ethanol precipitation, suction filtration, the dry aluminum fluoride nano material that to obtain.
According to mass percent, the aluminum fluoride nanocubes of 1 wt.% is joined in 100SN base oil, the oil sample of configuration is disperseed 1 hour with ultrasonic disperser.(experiment condition is: room temperature to investigate its tribological property with UMT-2 type ball disc type friction wear testing machine; Rotating speed 280r/min; Load 15N; Time 10min).Table 1 shows polishing scratch width (WSW), rubbing factor (μ) comparison of in base oil, adding aluminum fluoride nano particle.
table 1
| Oil product title | Base oil | Add aluminum fluoride nano particle (1%) |
| Polishing scratch width (WSW)/mm | 0.209 | 0.201 |
| Rubbing factor (μ) | 0.1055 | 0.0883 |
From table 1, add the lubricating oil of 1wt.% aluminum fluoride nano particle, obviously lower the rubbing factor in friction process, improve the fastness to wear of lubricating oil.
Aluminum fluoride nanocubes as antifriction additive of the present invention, can make an addition in lubricating oil, fat, reduces the friction system element in friction process, improves fastness to wear, the work-ing life of elongated component.
Claims (8)
1. an aluminum fluoride nano material, is characterized in that: described aluminum fluoride nano material is that the length of side is the nanocubes particle of 90-220nm.
2. the preparation method of a kind of aluminum fluoride nano material as claimed in claim 1, is characterized in that carrying out in accordance with the following steps: by Ti
3alC
2powder and hydrofluoric acid solution add in reactor, at high temperature react certain hour, after through distilled water and ethanol precipitation, suction filtration, the dry cube aluminum fluoride nano material that obtains; Described high temperature is 180-200 DEG C; Described certain hour refers to 24-48 hour.
3. the preparation method of a kind of aluminum fluoride nano material as claimed in claim 2, is characterized in that: described hydrofluoric acid solution concentration is 40wt%.
4. the preparation method of a kind of aluminum fluoride nano material as claimed in claim 2, is characterized in that: every ml hydrofluoric acid solution adds 0.05 gTi
3alC
2powder.
5. the preparation method of a kind of aluminum fluoride nano material as claimed in claim 2, is characterized in that described Ti
3alC
2the preparation method of powder is as follows:
(1) adopt planetary high-energy ball mill, titanium valve, aluminium powder, Graphite Powder 99 and glass putty ball milling are mixed;
(2) powder after ball milling is placed in to crucible, puts it in tubular react furnace, pass into Ar gas, be incubated 20 minutes after being heated to 1400 DEG C, cool to room temperature with the furnace, take out powder in crucible and make Ti
3alC
2powder.
6. the preparation method of a kind of aluminum fluoride nano material as claimed in claim 5, is characterized in that: described ball milling speed is 200 rpm, and the ball mill mixing time is 5-10 hour.
7. the preparation method of a kind of aluminum fluoride nano material as claimed in claim 5, is characterized in that: the ratio of the amount of substance of described Ti powder, Al powder, Graphite Powder 99, glass putty is 3:1:2:0.2.
8. a kind of aluminum fluoride nano material as claimed in claim 1 is as the purposes of wear reducing additive.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410176450.6A CN103922374A (en) | 2014-04-29 | 2014-04-29 | Aluminium fluoride nano material as well as preparation method and application thereof |
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|---|---|---|---|
| CN201410176450.6A CN103922374A (en) | 2014-04-29 | 2014-04-29 | Aluminium fluoride nano material as well as preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200343A (en) * | 2016-12-22 | 2017-09-26 | 常州轻工职业技术学院 | A kind of preparation method of the bar-shaped aluminum fluoride nano material as antifriction additive |
| CN110560108A (en) * | 2019-06-16 | 2019-12-13 | 浙江工业大学 | Ternary layered MAX phase ceramic material catalyst and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699159A (en) * | 2005-04-29 | 2005-11-23 | 北京交通大学 | Titanium aluminium carbide powder and synthesis method using tin as reactive adjuvant therefor |
-
2014
- 2014-04-29 CN CN201410176450.6A patent/CN103922374A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699159A (en) * | 2005-04-29 | 2005-11-23 | 北京交通大学 | Titanium aluminium carbide powder and synthesis method using tin as reactive adjuvant therefor |
Non-Patent Citations (2)
| Title |
|---|
| CHANG FY ET AL.: "Synthesis of a new graphene-like transition metal carbide by de-intercalating Ti3AlC2", 《MATERIALS LETTERS》, 15 October 2013 (2013-10-15) * |
| MAOQUN XUE ET AL.: "Preparation and tribological properties of nanoaluminium fluoride as additives to base oil", 《 MICRO & NANO LETTERS》, 26 March 2014 (2014-03-26) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200343A (en) * | 2016-12-22 | 2017-09-26 | 常州轻工职业技术学院 | A kind of preparation method of the bar-shaped aluminum fluoride nano material as antifriction additive |
| CN110560108A (en) * | 2019-06-16 | 2019-12-13 | 浙江工业大学 | Ternary layered MAX phase ceramic material catalyst and preparation method and application thereof |
| CN110560108B (en) * | 2019-06-16 | 2022-07-08 | 浙江工业大学 | Ternary layered MAX phase ceramic material catalyst and preparation method and application thereof |
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Application publication date: 20140716 |