CN1698998A - Method for preparing composite material with nano hybrid lubricant on surface - Google Patents

Method for preparing composite material with nano hybrid lubricant on surface Download PDF

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Publication number
CN1698998A
CN1698998A CN 200510025064 CN200510025064A CN1698998A CN 1698998 A CN1698998 A CN 1698998A CN 200510025064 CN200510025064 CN 200510025064 CN 200510025064 A CN200510025064 A CN 200510025064A CN 1698998 A CN1698998 A CN 1698998A
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lubricant
preparation
composite material
nano hybrid
described step
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CN 200510025064
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CN1305616C (en
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王浩伟
王慧
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Abstract

This invention relates to a method for preparing a nanometer confounding lubricant material, which belongs to materials engineering field. The method comprises the following steps: (1) anodic oxidation aluminum products: applying phosphoric acid and malic acid as the anodic oxidation liquid, creating a layer of poriness anodized film in the aluminum products surface. (2) preparing nanometer confounding lubricant: mixing MoS2 and PTFE powder absolutely, adding surface activator OP, then ball grinding in the high-energy ball grinder; ultrasonic dispersing in water. (3) filling of the lubricant: filling the lubricant to the porous aluminum oxide through ultrasonic hot dipping method; heating in the baking oven and insulation. Said invention uses synergistic effect of polyphase lubrication in nanometer dimension, which can increase the frictional factor of surface composite material.

Description

The preparation method of composite material with nano hybrid lubricant on surface
Invention field
That the present invention relates to is a kind of preparation method's of composite, particularly a kind of composite material with nano hybrid lubricant on surface preparation method, belongs to field of material engineering technology.
Background technology
After aluminium alloy carries out anodic oxidation, the surface can generate even, regular multiaperture pellumina, and its pore-size is nanoscale just, and lubricant is had very large adsorption capacity, help the filling of nanoscale lubricator, thereby can prepare aluminium matter composite surface material with self-lubricating property.
Find by prior art documents, people such as Xue Qunji are in " Surface Engineering ", 1997:35 (2) P7 writes articles " friction Surface Modification of Aluminum Materials ", the treatment process that this article proposes the existing self-lubricating anodised aluminium of having developed mainly contains following several: a. lubricant grease impregnation method, this method can be subdivided into two kinds of hot impregnation method and vacuum impregnation methods, technology is easy, is applicable to the lubricant grease of filling liquid.But,, adopt this method can not make in its micropore that is filled into oxide-film because its particle in solution is bigger for kollag.B. special fluorine draws the nurse processing method, this be a kind of in perforated membrane the technology of extrusion impregnating PTFE.But: 1, owing to adopt the method for extruding, make workpiece easy deformation, particularly some less workpiece; 2, this method is fine to the outer surface filling effect of workpiece, but there is no remarkable result for the filling of workpiece inwall and some complex parts.C. electrophoretic deposition, this method are to utilize the electrophoretic characteristic of dispersion liquid under electric field action that contains the kollag powder, make the kollag powder in the technology as the porous matter anodised aluminium surface deposition film forming of electrode.But test is found: because kollag powder particle diameter is general all big more than the aperture of anodic oxide coating minute aperture, so in fact the lubricity material is difficult to enter into porous matter anodic oxide coating.D. in-situ synthesis, this method comprises that two liquid flood reaction synthesis method and electrolytic synthesis alternately.Wherein, more noticeable and what demonstrated good development prospect is the electrolytic synthesis that the eighties is come out, this is a kind of in specific solution, by secondary or three electrolysis, utilizes the method for electrode reaction synthetic lubricity material of original position in the minute aperture of anodic oxide coating.But this technology yet exists some problems on performance.And above method all has the limitation of filling lubricant.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art and defective, a kind of preparation method of composite material with nano hybrid lubricant on surface is provided, make it utilize the cooperative effect of heterogeneous lubricator under the nanoscale, effectively improve the coefficient of friction of composite surface material, can reduce cost greatly, and easy and simple to handle, applied range.
The present invention is achieved by the following technical solutions, and the present invention adopts nanoscale to mix lubricant MoS 2, PTFE, be filled in the Woelm Alumina, be prepared into surface self-lubricating composite material, concrete steps are as follows:
(1) aluminum material anodic oxidation
Adopting concentration is that 4% phosphoric acid and 1% malic acid are as anodizing solution, at 1.5A/dm 2, aluminum material is carried out the 2h anodic oxidation under 8-10 ℃, its surface generates one deck porous anodic aluminium oxide film.
(2) nanoscale mixes the preparation of lubricant
With particle diameter is the MoS of 4-5 μ m 2And the PTFE powder is fully mixed in together, and its addition is controlled at 4: 6-7: 3, add 0.1-0.5% surfactant (OP), and in high energy ball mill, carry out ball milling then, ratio of grinding media to material is 10: 1; Rotating speed 500-600r/min, ball milling time 70-120h, ultrasonic dispersion in water behind the ball milling, its particle diameter is at 20-50nm.
MoS in the mechanical milling process 2The adding proportion that reaches the PTFE powder is one of frictional behaviour key factor of the final composite surface material that generates, and the present invention is with MoS 2And the adding proportion of PTFE powder is controlled at 4: 6-7: between 3.Surfactant to ball milling after the dispersiveness influence of nano hybrid lubricant very big, the surfactant (OP) that the present invention uses, when addition during at 0.1-0.5%, it is dispersed preferably that the nano hybrid particle is had in solution.Rotating speed and ball milling time are the important parameters of preparation nano hybrid particle: rotating speed is low excessively, and the time is too short, mixes particle and is difficult to reach nanoscale; Rotating speed is too high, overlong time, and the particle aggregation phenomenon is serious.The present invention is controlled at 500-600r/min and 70-120h respectively with rotational speed of ball-mill and time, has obtained effect preferably.
(3) filling of lubricant
Adopt ultrasonic hot dipping method will mix lubricant and be filled in the Woelm Alumina, supersonic frequency 50Hz, ultrasonic time 5min is heated to 150 ℃ then in baking oven, insulation 30min.
The present invention has substantive distinguishing features and marked improvement, general alumina-base material anode oxidation method prepares the surface self-lubricating material, the lubricant of filling is one matter, and the nano surface self-lubricating composite of the present invention's preparation has been filled nano level MoS in its perforated membrane 2And PTFE, both are obvious in the hybrid lubricant effect of nanoscale: its coefficient of friction and is filled MoS separately with same procedure between 0.05-0.15 2With the coefficient of friction of PTFE at 0.2-0.3.Self-lubrication treatment technology with other is compared, and the present invention has characteristics applied widely, easy and simple to handle, and the present invention to workpiece require lowly, can effectively fill the inwall and the complex part of workpiece.
The specific embodiment
Embodiment 1
The composite material with nano hybrid lubricant on surface preparation method: 1) adopting concentration is that 4% phosphoric acid and 1% malic acid are as anodizing solution, at 1.5A/dm 2, aluminum material is carried out the 2h anodic oxidation under 8 ℃, the surface generates porous oxide film; 2) the preparation nanoscale mixes lubricant, and the preparation method is as follows: particle diameter is the MoS of 4-5 μ m 2And the PTFE powder is according to 4: 6 ratio, add 0.1% surfactant (OP) and carry out ball milling, ratio of grinding media to material 10: 1, rotating speed is 500r/min, the ball milling time is 70h, behind the ball milling in the aqueous dispersions particle diameter at 40-50nm.3) porous oxide film is immersed in the dispersion liquid, lubricant is filled in ultrasonic immersing, supersonic frequency 50Hz, and ultrasonic time 5min is heated to 150 ℃ then in baking oven, insulation 30min.The composite surface material coefficient of friction that is obtained is 0.15.
Embodiment 2
1) to adopt concentration be that 4% phosphoric acid and 1% malic acid are as anodizing solution, at 1.5A/dm to aluminium 2, aluminum material is carried out the 2h anodic oxidation under 9 ℃, the surface generates porous oxide film; 2) the preparation nanoscale mixes lubricant, and the preparation method is as follows: particle diameter is the MoS of 4-5 μ m 2And the PTFE powder is according to 5: 5 ratio, add 0.5% surfactant (OP) and carry out ball milling, ratio of grinding media to material 10: 1, rotating speed is 600r/min, the ball milling time is 120h, behind the ball milling in the aqueous dispersions particle diameter at 30-50nm.3) porous oxide film is immersed in the dispersion liquid, lubricant is filled in ultrasonic immersing, supersonic frequency 50Hz, and ultrasonic time 5min is heated to 150 ℃ then in baking oven, insulation 30min.The composite surface material coefficient of friction that is obtained is 0.12
Embodiment 3
1) adopting concentration is that 4% phosphoric acid and 1% malic acid are as anodizing solution, at 1.5A/dm 2, aluminum material is carried out the 2h anodic oxidation under 10 ℃, the surface generates porous oxide film; 2) the preparation nanoscale mixes lubricant, and the preparation method is as follows: particle diameter is the MoS of 4-5 μ m 2And the PTFE powder is according to 7: 3 ratio, add 0.2% surfactant (OP) and carry out ball milling, ratio of grinding media to material 10: 1, rotating speed is 560r/min, the ball milling time is 90h, behind the ball milling in the aqueous dispersions particle diameter at 20-40nm.3) porous oxide film is immersed in the dispersion liquid, lubricant is filled in ultrasonic immersing, supersonic frequency 50Hz, and ultrasonic time 5min is heated to 150 ℃ then in baking oven, insulation 30min.The composite surface material coefficient of friction that is obtained is 0.05.

Claims (8)

1. the preparation method of a composite material with nano hybrid lubricant on surface is characterized in that, concrete steps are as follows:
(1) aluminum material anodic oxidation adopts phosphoric acid and malic acid as anodizing solution, and aluminum material is carried out anodic oxidation, and its surface generates one deck porous anodic aluminium oxide film;
(2) nanoscale mixes the preparation of lubricant, with MoS 2And the PTFE powder is fully mixed in together, adds surfactant OP, carries out ball milling then in high energy ball mill, ultrasonic dispersion in water behind the ball milling;
(3) filling of lubricant is adopted ultrasonic hot dipping method will mix lubricant and is filled in the Woelm Alumina, heats insulation then in baking oven.
2. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1 is characterized in that, the phosphoric acid in the described step 1: adopting concentration is that 4% phosphoric acid and 1% malic acid are as anodizing solution.
3. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1 is characterized in that, the anodic oxidation in the described step 1 is at 1.5A/dm 2, aluminum material is carried out 2h under 8-10 ℃.
4. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1 is characterized in that, in the described step 2 with MoS 2And the PTFE powder is fully mixed in together, is meant: be the MoS of 4-5 μ m with particle diameter 2And the PTFE powder is fully mixed in together.
5. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1 is characterized in that, the interpolation surfactant OP in the described step 2, and its addition is controlled at 4: 6-7: 3, interpolation 0.1-0.5% surfactant OP,
6. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1, it is characterized in that, in high energy ball mill, carry out ball milling in the described step 2, be meant: ratio of grinding media to material is 10: 1, rotating speed 500-600r/min, ball milling time 70-120h, ultrasonic dispersion in water behind the ball milling, its particle diameter is at 20-50nm.
7. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1, it is characterized in that the ultrasonic hot dipping method of the employing in the described step 3 is meant: adopt ultrasonic hot dipping method will mix lubricant and be filled in the Woelm Alumina, supersonic frequency 50Hz, ultrasonic time 5min.
8. the preparation method of composite material with nano hybrid lubricant on surface according to claim 1 is characterized in that, in baking oven, heating in the described step 3, and insulation is meant: be heated to 150 ℃ in baking oven, insulation 30min.
CNB2005100250648A 2005-04-14 2005-04-14 Method for preparing composite material with nano hybrid lubricant on surface Expired - Fee Related CN1305616C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101594952B (en) * 2006-10-27 2013-05-08 纳米技术金属有限公司 Atomized picoscale composite aluminum alloy and method therefor
CN106086990A (en) * 2016-08-04 2016-11-09 北京工业大学 A kind of method of the immobilized molybdenum bisuphide of porous titania thin films
CN107190304A (en) * 2016-03-14 2017-09-22 嘉兴福源激光科技有限公司 A kind of method that solid lubricant is planted in laser micropore template
CN107937955A (en) * 2017-12-28 2018-04-20 山东大学 A kind of method of aluminum alloy surface wearability under raising DRY SLIDING
CN111139507A (en) * 2019-12-20 2020-05-12 清华大学 Metal surface burning and coloring device based on electric control friction

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101250737B (en) * 2007-11-16 2010-07-14 苏州有色金属研究院有限公司 Self-lubricating surface composite material negative pressure impregnation filling preparation technique

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Publication number Priority date Publication date Assignee Title
JPS51119341A (en) * 1975-04-12 1976-10-19 Fujikura Ltd Process for strengthening anodic oxidation coating of aluminum or aluminum alloy
JPS56123398A (en) * 1980-02-29 1981-09-28 Toshiba Corp Surface treatment of metal
JP3751498B2 (en) * 2000-03-22 2006-03-01 本田技研工業株式会社 Piston for internal combustion engine made of aluminum alloy
KR20010104186A (en) * 2000-05-13 2001-11-24 이경재 A surface treatment method of ball joint for a car
CN1403633A (en) * 2002-10-10 2003-03-19 上海交通大学 Ultrasonic prepn process of self-lubricating surface composite material

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101594952B (en) * 2006-10-27 2013-05-08 纳米技术金属有限公司 Atomized picoscale composite aluminum alloy and method therefor
CN107190304A (en) * 2016-03-14 2017-09-22 嘉兴福源激光科技有限公司 A kind of method that solid lubricant is planted in laser micropore template
CN106086990A (en) * 2016-08-04 2016-11-09 北京工业大学 A kind of method of the immobilized molybdenum bisuphide of porous titania thin films
CN106086990B (en) * 2016-08-04 2019-02-01 北京工业大学 A kind of method of the immobilized molybdenum disulfide of porous titania thin films
CN107937955A (en) * 2017-12-28 2018-04-20 山东大学 A kind of method of aluminum alloy surface wearability under raising DRY SLIDING
WO2019128210A1 (en) * 2017-12-28 2019-07-04 山东大学 Method for improving surface abrasion resistance of aluminum alloy under dry friction condition
CN111139507A (en) * 2019-12-20 2020-05-12 清华大学 Metal surface burning and coloring device based on electric control friction
CN111139507B (en) * 2019-12-20 2021-04-02 清华大学 Metal surface burning and coloring device based on electric control friction

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